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Sample records for double hydroxide intercalated

  1. Electronic spectra of anions intercalated in layered double hydroxides

    Indian Academy of Sciences (India)

    Transition metal complexes intercalated in layered double hydroxides have a different electronic structure as compared to their free state owing to their confinement within the interlayer gallery. UV–Vis absorptions of the intercalated complex anions show a significant shift as compared to their free state. The ligand to metal ...

  2. Intercalation and controlled release properties of vitamin C intercalated layered double hydroxide

    International Nuclear Information System (INIS)

    Gao, Xiaorui; Lei, Lixu; O'Hare, Dermot; Xie, Juan; Gao, Pengran; Chang, Tao

    2013-01-01

    Two drug-inorganic composites involving vitamin C (VC) intercalated in Mg–Al and Mg–Fe layered double hydroxides (LDHs) have been synthesized by the calcination–rehydration (reconstruction) method. Powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), and UV–vis absorption spectroscopy indicate a successful intercalation of VC into the interlayer galleries of the LDH host. Studies of VC release from the LDHs in deionised water and in aqueous CO 3 2− solutions imply that Mg 3 Al–VC LDH is a better controlled release system than Mg 3 Fe–VC LDH. Analysis of the release profiles using a number of kinetic models suggests a solution-dependent release mechanism, and a diffusion-controlled deintercalation mechanism in deionised water, but an ion exchange process in CO 3 2− solution. - Graphical abstract: Vitamin C anions have been intercalated in the interlayer space of layered double hydroxide and released in CO 3 2− solution and deionised water. - Highlights: • Vitamin C intercalated Mg–Al and Mg–Fe layered double hydroxides were prepared. • Release property of vitamin C in aqueous CO 3 2− solution is better. • Avrami-Erofe’ev and first-order models provide better fit for release results. • Diffusion-controlled and ion exchange processes occur in deionised water. • An ion exchange process occurs in CO 3 2− solution

  3. Intercalation and controlled release properties of vitamin C intercalated layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Xiaorui, E-mail: gxr_1320@sina.com [College of Science, Hebei University of Engineering, Handan 056038 (China); School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189 (China); Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA (United Kingdom); Lei, Lixu [School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189 (China); O' Hare, Dermot [Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA (United Kingdom); Xie, Juan [College of Science, Hebei University of Engineering, Handan 056038 (China); Gao, Pengran [School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189 (China); Chang, Tao [College of Science, Hebei University of Engineering, Handan 056038 (China)

    2013-07-15

    Two drug-inorganic composites involving vitamin C (VC) intercalated in Mg–Al and Mg–Fe layered double hydroxides (LDHs) have been synthesized by the calcination–rehydration (reconstruction) method. Powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), and UV–vis absorption spectroscopy indicate a successful intercalation of VC into the interlayer galleries of the LDH host. Studies of VC release from the LDHs in deionised water and in aqueous CO{sub 3}{sup 2−} solutions imply that Mg{sub 3}Al–VC LDH is a better controlled release system than Mg{sub 3}Fe–VC LDH. Analysis of the release profiles using a number of kinetic models suggests a solution-dependent release mechanism, and a diffusion-controlled deintercalation mechanism in deionised water, but an ion exchange process in CO{sub 3}{sup 2−} solution. - Graphical abstract: Vitamin C anions have been intercalated in the interlayer space of layered double hydroxide and released in CO{sub 3}{sup 2−} solution and deionised water. - Highlights: • Vitamin C intercalated Mg–Al and Mg–Fe layered double hydroxides were prepared. • Release property of vitamin C in aqueous CO{sub 3}{sup 2−} solution is better. • Avrami-Erofe’ev and first-order models provide better fit for release results. • Diffusion-controlled and ion exchange processes occur in deionised water. • An ion exchange process occurs in CO{sub 3}{sup 2−} solution.

  4. Synthesis and characterization of laurate-intercalated Mg–Al layered double hydroxide prepared by coprecipitation

    DEFF Research Database (Denmark)

    Gerds, Nathalie Christiane; Katiyar, Vimal; Koch, Christian Bender

    2012-01-01

    Effective utilization of layered double hydroxides (LDH) for industrial applications requires the synthesis of pure and well-defined LDH phases. In the present study, dodecanoate (laurate) anions were intercalated into Mg–Al-layered double hydroxide (LDH-C12) by coprecipitation in the presence...

  5. NO and SCN -intercalated layered double hydroxides: structure and ...

    Indian Academy of Sciences (India)

    2018-02-05

    Feb 5, 2018 ... Nitrite ion; thiocyanate ion; layered double hydroxide; structure refinement. 1. Introduction. The layered .... the synthesis. The [Zn−Al−NO2] and [Zn–Al–SCN] LDHs were synthe- sized by coprecipitation at constant pH = 8 and temperature of 60 ... were obtained by the difference Fourier method embedded in.

  6. Facile synthesis of deoxycholate intercalated layered double hydroxide nanohybrids via a coassembly process

    International Nuclear Information System (INIS)

    Wu, Xiaowen; Wang, Shuang; Du, Na; Zhang, Renjie; Hou, Wanguo

    2013-01-01

    In this paper, we describe a synthesis strategy of deoxycholate (DC) intercalated layered double hydroxide (LDH) nanohybrids via a coassembly method at room temperature. For this strategy, LDH particles were delaminated to well-dispersed 2D nanosheets in formamide, and the resulting LDH nanosheets were then coassembled with DC anions into the DC intercalated LDH (DC-LDH) nanohybrids. The so-synthesized nanohybrids were characterized by XRD, TEM, FT-IR, elemental analyses and TG-DSC. It was found that the loading amount of DC in the nanohybrids could be easily controlled by changing the ratio of DC to LDH. In addition, the nanohybrids have similar characteristics with the DC-LDH nanohybrids synthesized by the hydrothermal method, including their DC loading, crystal structure, morphology and thermal gravimetric behavior. However, this strategy exhibited the advantages of short reaction time and mild experimental conditions compared with the hydrothermal method. - Graphical abstract: Deoxycholate intercalated layered double hydroxide nanohybrids were successfully synthesized via a coassembly strategy. In this strategy, the interlayer spaces of LDHs can be efficiently used for the intercalation of guest species. - Highlights: • Deoxycholate intercalated layered double hydroxide nanohybrids were synthesized via a coassembly strategy. • This strategy exhibited the advantages of short time and mild conditions. • This strategy can enable organic species to be readily intercalated into the LDH galleries

  7. Electronic spectra of anions intercalated in layered double hydroxides

    Indian Academy of Sciences (India)

    tions of the intercalated species (Boclair et al 2001). The metal contents of the samples were determined by atomic absorption spectroscopy (Varian Model AA240 Atomic. Absorption Spectrometer). Samples were digested in acid and total iron content in the case of ferrocyanide/ferricyanide and the total manganese content ...

  8. Intercalation of papain enzyme into hydrotalcite type layered double hydroxide

    Science.gov (United States)

    Zou, N.; Plank, J.

    2012-09-01

    Intercalation of proteolytic enzyme papain into hydrotalcite type LDH structure was achieved by controlled co-precipitation at pH=9.0 in the presence of papain. Characterization of the MgAl-papain-LDH phase was carried out using X-ray powder diffraction (XRD), elemental analysis, infrared spectroscopy (IR) and thermogravimetry (TG). According to XRD, papain was successfully intercalated. The d-value for the basal spacing of MgAl-papain-LDH was found at ˜5.3 nm. Consequently, original papain (hydrodynamic diameter ˜7.2 nm) attains a compressed conformation during intercalation.Formation of MgAl-papain-LDH was confirmed by elemental analysis and transmission electron microscopy (TEM). Under SEM, MgAl-papain-LDH phases appear as nanothin platelets which are intergrown to flower-like aggregates. Steric size and activity of the enzyme was retained after deintercalation from MgAl-LDH framework, as was evidenced by light scattering and UV/vis measurements. Thus, papain is not denatured during intercalation, and LDH is a suitable host structure which can provide a time-controlled release of the biomolecule.

  9. Dynamics of Intercalation/De-Intercalation of Rhodamine B during the Polymorphic Transformation of CdAl Layered Double Hydroxide to the Brucite-Like Cadmium Hydroxide

    KAUST Repository

    Saliba, Daniel

    2016-06-23

    Cadmium-Aluminum layered double hydroxide (CdAl LDH) is thermodynamically unstable and transforms to Cd(OH)2 and Al(OH)3 in a short period of time. We present a reaction-diffusion framework that enables us to use in situ steady-state fluorescence spectroscopy to study the kinetics of intercalation of a fluorescent probe (Rhodamine B (RhB)) during the formation of the CdAl LDH and its de-intercalation upon the conversion of the LDH phase to the β phase (Cd(OH)2). The method involves the diffusion of sodium hydroxide into a hydrogel gel matrix containing the aluminum and cadmium ions as well as the species we wish to incorporate in the interlayers of the LDH. The existence of RhB between the LDH layers and its expel during the transition into the β phase are proved via fluorescence microscopy, XRD and ssNMR. The activation energies of intercalation and de-intercalation of RhB are computed and show dependence on the cationic ratio of the corresponding LDH. We find that the energies of de- intercalation are systematically higher than those of intercalation proving that the dyes are stabilized due to the probe-brucite sheets interactions.

  10. Preparation and characterization of trans-RhCl(CO)(TPPTS)2-intercalated layered double hydroxides

    International Nuclear Information System (INIS)

    Zhang Xian; Wei Min; Pu Min; Li Xianjun; Chen Hua; Evans, David G.; Duan Xue

    2005-01-01

    trans-RhCl(CO)(TPPTS) 2 (TPPTS=tris(m-sulfonatophenyl)phosphine) has been intercalated into Zn-Al layered double hydroxides (LDHs) by the method of ion exchange. The structure, composition and thermal stability of the composite material have been characterized by powder X-ray diffraction, Fourier transform infrared and 31 P solid-state magic-angle spinning nuclear magnetic resonance spectroscopy, elemental analysis, thermogravimetry, and differential thermal analysis. The geometry of trans-RhCl(CO)(TPPTS) 2 was fully optimized using the PM3 semiempirical molecular orbital method, and a schematic model for the intercalated species has been proposed. The thermal stability of trans-RhCl(CO)(TPPTS) 2 is significantly enhanced by intercalation, which suggests that such materials may have prospective application as the basis of a supported catalyst system for the hydroformylation of higher olefins

  11. Intercalation of methotrexatum into layered double hydroxides via exfoliation-reassembly process

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Su-Qing; Li, Shu-Ping, E-mail: lishuping@njnu.edu.cn; Li, Xiao-Dong, E-mail: lixiaodong1@njnu.edu.cn

    2015-03-01

    Graphical abstract: The intercalation of methotrexatum (MTX) into layered double hydroxides (LDHs) via an exfoliation-reassembly process was studied and the resulting MTX/LDHs hybrids were evaluated by anticancer effects on A549 cells together with pristine LDHs and MTX itself, the results indicated that the hybrids obtained from low concentration of MTX solution presented much better anticancer effect. - Highlights: • Exfoliation-reassembly process is a good method to synthesize hybrids. • MTX/LDHs from low concentration of MTX solution presented better release property. • MTX/LDHs from low concentration of MTX solution presented good anticancer effects. - Abstract: In this paper, the intercalation of methotrexatum (MTX) into layered double hydroxides (LDHs) via an exfoliation-reassembly process was reported and the resulting hybrids were then characterized by X-ray diffraction (XRD) patterns, Fourier transform infrared (FTIR) spectroscopy and atomic force microscopy (AFM) patterns etc. In the synthesis procedure, LDHs particles were firstly delaminated into well-dispersed 2D nanosheets in formamide by ultrasonic treatment at room temperature, and then the resulting LDH nanosheets were reassembled in MTX solution to form MTX intercalated LDH (MTX/LDHs) hybrids. AFM images showed that during the exfoliation process a large part of LDHs particles were delaminated into single and double brucite layers. XRD patterns and FTIR investigations manifested the successful intercalation of MTX anions into LDHs interlayers for the final samples. It was also found out that the drug-loading capacity of the hybrids increased with the concentrations of MTX solutions, while the morphology became even aggregated. At last, the cell cytotoxicity of the hybrids was estimated by MTT assays on the human lung cancer cells (A549), and the results stated that MTX/LDHs hybrids had effective suppress role on the proliferation of cancer cells.

  12. Mechanochemical synthesis of Cu-Al and methyl orange intercalated Cu-Al layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Qu, Jun, E-mail: forsjun@whut.edu.cn [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); He, Xiaoman; Chen, Min; Hu, Huimin [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); Zhang, Qiwu, E-mail: zhangqw@whut.edu.cn [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); Liu, Xinzhong [College of Ecological Environment and Urban Construction, Fujian University of Technology, Fuzhou 350118 China (China)

    2017-04-15

    In this study, a mechanochemical route to synthesize a Cu-Al layered double hydroxide (LDH) and a methyl orange (MO) intercalated one (MO-LDH) was introduced, in which basic cupric carbonate (Cu{sub 2}(OH){sub 2}CO{sub 3}) and aluminum hydroxide (Al(OH){sub 3}) with Cu/Al molar ratio at 2/1 was first dry ground for 2 h and then agitated in water or methyl orange solution for another 4 h to obtain the LDH and MO-LDH products without any heating operation. The prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Thermogravimetry (TG), Differential scanning calorimetry (DSC) and Scanning electron microscopy (SEM). The products showed high crystallinity phase of Cu-Al and MO intercalated Cu-Al LDH with no evident impurities, proving that the craft introduced here was facile and effective. The new idea can be applied in other fields to produce organic-inorganic composites. - Highlights: • A facile mechanochemical route to synthesize Cu-Al and MO intercalated Cu-Al LDH. • The products possesses high crystalline of LDH phase with no impure phases. • The dry milling process induces the element substitution between the raw materials. • The agitation operation helps the grain growth of LDH.

  13. Synthesis, characterization, and controlled release antibacterial behavior of antibiotic intercalated Mg–Al layered double hydroxides

    International Nuclear Information System (INIS)

    Wang, Yi; Zhang, Dun

    2012-01-01

    Graphical abstract: The antibiotic anion released from Mg–Al LDHs provides a controlled release antibacterial activity against the growth of Micrococcus lysodeikticus in 3.5% NaCl solution. Highlights: ► Antibiotic anion intercalated LDHs were synthesized and characterized. ► The ion-exchange one is responsible for the release process. ► The diffusion through particle is the release rate limiting step. ► LDHs loaded with antibiotic anion have high antibacterial capabilities. -- Abstract: Antibiotic–inorganic clay composites including four antibiotic anions, namely, benzoate (BZ), succinate (SU), benzylpenicillin (BP), and ticarcillin (TC) anions, intercalated Mg–Al layered double hydroxides (LDHs) were synthesized via ion-exchange. Powder X-ray diffraction and Fourier transform infrared spectrum analyses showed the successful intercalation of antibiotic anion into the LDH interlayer. BZ and BP anions were accommodated in the interlayer region as a bilayer, whereas SU and TC anions were intercalated in a monolayer arrangement. Kinetic simulation of the release data indicated that ion-exchange was responsible for the release process, and the diffusion through the particles was the rate-limiting step. The antibacterial capabilities of LDHs loaded with antibiotic anion toward Micrococcus lysodeikticus growth were analyzed using a turbidimetric method. Significant high inhibition rate was observed when LDH nanohybrid was introduced in 3.5% NaCl solution. Therefore, this hybrid material may be applied as nanocontainer in active antifouling coating for marine equipment.

  14. Intercalation and structural aspects of macroRAFT agents into MgAl layered double hydroxides

    Directory of Open Access Journals (Sweden)

    Dessislava Kostadinova

    2016-12-01

    Full Text Available Increasing attention has been devoted to the design of layered double hydroxide (LDH-based hybrid materials. In this work, we demonstrate the intercalation by anion exchange process of poly(acrylic acid (PAA and three different hydrophilic random copolymers of acrylic acid (AA and n-butyl acrylate (BA with molar masses ranging from 2000 to 4200 g mol−1 synthesized by reversible addition-fragmentation chain transfer (RAFT polymerization, into LDH containing magnesium(II and aluminium(III intralayer cations and nitrates as counterions (MgAl-NO3 LDH. At basic pH, the copolymer chains (macroRAFT agents carry negative charges which allowed the establishment of electrostatic interactions with the LDH interlayer and their intercalation. The resulting hybrid macroRAFT/LDH materials displayed an expanded interlamellar domain compared to pristine MgAl-NO3 LDH from 1.36 nm to 2.33 nm. Depending on the nature of the units involved into the macroRAFT copolymer (only AA or AA and BA, the intercalation led to monolayer or bilayer arrangements within the interlayer space. The macroRAFT intercalation and the molecular structure of the hybrid phases were further characterized by Fourier transform infrared (FTIR and solid-state 13C, 1H and 27Al nuclear magnetic resonance (NMR spectroscopies to get a better description of the local structure.

  15. Synthesis, characterization, and controlled release antibacterial behavior of antibiotic intercalated Mg–Al layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yi [Shandong Provincial Key Lab of Corrosion Science, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071 (China); Zhang, Dun, E-mail: zhangdun@qdio.ac.cn [Shandong Provincial Key Lab of Corrosion Science, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071 (China)

    2012-11-15

    Graphical abstract: The antibiotic anion released from Mg–Al LDHs provides a controlled release antibacterial activity against the growth of Micrococcus lysodeikticus in 3.5% NaCl solution. Highlights: ► Antibiotic anion intercalated LDHs were synthesized and characterized. ► The ion-exchange one is responsible for the release process. ► The diffusion through particle is the release rate limiting step. ► LDHs loaded with antibiotic anion have high antibacterial capabilities. -- Abstract: Antibiotic–inorganic clay composites including four antibiotic anions, namely, benzoate (BZ), succinate (SU), benzylpenicillin (BP), and ticarcillin (TC) anions, intercalated Mg–Al layered double hydroxides (LDHs) were synthesized via ion-exchange. Powder X-ray diffraction and Fourier transform infrared spectrum analyses showed the successful intercalation of antibiotic anion into the LDH interlayer. BZ and BP anions were accommodated in the interlayer region as a bilayer, whereas SU and TC anions were intercalated in a monolayer arrangement. Kinetic simulation of the release data indicated that ion-exchange was responsible for the release process, and the diffusion through the particles was the rate-limiting step. The antibacterial capabilities of LDHs loaded with antibiotic anion toward Micrococcus lysodeikticus growth were analyzed using a turbidimetric method. Significant high inhibition rate was observed when LDH nanohybrid was introduced in 3.5% NaCl solution. Therefore, this hybrid material may be applied as nanocontainer in active antifouling coating for marine equipment.

  16. Highly Efficient Iodine Capture by Layered Double Hydroxides Intercalated with Polysulfides

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Shulan; Islam, Saiful M.; Shim, Yurina; Gu, Qingyang; Wang, Pengli; Li, Hao; Sun, Genban; Yang, Xiaojing; Kanatzidis, Mercouri G.

    2014-12-23

    We demonstrate strong iodine (I-2) vapor adsorption using Mg/Al layered double hydroxide (MgAl-LDH) nanocomposites intercalated with polysulfide (S-x(2-)) groups (S-x-LDH, x = 2, 4, 6). The as-prepared LDH/polysulfide hybrid materials display highly efficient iodine capture resulting from the reducing property of the intercalated polysulfides. During adsorption, the I-2 molecules are reduced to I-3(-) anions by the intercalated [S-x](2-) groups that simultaneously are oxidized to form S8. In addition to the chemical adsorption, additional molecular I-2 is physically captured by the LDH composites. As a result of these parallel processes, and despite their very low BET surface areas, the iodine capture capacities of S-2-LDH, S-4-LDH, and S-6-LDH are similar to 1.32, 1.52, and 1.43 g/g, respectively, with a maximum adsorption of 152% (wt %). Thermogravimetric and differential thermal analysis (TG-DTA), energy dispersive X-ray spectroscopy (EDS), and temperature-variable powder X-ray diffraction (XRD) measurements show the resulting I-3(-) ions that intercalated into the LDH gallery have high thermal stability (>= 350 degrees C). The excellent iodine adsorption performance combined with the facile preparation points to the S-x-LDH systems as potential superior materials for adsorption of radioactive iodine, a waste product of the nuclear power industry.

  17. DL-mandelic acid intercalated Zn-Al layered double hydroxide: A novel antimicrobial layered material.

    Science.gov (United States)

    Tang, Li-Ping; Cheng, Hui-Min; Cui, Shu-Mei; Wang, Xin-Rui; Song, Li-Ya; Zhou, Wei; Li, Shu-Jing

    2018-02-12

    DL-mandelic acid (MA) has been intercalated into Zn-Al layered double hydroxide (LDH) by an anion-exchange reaction. After intercalation of MA anions, the basal spacing of the LDH increased from 0.75 to 1.46 nm, suggesting that the MA anions were successfully intercalated into the interlayer galleries of the LDH. The structure and the thermal stability of the samples were characterized by XRD, FT-IR, TG-DTA. Studies of MA release from ZnAl-MA-LDH in hydrochloric solution (pH = 4) imply that ZnAl-MA-LDH is a better controlled release system than pure MA. Meanwhile, the mechanisms of slow release were assessed by using four commonly kinetic models. Finally, the antimicrobial activity of ZnAl-MA-LDH was tested against two kinds of bacteria and a fungus. The study confirms that the mandelic ions intercalated LDHs have the potential application as a slow release preservative in the future. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Layered double hydroxides as supports for intercalation and sustained release of antihypertensive drugs

    International Nuclear Information System (INIS)

    Xia Shengjie; Ni Zheming; Xu Qian; Hu Baoxiang; Hu Jun

    2008-01-01

    Zn/Al layered double hydroxides (LDHs) were intercalated with the anionic antihypertensive drugs Enalpril, Lisinopril, Captopril and Ramipril by using coprecipitation or ion-exchange technique. TG-MS analyses suggested that the thermal stability of Ena - , Lis - (arranged with monolayer, resulted from X-ray diffraction (XRD) and Fourier transform infrared spectra (FT-IR) analysis was enhanced much more than Cap - and Ram - (arranged with bilayer). The release studies show that the release rate of all samples markedly decreased in both pH 4.25 and 7.45. However, the release time of Ena - , Lis - were much longer compared with Cap - , Ram - in both pH 4.25 and 7.45, it is possible that the intercalated guests, arranged with monolayer in the interlayer, show lesser repulsive force and strong affinity with the LDH layers. And the release data followed both the Higuchi-square-root law and the first-order equation well. Based on the analysis of batch release, intercalated structural models as well as the TG-DTA results, we conclude that for drug-LDH, stronger the affinity between intercalated anions and the layers is, better the thermal property and the stability to the acid attack of drug-LDH, and the intercalated anions are easier apt to monolayer arrangement within the interlayer, were presented. - Graphical abstract: A series of antihypertensive drugs including Enalpril, Lisinopril, Captopril and Ramipril were intercalated into Zn/Al-NO 3 -LDHs successfully by coprecipitation or ion-exchange technique. We focus on the structure, thermal property and low/controlled release property of as-synthesized drug-LDH composite intended for the possibility of applying these LDH-antihypertensive nanohybrids in drug delivery and controlled release systems

  19. Preparation and inhibition properties of molybdate intercalated ZnAlCe layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Huajie; Wang, Jihui, E-mail: jhwang@tju.edu.cn; Zhang, Yu; Hu, Wenbin

    2016-09-05

    ZnAlCe layered double hydroxide intercalated by molybdate (ZnAlCe−MoO{sub 4} LDH) was successfully synthesized by using co-precipitation method, and the morphology, structure of ZnAlCe−MoO{sub 4} LDH were observed and characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) techniques. The inhibition behavior of ZnAlCe−MoO{sub 4} LDH for Q235 steel in 3.5%NaCl solution was determined by polarization curves, electrochemical impedance spectroscopy (EIS), inductively coupled plasma mass spectrometer (ICP-MS) and X-ray photoelectron spectrometer (XPS) methods. The results shows that the synthesized ZnAlCe−MoO{sub 4} LDH has a lamellar structure with a particle size of 0.1–2.0 μm, an average thickness of 30 nm, and a basal plane spacing of 0.898 nm. Compared with the addition of ZnAl layered double hydroxide intercalated by nitrate (ZnAl−NO{sub 3} LDH) and ZnAl layered double hydroxide intercalated by molybdate (ZnAl−MoO{sub 4} LDH) in 3.5% NaCl solution, Q235 steel in 3.5%NaCl + ZnAlCe−MoO{sub 4} LDH solution has a lower corrosion current density, larger polarization resistance and a higher inhibition efficiency. The addition of ZnAlCe−MoO{sub 4} LDH will reduce the chloride concentration in 3.5% NaCl solution by the anion exchanged with molybdate, and improve the corrosion resistance of Q235 steel owing to the formation of passive film with the composition of ferrous or iron molybdate and deposition film with zinc and cerium hydroxides. - Highlights: • ZnAlCe−MoO{sub 4} LDH compound was successfully synthesized by co-precipitation method. • ZnAlCe−MoO{sub 4} LDH has a better inhibition effect to Q235 steel in 3.5%NaCl solution. • The Cl{sup −} ions in solution was partially exchanged with MoO{sub 4}{sup 2−} ions in host layers. • The passive film and deposition film were formed by the release of LDH compound.

  20. Synthesis, characterization, and controlled release anticorrosion behavior of benzoate intercalated Zn-Al layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yi [Shandong Provincial Key Lab of Corrosion Science, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071 (China); Zhang, Dun, E-mail: zhangdun@qdio.ac.cn [Shandong Provincial Key Lab of Corrosion Science, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071 (China)

    2011-11-15

    Graphical abstract: The benzoate anion released from Zn-Al LDHs provides a more effective long-term protection against corrosion of Q235 carbon steel in 3.5% NaCl solution. Highlights: {yields} A benzoate anion corrosion inhibitor intercalated Zn-Al layered double hydroxides (LDHs) has been assembled by coprecipitation method. {yields} The kinetic simulation indicates that the ion-exchange one is responsible for the release process and the diffusion through particle is the rate limiting step. {yields} A significant reduction of the corrosion rate is observed when the LDH nanohybrid is present in the corrosive media. -- Abstract: Corrosion inhibitor-inorganic clay composite including benzoate anion intercalated Zn-Al layered double hydroxides (LDHs) are assembled by coprecipitation. Powder X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectrum analyses indicate that the benzoate anion is successfully intercalated into the LDH interlayer and the benzene planes are vertically bilayer-positioned as a quasi-guest ion-pair form in the gallery space. Kinetic simulation for the release data, XRD and FT-IR analyses of samples recovered from the release medium indicate that ion-exchange is responsible for the release process and diffusion through the particle is also indicated to be the rate-limiting step. The anticorrosion capabilities of LDHs loaded with corrosion inhibitor toward Q235 carbon steel are analyzed by polarization curve and electrochemical impedance spectroscopy methods. Significant reduction of corrosion rate is observed when the LDH nanohybrid is present in the corrosive medium. This hybrid material may potentially be applied as a nanocontainer in self-healing coatings.

  1. Anion-intercalated layered double hydroxides modified test strips for detection of heavy metal ions.

    Science.gov (United States)

    Wang, Nan; Sun, Jianchao; Fan, Hai; Ai, Shiyun

    2016-01-01

    In this work, a novel approach for facile and rapid detection of heavy metal ions using anion-intercalated layered double hydroxides (LDHs) modified test strips is demonstrated. By intercalating Fe(CN)6(4-) or S(2-) anions into the interlayers of LDHs on the filter paper, various heavy metal ions can be easily detected based on the color change before and after reaction between the anions and the heavy metal ions. Upon the dropping of heavy metal ions solutions to the test strips, the colors of the test strips changed instantly, which can be easily observed by naked eyes. With the decrease of the concentration, the color depth changed obviously. The lowest detection concentration can be up to 1×10(-6) mol L(-1). Due to the easily intercalation of anions into the interlayer of the LDHs on test trips, this procedure provides a general method for the construction of LDHs modified test strips for detection of heavy metal ions. The stability of the prepared test strips is investigated. Furthermore, all the results were highly reproducible. The test strips may have potential applications in environmental monitoring fields. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Drug intercalation in layered double hydroxide clay: Application in the development of a nanocomposite film for guided tissue regeneration

    DEFF Research Database (Denmark)

    Chakraborti, M.; Jackson, J.K.; Plackett, David

    2011-01-01

    of release by intercalation of alendronate anions in magnesium/aluminum layered double hydroxide (LDH) clay nanoparticles and dispersed in the PLGA film matrix. Tetracycline, loaded as free drug into the film together with alendronate–LDH clay complex released more rapidly than alendronate, but showed...

  3. Methotrexate intercalated layered double hydroxides with the mediation of surfactants: Mechanism exploration and bioassay study

    Energy Technology Data Exchange (ETDEWEB)

    Dai, Chao-Fan; Tian, De-Ying; Li, Shu-Ping, E-mail: lishuping@njnu.edu.cn; Li, Xiao-Dong

    2015-12-01

    Methotrexatum intercalated layered double hydroxides (MTX/LDHs) hybrids were synthesized by the co-precipitation method and three kinds of nonionic surfactants with different hydrocarbon chain lengths were used. The resulting hybrids were then characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and transmission electron microscopy (TEM). XRD and FTIR investigations manifest the successful intercalation of MTX anions into the interlayer of LDHs. TEM graphs indicate that the morphology of the hybrids changes with the variation of the chain length of the surfactants, i.e., the particles synthesized using polyethylene glycol (PEG-7) present regular disc morphology with good monodispersity, while samples with the mediation of alkyl polyglycoside (APG-14) are heavily aggregated and samples with the addition of polyvinylpyrrolidone (PVP-10) exhibit irregular branches. Furthermore, the release and bioassay experiments show that monodisperse MTX/LDHs present good controlled-release and are more efficient in the suppression of the tumor cells. - Highlights: • Surfactants could be used to modify the dispersing state of MTX/LDHs hybrids. • Surfactants have great effect on the morphology of MTX/LDHs hybrids. • MTX/LDHs with good monodisperse degree are more efficient in the suppression of the tumor cells.

  4. Heterogeneous photocatalytic degradation of pesticides using decatungstate intercalated macroporous layered double hydroxides.

    Science.gov (United States)

    Da Silva, Eliana S; Prevot, Vanessa; Forano, Claude; Wong-Wah-Chung, Pascal; Burrows, Hugh D; Sarakha, Mohamed

    2014-10-01

    Decatungstate W10O32(4-) was efficiently intercalated between the layers of three-dimensionally ordered macroporous Mg2Al-layered double hydroxide. The structural and textural properties of as-prepared intercalated compound were characterized using different solid-state characterization techniques such as X-ray powder diffraction, FTIR and Raman spectroscopies and electronic microscopy. The photocatalytic properties of immobilized W10O32 (4-) within Mg2Al structure were investigated using 2-(1-naphthyl) acetamide (NAD) as a model of pesticide. The influence of different parameters such as amount of catalyst, pH and oxygen concentration were investigated. An optimal NAD degradation was obtained for a photocatalyst concentration of 60 mg l(-1). Under our experimental conditions, this heterogeneous photocatalyst induces photodegradation of 60 % of NAD after 17 h of irradiation at 365 nm and at pH 6.6. Interestingly, pesticide photodegradation leads to the mineralization of substrates to H2O and CO2 and the photocatalyst can be recycled and reused without any loss of activity over four cycles.

  5. Biocompatible nanocomposite of carboxymethyl cellulose and functionalized carbon-norfloxacin intercalated layered double hydroxides.

    Science.gov (United States)

    Allou, N'guadi Blaise; Yadav, Archana; Pal, Mintu; Goswamee, Rajib Lochan

    2018-04-15

    In recent years, the development of systems with progressive drug release properties, which is an effective technique for the use of drugs, has aroused great interest in the field of controlled release formulations. In this work, hybrid materials containing citric acid cross-linked carboxymethyl cellulose (CMC) and norfloxacin (NOR) intercalated layered double hydroxide (LDH) deposited over the surface of functionalized carbon (AC) were prepared. The synthesized CMC@AC-LDHNOR nanohybrids were characterized using different techniques and in vitro NOR release behaviors were investigated in phosphate buffer saline, pH 7.4 at 37 °C. On the basis of the release profiles, it was found that NOR release was delayed when it was intercalated in AC-LDH which in presence of modified CMC decreases further. The nanohybrids indicated enhancement of antibacterial activity against gram-negative and gram-positive bacteria. The MTT assay showed their non-toxic behavior against ovarian normal epithelial and cancer cells, suggesting their potential use as drug carriers. Copyright © 2018 Elsevier Ltd. All rights reserved.

  6. Engineering of (10-hydroxycamptothecin intercalated layered double hydroxide)@liposome nanocomposites with excellent water dispersity

    Science.gov (United States)

    Zhang, Yongfang; Wu, Xiaowen; Mi, Yuwei; Li, Haiping; Hou, Wanguo

    2017-09-01

    A hierarchical nanocomposite of 10-hydroxycamptothecin (HCPT), a nonionic and lipophilic anticancer drug, intercalated layered double hydroxide (LDH) encapsulated in liposomes was constructed. HCPT molecules were first incorporated into sodium cholate (Ch) micelles, and the resultant negatively charged HCPT-loaded Ch micelles were then co-assembled with positively charged LDH single-layer nanosheets, forming a HCPT/Ch intercalated LDH (HCPT-Ch-LDH) host-gest nanohybrid. The nanohybrid particles were further coated with liposomes (LSs), gaining a core-shell nanocomposite, denoted as (HCPT-Ch-LDH)@LS. The so-obtained samples were characterized using TEM, SAXS, FT-IR, DLS, and elemental analyses. Special emphasis was placed on the effect of liposome-coating for the HCPT-Ch-LDH on its water dispersity and drug-release. The results showed that the nanocomposite has excellent water dispersity and enhanced drug sustained-release performance in comparison with the HCPT-Ch-LDH, demonstrating that the liposome-coating for drug-LDH nanohybrids is an effective strategy to enhance their water dispersity and sustained-release performances. This work provides an effective strategy for engineering of LDH-based delivery systems for nonionic and lipophilic drugs.

  7. Methotrexatum intercalated layered double hydroxides: Statistical design, mechanism explore and bioassay study

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xiao-Feng [Department of Gastroenterology, Weihai municipal hospital, Weihai 264200 (China); Liu, Su-Qing [Jiangsu Key Laboratory of Biofunctional Material, College of Chemistry and Material Science, Nanjing Normal University, Nanjing 210023 (China); Li, Shu-Ping, E-mail: lishuping@njnu.edu.cn [Jiangsu Key Laboratory of Biofunctional Material, College of Chemistry and Material Science, Nanjing Normal University, Nanjing 210023 (China)

    2015-04-01

    A series of methotrexatum intercalated layered double hydroxide (MTX/LDH for short) hybrids have been synthesized by a mechanochemical–hydrothermal method, the statistical experiments are planned and conducted to find out the critical factor influencing the physicochemical properties. Four variables, i.e., addition of NaOH solution, grinding duration, hydrothermal temperature and time, are chosen to play as the examined factors in the orthogonal design. Furthermore, three respective levels, i.e., high, medium and low levels, are conducted in the design. The resulting hybrids are then characterized by X-ray diffraction (XRD) patterns, transmission electron microscope (TEM) graphs and Zeta potentials. XRD diffractions indicate that MTX anions have been successfully intercalated into LDH interlayers and the amount of NaOH solution can change the gallery height greatly. The information from TEM graphs and Zeta potentials state that the increase of alkali solution gives rise to regular morphology and the increase of Zeta potentials. As a result of the statistical analysis, addition of alkali solution is the major factor affecting the morphology and drug-loading capacity. At last, the mechanism of particle growth is explored emphatically, and the anticancer efficacy of some MTX/LDH hybrids is estimated by MTT assay on A549 cells as well. - Graphical abstract: Schematic illustration of synthesis and properties of MTX intercalated LDH hybrids. - Highlights: • Increasing NaOH solution gives rise to high drug-loading capacity. • Increasing the alkali solution leads to high layer charge and regular morphology. • The monodispersity has critical effect on the tumor suppression efficiency.

  8. Mechanochemical synthesis of dodecyl sulfate anion (DS-) intercalated Cu-Al layered double hydroxide

    Science.gov (United States)

    Qu, Jun; He, Xiaoman; Lei, Zhiwu; Zhang, Qiwu; Liu, Xinzhong

    2017-12-01

    Dodecyl sulfate anion (DS-) was successfully intercalated into the gallery space of Cu-Al layered double hydroxides (LDH) by a non-heating mechanochemical route, in which basic cupric carbonate (Cu2(OH)2CO3) and aluminum hydroxide (Al(OH)3) were first dry ground and then agitated in SDS solution under ambient environment. The organics modified Cu-Al LDH showed good adsorption ability toward 2,4-dichlorophenoxyacetic acid (2, 4-D). The prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), CHS elemental analysis and Scanning electron microscopy (SEM). The LDH precursor prepared by ball-milling could directly react with SDS molecules forming a pure phase of DS- pillared Cu-Al LDH, which was not observed with the LDH product through the ion-exchange of DS- at room temperature. The process introduced here may be applied to manufacture other types of organic modified composites for pollutants removal and other applications.

  9. Preparation of layered double hydroxides intercalated with organic anions and their application in LDH/poly(butyl methacrylate) nanocomposites

    Czech Academy of Sciences Publication Activity Database

    Kovanda, F.; Jindrová, E.; Lang, Kamil; Kubát, Pavel; Sedláková, Zdeňka

    2010-01-01

    Roč. 48, 1-2 (2010), s. 260-270 ISSN 0169-1317 R&D Projects: GA AV ČR KAN100500651 Institutional research plan: CEZ:AV0Z40320502; CEZ:AV0Z40400503; CEZ:AV0Z40500505 Keywords : Layered double hydroxides * intercalation * poly(butyl methacrylate) nanocomposite * photoactive materials Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.303, year: 2010

  10. Synthesis and UV absorption properties of 5-sulfosalicylate-intercalated Zn Al layered double hydroxides

    Science.gov (United States)

    Zhang, Linyan; Lin, Yanjun; Tuo, Zhenjun; Evans, David G.; Li, Dianqing

    2007-04-01

    5-sulfosalicylic acid (SSA) anions have been intercalated into layered double hydroxides (LDHs) by an anion-exchange reaction using ZnAl-NO 3-LDHs as a precursor. The samples were characterized by XRD, FT-IR, TG-DTA/MS and UV-visible spectroscopy. The results show that the NO 3- anions in the precursor have been completely replaced by SSA anions to give ZnAl-SSA-LDHs having a high degree of crystallinity. Detailed studies reveal the existence of a supramolecular structure in ZnAl-SSA-LDHs involving electrostatic attraction between opposite charges, hydrogen bonding and other weak chemical bonding interactions between host layers and SSA anions. The thermal stability of ZnAl-SSA-LDHs is considerably enhanced compared with that of a mixture of ZnAl-NO 3-LDHs and SSA. After addition of 2.0 wt% ZnAl-SSA-LDHs to polypropylene (PP), the resistance of the polymer to UV degradation is significantly improved.

  11. Tribological performance of Mg/Al/Ce layered double hydroxides nanoparticles and intercalated products as lubricant additives

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shuo; Qin, Haojing; Zuo, Ranfang; Bai, Zhimin, E-mail: zhimibai@cugb.edu.cn

    2015-10-30

    Highlights: • Mg/Al/Ce layered double hydroxides (LDHs) were synthesized by coprecipitation. • Mg/Al/Ce LDHs were intercalated with succinic acid and lauric acid respectively. • LDHs intercalated with lauric acid had the best friction properties among products. • Sliding of layers, good dispersity and a protective film decided the performance. - Abstract: Mg/Al/Ce ternary layered double hydroxides (LDHs) were synthesized via coprecipitation and intercalated by succinic acid and lauric acid through ion exchange method respectively. The LDHs products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transform infrared (FT-IR). Tribological properties of LDHs as lubricant additives were evaluated by four-ball friction and air compressor test. The results indicated that Mg/Al/Ce LDHs were prepared successfully with Ce/Al molar ratio of 0.05 and crystallization temperature of 140 °C. The interlayer spacing of LDHs precursor was expanded by succinic acid and lauric acid to 8.838 and 17.519 Å respectively. All the three LDHs products can reduce friction and wear of engine lubricating oil in the tests. LDHs intercalated with lauric acid showed best tribological performance among them which was attributed to sliding each other between laminates, good dispersibility in oil medium and a protective tribofilm formed on the worn surface.

  12. Intercalation behavior of amino acids into Zn-Al-layered double hydroxide by calcination-rehydration reaction

    Science.gov (United States)

    Aisawa, Sumio; Kudo, Hiroko; Hoshi, Tomomi; Takahashi, Satoshi; Hirahara, Hidetoshi; Umetsu, Yoshio; Narita, Eiichi

    2004-11-01

    The intercalation of amino acids for the Zn-Al-layered double hydroxide (LDH) has been investigated by the calcination-rehydration reaction at 298 K using mainly phenylalanine (Phe) as a guest amino acid. The Zn-Al oxide precursor prepared by the calcination of Zn-Al-carbonated LDH at 773 K for 2 h was used as the host material. The amount of Phe intercalated by the rehydration was remarkably influenced by the initial solution pH and reached ca. 2.7 times for anion exchange capacity (AEC) of the LDH at neutral and weak alkaline solutions, suggesting that Phe was intercalated as amphoteric ion form into the LDH interlayer. As Phe is intercalated for the LDH as monovalent anion in alkaline solution, the amount of Phe intercalated at pH 10.5 corresponded with AEC of the LDH. The solid products were found to have the expanded LDH structure, which confirmed that Phe was intercalated into the LDH interlayer as amphoteric ion or anion form. The basal spacing, d003, of the Phe/LDH was 1.58 nm at pH 7.0 and 0.80 nm at pH 10.5; two kinds of expansion suggested for Phe in the interlayer space as vertical (pH 7.0) and horizontal (pH 10.5) orientations. The intercalation behavior of various amino acids for the LDH was also found to be greatly influenced by the feature of the amino acid side-chain, namely, its carbon-chain length, structure and physicochemical property. In particular, α-amino acids possessing a hydrophobic or negative-charged side-chain were preferentially intercalated for the LDH.

  13. Dysprosium-containing layered double hydroxides nanoparticles intercalated with biologically active species as an approach for theranostic systems

    KAUST Repository

    Arratia-Quijada, Jenny

    2015-10-23

    A layered double hydroxide structure including dysprosium cations was prepared by co-precipitation. The nanoparticles showed a linear relationship with the reciprocal relaxation spin-lattice (T1) time of water protons which is reflected as contrast in aqueous suspensions analyzed by magnetic resonance imaging. The interlayer space of dysprosium containing LDH was successfully intercalated with folate, ibuprofen and gallate ions, which are key molecules for recognition of some cancer cells and treatment of diseases. The paramagnetic property of the dysprosium-containing LDH detected in this work beside the ability to transport drugs open up the opportunity to design theranostic materials in a single crystal phase with nanometric dimensions.

  14. Mg-Al layered double hydroxide intercalated with porphyrin anions: molecular simulations and experiments

    Czech Academy of Sciences Publication Activity Database

    Kovář, P.; Pospíšil, M.; Káfuňková, Eva; Lang, Kamil; Kovanda, F.

    2010-01-01

    Roč. 16, č. 2 (2010), s. 223-233 ISSN 1610-2940 R&D Projects: GA ČR(CZ) GA203/06/1244; GA AV ČR KAN100500651 Institutional research plan: CEZ:AV0Z40320502 Keywords : layered double hydroxide * porphyrin * molecular simulations Subject RIV: CA - Inorganic Chemistry Impact factor: 1.871, year: 2010

  15. Dysprosium-containing layered double hydroxides nanoparticles intercalated with biologically active species as an approach for theranostic systems

    Energy Technology Data Exchange (ETDEWEB)

    Arratia-Quijada, Jenny [Departamento de Ciencias de la Salud, Centro Universitario Tonalá, Universidad de Guadalajara, Av. Nuevo Periférico No. 555, C.P. 48525, Tonalá, Jalisco (Mexico); Sánchez Jiménez, Cecilia [Departamento de Química, Universidad de Guadalajara, Boulevard Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico); Gurinov, Andrey [Research Resources Center for Magnetic Resonance, St. Petersburg State University, Universitetskiy pr. 26, 198504 St. Petersburg (Russian Federation); NMR Core Lab, King Abdullah University of Science and Technology, Thuwal 23955-6900 (Saudi Arabia); Pérez Centeno, Armando; Ceja Andrade, Israel [Departamento de Física, Universidad de Guadalajara, Boulevard Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico); Carbajal Arízaga, Gregorio Guadalupe, E-mail: gregoriocarbajal@yahoo.com.mx [Departamento de Química, Universidad de Guadalajara, Boulevard Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico)

    2016-01-15

    Graphical abstract: - Highlights: • LDH structure including dysprosium was prepared by co-precipitation. • LDH was capable to produce contrast in the T1 mode of MRI. • LDH were intercalated with folate, ibuprofen and gallate ions. - Abstract: A layered double hydroxide structure including dysprosium cations was prepared by co-precipitation. The nanoparticles showed a linear relationship with the reciprocal relaxation spin-lattice (T1) time of water protons which is reflected as contrast in aqueous suspensions analyzed by magnetic resonance imaging. The interlayer space of dysprosium containing LDH was successfully intercalated with folate, ibuprofen and gallate ions, which are key molecules for recognition of some cancer cells and treatment of diseases. The paramagnetic property of the dysprosium-containing LDH detected in this work beside the ability to transport drugs open up the opportunity to design theranostic materials in a single crystal phase with nanometric dimensions.

  16. Dysprosium-containing layered double hydroxides nanoparticles intercalated with biologically active species as an approach for theranostic systems

    International Nuclear Information System (INIS)

    Arratia-Quijada, Jenny; Sánchez Jiménez, Cecilia; Gurinov, Andrey; Pérez Centeno, Armando; Ceja Andrade, Israel; Carbajal Arízaga, Gregorio Guadalupe

    2016-01-01

    Graphical abstract: - Highlights: • LDH structure including dysprosium was prepared by co-precipitation. • LDH was capable to produce contrast in the T1 mode of MRI. • LDH were intercalated with folate, ibuprofen and gallate ions. - Abstract: A layered double hydroxide structure including dysprosium cations was prepared by co-precipitation. The nanoparticles showed a linear relationship with the reciprocal relaxation spin-lattice (T1) time of water protons which is reflected as contrast in aqueous suspensions analyzed by magnetic resonance imaging. The interlayer space of dysprosium containing LDH was successfully intercalated with folate, ibuprofen and gallate ions, which are key molecules for recognition of some cancer cells and treatment of diseases. The paramagnetic property of the dysprosium-containing LDH detected in this work beside the ability to transport drugs open up the opportunity to design theranostic materials in a single crystal phase with nanometric dimensions.

  17. A comparison of corrosion inhibition of magnesium aluminum and zinc aluminum vanadate intercalated layered double hydroxides on magnesium alloys

    Science.gov (United States)

    Guo, Lian; Zhang, Fen; Lu, Jun-Cai; Zeng, Rong-Chang; Li, Shuo-Qi; Song, Liang; Zeng, Jian-Min

    2018-04-01

    The magnesium aluminum and zinc aluminum layered double hydroxides intercalated with NO3 -(MgAl-NO3-LDH and ZnAl-NO3-LDH) were prepared by the coprecipitation method, and the magnesium aluminum and the zinc aluminum layered double hydroxides intercalated with VO x -(MgAl-VO x -LDH and ZnAl-VO x -LDH) were prepared by the anion-exchange method. Morphologies, microstructures and chemical compositions of LDHs were investigated by SEM, EDS, XRD, FTIR, Raman and TG analyses. The immersion tests were carried to determine the corrosion inhibition properties of MgAl-VO x -LDH and ZnAl-VO x -LDH on AZ31 Mg alloys. The results showed that ZnAl-VO x -LDH possesses the best anion-exchange and inhibition abilities. The influence of treatment parameters on microstructures of LDHs were discussed. Additionally, an inhibition mechanism for ZnAl-VO x -LDH on the AZ31 magnesium alloy was proposed and discussed.

  18. In situ oligomerization of 2-(thiophen-3-yl)acetate intercalated into Zn{sub 2}Al layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Tronto, Jairo, E-mail: jairotronto@ufv.br [Universidade Federal de Viçosa, Instituto de Ciências Exatas e Tecnológicas, Campus de Rio Parsanaíba, Rodovia BR 354 km 310, Cx. Postal 22, CEP, 38.810-000 Rio Paranaíba, MG (Brazil); Pinto, Frederico G.; Costa, Liovando M. da [Universidade Federal de Viçosa, Instituto de Ciências Exatas e Tecnológicas, Campus de Rio Parsanaíba, Rodovia BR 354 km 310, Cx. Postal 22, CEP, 38.810-000 Rio Paranaíba, MG (Brazil); Leroux, Fabrice; Dubois, Marc [Clermont Université, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, BP 10448, F-63000 Clermont-Ferrand (France); CNRS, UMR 6296, ICCF, BP 80026, F-6317 Clermont-Ferrand (France); Valim, João B. [Universidade de São Paulo, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Departamento de Química, Av. dos Bandeirantes 3900, CEP 14.040-901, Ribeirão Preto, SP (Brazil)

    2015-01-15

    A layered double hydroxide (LDH) with cation composition Zn{sub 2}Al was intercalated with 2-(thiophen-3-yl)acetate (3-TA) monomers. To achieve in situ polymerization and/or oligomerization of the intercalated monomers, soft thermal treatments were carried out, and subsequent hybrid LDH materials were analyzed by means of several characterization techniques using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), {sup 13}C CP–MAS nuclear magnetic resonance (NMR), electron spin resonance (EPR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), inductively coupled plasma optical emission spectroscopy (ICP–OES), and elemental analysis. PXRD analysis suggested that the intercalated monomers formed a bilayer. Thermal treatment of the hybrid LDH assembly above 120 °C provokes partially the breakdown of the layered structure, generating the phase zincite. EPR results indicated that vicinal monomers (oligomerization) were bound to each other after hydrothermal or thermal treatment, leading to a polaron response characteristic of electron conductivity localized on a restricted number of thiophene-based monomer segments. Localized unpaired electrons exist in the material and interact with the {sup 27}Al nuclei of the LDH layers by superhyperfine coupling. These unpaired electrons also interact with the surface of ZnO (O{sup 2−} vacancies), formed during the thermal treatments. - Graphical abstract: We synthesized a layered double hydroxide (LDH) with cation composition Zn{sub 2}Al, intercalated with 2-(thiophen-3-yl)acetate (3-TA) monomers, by coprecipitation at constant pH. We thermally treated the material, to achieve in situ polymerization and/or oligomerization of the intercalated monomers. - Highlights: • A Zn{sub 2}Al–LDH was intercalated with 2-(thiophen-3-yl)acetate monomers. • To achieve in situ oligomerization of the monomers, thermal treatments were made.

  19. Influence of carbonate intercalation in the surface-charging behavior of Zn-Cr layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, R., E-mail: rrojas@mail.fcq.unc.edu.ar [INFIQC, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, 5000 Cordoba (Argentina); Barriga, C. [Departamento de Quimica Inorganica e Ingenieria Quimica, Edificio Marie Curie, Campus de Rabanales, Universidad de Cordoba, 14071 Cordoba (Spain); De Pauli, C.P. [INFIQC, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, 5000 Cordoba (Argentina); Avena, M.J. [Departamento de Quimica, Universidad Nacional del Sur, Avenida Alem 1253, 8000 Bahia Blanca (Argentina)

    2010-01-15

    The influence of interlayer composition in the surface charge and reactivity of layered double hydroxides (LDHs) has been explored. With this purpose, a chloride-intercalated Zn-Cr-LDH has been synthesized by the constant pH coprecipitation method and afterwards exchanged with carbonate to obtain solids with different Cl{sup -}/CO{sub 3}{sup 2-} ratios. The solids structure has been characterized by elemental chemical analysis, powder X-ray diffraction and infrared spectroscopy, while its surface-charging behavior and reactivity have been studied by acid-base potentiometric titrations and electrophoretic mobility determinations. The chloride-intercalated sample shows an increasing hydroxyl adsorption with increasing pH and decreasing support electrolyte concentration and the particles present positive electrophoretic mobility in the measured pH range. As carbonate content increases in the samples, the total OH{sup -} uptake diminishes and the samples show an isoelectric point at pH around 10. When the gallery is totally occupied by carbonate anions, the OH uptake vs. pH curves registered at different electrolyte concentrations merge at around pH 10. A LDH-water interface model has been used to give an interpretation to the experimental data. The model indicates that as carbonate content increases, the sample behavior becomes similar to that of a metal (hydr)oxide and that surface (bi)carbonate anions undergo acid-base reactions.

  20. Synthesis and characterization of Zn-Ti layered double hydroxide intercalated with cinnamic acid for cosmetic application

    Science.gov (United States)

    Li, Yong; Tang, Liping; Ma, Xinxu; Wang, Xinrui; Zhou, Wei; Bai, Dongsheng

    2017-08-01

    The use of sunscreen is recently growing and their efficacy and safety must be taken into account since they are applied on the skin frequently. In this work, an organic ultraviolet (UV) ray absorbent, cinnamic acid (CA) was intercalated into Zn-Ti layered double hydroxide (LDH) by anion-exchange reaction. ZnTi-CA-LDH, a new type of host-guest UV-blocking material has been synthesized. Detailed structural and surface morphology of ZnTi-CA-LDH were characterized by XRD, FT-IR, SEM and TEM. ZnTi-CA-LDH exhibits a superior UV blocking ability compared to pure CA and ZnTi-CO3-LDH. The thermal stability of the intercalated ZnTi-CA-LDH was investigated by TG-DTA, which showed that the thermostability of CA was markedly enhanced after intercalation into ZnTi-CO3-LDH. The EPR data showed greatly decreased photocatalytic activity compared to common inorganic UV blocking agents TiO2 and ZnO. Furthermore, the sample was formulated in a sunscreen cream to study the matrix protective effect towards UV rays.

  1. New layered double hydroxides by prepared by the intercalation of gibbsite

    Energy Technology Data Exchange (ETDEWEB)

    Rees, Jennifer R.; Burden, Chloe S.; Fogg, Andrew M., E-mail: andrewmfogg@hotmail.com

    2015-04-15

    New layered double hydroxides (LDHs) with the composition [MAl{sub 4}(OH){sub 12}]Cl{sub 2}·1.5H{sub 2}O (M=Co, Ni) have been prepared by reacting gibbsite, γ-Al(OH){sub 3}, with the appropriate chloride salt in a synthesis in which the water of crystallization is the only solvent present and fully characterized. These LDHs have been shown to undergo facile anion exchange reactions with both organic and inorganic anions at room temperature making them comparable to other LDHs in this respect. Reactions under the same conditions with CuCl{sub 2}·2H{sub 2}O and ZnCl{sub 2} failed to form the desired LDHs but those with nitrate salts did lead to the formation of the previously reported [MAl{sub 4}(OH){sub 12}](NO{sub 3}){sub 2}·1.5H{sub 2}O (M=Co, Ni) compounds. - Graphical abstract: New layered double hydroxides (LDHs) with the composition [MAl{sub 4}(OH){sub 12}]Cl{sub 2}·1.5H{sub 2}O (M=Co, Ni) have been prepared by reacting gibbsite, γ-Al(OH){sub 3}, with the appropriate chloride salt in a synthesis in which no additional solvent is used and fully characterized. These LDHs have been shown to undergo facile anion exchange reactions with both organic and inorganic anions at room temperature. - Highlights: • Synthesis of new layered double hydroxides, [MAl{sub 4}(OH){sub 12}]Cl{sub 2}·1.5H{sub 2}O (M=Co, Ni). • Demonstration of the anion exchange capacity with both organic and inorganic anions. • Demonstration of the generality of the synthesis for LDHs.

  2. New layered double hydroxides by prepared by the intercalation of gibbsite

    International Nuclear Information System (INIS)

    Rees, Jennifer R.; Burden, Chloe S.; Fogg, Andrew M.

    2015-01-01

    New layered double hydroxides (LDHs) with the composition [MAl 4 (OH) 12 ]Cl 2 ·1.5H 2 O (M=Co, Ni) have been prepared by reacting gibbsite, γ-Al(OH) 3 , with the appropriate chloride salt in a synthesis in which the water of crystallization is the only solvent present and fully characterized. These LDHs have been shown to undergo facile anion exchange reactions with both organic and inorganic anions at room temperature making them comparable to other LDHs in this respect. Reactions under the same conditions with CuCl 2 ·2H 2 O and ZnCl 2 failed to form the desired LDHs but those with nitrate salts did lead to the formation of the previously reported [MAl 4 (OH) 12 ](NO 3 ) 2 ·1.5H 2 O (M=Co, Ni) compounds. - Graphical abstract: New layered double hydroxides (LDHs) with the composition [MAl 4 (OH) 12 ]Cl 2 ·1.5H 2 O (M=Co, Ni) have been prepared by reacting gibbsite, γ-Al(OH) 3 , with the appropriate chloride salt in a synthesis in which no additional solvent is used and fully characterized. These LDHs have been shown to undergo facile anion exchange reactions with both organic and inorganic anions at room temperature. - Highlights: • Synthesis of new layered double hydroxides, [MAl 4 (OH) 12 ]Cl 2 ·1.5H 2 O (M=Co, Ni). • Demonstration of the anion exchange capacity with both organic and inorganic anions. • Demonstration of the generality of the synthesis for LDHs

  3. Ultrasonically-enhanced mechanochemical synthesis of CaAl-layered double hydroxides intercalated by a variety of inorganic anions.

    Science.gov (United States)

    Szabados, Márton; Mészáros, Rebeka; Erdei, Szabolcs; Kónya, Zoltán; Kukovecz, Ákos; Sipos, Pál; Pálinkó, István

    2016-07-01

    CaAl-layered double hydroxides (CaAl-LDHs) were synthesised with various interlayer anions (CO3(2-), F(-), Cl(-), Br(-) and I(-)) by mechanochemical pre-treatment followed by ultrasonic irradiation in aqueous media. The parameters of the syntheses (duration of pre-milling and sonication, quality of the aqueous media, temperature) were altered in order to optimise the procedure and to understand the formation of LDH and other secondary products. The products were characterised by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The optimisation resulted in close-to-phase-pure CaAl-LDHs, not only with carbonate and chloride interlayer anions, but the hard-to-intercalate bromide and iodide as well. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Layered double hydroxide using hydrothermal treatment: morphology evolution, intercalation and release kinetics of diclofenac sodium

    Science.gov (United States)

    Joy, Mathew; Iyengar, Srividhya J.; Chakraborty, Jui; Ghosh, Swapankumar

    2017-12-01

    The present work demonstrates the possibilities of hydrothermal transformation of Zn-Al layered double hydroxide (LDH) nanostructure by varying the synthetic conditions. The manipulation in washing step before hydrothermal treatment allows control over crystal morphologies, size and stability of their aqueous solutions. We examined the crystal growth process in the presence and the absence of extra ions during hydrothermal treatment and its dependence on the drug (diclofenac sodium (Dic-Na)) loading and release processes. Hexagonal plate-like crystals show sustained release with ˜90% of the drug from the matrix in a week, suggesting the applicability of LDH nanohybrids in sustained drug delivery systems. The fits to the release kinetics data indicated the drug release as a diffusion-controlled release process. LDH with rod-like morphology shows excellent colloidal stability in aqueous suspension, as studied by photon correlation spectroscopy.

  5. A solid state NMR study of Layered double hydroxides intercalated with para-amino salicylate, a tuberculosis drug

    DEFF Research Database (Denmark)

    Jensen, Nicholai Daugaard; Bjerring, Morten; Nielsen, Ulla Gro

    2016-01-01

    Para-amino salicylate (PAS), a tubercolosis drug, was intercalated in three different layered double hydroxides (MgAl, ZnAl, and CaAl-LDH) and the samples were studied by multi-nuclear (1H, 13C, and 27Al) solid state NMR (SSNMR) spectroscopy in combination with powder X-ray diffraction (PXRD....... Moreover, 13C MAS NMR and infra-red spectroscopy show that PAS did not decompose during synthesis. Large amounts (20-41%) of amorphous aluminum impurities were detected in the structure using 27Al single pulse and 3QMAS NMR spectra, which in combination with 1H single and double quantum experiments also...... showed that the M(II):Al ratio was higher than predicted from the bulk metal composition of MgAl-PAS and ZnAl-PAS. Moreover, the first high-resolution 1H SSNMR spectra of a CaAl LDH is reported and assigned using 1H single and double quantum experiments in combination with 27Al{1H} HETCOR....

  6. Intercalation of tartrazine into ZnAl and MgAl layered double hydroxides

    Czech Academy of Sciences Publication Activity Database

    Beneš, L.; Melánová, Klára; Zima, Vítězslav; Svoboda, Jan

    2005-01-01

    Roč. 70, č. 2 (2005), s. 259-267 ISSN 0010-0765 Institutional research plan: CEZ:AV0Z40500505 Keywords : intercalation * hydrotalcite Subject RIV: CA - Inorganic Chemistry Impact factor: 0.949, year: 2005

  7. OXIDATION OF CYCLOHEXANOL ON PHOSPHOTUNGSTIC ACID ANION INTERCALATED LAYERED DOUBLE HYDROXIDES WITH AQUEOUS H2O2 AS OXIDANT

    Directory of Open Access Journals (Sweden)

    Xueli Bai

    Full Text Available The layered double hydroxides (LDH of Mg2AlNi and Mg3Al pillared by Keggin-type phosphotungstic acid anion (POM, i.e. Mg2AlNi-POM LDH and Mg3Al-POM LDH were synthesized by an ion-exchange method. The synthesized POM intercalated LDH compounds were characterized using various techniques such as FTIR, XRD, TGA and BET. The observed results show that the obtained catalysts retain the layer structure of LDH. Compared with the binary Mg3Al-POM LDH, the ternary Mg2AlNi-POM LDH catalyst indicated a higher thermal and chemical stability. The catalytic activity of the resulting LDH-POM was also assessed in the green oxidation of cyclohexanol with aqueous H2O2 as an oxidant. The Mg2AlNi-POM LDH showed a much higher conversion and selectivity for cyclohexanone than the corresponding Mg3Al-POM LDH catalyst.

  8. Organic–inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides with intercalated phacolysin as ocular delivery system

    Energy Technology Data Exchange (ETDEWEB)

    Qin, Zhiguo; Zhang, Jie; Chi, Huibo; Cao, Feng, E-mail: cpufengc@163.com [China Pharmaceutical University, Department of Pharmaceutics, School of Pharmacy (China)

    2015-12-15

    This study was mainly aimed to evaluate the potential use of a novel ocular drug delivery system, organic–inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides (LDH). Organic polymers of chitosan–glutathione (CG) and pre-activated chitosan–glutathione (CG-2MNA) were successfully synthesized and characterized. LDH with intercalated phacolysin (PCL), including larger hexagonal LDH–PCL (Lh-LDH–PCL), larger spherical LDH–PCL (Ls-LDH–PCL), smaller hexagonal LDH–PCL (Sh-LDH–PCL), CG hybrid LDH–PCL (LDH–PCL-CG), and CG-2MNA hybrid LDH–PCL (LDH–PCL-CG-2MNA), were prepared. The nanocomposites with particle size of 107.2–274.9 nm were characterized by powder X-ray diffraction, Fourier transform infrared, transmission electron micrographs, etc. In vivo precorneal retention studies showed that the detectable time of all nanocomposites was prolonged from 2 to 6 h in comparison to PCL saline. Accordingly, the AUC{sub 0–6h} values of Lh-LDH–PCL, Ls-LDH–PCL, Sh-LDH–PCL, LDH–PCL-CG, and LDH–PCL-CG-2MNA nanocomposites were increased by 2.27-, 2.08-, 3.08-, 4.67-, and 3.36-fold, respectively. The Draize test and hematoxylin and eosin staining demonstrated that modified LDH had no eye irritation after single and repeated administration. These results indicated that chitosan derivatives-LDH hybrid nanocomposite dispersion could be a promising ocular drug delivery system to improve precorneal retention time of drugs.Graphical AbstractThiolated chitosan-LDH hybrid nanocomposite dispersion could be a promising ocular drug delivery system to improve precorneal retention time of drugs and may facilitate penetration of drugs into tissues of the eyes.

  9. Organic-inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides with intercalated phacolysin as ocular delivery system

    Science.gov (United States)

    Qin, Zhiguo; Zhang, Jie; Chi, Huibo; Cao, Feng

    2015-12-01

    This study was mainly aimed to evaluate the potential use of a novel ocular drug delivery system, organic-inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides (LDH). Organic polymers of chitosan-glutathione (CG) and pre-activated chitosan-glutathione (CG-2MNA) were successfully synthesized and characterized. LDH with intercalated phacolysin (PCL), including larger hexagonal LDH-PCL (Lh-LDH-PCL), larger spherical LDH-PCL (Ls-LDH-PCL), smaller hexagonal LDH-PCL (Sh-LDH-PCL), CG hybrid LDH-PCL (LDH-PCL-CG), and CG-2MNA hybrid LDH-PCL (LDH-PCL-CG-2MNA), were prepared. The nanocomposites with particle size of 107.2-274.9 nm were characterized by powder X-ray diffraction, Fourier transform infrared, transmission electron micrographs, etc. In vivo precorneal retention studies showed that the detectable time of all nanocomposites was prolonged from 2 to 6 h in comparison to PCL saline. Accordingly, the AUC0-6h values of Lh-LDH-PCL, Ls-LDH-PCL, Sh-LDH-PCL, LDH-PCL-CG, and LDH-PCL-CG-2MNA nanocomposites were increased by 2.27-, 2.08-, 3.08-, 4.67-, and 3.36-fold, respectively. The Draize test and hematoxylin and eosin staining demonstrated that modified LDH had no eye irritation after single and repeated administration. These results indicated that chitosan derivatives-LDH hybrid nanocomposite dispersion could be a promising ocular drug delivery system to improve precorneal retention time of drugs.

  10. Organic–inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides with intercalated phacolysin as ocular delivery system

    International Nuclear Information System (INIS)

    Qin, Zhiguo; Zhang, Jie; Chi, Huibo; Cao, Feng

    2015-01-01

    This study was mainly aimed to evaluate the potential use of a novel ocular drug delivery system, organic–inorganic hybrid nanocomposites based on chitosan derivatives and layered double hydroxides (LDH). Organic polymers of chitosan–glutathione (CG) and pre-activated chitosan–glutathione (CG-2MNA) were successfully synthesized and characterized. LDH with intercalated phacolysin (PCL), including larger hexagonal LDH–PCL (Lh-LDH–PCL), larger spherical LDH–PCL (Ls-LDH–PCL), smaller hexagonal LDH–PCL (Sh-LDH–PCL), CG hybrid LDH–PCL (LDH–PCL-CG), and CG-2MNA hybrid LDH–PCL (LDH–PCL-CG-2MNA), were prepared. The nanocomposites with particle size of 107.2–274.9 nm were characterized by powder X-ray diffraction, Fourier transform infrared, transmission electron micrographs, etc. In vivo precorneal retention studies showed that the detectable time of all nanocomposites was prolonged from 2 to 6 h in comparison to PCL saline. Accordingly, the AUC 0–6h values of Lh-LDH–PCL, Ls-LDH–PCL, Sh-LDH–PCL, LDH–PCL-CG, and LDH–PCL-CG-2MNA nanocomposites were increased by 2.27-, 2.08-, 3.08-, 4.67-, and 3.36-fold, respectively. The Draize test and hematoxylin and eosin staining demonstrated that modified LDH had no eye irritation after single and repeated administration. These results indicated that chitosan derivatives-LDH hybrid nanocomposite dispersion could be a promising ocular drug delivery system to improve precorneal retention time of drugs.Graphical AbstractThiolated chitosan-LDH hybrid nanocomposite dispersion could be a promising ocular drug delivery system to improve precorneal retention time of drugs and may facilitate penetration of drugs into tissues of the eyes

  11. Soft-chemical synthesis and catalytic activity of Ni-Al and Co-Al layered double hydroxides (LDHs intercalated with anions with different charge density

    Directory of Open Access Journals (Sweden)

    Takahiro Takei

    2014-09-01

    Full Text Available Co-Al and Ni-Al layered double hydroxides (LDHs intercalated with three types of anionic molecules, dodecylsulfate (C12H25SO4−, DS, di-2-ethylsulfosuccinate ([COOC2H3EtBu]2C2H3SO3−, D2ES, and polytungstate (H2W12O4210−, HWO were prepared by means of ion-exchange and co-precipitation processes. With the use of DS and D2ES as intercalation agents, high crystallinity was maintained after intercalation into the LDHs. In the case of HWO, the intercalated LDHs could be obtained by ion-exchange as well as co-precipitation with a decline in the crystallinity; however, unreacted LDH was detected in the ion-exchange samples, and some unwanted phases such as hydroxide and pyrochlore were generated by the co-precipitation process. The maximum specific surface area and pore volume of the Ni-Al sample with intercalated HWO, prepared by the ion-exchange process were 74 m2/g and 0.174 mL/g, respectively. The occupancies of DS, D2ES, and HWO within the interlayer space were approximately 0.3–0.4, 0.5–0.6, and 0.1–0.2, respectively, in the Co-Al and Ni-Al LDHs. Analysis of the catalytic activity demonstrated that the DS-intercalated Ni-Al LDH sample exhibited relatively good catalytic activity for conversion of cyclohexanol to cyclohexanone.

  12. Preparation of an anionic azo pigment-pillared layered double hydroxide and the thermo- and photostability of the resulting intercalated material

    International Nuclear Information System (INIS)

    Guo Shengchang; Li Dianqing; Zhang Weifeng; Pu Min; Evans, David G.; Duan Xue

    2004-01-01

    A large anionic pigment has been intercalated into a layered double hydroxide (LDH) host by ion-exchange of an Mg/Al LDH-nitrate precursor with a solution of C.I. Pigment Red 48:2 (the calcium salt of 4-((5-chloro-4-methyl-2-sulfophenyl)azo)-3-hydroxy-2-naphthalene-carboxylic acid), in ethane-1,2-diol. After intercalation of the pigment, the interlayer distance in the LDH increases from 0.86 to 1.72nm. Infrared spectra and TG-DTA curves reveal the presence of a complex system of supramolecular host-guest interactions. The UV-visible diffuse reflectance spectra of C.I. Pigment Red 48:2 show marked changes after heating at 200 deg. C and above, whereas there are no significant changes in the spectra of the intercalated pigment after heating at temperatures up to 300 deg. C, showing that the thermostability is markedly enhanced by intercalation in the LDH host. The pigment-intercalated LDHs exhibits much higher photostability to UV light than the pristine pigment, in the case of both the pure solids and their composites with polypropylene, as shown by measurement of CIE 1976 L*a*b* color difference (ΔE) values

  13. Magnetic nanocomposites with drug-intercalated layered double hydroxide shell supported on commercial magnetite and laboratory-made magnesium ferrite core materials

    Energy Technology Data Exchange (ETDEWEB)

    Ay, Ahmet Nedim, E-mail: ay@hacettepe.edu.tr; Konuk, Deniz; Zuemreoglu-Karan, Birguel

    2011-07-20

    Mg-Al-layered double hydroxide intercalated with a model drug, salicylate, was deposited on laboratory-made magnesium ferrite and commercial magnetite nanoparticles. The obtained core-shell nanocomposites have been characterized by a variety of methods. The combined information from X-ray diffraction patterns, electron diffraction patterns, FTIR spectra, X-ray photoelectron spectra, electron microscopy images, thermogravimetric analysis and microchemical analysis has indicated a similar nature and composition for the two samples. Magnetic measurements have revealed that although the inherent magnetization of magnetite was significantly higher, the nanocomposites displayed nearly similar magnetic properties.

  14. Enrichment of rare earth metal ions by the highly selective adsorption of phytate intercalated layered double hydroxide.

    Science.gov (United States)

    Jin, Cheng; Liu, Huimin; Kong, Xianggui; Yan, Hong; Lei, Xiaodong

    2018-02-27

    Phytate intercalated MgAl layered double hydroxide (MgAl-LDH) was prepared by an anion exchange method with the precursor NO 3 - containing MgAl-LDH. The final as-synthesized product [Mg 0.69 Al 0.31 (OH) 2 ] (phytateNa 6 ) 0.05 (NO 3 ) 0.01 ·mH 2 O (phytate-LDH) has highly selective adsorption ability for some metal ions and can be used to enrich rare earth metal ions in mixed solution, such as Pr 3+ and Ce 3+ from a mixed solution of them with Pb 2+ and Co 2+ . At first, phytate-LDH has good adsorption performance for these ions in single metal ion solutions. At low concentration (below 10 mg L -1 ), all the capture rates of the four metal ions were more than 97%, for highly toxic Pb 2+ it was even up to nearly 100%, and a high capture rate (99.87%) was maintained for Pb 2+ at a high concentration (100 mg L -1 ). When all the four metal ions are co-existing in aqueous solution, the selectivity order is Pb 2+ ≫ Pr 3+ ≈ Ce 3+ > Co 2+ . In a solution containing mixtures of the three metal ions of Pr 3+ , Ce 3+ , and Co 2+ , the selectivity order is Pr 3+ ≈ Ce 3+ ≫ Co 2+ , and in a solution containing mixtures of Pr 3+ with Co 2+ and Ce 3+ with Co 2+ , the selectivity orders are Pr 3+ ≫ Co 2+ and Ce 3+ ≫ Co 2+ , respectively. The high selectivity and adsorption capacities for Pb 2+ , Co 2+ , Pr 3+ , and Ce 3+ result in the efficient removal of Pb 2+ and enrichment of the rare earth metal ions Pr 3+ and Ce 3+ by phytate-LDH. Based on the elemental analysis, it is found that the difference of the adsorption capacities is mainly due to the different coordination number of them with phytate-LDH. With molecular simulation, we believe that the adsorption selectivity is due to the difference of the binding energy between the metal ion and phytate-LDH. Therefore, the phytate-LDH is promising for the enrichment and/or purification of the rare earth metal ions and removal of toxic metal ions from waste water.

  15. Simultaneous intercalation and release of 2,4-dichloro- and 4-chloro-phenoxy acetates into Zn/Al layered double hydroxide

    Directory of Open Access Journals (Sweden)

    Abbas Matrod Bashi

    2016-11-01

    Full Text Available A new nanohybrid compound was formed by the concurrent insertion of 2,4-dichlorophenoxy acetate (DPA used as herbicides and 4-chlorophenoxy acetate (CPA as plant growth regulator, the two guest anions into the interlamellar space of the host Zn/Al layered double hydroxide (LDH using co-precipitation or spontaneous self-assembly method. Two different basal spacings of 2.54 and 1.97 nm were detected by PXRD of the nanohybrid accounting for the presence of two distinct intercalated phases. Direct insertion mass spectroscopy (DIMS analyses confirm that both anions are intercalated to give a biphasic well ordered nanohybrid material. The study of the release properties shows that both ions were released, but with different rates. This opens up the possibility of using such a biphasic nanohybrid for controlled release of more than one active anionic agent at different controlled rates.

  16. In Situ Formation of Decavanadate-Intercalated Layered Double Hydroxide Films on AA2024 and their Anti-Corrosive Properties when Combined with Hybrid Sol Gel Films

    Directory of Open Access Journals (Sweden)

    Junsheng Wu

    2017-04-01

    Full Text Available A layered double hydroxide (LDH film was formed in situ on aluminum alloy 2024 through a urea hydrolysis method, and a decavanadate-intercalated LDH (LDH-V film fabricated through the dip coating method. The microstructural and morphological characteristics were investigated by scanning electron microscopy (SEM. The corrosion-resistant performance was analyzed by electrochemical impedance spectroscopy (EIS, scanning electrochemical microscopy (SECM, and a salt-spray test (SST.The SEM results showed that a complete and defect-free surface was formed on the LDH-VS film. The anticorrosion results revealed that the LDH-VS film had better corrosion-resistant properties than the LDH-S film, especially long-term corrosion resistance. The mechanism of corrosion protection was proposed to consist of the self-healing effect of the decavanadate intercalation and the shielding effect of the sol-gel film.

  17. Toxicity and Metabolism of Layered Double Hydroxide Intercalated with Levodopa in a Parkinson’s Disease Model

    Directory of Open Access Journals (Sweden)

    Aminu Umar Kura

    2014-04-01

    Full Text Available Layered hydroxide nanoparticles are generally biocompatible, and less toxic than most inorganic nanoparticles, making them an acceptable alternative drug delivery system. Due to growing concern over animal welfare and the expense of in vivo experiments both the public and the government are interested to find alternatives to animal testing. The toxicity potential of zinc aluminum layered hydroxide (ZAL nanocomposite containing anti-Parkinsonian agent may be determined using a PC 12 cell model. ZAL nanocomposite demonstrated a decreased cytotoxic effect when compared to levodopa on PC12 cells with more than 80% cell viability at 100 µg/mL compared to less than 20% cell viability in a direct levodopa exposure. Neither levodopa-loaded nanocomposite nor the un-intercalated nanocomposite disturbed the cytoskeletal structure of the neurogenic cells at their IC50 concentration. Levodopa metabolite (HVA released from the nanocomposite demonstrated the slow sustained and controlled release character of layered hydroxide nanoparticles unlike the burst uptake and release system shown with pure levodopa treatment.

  18. Nanostructural drug-inorganic clay composites: Structure, thermal property and in vitro release of captopril-intercalated Mg Al-layered double hydroxides

    Science.gov (United States)

    Zhang, Hui; Zou, Kang; Guo, Shaohuan; Duan, Xue

    2006-06-01

    A nanostructural drug-inorganic clay composite involving a pharmaceutically active compound captopril (Cpl) intercalated Mg-Al-layered double hydroxides (Cpl-LDHs) with Mg/Al molar ratio of 2.06 has been assembled by coprecipitation method. Powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR) and Raman spectra analysis indicate a successful intercalation of Cpl between the layers with a vertical orientation of Cpl disulphide-containing S-S linkage. SEM photo indicates that as-synthesized Cpl-LDHs possess compact and non-porous structure with approximately and linked elliptical shape particles of ca. 50 nm. TG-DTA analyses suggest that the thermal stability of intercalated organic species is largely enhanced due to host-guest interaction involving the hydrogen bond compared to pure form before intercalation. The in vitro release studies show that both the release rate and release percentages markedly decrease with increasing pH from 4.60 to 7.45 due to possible change of release mechanism during the release process. The kinetic simulation for the release data, and XRD and FT-IR analyses for samples recovered from release media indicate that the dissolution mechanism is mainly responsible for the release behaviour of Cpl-LDHs at pH 4.60, while the ion-exchange one is responsible for that at pH 7.45.

  19. Mössbauer, XRD and TEM Study on the Intercalation and the Release of Drugs in/from Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    E. Kuzmann

    2015-12-01

    Full Text Available Layered double hydroxides (LDHs are one of the very important nano-carriers for drug delivery, due to their many advantageous features, such as the ease and low-cost of preparation, low cytotoxicity, good biocompatibility, protection for the intercalated drugs, and the capacity to facilitate the uptake of the loaded drug in the cells. In our previous studies, Mössbauer spectroscopy was applied to monitor structural changes occurring during the incorporation of Fe(III in MgFe- and CaFe-LDHs, and the intercalation of various organic compounds in anionic form. Recently, we have successfully elaborated a protocol for the intercalation and release of indol-2-carboxylate and L-cysteinate in CaFe-LDH. The corresponding structural changes in the LDH samples were studied by XRD, HR-TEM and 57Fe Mössbauer spectroscopy. The Mössbauer spectra reflected small but significant changes upon both the intercalation and the release of drugs. The changes in the basal distances could be followed by XRD measurements, and HR-TEM images made these changes visible.

  20. Oxidation of Dodecanoate Intercalated Iron(II)–Iron(III) Layered Double Hydroxide to Form 2D Iron(III) (Hydr)oxide Layers

    DEFF Research Database (Denmark)

    Huang, Li‐Zhi; Ayala‐Luis, Karina B.; Fang, Liping

    2013-01-01

    .00(OH)5.31(C12H23O2)0.66(SO4)0.51 and FeIII3O2.18(OH)3.13(C12H23O2)0.56(SO4)0.47, respectively. oxGRC12 has the same planar layer structure as GRC12, as revealed by identical powder X‐ray diffraction patterns. The electrostatic interactions between the interlayer dodecanoate (C12) anions and the iron...... hydroxide planar layer were preserved during the oxidation, as shown by FTIR spectroscopy. The high positive charge in the hydroxide layer produced by the oxidation of iron(II) to iron(III) is partially compensated by the deprotonation of hydroxy groups, as shown by X‐ray photoelectron spectroscopy...... between the alkyl chains of the intercalated dodecanoate anions play a crucial role in stabilizing the structure and hindering the collapse of the iron(II)–iron(III) (hydr)oxide structure during oxidation. This is the first report describing the formation of a stable planar layered octahedral iron...

  1. Preparation and characterization of lactate-intercalated Co-Fe layered double hydroxides and exfoliated nanosheet film with low infrared emissivity

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Yunxia [School of Chemistry and Chemical Engineering, Southeast University, Optoelectronic Functional Materials and Engineering Laboratory, Jiangsu, Nanjing 211189 (China); Zhou Yuming, E-mail: ymzhou@seu.edu.cn [School of Chemistry and Chemical Engineering, Southeast University, Optoelectronic Functional Materials and Engineering Laboratory, Jiangsu, Nanjing 211189 (China); Zhang Tao; He Man; Wang Yongjuan [School of Chemistry and Chemical Engineering, Southeast University, Optoelectronic Functional Materials and Engineering Laboratory, Jiangsu, Nanjing 211189 (China); Yang Xiaoming [Suzhou Sidike New Material Technology Co., Ltd., Suzhou 215400 (China); Yang Yong [School of Chemistry and Chemical Engineering, Southeast University, Optoelectronic Functional Materials and Engineering Laboratory, Jiangsu, Nanjing 211189 (China)

    2012-12-15

    Highlights: Black-Right-Pointing-Pointer We use ferrous, cobalt powders and lactic acid to synthesis lactate-intercalated Co-Fe layered double hydroxides successfully. Black-Right-Pointing-Pointer A possible orientation of the intercalated lactate between the layers is carried out. Black-Right-Pointing-Pointer The thin nanosheet film is fabricated and the surface is very smooth and flat. Black-Right-Pointing-Pointer The infrared emissivity value of Co-Fe LDHs is lower than that of Zn-Al or Mg-Al LDHs, and the value is further reduced after forming a thin film. - Abstract: Lactate-intercalated Co-Fe layered double hydroxides (LDHs) were successfully prepared by coprecipitation and hydrothermal method. In this process, divalent metal ions as precursors can be obtained from the reduction reaction of lactic acid and metal powder (cobalt and ferrous). In order to obtain Fe{sup 3+}, H{sub 2}O{sub 2} (30%) was used to oxidize Fe{sup 2+}. Meanwhile, the produced lactate was intercalated into the LDHs interlayers to compensate the positively charged layers. The as-synthesized LDHs were studied by element chemical analysis, powder X-ray diffraction (XRD), FT-IR spectroscopy, thermogravitry (TG) and differential scanning calorimetry (DSC), TEM. The results indicated that the basal spacing value of the LDHs was larger than that of lactate-intercalated Mg-Al or Zn-Al LDHs. It proved that the lactate anions were inserted into the gallery in the form of dimers which made it easy to be delaminated in water. The obtained nanosheets were deposited on the substrates to form the film which was characterized by TEM and AFM, and infrared emissivity value (8-14 {mu}m) was also investigated. The infrared emissivity values of Co-Fe LDHs were lower than that of Zn-Al which took advantage of the special electronic structure in Co and Fe. Besides, the orderly structure and the reduction of the interfacial deficiency of the film made the values further reduced.

  2. Real-time tracking of hydrogen peroxide secreted by live cells using MnO{sub 2} nanoparticles intercalated layered doubled hydroxide nanohybrids

    Energy Technology Data Exchange (ETDEWEB)

    Asif, Muhammad; Aziz, Ayesha [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, Hubei Key Laboratory of Material Chemistry and Service Failure, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, 1037 Luoyu Road, Wuhan, 430074 (China); Dao, Anh Quang [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, Hubei Key Laboratory of Material Chemistry and Service Failure, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, 1037 Luoyu Road, Wuhan, 430074 (China); Hue Industrial College, 70 Nguyen Hue, Hue, Thua Thien Hue, 531081 (Viet Nam); Hakeem, Abdul; Wang, Haitao; Dong, Shuang; Zhang, Guoan [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, Hubei Key Laboratory of Material Chemistry and Service Failure, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, 1037 Luoyu Road, Wuhan, 430074 (China); Xiao, Fei [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, Hubei Key Laboratory of Material Chemistry and Service Failure, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, 1037 Luoyu Road, Wuhan, 430074 (China); Shenzhen Institute of Huazhong University of Science & Technology, Shenzhen, 518000 (China); Liu, Hongfang, E-mail: liuhf@hust.edu.cn [Key Laboratory for Large-Format Battery Materials and System, Ministry of Education, Hubei Key Laboratory of Material Chemistry and Service Failure, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, 1037 Luoyu Road, Wuhan, 430074 (China); Shenzhen Institute of Huazhong University of Science & Technology, Shenzhen, 518000 (China)

    2015-10-22

    We report a facile and green method for the fabrication of new type of electrocatalysts based on MnO{sub 2} nanoparticles incorporated on MgAl LDH P-type semiconductive channel and explore its practical applications as high-performance electrode materials for electrochemical biosensor. A series of MgAl layered doubled hydroxide (LDH) nanohybrids with fixed Mg/Al (M{sup 2+}/M{sup 3+} atomic ratio of 3) and varied amount of MnCl{sub 2}.4H{sub 2}O are fabricated by a facile co-precipitation method. This approach demonstrates the combination of distinct properties including excellent intercalation features of LDH for entrapping nanoparticles and high loading of MnO{sub 2} nanoparticles in the host layers of LDH. Among all samples, Mn5–MgAl with 0.04% loaded manganese has a good crystalline morphology. A well-dispersed MnO{sub 2} nanoparticles encapsulated into the host matrix of hydrotalcite exhibit enhanced electrocatalytic activity towards the reduction of H{sub 2}O{sub 2} as well as excellent stability, selectivity and reproducibility due to synergistic effect of good catalytic ability of MnO{sub 2} and conductive MgAl LDH. Glass carbon electrode (GCE) modified with Mn5–MgAl possesses a wide linear range of 0.05–78 mM, lowest detection limit 5 μM (S/N = 3) and detection sensitivity of 0.9352 μAmM{sup −1}. This outstanding performance enables it to be used for real-time tracking of H{sub 2}O{sub 2} secreted by live HeLa cells. This work may provide new insight in clinical diagnosis, on-site environmental analysis and point of care testing devices. - Highlights: • MnO{sub 2}MgAl nanohybrids have been fabricated by a facile and robust co-precipitation approach. • MgAl layered doubled hydroxide can be used for the intercalation of MnO{sub 2} nanoparticles. • MgAl layered doubled hydroxide nanohybrid serves as p-type semiconductive channel for efficient electrocatalysis. • The nanohybrid electrode demonstrates excellent electrochemical performance

  3. Reversible hydration and aqueous exfoliation of the acetate-intercalated layered double hydroxide of Ni and Al: Observation of an ordered interstratified phase

    International Nuclear Information System (INIS)

    Manohara, G.V.; Vishnu Kamath, P.; Milius, Wolfgang

    2012-01-01

    Acetate-intercalated layered double hydroxides (LDHs) of Ni and Al undergo reversible hydration in the solid state in response to the ambient humidity. The LDH with a high layer charge (0.33/formula unit) undergoes facile hydration in a single step, whereas the LDH with a lower layer charge (0.24/formula unit) exhibits an ordered interstratified intermediate, comprising the hydrated and dehydrated layers stacked alternatively. This phase, also known as the staged S-2 phase, coexists with the end members suggesting the existence of a solution-type equilibrium between the S-2 phase and the end members of the hydration cycle. These LDHs also undergo facile aqueous exfoliation into 2–5 nm-thick tactoids with a radial dimension of 0.2–0.5 μm. - Graphical abstract: Schematic of the hydrated, dehydrated and interstratified phases observed during the hydration–dehydration of Ni/Al–CH 3 COO LDH. Highlights: ► Ni/Al-acetate LDHs were synthesized by HPFS method by hydrolysis of acetamide. ► Intercalated acetate ion shows reversible hydration with variation in humidity. ► An ordered interstratified phase was observed during hydration/dehydration cycle. ► A solution type equilibrium is observed between hydration–dehydration phases. ► These LDHs undergo facile aqueous exfoliation.

  4. Reversible intercalation of ammonia molecules into a layered double hydroxide structure without exchanging nitrate counter-ions

    International Nuclear Information System (INIS)

    Carbajal Arizaga, Gregorio Guadalupe; Wypych, Fernando; Castillon Barraza, Felipe; Contreras Lopez, Oscar Edel

    2010-01-01

    A zinc/aluminum LDH was precipitated with recycled ammonia from a chemical vapor deposition reaction. The LDH presented a crystalline phase with basal distance of 8.9 A, typical for nitrate-containing LDHs, and another phase with a basal distance of 13.9 A. Thermal treatment at 150 o C eliminated the phase with the bigger basal distance leaving only the anhydrous nitrate-intercalated LDH structure with 8.9 A. Intense N-H stretching modes in the FTIR spectra suggested that the expansion was due to intercalation of ammonia in the form of [NH 4 (NH 3 ) n ] + species. When additional samples were precipitated with pure ammonia, the conventional LDH nitrate structure was obtained (8.9 A basal distance) at pH=7, as well as a pure crystalline phase with 13.9 A basal distance at pH=10 due to ammonia intercalation that can be removed by heating at 150 o C or by stirring in acetone, confirming a unusual sensu stricto intercalation process into a LDH without exchanging nitrate ions. - Graphical abstract: LDH-nitrate precipitated with ammonia expands the interlayer space if ammonia is bubbled up to pH 10. The basal distance decreased when the compound was heated at 150 o C or stirred in acetone. Nitrate ions are not exchanged.

  5. Influence of Hydrothermal Treatment on Physicochemical Properties and Drug Release of Anti-Inflammatory Drugs of Intercalated Layered Double Hydroxide Nanoparticles

    Directory of Open Access Journals (Sweden)

    Zi Gu

    2014-05-01

    Full Text Available The synthesis method of layered double hydroxides (LDHs determines nanoparticles’ performance in biomedical applications. In this study, hydrothermal treatment as an important synthesis technique has been examined for its influence on the physicochemical properties and the drug release rate from drug-containing LDHs. We synthesised MgAl–LDHs intercalated with non-steroidal anti-inflammatory drugs (i.e., naproxen, diclofenac and ibuprofen using a co-precipitation method with or without hydrothermal treatment (150 °C, 4 h. After being hydrothermally treated, LDH–drug crystallites increased in particle size and crystallinity, but did not change in the interlayer anion orientation, gallery height and chemical composition. The drug release patterns of all studied LDH–drug hybrids were biphasic and sustained. LDHs loaded with diclofenac had a quicker drug release rate compared with those with naproxen and ibuprofen, and the drug release from the hydrothermally-treated LDH–drug was slower than the freshly precipitated LDH–drug. These results suggest that the drug release of LDH–drugs is influenced by the crystallite size of LDHs, which can be controlled by hydrothermal treatment, as well as by the drug molecular physicochemical properties.

  6. Intercalation of p-methycinnamic acid anion into Zn-Al layered double hydroxide to improve UV aging resistance of asphalt

    Directory of Open Access Journals (Sweden)

    Chao Peng

    2015-02-01

    Full Text Available A UV absorber, p-methycinnamic acid (PMCA, was intercalated into Zn-Al layered double hydroxide (LDH by calcination recovery. Fourier transform infrared spectroscopy showed that the PMCA anions completely replaced the CO32− anions in the interlayer galleries of Zn-Al-LDH containing PMCA anions (Zn-Al-PMCA-LDH. X-ray diffraction and transmission electron microscopy showed that the interlayer distance increased from 0.78 nm to 1.82 nm after the substitution of PMCA anions for CO32− anions. The similar diffraction angles of the CO32− anion-containing Zn-Al-LDH (Zn-Al-CO32−-LDH and the Zn-Al-CO32−-LDH/styrene–butadiene–styrene (SBS modified asphalt implied that the asphalt molecules do not enter into the LDH interlayer galleries to form separated-phase structures. The different diffraction angles of Zn-Al-PMCA-LDH and Zn-Al-PMCA-LDH/SBS modified asphalt indicated that the asphalt molecules penetrated into the LDH interlayer galleries to form an expanded-phase structure. UV-Vis absorbance analyses showed that Zn-Al-PMCA-LDH was better able to block UV light due to the synergistic effects of PMCA and Zn-Al-LDH. Conventional physical tests and atomic force microscopy images of the SBS modified asphalt, Zn-Al-CO32−-LDH/SBS modified asphalt and Zn-Al-PMCA-LDH/SBS modified asphalt before and after UV aging indicated that Zn-Al-PMCA-LDH improved the UV aging resistance of SBS modified asphalts.

  7. Layered double hydroxides

    DEFF Research Database (Denmark)

    López Rayo, Sandra; Imran, Ahmad; Hansen, Hans Chr. Bruun

    2017-01-01

    A novel zinc (Zn) fertilizer concept based on Zn doped layered double hydroxides (Zn-doped Mg-Fe-LDHs) has been investigated. Zn-doped Mg-Fe-LDHs were synthetized, their chemical composition was analyzed and their nutrient release was studied in buffered solutions with different pH values. Uptake...

  8. Electric and dielectric behavior of copper-chromium layered double hydroxide intercalated with dodecyl sulfate anions using impedance spectroscopy

    Science.gov (United States)

    Elhatimi, Wafaa; Bouragba, Fatima Zahra; Lahkale, Radouane; Sadik, Rachid; Lebbar, Nacira; Siniti, Mustapha; Sabbar, Elmouloudi

    2018-05-01

    The Cu2Cr-DS-LDH hybrid was successfully prepared by the anion exchange method at room temperature. The structure, the chemical composition and the physico-chemical properties of the sample were determined using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA) and inductively coupled plasma (ICP). In this work, the electrical and dielectric properties investigated are determined using impedance spectroscopy (IS) in a frequency range of 1 Hz to 1 MHz. Indeed, the Nyquist diagram modelized by an electrical equivalent circuit showed three contributions attributed respectively to the polarization of grains, grains boundaries and interface electrode-sample. This modelization allowed us to determine the intrinsic electrical parameters of the hybrid (resistance, pseudo-capacitance and relaxation time). The presence of the non-Debye relaxation phenomena was confirmed by the frequency analysis of impedance. Moreover, the evolution of the alternating current conductivity (σac) studied obeys the double power law of Jonscher. The ionic conduction of this material was generated through a jump movement by translation of the charge carriers. As for the dielectric behavior of the material, the evolution of dielectric constant as a function of frequency shows relatively high values in a frequency range between 10 Hz and 1 KHz. The low values of the loss tangent obtained in this frequency zone can valorize this LDH hybrid.

  9. The Effect of Single, Binary and Ternary Anions of Chloride, Carbonate and Phosphate on the Release of 2,4-Dichlorophenoxyacetate Intercalated into the Zn-Al-layered Double Hydroxide Nanohybrid.

    Science.gov (United States)

    Hussein, Mohd Zobir; Jaafar, Adila Mohamad; Yahaya, Asmah Hj; Zainal, Zulkarnain

    2009-08-04

    Intercalation of beneficial anion into inorganic host has lead to an opportunity to synthesize various combinations of new organic-inorganic nanohybrids with various potential applications; especially, for the controlled release formulation and storage purposes. Investigation on the release behavior of 2,4-dichlorophenoxyacetate (2,4-D) intercalated into the interlayer of Zn-Al-layered double hydroxide (ZAN) have been carried out using single, binary and ternary aqueous systems of chloride, carbonate and phosphate. The release behavior of the active agent 2,4-D from its double-layered hydroxide nanohybrid ZANDI was found to be of controlled manner governed by pseudo-second order kinetics. It was found that carbonate medium yielded the highest accumulated release of 2,4-D, while phosphate in combination with carbonate and/or nitrate speeds up the release rate of 2,4-D. These results indicate that it is possible to design and develop new delivery system of latex stimulant compound with controlled release property based on 2,4-D that is known as a substance to increase latex production of rubber tree, Hevea brasiliensis.

  10. The Effect of Single, Binary and Ternary Anions of Chloride, Carbonate and Phosphate on the Release of 2,4-Dichlorophenoxyacetate Intercalated into the Zn–Al-layered Double Hydroxide Nanohybrid

    Directory of Open Access Journals (Sweden)

    Zainal Zulkarnain

    2009-01-01

    Full Text Available Abstract Intercalation of beneficial anion into inorganic host has lead to an opportunity to synthesize various combinations of new organic–inorganic nanohybrids with various potential applications; especially, for the controlled release formulation and storage purposes. Investigation on the release behavior of 2,4-dichlorophenoxyacetate (2,4-D intercalated into the interlayer of Zn–Al-layered double hydroxide (ZAN have been carried out using single, binary and ternary aqueous systems of chloride, carbonate and phosphate. The release behavior of the active agent 2,4-D from its double-layered hydroxide nanohybrid ZANDI was found to be of controlled manner governed by pseudo-second order kinetics. It was found that carbonate medium yielded the highest accumulated release of 2,4-D, while phosphate in combination with carbonate and/or nitrate speeds up the release rate of 2,4-D. These results indicate that it is possible to design and develop new delivery system of latex stimulant compound with controlled release property based on 2,4-D that is known as a substance to increase latex production of rubber tree,Hevea brasiliensis.

  11. Layered hydroxides intercalated with organic anions and their application in preparation of LDH/polymer nanocomposites

    Czech Academy of Sciences Publication Activity Database

    Kovanda, F.; Jindová, E.; Doušová, B.; Koloušek, D.; Pleštil, Josef; Sedláková, Zdeňka

    2009-01-01

    Roč. 6, č. 1 (2009), s. 111-119 ISSN 1214-9705 R&D Projects: GA AV ČR KAN100500651 Institutional research plan: CEZ:AV0Z40500505 Keywords : hydrotalcite * layered double hydroxides * intercalation Subject RIV: CD - Macromolecular Chemistry Impact factor: 0.275, year: 2009

  12. High-temperature X-ray powder diffraction as a tool for characterization of smectites, layered double hydroxides, and their intercalates with porphyrins

    Czech Academy of Sciences Publication Activity Database

    Píšková, A.; Bezdička, Petr; Hradil, David; Káfuňková, E.; Lang, Kamil; Večerníková, Eva; Kovanda, F.; Grygar, Tomáš

    2010-01-01

    Roč. 49, č. 4 (2010), s. 363-371 ISSN 0169-1317 R&D Projects: GA ČR(CZ) GA203/06/1244; GA AV ČR KAN100500651; GA AV ČR IAA3032401 Institutional research plan: CEZ:AV0Z40320502 Keywords : smectite * Layer ed double hydroxides * thermal decomposition Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.303, year: 2010

  13. Intercalation of ethylene glycol into yttrium hydroxide layered materials.

    Science.gov (United States)

    Xi, Yuanzhou; Davis, Robert J

    2010-04-19

    Intercalation of ethylene glycol into layered yttrium hydroxide containing nitrate counterions was accomplished by heating the reagents in a methanol solution of sodium methoxide under autogenous pressure at 413 K for 20 h. The resulting crystalline material had an expanded interlayer distance of 10.96 A, confirming the intercalation of an ethylene glycol derived species. Characterization of the material by FT-IR spectroscopy, thermogravimetric analysis, and the catalytic transesterification of tributyrin with methanol was consistent with direct bonding of ethylene glycolate anions (O(2)C(2)H(5)(-)) to the yttrium hydroxide layers, forming Y-O-C bonds. The layers of the material are proposed to be held together by H-bonding between the hydroxyls of grafted ethylene glycol molecules attached to adjacent layers. Glycerol can also be intercalated into yttrium hydroxide layered materials by a similar method.

  14. 5-Fluorouracil intercalated iron oxide@layered double hydroxide core-shell nano-composites with isotropic and anisotropic architectures for shape-selective drug delivery applications.

    Science.gov (United States)

    Tuncelli, Gülsevde; Ay, Ahmet Nedim; Zümreoglu-Karan, Birgül

    2015-10-01

    We report the synthesis, characterization and in vitro release behavior of anti-cancer drug carrying iron oxide@layered double hydroxide core-shell nanocomposites with sizes ranging from 40 to 300 nm, good drug loading capacities and soft ferromagnetic properties. HRTEM analyses verified that nearly spherical isotropic carriers were obtained by coating spherical magnetite particles while anisotropic carriers were obtained by coating spindle-shaped hematite particles. They both displayed a fluctuating in vitro release profile with a higher release percentage for the anisotropic carrier. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Superconductivity and magnetism in iron sulfides intercalated by metal hydroxides.

    Science.gov (United States)

    Zhou, Xiuquan; Eckberg, Christopher; Wilfong, Brandon; Liou, Sz-Chian; Vivanco, Hector K; Paglione, Johnpierre; Rodriguez, Efrain E

    2017-05-01

    Inspired by naturally occurring sulfide minerals, we present a new family of iron-based superconductors. A metastable form of FeS known as the mineral mackinawite forms two-dimensional sheets that can be readily intercalated by various cationic guest species. Under hydrothermal conditions using alkali metal hydroxides, we prepare three different cation and metal hydroxide-intercalated FeS phases including (Li 1- x Fe x OH)FeS, [(Na 1- x Fe x )(OH) 2 ]FeS, and K x Fe 2- y S 2 . Upon successful intercalation of the FeS layer, the superconducting critical temperature T c of mackinawite is enhanced from 5 K to 8 K for the (Li 1- x Fe x OH) δ + intercalate. Layered heterostructures of [(Na 1- x Fe x )(OH) 2 ]FeS resemble the natural mineral tochilinite, which contains an iron square lattice interleaved with a hexagonal hydroxide lattice. Whilst heterostructured [(Na 1- x Fe x )(OH) 2 ]FeS displays long-range magnetic ordering near 15 K, K x Fe 2- y S 2 displays short range antiferromagnetism.

  16. Alkali metal and alkali metal hydroxide intercalates of the layered transition metal disulfides

    International Nuclear Information System (INIS)

    Kanzaki, Y.; Konuma, M.; Matsumoto, O.

    1981-01-01

    The intercalation reaction of some layered transition metal disulfides with alkali metals, alkali metal hydroxides, and tetraalkylammonium hydroxides were investigated. The alkali metal intercalates were prepared in the respective metal-hexamethylphosphoric triamide solutions in vaccuo, and the hydroxide intercalates in aqueous hydroxide solutions. According to the intercalation reaction, the c-lattice parameter was increased, and the increase indicated the expansion of the interlayer distance. In the case of alkali metal intercalates, the expansion of the interlayer distance increased continuously, corresponding to the atomic radius of the alkali metal. On the other hand, the hydroxide intercalates showed discrete expansion corresponding to the effective ionic radius of the intercalated cation. All intercalates of TaS 2 amd NbS 2 were superconductors. The expansion of the interlayer distance tended to increase the superconducting transition temperature in the intercalates of TaS 2 and vice versa in those of NbS 2 . (orig.)

  17. A new route to prepare nanocomposites based on polyvinyl chloride and MgAl layered double hydroxide intercalated with laurylether phosphate

    Directory of Open Access Journals (Sweden)

    2009-09-01

    Full Text Available The MgAl layered double hydroxide (LDH with laurylether phosphate was prepared using reconstruction method. Delamilation of the LDH with laurylether phosphate (LDH-PK in tetrahydrofuran was characterized by AFM (atomic force microscopy, indicating that a large part of the LDH was delaminated into single, double and multi layers. The delaminated LDH-PK suspension was then used with polyvinyl chloride (PVC to prepare a series of high-LDH-loading nanocomposites. Both the XRD (X-ray diffraction patterns and TEM (transmission electron microscopy photographs of the as-prepared PVC/LDH nanocomposites indicated that the LDH nanolayers dispersed uniformly in the PVC matrix. With differential scanning calorimetry (DSC the glass transition temperatures of PVC phases in the PVC/LDH nanocomposites were measured and a slightly lower value than that of pristine PVC has been observed. Thermogravimetric analysis results show that the presence of LDH enhanced the dehydrochlorination temperature (Tmax1, reduced the maximum degradation rate (Rmax1 and the 5% weight loss temperature, and promoted the char formation of PVC. However, the thermal degradation temperature (Tmax2 and thermal degradation rate (Rmax2 of the dehydrochlorinated PVC were slightly affected by the presence of LDH. The apparent activation energies were calculated by the method of Flynn-Wall-Ozawa in nitrogen at four different heating rates, showing that the nanofiller increased the apparent activation energies by 10–26 kJ/mol when compared with pristine PVC, probably implying that the LDH nanolayers improve the stability of chlorine atom on the PVC chains.

  18. Influence of sodium dodecyl sulfate concentration on the photocatalytic activity and dielectric properties of intercalated sodium dodecyl sulfate into Zn–Cd–Al layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Abdullah Ahmed Ali, E-mail: abdullah2803@gmail.com [Department of Physics, Faculty of Applied Science, Thamar University, Dhamar 87246 (Yemen); Talib, Zainal Abidin [Department of Physics, Faculty of Science, Universiti Putra Malaysia, UPM, Serdang, Selangor 43400 (Malaysia); Hussein, Mohd Zobir [Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, UPM, Serdang, Selangor 43400 (Malaysia)

    2015-02-15

    Highlights: • Zn–Cd–Al–LDH–DS were synthesized with different SDS concentrations. • Photocatalytic activity of samples was improved by increasing SDS concentration. • Dielectric response of LDH can be described by anomalous low frequency dispersion. • The dc conductivity values were calculated for Zn–Cd–Al–LDH–DS samples. • ESR spectra exhibited the successful intercalation of DS molecule into LDH gallery. - Abstract: Sodium dodecyl sulfate (SDS) has been successfully intercalated into Zn–Cd–Al–LDH precursor with different SDS concentrations (0.2, 0.3, 0.4, 0.5 and 1 mol L{sup −1}) using the coprecipitation method at (Zn{sup 2+} + Cd{sup 2+})/Al{sup 3+} molar ratio of 13 and pH 8. The structural, morphological, texture and composition properties of the synthesized (Zn–Cd–Al–LDH–DS) nanostructure were investigated using powder X-ray diffraction (PXRD), scanning electron microscope (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR), respectively. The photocatalytic activity of these materials was developed by increasing the concentration of intercalated SDS. The absorbance spectra have been used to detect an anion in the LDH interlayer before and after the intercalation process, which confirmed the presence of the dodecyl sulfate (DS{sup −}) anion into LDH gallery after intercalation. The anomalous low frequency dispersion (ALFD) has been used to describe the dielectric response of Zn–Cd–Al–LDH–DS nanostructure using the second type of universal power law. At low frequency, the polarization effect of electrodes caused the rising in dielectric constant and loss values. An important result of the dielectric measurements is the calculated dc conductivity values, which are new in dielectric spectroscopy of LDH materials. An important result of the electron spin resonance (ESR) spectra exhibited the successful intercalation of DS molecule into LDH gallery. The g-factor value was affected by

  19. Kinetics and equilibrium studies on the treatment of nitric acid with Mg-Al oxide obtained by thermal decomposition of NO3(-)-intercalated Mg-Al layered double hydroxide.

    Science.gov (United States)

    Kameda, Tomohito; Fubasami, Yuki; Yoshioka, Toshiaki

    2011-10-15

    Mg-Al oxide obtained by thermal decomposition of NO(3)(-)-intercalated Mg-Al layered double hydroxide (NO(3)·Mg-Al LDH) was found to treat HNO(3), acting as both a neutralizer and fixative for NO(3)(-). The degree of NO(3)(-) removal increased with time, Mg-Al oxide quantity, and temperature. The NO(3)(-) removal could be represented by a first-order reaction. The apparent activation energy was 52.9 kJ mol(-1), confirming that NO(3)(-) removal by Mg-Al oxide proceeded under chemical reaction control. Furthermore, the adsorption of NO(3)(-) on Mg-Al oxide could be expressed by a Langmuir-type adsorption isotherm. The maximum adsorption amount and equilibrium adsorption constant were 3.8 mmol g(-1) and 1.33, respectively. The Gibbs free energy change was -18 kJ mol(-1), confirming that the uptake of NO(3)(-) from HNO(3) by Mg-Al oxide proceeded spontaneously. Copyright © 2011 Elsevier Inc. All rights reserved.

  20. Synthesis of graphene oxide-intercalated alpha-hydroxides by metathesis and their decomposition to graphene/metal oxide composites

    OpenAIRE

    Nethravathi, C; Rajamathi, Michael; Ravishankar, N; Basit, Lubna; Felser, Claudia

    2010-01-01

    Graphene oxide-intercalated alpha-metal hydroxides were prepared using layers from the delaminated colloidal dispersions of cetyltrimethylammonium-intercalated graphene oxide and dodecylsulfate-intercalated alpha-hydroxide of nickel/cobalt as precursors. The reaction of the two dispersions leads to de-intercalation of the interlayer ions from both the layered solids and the intercalation of the negatively charged graphene oxide sheets between the positively charged layers of the alpha-hydroxi...

  1. Fabrication of a novel NiFe2O4/Zn-Al layered double hydroxide intercalated with EDTA composite and its adsorption behavior for Cr(VI) from aqueous solution

    Science.gov (United States)

    Deng, Lin; Shi, Zhou; Wang, Li; Zhou, Shiqing

    2017-05-01

    A novel magnetic NiFe2O4/Zn-Al layered double hydroxide intercalated with EDTA composite (NiFe2O4/ZnAl-EDTA LDH) was prepared through modified coprecipitation method and employed for adsorptive removal of Cr(VI) from aqueous solution. The adsorbents were characterized using Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), vibrating sample magnetometer (VSM), and X-ray photoelectron spectroscopy (XPS). Factors affecting the Cr(VI) adsorption, such as initial solution pH, adsorbent dosage, contact time, initial Cr(VI) concentration, temperature and coexisting ions, were studied systematically. Experiments results show that the magnetic NiFe2O4/ZnAl-EDTA LDH exhibits high adsorption efficiency within a wide pH range of 3.0-7.0 (R>80% at Cr(VI) concentration 50 mg L-1, contact time 360 min, and adsorbent dosage 2 g/L) and quick separation property. The adsorption process is fitted well with the Langmuir isotherm and pseudo-second-order kinetic model. The maximum theoretical adsorption capacity is found to be 77.22 mg g-1 at pH 6.0 and 318 K. The positive ΔH value (2.907 kJ mol-1) and negative ΔG value (-4.722 kJ mol-1) at 298-318 K reveals that the adsorption process is feasible, spontaneous and endothermic. Coexisting anions (PO43-, SO42-, CO32-, HCO3-, Cl-, and NO3-) have no significant effect on Cr(VI) removal. The mechanism study indicates that the adsorption of Cr(VI) onto NiFe2O4/ZnAl-EDTA LDH mainly involves electrostatic attraction and ion exchange interaction. It is interesting to note that a proportion of Cr(VI) adsorbed on the adsorbent surface are reduced to Cr(III) during the adsorption process. Results from this study demonstrate the potential utility of the magnetic NiFe2O4/ZnAl-EDTA LDH that could be developed into a viable technology for efficient removal of Cr(VI) from aqueous solution.

  2. Accessing the biocompatibility of layered double hydroxide by intramuscular implantation: histological and microcirculation evaluation

    OpenAIRE

    Cunha, Vanessa Roberta Rodrigues; de Souza, Rodrigo Barbosa; da Fonseca Martins, Ana Maria Cristina Rebello Pinto; Koh, Ivan Hong Jun; Constantino, Vera Regina Leopoldo

    2016-01-01

    Biocompatibility of layered double hydroxides (LDHs), also known as hydrotalcite-like materials or double metal hydroxides, was investigated by in vivo assays via intramuscular tablets implantation in rat abdominal wall. The tablets were composed by chloride ions intercalated into LDH of magnesium/aluminum (Mg2Al-Cl) and zinc/aluminum (Zn2Al-Cl). The antigenicity and tissue integration capacity of LDHs were assessed histologically after 7 and 28 days post-implantation. No fibrous capsule near...

  3. A new approach to reducing the flammability of layered double hydroxide (LDH)-based polymer composites: preparation and characterization of dye structure-intercalated LDH and its effect on the flammability of polypropylene-grafted maleic anhydride/d-LDH composites.

    Science.gov (United States)

    Kang, Nian-Jun; Wang, De-Yi; Kutlu, Burak; Zhao, Peng-Cheng; Leuteritz, Andreas; Wagenknecht, Udo; Heinrich, Gert

    2013-09-25

    Dye structure-intercalated layered double hydroxide (d-LDH) was synthesized using a one-step method, and its intercalated behaviors have been characterized by Fourier transform infrared spectroscopy (FTIR), wide angle X-ray scattering (WAXS), scanning electron microscopy, thermogravimetric analysis (TGA), etc. As a novel functional potential fire-retarding nanofiller, it was used to prepare a polypropylene-grafted maleic anhydride (PP-g-MA)/d-LDH composite by refluxing the mixture of d-LDH and PP-g-MA in xylene, aiming to investigate its effect on the flammability of the PP-g-MA composite. The morphological properties, thermal stability, and flame retardant properties of the PP-g-MA/d-LDH composite were determined by FTIR, WAXS, transmission electron microscopy, TGA, and microscale combustion calorimetry. Compared with NO3-LDH (unmodified LDH) and LDH intercalated by sodium dodecylbenzenesulfonate (conventional organo-modified LDH), d-LDH can significantly decrease the heat release rate and the total heat release of the PP-g-MA composite, offering a new approach to imparting low flammability to LDH-based polymer composites.

  4. Acetyl salicylic acid–ZnAl layered double hydroxide functional nanohybrid for skin care application

    CSIR Research Space (South Africa)

    Mosangi, Damodar

    2016-10-01

    Full Text Available In this study, a pharmaceutically active ingredient, acetyl salicylic acid (ASA), was intercalated into ZnAl layered double hydroxide (LDH). The LDH–ASA nanohybrid material was characterized by XRD, FTIR, SEM, ICP-MS, TEM and TGA. Successful...

  5. Inorganic layered double hydroxides as a 4-hexyl resorcinol delivery system for topical applications

    CSIR Research Space (South Africa)

    Mosangi, Damodar

    2016-08-01

    Full Text Available In this study, the hydrophobic even skin tone active, 4-hexylresorcinol (HR), was intercalated into a zinc aluminium layered double hydroxide (ZnAl-LDH) by a co-precipitation method and used as a controlled release ingredient in skin care...

  6. molecules in a functionalized layered double hydroxide

    Indian Academy of Sciences (India)

    Unknown

    included within the functionalized Mg–Al layered double hydroxide solid are similar to that of dilute so- lutions of the PAH in non-polar ... thermally stable over a wide temperature range with their emission properties practically unaltered. Keywords. Layered double ..... deformation, C–C skeletal stretch. 1020. 1024. 1024. –.

  7. Development of controlled drug release formulation based on pamoate-zinc-aluminium-layered double hydroxide nano composite

    International Nuclear Information System (INIS)

    Zaemah Jubri

    2008-01-01

    Controlled drug release formulation of pamoate was developed by the intercalation of pamoate anion into Zn-Al-layered double hydroxide (LDH). The resulting layered organic-inorganic hybrid nano composite material was formed using pamoate as guest anion intercalated into the Zn-Al layered double hydroxide inorganic host by direct co-precipitation method. As a result of successful intercalation of pamoate ion into the interlayer structure of Zn-Al-LDH, an expansion of the interlayer spacing, from 8.9 Angstrom in the layered double hydroxide to 18.1 Angstrom in the nano composite (ZAP) could be observed in the powder X-ray diffractogram. The reverse process, for example the de intercalation or release of the guest, pamoate was found to be rapid initially, followed by a more sustained release thereafter and this behavior was dependent on the pH of the release medium, the aqueous solution. The mechanism of release has been interpreted on the basis of the ion-exchange process between the pamoate anion intercalated in the lamella host and nitrate, or hydroxyl anions in the aqueous solution. This study suggest that layered double hydroxide can be used as a carrier for drugs that allow safe and controlled delivery of various bio agents into target with high efficiency. (author)

  8. Synthesis and structure refinement of layered double hydroxides of ...

    Indian Academy of Sciences (India)

    Administrator

    )-oxygen bond in this compound as opposed to the Co–Ga hydroxide. These observations are supported by IR spectra. Keywords. Layered double hydroxide; Rietveld refinement; urea hydrolysis. 1. Introduction. The synthesis, structure and properties of layered double hydroxides (LDHs) have been widely studied in recent.

  9. Intercalation of 2 - Naphtol - 3,6 - disulfonate, 9,10 - Anthraquinone - 2,6 - disulfonate, and 9,10 - Anthraquinone - 2 - sulfonate Anions into Zn - Al Layered Double Hydroxide

    Czech Academy of Sciences Publication Activity Database

    Beneš, L.; Zima, Vítězslav; Svoboda, Jan; Melánová, Klára

    2005-01-01

    Roč. 53, č. 1-2 (2005), s. 41-46 ISSN 0923-0750 R&D Projects: GA ČR(CZ) GA203/05/2306 Institutional research plan: CEZ:AV0Z40500505 Keywords : intercalate Subject RIV: CA - Inorganic Chemistry Impact factor: 1.020, year: 2005

  10. Benzoate Anion-Intercalated Layered Cobalt Hydroxide Nanoarray: An Efficient Electrocatalyst for the Oxygen Evolution Reaction.

    Science.gov (United States)

    Ge, Ruixiang; Ren, Xiang; Ji, Xuqiang; Liu, Zhiang; Du, Gu; Asiri, Abdullah M; Sun, Xuping; Chen, Liang

    2017-10-23

    Efficient oxygen evolution reaction (OER) catalysts are highly desired to improve the overall efficiency of electrochemical water splitting. We develop a benzoate anion-intercalated layered cobalt hydroxide nanobelt array on nickel foam (benzoate-Co(OH) 2 /NF) through a one-pot hydrothermal process. As a 3 D electrode, benzoate-Co(OH) 2 /NF with an expanded interlayer spacing (14.72 Å) drives a high OER catalytic current density of 50 mA cm -2 at an overpotential of 291 mV, outperforming its carbonate anion-intercalated counterpart with a lower interlayer spacing of 8.81 Å (337 mV overpotential at 50 mA cm -2 ). Moreover, this benzoate-Co(OH) 2 /NF can maintain its catalytic activity for 21 h. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Rare earth and zinc layered hydroxide salts intercalated with the 2-aminobenzoate anion as organic luminescent sensitizer

    Energy Technology Data Exchange (ETDEWEB)

    Cursino, Ana Cristina Trindade, E-mail: anacursino@ufpr.br [CEPESQ – Research Centre of Applied Chemistry, Department of Chemistry, Universidade Federal do Paraná – P.O. Box 19081, 81531-980 Curitiba, PR (Brazil); Rives, Vicente, E-mail: vrives@usal.es [GIR-QUESCAT – Department of Inorganic Chemistry, Universidad de Salamanca, Plaza de la Merced S/N, 37998 Salamanca (Spain); Arizaga, Gregorio Guadalupe Carbajal, E-mail: gregoriocarbajal@yahoo.com.mx [Universidad de Guadalajara, Department of Chemistry, Boulevard Marcelino García Barragán 1421, C.P. 44430 Guadalajara, Jalisco (Mexico); Trujillano, Raquel, E-mail: rakel@usal.es [GIR-QUESCAT – Department of Inorganic Chemistry, Universidad de Salamanca, Plaza de la Merced S/N, 37998 Salamanca (Spain); Wypych, Fernando, E-mail: wypych@ufpr.br [CEPESQ – Research Centre of Applied Chemistry, Department of Chemistry, Universidade Federal do Paraná – P.O. Box 19081, 81531-980 Curitiba, PR (Brazil)

    2015-10-15

    Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide salts intercalated with nitrate anions were synthesized, followed by exchange with 2-aminobenzoate. The UV absorption ability was improved after intercalation/grafting in relation to that shown by the parent material. - Highlights: • Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide were synthesized. • Intercalated nitrate anions were exchanged by 2-aminobenzoate. • In all the 2-aminobenzoate containing compounds, the grafting reaction was detected. • The UV absorption ability was improved after the exchange reactions. • Rare earth hydroxide salts are potential matrixes to produce luminescent materials. - Abstract: Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide salts intercalated with nitrate anions were synthesized, followed by exchange with 2-aminobenzoate. The obtained compounds were characterized by powder X-ray diffraction (PXRD), Fourier transform infrared (FTIR) and ultraviolet visible (UV–vis) spectroscopies, fluorescence measurements and thermal analysis (TGA/DTA). The results from FTIR spectroscopy suggest a direct coordination of 2-aminobenzoate to the metal cations of the inorganic layered structure. The organic derivative products from the intercalation reactions absorb a broader range of UV-light in relation to that shown by the parent material; the photoluminescence measurements present a strong violet, blue and green luminescence under UV-light excitation for layered compounds with, Zn, Y and Tb, respectively. Rare earth hydroxide salts (RE-LHS) are potential alternative matrices for the immobilization of organic species to produce luminescent materials.

  12. Rare earth and zinc layered hydroxide salts intercalated with the 2-aminobenzoate anion as organic luminescent sensitizer

    International Nuclear Information System (INIS)

    Cursino, Ana Cristina Trindade; Rives, Vicente; Arizaga, Gregorio Guadalupe Carbajal; Trujillano, Raquel; Wypych, Fernando

    2015-01-01

    Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide salts intercalated with nitrate anions were synthesized, followed by exchange with 2-aminobenzoate. The UV absorption ability was improved after intercalation/grafting in relation to that shown by the parent material. - Highlights: • Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide were synthesized. • Intercalated nitrate anions were exchanged by 2-aminobenzoate. • In all the 2-aminobenzoate containing compounds, the grafting reaction was detected. • The UV absorption ability was improved after the exchange reactions. • Rare earth hydroxide salts are potential matrixes to produce luminescent materials. - Abstract: Rare earth (RE = Eu, Y and Tb) and zinc layered hydroxide salts intercalated with nitrate anions were synthesized, followed by exchange with 2-aminobenzoate. The obtained compounds were characterized by powder X-ray diffraction (PXRD), Fourier transform infrared (FTIR) and ultraviolet visible (UV–vis) spectroscopies, fluorescence measurements and thermal analysis (TGA/DTA). The results from FTIR spectroscopy suggest a direct coordination of 2-aminobenzoate to the metal cations of the inorganic layered structure. The organic derivative products from the intercalation reactions absorb a broader range of UV-light in relation to that shown by the parent material; the photoluminescence measurements present a strong violet, blue and green luminescence under UV-light excitation for layered compounds with, Zn, Y and Tb, respectively. Rare earth hydroxide salts (RE-LHS) are potential alternative matrices for the immobilization of organic species to produce luminescent materials

  13. Effect of adsorbed/intercalated anionic dyes into the mechanical properties of PVA: layered zinc hydroxide nitrate nanocomposites.

    Science.gov (United States)

    Marangoni, Rafael; Mikowski, Alexandre; Wypych, Fernando

    2010-11-15

    Zinc hydroxide nitrate (ZHN) was adsorbed with anions of blue dyes (Chicago sky blue, CSB; Evans blue, EB; and Niagara blue, NB) and intercalated with anions of orange dyes (Orange G, OG; Orange II, OII; methyl orange, MO). Transparent, homogeneous and colored nanocomposite films were obtained by casting after dispersing the pigments (dye-intercalated/adsorbed into LHSs) into commercial poly(vinyl alcohol) (PVA). The films were characterized by XRD, UV-Vis spectroscopy, and mechanical testing. The mechanical properties of the PVA compounded with the dye-intercalated/adsorbed ZHN were evaluated, and reasonable increases in Young's modulus and ultimate tensile strength were observed, depending on the amount and choice of layered filler. These results demonstrate the possibility of using a new class of layered hydroxide salts intercalated and adsorbed with anionic dyes to prepare multifunctional polymer nanocomposite materials. Copyright © 2010 Elsevier Inc. All rights reserved.

  14. Controlled release formulation of an anti-depression drug based on a L-phenylalanate-zinc layered hydroxide intercalation compound

    Science.gov (United States)

    Hashim, Norhayati; Sharif, Sharifah Norain Mohd; Isa, Illyas Md; Hamid, Shahidah Abdul; Hussein, Mohd Zobir; Bakar, Suriani Abu; Mamat, Mazidah

    2017-06-01

    The intercalation of L-phenylalanate (LP) into the interlayer gallery of zinc layered hydroxide (ZLH) has been successfully executed using a simple direct reaction method. The synthesised intercalation compound, zinc layered hydroxide-L-phenylalanate (ZLH-LP), was characterised using PXRD, FTIR, CHNS, ICP-OES, TGA/DTG, FESEM and TEM. The PXRD patterns of the intercalation compound demonstrate an intense and symmetrical peak, indicating a well-ordered crystalline layered structure. The appearance of an intercalation peak at a low angle of 2θ with a basal spacing of 16.3 Å, signifies the successful intercalation of the L-phenylalanate anion into the interlayer gallery of the host. The intercalation is also validated by FTIR spectroscopy and CHNS elemental analysis. Thermogravimetric analysis confirms that the ZLH-LP intercalation compound has higher thermal stability than the pristine L-phenylalanine. The observed percentage of L-phenylalanate accumulated release varies in each release media, with 84.5%, 79.8%, 63.8% and 61.8% release in phosphate buffer saline (PBS) solution at pH 4.8, deionised water, PBS solution at pH 7.4 and NaCl solution, respectively. The release behaviour of LP from its intercalation compounds in deionised water and PBS solution at pH 4.8 follows pseudo second order, whereas in NaCl solution and PBS solution at pH 7.4, it follows the parabolic diffusion model. This study shows that the synthesised ZLH-LP intercalation compound can be used for the formation of a new generation of materials for targeted drug release with controlled release properties.

  15. Synthesis and properties of Mg2Al layered double hydroxides containing 5-fluorouracil

    International Nuclear Information System (INIS)

    Wang Zhongliang; Wang Enbo; Gao Lei; Xu Lin

    2005-01-01

    A pharmaceutically active compound, 5-fluorouracil (5-FU) has been firstly intercalated into layered double hydroxide with the restructure method. Powder X-ray diffraction and spectroscopic analysis indicate that 5-FU molecule is stabilized in the host interlayer by electrostatic interaction and intermolecular interaction, and that the orientation of 5-FU is different when changing the pattern of aging treatment or the swelling agent. The release studies show that a rapid release of the drug during the first 40min is followed by a more sustained one, and that the total amount of drug released from hybrid material into the aqueous solution is almost 87% and 74% at pH 4 and 7, respectively. The studies mentioned above suggest that layered double hydroxide might be used as the basis of a tunable drug delivery carrier

  16. Polymethyl methacrylate and polystyrene with layered double hydroxide nano composites: In situ synthesis, morphology and thermal properties

    International Nuclear Information System (INIS)

    Botan, Rodrigo; Nogueira, Telma R.; Lona, Liliane M.F.; Wypych, Fernando

    2011-01-01

    Over the past decade, polymer nanocomposites have attracted interest, both in industry and in academia, because they often exhibit remarkable improvement in their properties when compared with pure polymer or conventional micro and macro-composites using low levels of reinforcements. In this work polymethyl methacrylate and polystyrene reinforced with layered double hydroxide, which was intercalated with sodium dodecyl sulfate were synthesized by in situ bulk polymerization. The nanocomposites were characterized and compared by X-ray diffraction, thermogravimetric analysis and flammability test. The X-ray diffraction demonstrated that synthesized nanocomposites showed a high global dispersion of layered double hydroxide, suggesting exfoliated morphology. The result of thermogravimetric analysis and flammability test for synthesized polystyrene/ layered double hydroxide nanocomposite presented a significant improvement in thermal stability and flammability property when compared with pure polymer. (author)

  17. Synthesis and characterization of 10-hydroxycamptothecin - sebacate - layered double hydroxide nanocomposites

    Science.gov (United States)

    Pang, Xiujiang; Ma, Xiuming; Li, Dongxiang; Hou, Wanguo

    2013-02-01

    10-Hydroxycamptothecin (HCPT) as a hydrophobic anticancer drug brings many challenges in the clinical applications due to its poor water solubility and the presence of a chemically unstable lactone ring. In this work, the nanocomposites of HCPT intercalated layered double hydroxide (LDH) were prepared by a secondary intercalation method, and the encapsulated HCPT could keep the biologically active lactone form. A Zn-Al-NO3 LDH was pillared with sebacate anions by a co-precipitation method in an aqueous medium, and then HCPT was intercalated into the LDH's gallery via hydrophobic interaction in an ethanol medium. The parallel alkyl chains of perpendicularly arranged sebacate anions in the LDH gallery provide a hydrophobic space for the drug intercalation. The in vitro release kinetics of HCPT from the nanocomposites could be fitted with the pseudo-second-order kinetic model, and the diffusion of HCPT through the LDH particles played an important role in controlling the drug release. The nanocomposites can be considered as a potential drug delivery system.

  18. Electronic spectra of anions intercalated in layered double hydroxides

    Indian Academy of Sciences (India)

    Frost R L, Musumeci A W, Bouzaid J, Adebajo M O, Martens W N and Kloprogge J T 2005 J. Solid State Chem. 178 1940. Giannelis E P, Nocera D G and Pinnavaia T J 1987 Inorg. Chem. 26 203. Gray H B and Beach N A 1963 J. Am. Chem. Soc. 85 2922. Hansen H C B and Koch C B 1994 Clays Clay Miner. 42 170.

  19. NO and SCN -intercalated layered double hydroxides: structure and ...

    Indian Academy of Sciences (India)

    2018-02-05

    Feb 5, 2018 ... C (18 h). 2.2 Materials characterization. The samples were characterized by powder X-ray diffraction. (PXRD) with a Bruker D8 Advance powder diffractometer. (source CuKα radiation, Ni filter, λ = 1.5418 Å) operating in reflection geometry. For structure refinement, data were col- lected at a scan rate of 0.12.

  20. Synthesis and release behavior of composites of camptothecin and layered double hydroxide

    International Nuclear Information System (INIS)

    Dong Lun; Yan Li; Hou Wanguo; Liu Shaojie

    2010-01-01

    A simple method, reconstruction of calcinated layered double hydroxides (CLDH) in an organic (ethanol)-water mixed solvent medium containing drug, was developed to intercalate partially a non-ionic and poorly water-soluble drug (camptothecin) into the gallery of layered double hydroxides (LDHs) to form the drug-LDH composites. The purpose of choosing organic-water mixed solvent is to increase remarkably the solubility of camptothecin (CPT) in the reconstruction medium. A probable morphology of CPT molecules in the gallery of LDHs is that CPT molecules arrange as monolayer with the long axis parallel to the LDH layers. The in vitro drug release from the composites was remarkably lower than that from the corresponding physical mixture, which shows these drug-inorganic composites can be used as a potential drug delivery system. - Graphical abstract: A simple method, reconstruction of calcinated LDHs in an organic-water medium containing drug, was developed to intercalate non-ionic and poorly water-soluble camptothecin into the gallery of LDHs.

  1. Development of polymer nanocomposites based on layered double hydroxides

    Directory of Open Access Journals (Sweden)

    Sipusic, J.

    2009-05-01

    Full Text Available Polymeric nanocomposites are commonly considered as systems composed of a polymeric matrix and - usually inorganic - filler. The types of nanofillers are indicated in Fig. 1. Beside wellknown layered silicate fillers, recent attention is attracted to layered double hydroxide fillers (LDH, mainly of synthetic origin. The structure of LDH is based on brucite, or magnesium hydroxide, Mg(OH2 and is illustrated in Fig. 2. The modification of LDHs is commonly done by organic anions, to increase the original interlayer distance and to improve the organophilicity of the filler, keeping in mind their final application as fillers for, usually hydrophobic, polymer matrices. We have used the modified rehydration procedure for preparing organically modified LDH. The stoichiometric quantities of Ca33Al2O6, CaO and benzoic (B (or undecenoic (U acid were mixed with water and some acetone. After long and vigorous shaking, the precipitated fillers were washed, dried and characterized. X-ray diffraction method (XRD has shown the increase of the original interlayer distance for unmodified LDH (OH–-saturated of 0.76 nm to the 1.6 nm in LDH-B or LDH-U fillers (Fig. 3. Infrared spectroscopy method (FTIR has confirmed the incorporation of benzoic anion within the filler layers (Fig. 4. For the preparation of LDH-B and LDH-U composites with polystyrene (PS, poly(methyl methacrylate (PMMA and copolymer (SMMA matrices, a two-step in situ bulk radical polymerization was selected (Table 1 for recipes, azobisisobutyronitrile as initiator, using conventional stirred tank reactor in the first step, and heated mold with the movable wall (Fig. 6 in the second step of polymerization. All the prepared composites with LDH-U fillers were macroscopically phase-separated, as was the PMMA/LDH-B composite.PS/LDH-B and SMMA/LDH-B samples were found to be transparent and were further examined for deduction of their structure (Fig. 5 and thermal properties. FTIR measurements showed that

  2. Organo-layered double hydroxides composite thin films deposited by laser techniques

    Science.gov (United States)

    Birjega, R.; Vlad, A.; Matei, A.; Dumitru, M.; Stokker-Cheregi, F.; Dinescu, M.; Zavoianu, R.; Raditoiu, V.; Corobea, M. C.

    2016-06-01

    We used laser techniques to create hydrophobic thin films of layered double hydroxides (LDHs) and organo-modified LDHs. A LDH based on Zn-Al with Zn2+/Al3+ ratio of 2.5 was used as host material, while dodecyl sulfate (DS), which is an organic surfactant, acted as guest material. Pulsed laser deposition (PLD) and matrix assisted pulsed laser evaporation (MAPLE) were employed for the growth of the films. The organic anions were intercalated in co-precipitation step. The powders were subsequently used either as materials for MAPLE, or they were pressed and used as targets for PLD. The surface topography of the thin films was investigated by atomic force microscopy (AFM), the crystallographic structure of the powders and films was checked by X-ray diffraction. FTIR spectroscopy was used to evidence DS interlayer intercalation, both for powders and the derived films. Contact angle measurements were performed in order to establish the wettability properties of the as-prepared thin films, in view of functionalization applications as hydrophobic surfaces, owing to the effect of DS intercalation.

  3. Oxidative leaching of chromium from layered double hydroxides ...

    Indian Academy of Sciences (India)

    Unknown

    Abstract. The layered double hydroxide (LDH) of Zn with Cr on treatment with a hypochlorite solution releases chromate ions as a result of oxidative leaching by a dissolution–reprecipitation mechanism. The resi- due is found to be ε-Zn(OH)2. The LDH of Mg with Cr on the other hand is resistant to oxidative leaching. In.

  4. Oxidative leaching of chromium from layered double hydroxides ...

    Indian Academy of Sciences (India)

    The layered double hydroxide (LDH) of Zn with Cr on treatment with a hypochlorite solution releases chromate ions as a result of oxidative leaching by a dissolution–reprecipitation mechanism. The residue is found to be -Zn(OH)2. The LDH of Mg with Cr on the other hand is resistant to oxidative leaching. In contrast, a ...

  5. Interaction of pristine hydrotalcite-like layered double hydroxides ...

    Indian Academy of Sciences (India)

    Metal oxides in general have surface acidic sites, but for exceptional circumstances, are not expected to mineralize CO2. Given their intrinsic basicity and an expandable interlayer gallery, the hydrotalcite-like layered double hydroxides (LDHs) are expected to be superior candidate materials for CO2 mineralization.

  6. Interaction of pristine hydrotalcite-like layered double hydroxides ...

    Indian Academy of Sciences (India)

    -like layered double hydroxides (LDHs) are expected to be superior candidate materials for CO2 mineralization. However, the ... of the [Mg–Al–CO3] LDH is only marginally delayed in flowing CO2 in comparison with flowing N2, showing only.

  7. Synthesis of protocatechuic acid–zinc/aluminium–layered double hydroxide nanocomposite as an anticancer nanodelivery system

    Energy Technology Data Exchange (ETDEWEB)

    Barahuie, Farahnaz [Materials Synthesis and Characterisation Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Hussein, Mohd Zobir, E-mail: mzobir@upm.edu.my [Materials Synthesis and Characterisation Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Gani, Shafinaz Abd [Department of Biochemistry, Faculty of Biotechnology and Biomolecular Sciences, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Fakurazi, Sharida [Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Department of Human Anatomy, Faculty of Medicine and Health Sciences, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia); Zainal, Zulkarnain [Materials Synthesis and Characterisation Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor (Malaysia)

    2015-01-15

    Protocatechuic acid, an active anticancer agent, has been intercalated into Zn/Al–layered double hydroxide at Zn/Al=2) using two different preparation methods, co-precipitation and ion-exchange, which are labelled as PZAE and PZAC, respectively. The release of protocatechuate from the nanocomposites occurred in a controlled manner and was fitted satisfactorily to pseudo-second order kinetics. The basal spacing of the resulting nanocomposites PZAE and PZAC was 10.2 and 11.0 Å, respectively, indicating successful intercalation of protocatechuate anions into the interlayer galleries of Zn/Al–NO{sub 3}–LDH in a monolayer arrangement with angles of 24 and 33° from the z-axis in PZAE and PZAC, respectively. The formation of nanocomposites was further confirmed by a Fourier transform infrared study. Thermogravimetric and differential thermogravimetric analyses indicated that the thermal stability of the intercalated protocatechuic acid was significantly enhanced compared to its free protocatechuic acid, and the drug content in the nanocomposites was estimated to be approximately 32.6% in PZAE and 29.2% in PZAC. Both PZAE and PZAC nanocomposites inhibit the growth of human cervical, liver and colorectal cancer cell lines and exhibit no toxic effects towards normal fibroblast 3T3 cell after 72 h of treatment. - Graphical abstract: Protocatechuate anions were arranged in monolayer mode with the angle of 24° for PZAE and 33° for PZAC from Z axis to maximize interaction between carboxylate groups and brucite-like layers. - Highlights: • Two methods gave nanocomposites with slightly different physico-chemical properties. • PZAE and PZAC have the potential to be used as a controlled release formulation. • The thermal stability of PA is markedly enhanced upon the intercalation process. • Higher cancer cell growth inhibition for PZAE and PZAC nanocomposites than for PA.

  8. Synthesis and Controlled Release Property of Levodopa from Its Zn-Al-Layered Double Hydroxide Nano hybrid

    International Nuclear Information System (INIS)

    Mohd Zobir Hussein; Sariwani Abdul Ghani; Mohd Zobir Hussein; Abdul Halim Abdullah

    2011-01-01

    A new inorganic-based drug delivery system, levodopa-layered double hydroxide nano hybrid compound was synthesized for a controlled release formulation through co-precipitation method. The nano hybrid was synthesized using a layered double hydroxide material of Zn-Al layered double hydroxide type as a host in which nitrate anions present in the host galleries were ion-exchanged with levodopa anion. The results from PXRD, FTIR and thermal analysis (TG/DTA) indicated the presence of the levodopa anion that has been successfully intercalated into the layered double hydroxide for the formation of nano hybrid. The release of the active agent, levodopa from the interlayer of the nano hybrid was found to be of controlled manner governed by the pseudo-second order kinetic. It was found that the release of levodopa in phosphate buffer solution medium is of controlled manner while chloride speeds up the release rate of levodopa. The material has good potential as a new generation of drug with slow release capability which can be used for drug delivery system. (author)

  9. Recent advances in polymer supporting layered double hydroxides nanocomposite for electrochemical biosensors

    Science.gov (United States)

    Dhanasekaran, T.; Padmanaban, A.; Gnanamoorthy, G.; Manigandan, R.; Praveen Kumar, S.; Stephen, A.; Narayanan, V.

    2018-01-01

    In recent years, layered double hydroxides (LDHs) materials having emerging due to their ability of intercalate a variety of anions, either organic or inorganic molecules. The most significance of the LDHs has been found potential applications in catalysis, wastewater treatment, and electrochemical sensors. The Mg-Al LDHs (MAL) and Poly-o-phenylenediamine @ Mg-Al LDHs (P-MAL) was prepared via simple one step hydrothermal method. As prepared material was characterized using many techniques such as, the structural and crystal phase was determined from XRD and Raman analyses. The functional groups were depicted using FT-IR spectroscopy. The optical propertied studied using diffuse reflectance spectroscopy UV-vis spectroscopy and the emission property were analyzed from Photoluminescence spectroscopy. The surface morphology and average particle size was analyzed using FESEM microscopy. The prepared polymer composite material P-MAL was further used for highly sensitive electrochemical detection towards dopamine (DA).

  10. Anion capture with calcium, aluminium and iron containing layered double hydroxides

    Science.gov (United States)

    Phillips, J. D.; Vandeperre, L. J.

    2011-09-01

    The competitive adsorption of nitrate, chloride and carbonate in layered double hydroxides (LHD) with the general formula Ca(1-x)2+Al(1-y)3+,Fe(y)3+x(OH)2xNO3-·nHO was investigated. Both normal ion exchange by exposure to a solution containing different anions, as well as addition of calcined material to solution thereby exploiting the memory effect of LDHs was studied. Changes in the interlayer anion changed the interlayer spacing of the LDH. The order of preference of intercalation was Cl≈CO32->NO3-. When multiple anions were present in the exchange solution, LDHs with several distinct interlayer spacing were produced indicating that LDHs with different anions in the interlayer existed at the same time. However for extended exchange times (14 days) where high concentrations of carbonate anion were present, the layered structure was destroyed resulting in the formation of calcite, CaCO 3.

  11. Defluoridation of groundwater by calcined Mg/Al layered double hydroxide

    Directory of Open Access Journals (Sweden)

    A. Elhalil

    2016-03-01

    Full Text Available The present study evaluated calcined Mg/Al layered double hydroxide (CLDH availability for the removal of fluoride from local groundwaters. The Mg/Al layered double hydroxide (LDH was synthesized by co-precipitation method and characterized by XRD, FT-IR and TGA-TDA analyses. Batch defluoridation experiments were performed under various conditions such as calcination, solution pH, contact time, temperature, material dosage and reuse. Experimental results indicate that fluoride removal strongly increased after calcination of the LDH up to 600 °C. The maximum fluoride removal was obtained at solution pH of 6.85. Kinetics of fluoride removal followed the pseudo-second order kinetic model. The rise in solution temperature strongly enhances the removal efficiency. The adsorption mechanism involved surface adsorption, ion exchange interaction and original LDH structure reconstruction by rehydration of mixed metal oxides and concomitant intercalation of fluoride ions into the interlayer region. The optimum dosages required to meet the national standard for drinking water quality were found to be 0.29 and 0.8 g/L, respectively, for Bejaad and Settat goundwaters. A decrease in the fluoride uptake with increasing the number of regeneration cycles was observed.

  12. Accessing the biocompatibility of layered double hydroxide by intramuscular implantation: histological and microcirculation evaluation.

    Science.gov (United States)

    Cunha, Vanessa Roberta Rodrigues; de Souza, Rodrigo Barbosa; da Fonseca Martins, Ana Maria Cristina Rebello Pinto; Koh, Ivan Hong Jun; Constantino, Vera Regina Leopoldo

    2016-08-02

    Biocompatibility of layered double hydroxides (LDHs), also known as hydrotalcite-like materials or double metal hydroxides, was investigated by in vivo assays via intramuscular tablets implantation in rat abdominal wall. The tablets were composed by chloride ions intercalated into LDH of magnesium/aluminum (Mg2Al-Cl) and zinc/aluminum (Zn2Al-Cl). The antigenicity and tissue integration capacity of LDHs were assessed histologically after 7 and 28 days post-implantation. No fibrous capsule nearby the LDH was noticed for both materials as well any sign of inflammatory reactions. Sidestream Dark Field imaging, used to monitor in real time the microcirculation in tissues, revealed overall integrity of the microcirculatory network neighboring the tablets, with no blood flow obstruction, bleeding and/or increasing of leukocyte endothelial adhesion. After 28 days Mg2Al-Cl promoted multiple collagen invaginations (mostly collagen type-I) among its fragments while Zn2Al-Cl induced predominantly collagen type-III. This work supports previous results in the literature about LDHs compatibility with living matter, endorsing them as functional materials for biomedical applications.

  13. The role of oleate-functionalized layered double hydroxide in the melt compounding of polypropylene nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Donato, Ricardo K., E-mail: ricardokeitel@iq.ufrgs.br [Laboratory of Technological Processes and Catalysis, Institute of Chemistry, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970, Porto Alegre, RS (Brazil); Luza, Leandro, E-mail: leandro.luza@ufrgs.br [Laboratory of Technological Processes and Catalysis, Institute of Chemistry, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970, Porto Alegre, RS (Brazil); Silva, Renato F. da, E-mail: renato.figueira@ufrgs.br [Laboratory of Technological Processes and Catalysis, Institute of Chemistry, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970, Porto Alegre, RS (Brazil); Moro, Celso C., E-mail: celso@iq.ufrgs.br [Institute of Chemistry, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970, Porto Alegre, RS (Brazil); Guzatto, Rafael, E-mail: guzatto@gmail.com [Laboratory of Instrumentation and Molecular Dynamics, Institute of Chemistry, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970, Porto Alegre, RS (Brazil); Samios, Dimitrios, E-mail: dsamios@iq.ufrgs.br [Laboratory of Instrumentation and Molecular Dynamics, Institute of Chemistry, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970, Porto Alegre, RS (Brazil); Matejka, Libor, E-mail: matejka@imc.cas.cz [Institute of Macromolecular Chemistry, Academy of Sciences of the Czech Republic, Heyrovsky Sq. 2, Prague 6, 162 06 (Czech Republic); Dimzoski, Bojan, E-mail: dimzoski@imc.cas.cz [Institute of Macromolecular Chemistry, Academy of Sciences of the Czech Republic, Heyrovsky Sq. 2, Prague 6, 162 06 (Czech Republic); and others

    2012-12-01

    In this research, the oleate-functionalized magnesium and aluminum layered double hydroxide (LDH; Mg:Al = 3:1) o-LDH was applied as nanofiller in the melt blending of polypropylene (PP) nanocomposites, in order to understand its role in this process. o-LDH was prepared using the memory effect of the calcined carbonated LDH. Blending of PP and low o-LDH filler contents of 0.45 and 0.90 wt.% afforded the nanocomposites PP0.45 and PP0.90, respectively, which were characterized by transmission electron microscopy, X-ray diffraction, small angle X-ray scattering, thermo-gravimetric analysis, differential scanning calorimetry and dynamic mechanical analysis. The oleate LDH surface functionalization enhanced the system compatibility as a relative regular dispersion of o-LDH tactoids was observed within the matrix, together with partial PP intercalation. This o-LDH incorporation increased the PP relative crystallinity, induced crystalline orientation and decreased the glass transition temperature. Furthermore, the nanocomposites showed improved initial resistance to decomposition and stiffness. These results showed that the o-LDH acted as both nucleating agent and plasticizer, and that the presented approach can be used for the development of PP nanocomposites with distinguished properties. Highlights: Black-Right-Pointing-Pointer Nanofiller induced orientation of the crystalline polypropylene phase. Black-Right-Pointing-Pointer Renewable feedstock as compatibilizer in the preparation of nanocomposites Black-Right-Pointing-Pointer Layered double hydroxide as nucleating agent and plasticizer.

  14. Kinetics and mechanism of ionic intercalation/de-intercalation during the formation of α-cobalt hydroxide and its polymorphic transition to β-cobalt hydroxide: Reaction-diffusion framework

    KAUST Repository

    Rahbani, Janane

    2012-01-01

    We study the kinetics and mechanism of intercalation and de-intercalation of small anions during the formation of crystalline α-Co(OH) 2 and its transformation to β-Co(OH) 2 within a reaction-diffusion framework. We therein use fluorescence spectroscopy with Rhodamine 6G (Rh6G) as a probe as well as other spectroscopic and imaging techniques. The method is based on the reaction and diffusion of hydroxide ions into a gel matrix containing the Co(ii) ions, the conjugate anions to be intercalated and Rh6G. The advantage of this simple method is that it allows us to separate throughout space the various stages during the formation of α-Co(OH) 2 and its transformation to β-Co(OH) 2, thus enabling fluorescence measurements of the those stages by simply focusing on different areas of the tube. It also permits us to extract with ease the solids for characterization and image analysis. The macroscopic evolution of the system, which consists of a leading blue front designating the formation of α-Co(OH) 2 followed by a sharp blue/pink interface designating the transformation to the pink β-Co(OH) 2, exhibits different dynamics depending on the anion present in the gel. At a certain stage, the blue/pink interface stops its propagation and only the blue front continues. This represents clear evidence of the dependence of the kinetics of intercalation and de-intercalation on the nature of the anion. The coexisting polymorphs were collected and characterized using XRD, FTIR, Raman and UV-Vis. The fluorescence images of the α-Co(OH) 2 reveal clearly the presence of Rh6G between its layers, whereas images from the β polymorph indicate the opposite. Moreover, the fluorescence of Rh6G is monitored during the formation of α-Co(OH) 2 and its conversion to β-Co(OH) 2. During the formation, the fluorescence intensity and lifetime are significantly increased whereas the opposite happens during the transformation to the β phase. We are able to calculate the activation energies

  15. Synthesis, structure refinement and chromate sorption characteristics of an Al-rich bayerite-based layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Britto, Sylvia, E-mail: sylviabritto11@gmail.com; Kamath, P. Vishnu

    2014-07-01

    “Imbibition” of Zn{sup 2+} ions into the cation vacancies of bayerite–Al(OH){sub 3} and NO{sub 3}{sup −} ions into the interlayer gallery yields an Al-rich layered double hydroxide with Al/Zn ratio ∼3. NO{sub 3}{sup −} ions are intercalated with their molecular planes inclined at an angle to the plane of the metal hydroxide slab and bonded to it by hydrogen bonds. Rietveld refinement of the structure shows that the monoclinic symmetry of the precursor bayerite is preserved in the product, showing that the imbibition is topochemical in nature. The nitrate ion is labile and is quantitatively replaced by CrO{sub 4}{sup 2−} ions from solution. The uptake of CrO{sub 4}{sup 2−} ions follows a Langmuir adsorption isotherm, thus showing that the hydroxide is a candidate material for green chemistry applications for the removal of CrO{sub 4}{sup 2−} ions from waste water. Rietveld refinement of the structure of the hydroxide after CrO{sub 4}{sup 2−} inclusion reveals that the CrO{sub 4}{sup 2−} ion is intercalated with one of its 2-fold axes parallel to the b-crystallographic axis of the crystal, also the principal 2 axis of the monoclinic cell. - Graphical abstract: The structure of the [Zn–Al4-nitrate] LDH viewed along the a-axis. - Highlights: • Synthesis of Al-rich layered double hydroxide with Al/Zn ratio ∼3. • Rietveld refinement indicates that the imbibition of Zn into Al(OH){sub 3} is topochemical in nature. • The uptake of CrO{sub 4}{sup 2−} ions follows a Langmuir adsorption isotherm.

  16. Mesoporous mixed metal oxides derived from P123-templated Mg-Al layered double hydroxides

    International Nuclear Information System (INIS)

    Wang Jun; Zhou Jideng; Li Zhanshuang; He Yang; Lin Shuangshuang; Liu Qi; Zhang Milin; Jiang Zhaohua

    2010-01-01

    We report the preparation of mesoporous mixed metal oxides (MMOs) through a soft template method. Different amounts of P123 were used as structure directing agent to synthesize P123-templated Mg-Al layered double hydroxides (LDHs). After calcination of as-synthesized LDHs at 500 o C, the ordered mesopores were obtained by removal of P123. The mesoporous Mg-Al MMOs fabricated by using 2 wt% P123 exhibited a high specific surface area of 108.1 m 2 /g, and wide distribution of pore size (2-18 nm). An investigation of the 'memory effect' of the mesoporous MMOs revealed that they were successfully reconstructed to ibuprofen intercalated LDHs having different gallery heights, which indicated different intercalation capacities. Due to their mesoporosity these unique MMOs have particular potential as drug or catalyst carriers. - Graphical abstract: Ordered mesoporous Mg-Al MMOs can be obtained through the calcination of P123-templated Mg-Al-CO 3 LDHs. The pore diameter is 2.2 nm. At the presence of ibuprofen, the Mg-Al MMOs can recover to Mg-Al-IBU LDHs, based on its 'remember effect'. Display Omitted

  17. Electrospun fibers of layered double hydroxide/biopolymer nanocomposites as effective drug delivery systems

    International Nuclear Information System (INIS)

    Miao, Yue-E.; Zhu Hong; Chen Dan; Wang Ruiyu; Tjiu, Weng Weei; Liu Tianxi

    2012-01-01

    Ibuprofen intercalated layered double hydroxide (LDH-IBU)/polycaprolactone (PCL) and LDH-IBU/polylactide (PLA) nanocomposite fibers are electrospun based on a combination of LDH-IBU with two kinds of biopolymers (i.e. PCL and PLA), to act as effective drug delivery systems. Ibuprofen (IBU) is chosen as a model drug, which is intercalated in MgAl-LDH by coprecipitation. Poly(oxyethylene-b-oxypropylene-b-oxyethylene) (Pluronic) is also added into PLA-based fibers as hydrophilicity enhancer and release modulator. LDH-IBU nanoparticles are uniformly dispersed throughout the nanocomposite fibers, as evidenced by transmission electron microscopy (TEM) observations. In vitro drug release studies show that initial IBU liberation from LDH-IBU/PCL composite fibers is remarkably slower than that from IBU/PCL fibers due to the sustained release property of LDH-IBU and heterogeneous nucleation effect of LDH-IBU on PCL chain segments. Surprisingly, the initial IBU release from LDH-IBU/PLA and LDH-IBU/PLA/Pluronic composite fibers is faster than that from the corresponding IBU/PLA and IBU/PLA/Pluronic fibers. This effect can be attributed to the strong interaction between alkyl groups in IBU molecules and methyl substituent groups of PLA as well as the hydrophilicity of LDH-IBU, which lead to an easier diffusion of water with a faster release of IBU from LDH-IBU/PLA and LDH-IBU/PLA/Pluronic composite fibers. - Graphical abstract: Ibuprofen intercalated layered double hydroxide (LDH-IBU)/polycaprolactone (PCL) and LDH-IBU/polylactide (PLA) nanocomposite fibers are electrospun based on the combination of LDHs with two kinds of biopolymers (i.e. PCL and PLA). LDH-IBU nanoparticles are uniformly dispersed throughout all the electrospun nanocomposite fibers even at a high loading level of 5 wt%. By combining the tunable drug release property of LDHs and electrospinning technique, the new drug delivery system is anticipated for effective loading and sustained release of drugs

  18. Electrospun fibers of layered double hydroxide/biopolymer nanocomposites as effective drug delivery systems

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Yue-E.; Zhu Hong; Chen Dan; Wang Ruiyu [State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular Science, Fudan University, Shanghai 200433 (China); Tjiu, Weng Weei [Institute of Materials Research and Engineering, A-STAR (Agency for Science, Technology and Research), 3 Research Link, Singapore 117602 (Singapore); Liu Tianxi, E-mail: txliu@fudan.edu.cn [State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular Science, Fudan University, Shanghai 200433 (China)

    2012-06-15

    Ibuprofen intercalated layered double hydroxide (LDH-IBU)/polycaprolactone (PCL) and LDH-IBU/polylactide (PLA) nanocomposite fibers are electrospun based on a combination of LDH-IBU with two kinds of biopolymers (i.e. PCL and PLA), to act as effective drug delivery systems. Ibuprofen (IBU) is chosen as a model drug, which is intercalated in MgAl-LDH by coprecipitation. Poly(oxyethylene-b-oxypropylene-b-oxyethylene) (Pluronic) is also added into PLA-based fibers as hydrophilicity enhancer and release modulator. LDH-IBU nanoparticles are uniformly dispersed throughout the nanocomposite fibers, as evidenced by transmission electron microscopy (TEM) observations. In vitro drug release studies show that initial IBU liberation from LDH-IBU/PCL composite fibers is remarkably slower than that from IBU/PCL fibers due to the sustained release property of LDH-IBU and heterogeneous nucleation effect of LDH-IBU on PCL chain segments. Surprisingly, the initial IBU release from LDH-IBU/PLA and LDH-IBU/PLA/Pluronic composite fibers is faster than that from the corresponding IBU/PLA and IBU/PLA/Pluronic fibers. This effect can be attributed to the strong interaction between alkyl groups in IBU molecules and methyl substituent groups of PLA as well as the hydrophilicity of LDH-IBU, which lead to an easier diffusion of water with a faster release of IBU from LDH-IBU/PLA and LDH-IBU/PLA/Pluronic composite fibers. - Graphical abstract: Ibuprofen intercalated layered double hydroxide (LDH-IBU)/polycaprolactone (PCL) and LDH-IBU/polylactide (PLA) nanocomposite fibers are electrospun based on the combination of LDHs with two kinds of biopolymers (i.e. PCL and PLA). LDH-IBU nanoparticles are uniformly dispersed throughout all the electrospun nanocomposite fibers even at a high loading level of 5 wt%. By combining the tunable drug release property of LDHs and electrospinning technique, the new drug delivery system is anticipated for effective loading and sustained release of drugs

  19. MgAl- Layered Double Hydroxide Nanoparticles for controlled release of Salicylate.

    Science.gov (United States)

    Mondal, Soumini; Dasgupta, Sudip; Maji, Kanchan

    2016-11-01

    Layered double hydroxides (LDHs), have been known for many decades as catalyst and ceramic precursors, traps for anionic pollutants, and additives for polymers. Recently, their successful synthesis on the nanometer scale opened up a whole new field for their application in nanomedicine. Here we report the efficacy of Mg1-xAlx (NO3)x (OH)2 LDH nanoparticles as a carrier and for controlled release of one of the non-steroidal anti-inflammatory drugs (NSAID), sodium salicylate. Mg1-xAlx (NO3)x (OH)2.nH2O nanoparticles were synthesized using co-precipitation method from an aqueous solution of Mg(NO3)2.6H2O and Al(NO3)3.9H2O. Salicylate was intercalated in the interlayer space of Mg-Al LDH after suspending nanoparticles in 0.0025(M) HNO3 and 0.75 (M) NaNO3 solution and using anion exchange method under N2 atmosphere. The shift in the basal planes like (003) and (006) to lower 2θ value in the XRD plot of intercalated sample confirmed the increase in basal spacing in LDH because of intercalation of salicylate into the interlayer space of LDH. FTIR spectroscopy of SA-LDH nano hybrid revealed a red shift in the frequency band of carboxylate group in salicylate indicating an electrostatic interaction between cationic LDH sheet and anionic drug. Differential thermal analysis of LDH-SA nanohybrid indicated higher thermal stability of salicylate in the intercalated form into LDH as compared to its free state. DLS studies showed a particle size distribution between 30-60 nm for pristine LDH whereas salicylate intercalated LDH exhibited a particle size distribution between 40-80nm which is ideal for its efficacy as a superior carrier for drugs and biomolecules. The cumulative release kinetic of salicylate from MgAl-LDH-SA hybrids in phosphate buffer saline (PBS) at pH7.4 showed a sustained release of salicylate up to 72h that closely resembled first order release kinetics through a combination of drug diffusion and dissolution of LDH under physiological conditions. Also the

  20. Dual nutraceutical nanohybrids of folic acid and calcium containing layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Tae-Hyun; Oh, Jae-Min, E-mail: jaemin.oh@yonsei.ac.kr

    2016-01-15

    Dual nutraceutical nanohybrids consisting of organic nutrient, folic acid (FA), and mineral nutrient, calcium, were prepared based on layered double hydroxide (LDH) structure. Among various hybridization methods such as coprecipitation, ion exchange, solid phase reaction and exfoliation-reassembly, it was found that exfoliation-reassembly was the most effective in terms of intercalation of FA moiety between Ca-containing LDH layers. X-ray diffraction patterns and infrared spectra indicated that FA molecules were well stabilized in the interlayer space of LDHs through electrostatic interaction. From the atomic force and scanning electron microscopic studies, particle thickness of LDH was determined to be varied with tens, a few and again tens of nanometers in pristine, exfoliated and reassembled state, respectively, while preserving particle diameter. The result confirmed layer-by-layer hybrid structure of FA and LDHs was obtained by exfoliation-reassembly. Solid UV–vis spectra showed 2-dimensional molecular arrangement of FA moiety in hybrid, exhibiting slight red shift in n→π* and π→π* transition. The chemical formulae of FA intercalated Ca-containing LDH were determined to Ca{sub 1.30}Al(OH){sub 4.6}FA{sub 0.74}·3.33H{sub 2}O and Ca{sub 1.53}Fe(OH){sub 5.06}FA{sub 2.24}·9.94H{sub 2}O by inductively coupled plasma-atomic emission spectroscopy, high performance liquid chromatography and thermogravimetry, showing high nutraceutical content of FA and Ca. - Highlights: • We successfully intercalated FA molecules into Ca-containing LDHs. • Exfoliation-reassembly was proven to be the most effective. • The interaction between LDH and FA were studied by FT-IR and UV–vis spectra. • Thermal stability of FA were enhanced by electrostatic interaction with LDH layers.

  1. LAYERED DOUBLE HYDROXIDES: NANOMATERIALS FOR APPLICATIONS IN AGRICULTURE

    Directory of Open Access Journals (Sweden)

    Luíz Paulo Figueredo Benício

    2015-02-01

    Full Text Available The current research aims to introduce Layered Double Hydroxides (LDH as nanomaterials to be used in agriculture, with particular reference to its use as storage and slow release matrix of nutrients and agrochemicals for plant growing. Structural characteristics, main properties, synthesis methods and characterization of LDH were covered in this study. Moreover, some literature data have been reported to demonstrate their potential for storage and slow release of nitrate, phosphate, agrochemicals, besides as being used as adsorbent for the wastewater treatment. This research aims to expand, in near future, the investigation field on these materials, with application in agriculture, increasing the interface between chemistry and agronomy.

  2. Membrane interactions and antimicrobial effects of layered double hydroxide nanoparticles

    DEFF Research Database (Denmark)

    Malekkhaiat Häffner, S; Nyström, L; Nordström, R

    2017-01-01

    ) on layered double hydroxide (LDH) interactions with both bacteria-mimicking and mammalian-mimicking lipid membranes. LDH binding to bacteria-mimicking membranes, extraction of anionic lipids, as well as resulting membrane destabilization, was found to increase with decreasing particle size, also translating...... into size-dependent synergistic effects with the antimicrobial peptide LL-37. Due to strong interactions with anionic lipopolysaccharide and peptidoglycan layers, direct membrane disruption of both Gram-negative and Gram-positive bacteria is suppressed. However, LDH nanoparticles cause size-dependent charge...

  3. Inorganic-Organic Nanohybrid Materials of Layered Zinc Hydroxide Nitrate with Intercalated Salicylate: Preparation, Characterization and UV-Blocking Properties

    Science.gov (United States)

    Liu, Jiexiang; Zhang, Yongqing; Zhang, Xiaoguang

    2016-02-01

    Intercalation of salicylate (Sal) into layered zinc hydroxide nitrate (ZHN) nanohybrid materials was successfully synthesized by the coprecipitation method. The effect of pH, crystallization method, temperature and time of hydrothermal treatment on preparation was investigated in detail and compared. The products were confirmed by X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR), thermogravimetry and differential thermal analysis (TG-DTA), and scanning electron microscope (SEM). The results revealed that ZHN-Sal with pure phase and good crystallinity was obtained at pH = 6.0-6.5, 60∘C and 3h of temperature and time of hydrothermal treatment. The TG-DTA data indicated that the intercalated Sal had a high stability compared to the isolated. And the phases and compositions of the sample calcined at increasing temperatures were also identified by XRPD and FTIR techniques. Furthermore, ZHN-Sal exhibited an improved UV-blocking ability, showing it can be used as a potential alternative matrix for the UV blocker.

  4. Hydroxy double salts loaded with bioactive ions: Synthesis, intercalation mechanisms, and functional performance

    International Nuclear Information System (INIS)

    Kaassis, Abdessamad Y.A.; Xu, Si-Min; Guan, Shanyue; Evans, David G.; Wei, Min; Williams, Gareth R.

    2016-01-01

    The intercalation of the anions of diclofenac (Dic), naproxen (Nap), and valproic acid (Val) into three hydroxy double salts (HDSs) has been explored in this work. Experiments were performed with [Co 1.2 Zn 3.8 (OH) 8 ](NO 3 ) 2 ·2H 2 O (CoZn-NO 3 ), [Ni 2 Zn 3 (OH) 8 ](NO 3 ) 2 ·2H 2 O (NiZn-NO 3 ) and [Zn 5 (OH) 8 ](NO 3 ) 2 ·2H 2 O (Zn-NO 3 ). It proved possible to intercalate diclofenac and naproxen into all three HDSs. In contrast, Val could be intercalated into CoZn-NO 3 but when it was reacted with Zn-NO 3 the HDS structure was destroyed, and the product comprised ZnO. Successful intercalation was verified by X-ray diffraction, IR spectroscopy, and elemental microanalysis. Molecular dynamics simulations showed the Dic and Nap ions to arrange themselves in an “X” shape in the interlayer space, forming a bilayer. Val was found to adopt a position with its aliphatic groups parallel to the HDS layer, again in a bilayer. In situ time resolved X-ray diffraction experiments revealed that intercalation of Dic and Nap into CoZn-NO 3 and Zn-NO 3 is mechanistically complex, with a number of intermediate phases observed. In contrast, the intercalation of all three guests into NiZn-NO 3 and of Val into CoZn-NO 3 are simple one step reactions proceeding directly from the starting material to the product. The HDS-drug composites were found to have sustained release profiles. - Graphical abstract: Seven new drug intercalates of hydroxy double salts (HDSs) have been prepared and characterised. The intercalation mechanisms have been explored, and the drug release properties of the HDS/drug composites quantified. Display Omitted

  5. [Role of layered double hydroxide (LDH) in the protection of herring testis DNA from heavy metals].

    Science.gov (United States)

    Tang, Yi-Ni; Wu, Ping-Xiao; Zhu, Neng-Wu

    2012-10-01

    The role of layered double hydroxide (LDH) in the protection of herring testis DNA from heavy metals Cd2+ and Pb2+ was studied by X-ray diffraction ( XRD) spectra, Fourier transform infrared (FTIR) spectra, Scanning Electron Microscopy (SEM), Cyclic Voltammetry and Ultraviolet Spectrometry. Size expansion of the basal spacing (003) from 0. 76 nm in LDH to 2. 30 nm was observed in the resulting DNA-LDH nanohybrids and it gave peaks corresponding to C=O (1 534 cm(-1) and 1488 cm(-1)) in skeleton and bases, C-O stretching vibration (1228 cm(-1)), and P-O symmetrical stretching vibration (1096 cm(-1)) in functional groups of DNA, indicating that DNA were intercalated into the LDH by the ion exchange. However, the displacement of NO3(-) was not fully complete (partial intercalation of DNA). The DNA outside LDH interlayers was absorbed on the surface of LDH. The cyclic voltammetric curves showed that DNA in the composites exhibited a very similar peaks, which corresponded to the two reduction current peaks (E(P) = - 1.2 mV and E(P) = -2.4 mV) of free DNA. Also there was no cathode sag emerging in cyclic voltammetric curves, suggesting that both Cd2+ and Pb2+ cannot insert into the groove of DNA to associate with base pairs or other groups when DNA was bound on LDH. The results showed that, on the one hand, both Cd2+ and Pb2+ were absorbed on the external surface of LDH for immobilization, on the other hand, the layer of LDH provided ideal space for DNA by the action of protecting DNA molecules from Cd2+ and Pb2+.

  6. Adsorption of Anionic Dyes from Aqueous Solutions by Calcined and Uncalcined Mg/ Al Layered Double Hydroxide

    International Nuclear Information System (INIS)

    Siti Mariam Sumari; Zaini Hamzah; Kantasamy, N.

    2016-01-01

    The uptake of Acid Blue 29 (AB29), Reactive Orange 16 (RO16) and Reactive Red 120 (RR120) from aqueous solutions by calcined (CLDH) and uncalcined Mg/Al layered double hydroxide (LDH) has been investigated. The adsorption process was conducted in a batch mode at 25 degree Celcius. Anionic dye removal was more efficient using the CLDH rather than LDH. The adsorption process by CLDH involved reconstruction and hydration of the calcined LDH and intercalation of AB29, RO16 and RR120. Physical characterization using X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform Infrared (FTIR) were used to ascertain the memory effect phenomenon that is structural reconstruction to regain its original LDH after rehydration. To gain insight into the mechanism of adsorption by CLDH, the pseudo-first order (PFO) and pseudo-second order (PSO) and intraparticle diffusion (IPD) kinetic models were used to analyse experimental data. Based on the correlation coefficient (R 2 ), the PSO has better fitting (R 2 =0.987-1.00) compared to PFO (R 2 =0.867-0.990). Furthermore the values of maximum adsorption capacity, (q e ) calculated from PSO model are consistent with the experimental q e indicating that the experimental kinetic data for AB29, RO16 and RR120 adsorption by CLDH are suitable for this model. Recycling of the adsorbent, in cycles of calcination-reconstruction process promised a possibility of regeneration of CLDH. (author)

  7. Hydroxy double salts loaded with bioactive ions: Synthesis, intercalation mechanisms, and functional performance

    Energy Technology Data Exchange (ETDEWEB)

    Kaassis, Abdessamad Y.A. [UCL School of Pharmacy, University College London, 29-39 Brunswick Square, London WC1N 1AX (United Kingdom); Xu, Si-Min; Guan, Shanyue; Evans, David G. [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Wei, Min, E-mail: weimin@mail.buct.edu.cn [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Williams, Gareth R., E-mail: g.williams@ucl.ac.uk [UCL School of Pharmacy, University College London, 29-39 Brunswick Square, London WC1N 1AX (United Kingdom)

    2016-06-15

    The intercalation of the anions of diclofenac (Dic), naproxen (Nap), and valproic acid (Val) into three hydroxy double salts (HDSs) has been explored in this work. Experiments were performed with [Co{sub 1.2}Zn{sub 3.8}(OH){sub 8}](NO{sub 3}){sub 2}·2H{sub 2}O (CoZn-NO{sub 3}), [Ni{sub 2}Zn{sub 3}(OH){sub 8}](NO{sub 3}){sub 2}·2H{sub 2}O (NiZn-NO{sub 3}) and [Zn{sub 5}(OH){sub 8}](NO{sub 3}){sub 2}·2H{sub 2}O (Zn-NO{sub 3}). It proved possible to intercalate diclofenac and naproxen into all three HDSs. In contrast, Val could be intercalated into CoZn-NO{sub 3} but when it was reacted with Zn-NO{sub 3} the HDS structure was destroyed, and the product comprised ZnO. Successful intercalation was verified by X-ray diffraction, IR spectroscopy, and elemental microanalysis. Molecular dynamics simulations showed the Dic and Nap ions to arrange themselves in an “X” shape in the interlayer space, forming a bilayer. Val was found to adopt a position with its aliphatic groups parallel to the HDS layer, again in a bilayer. In situ time resolved X-ray diffraction experiments revealed that intercalation of Dic and Nap into CoZn-NO{sub 3} and Zn-NO{sub 3} is mechanistically complex, with a number of intermediate phases observed. In contrast, the intercalation of all three guests into NiZn-NO{sub 3} and of Val into CoZn-NO{sub 3} are simple one step reactions proceeding directly from the starting material to the product. The HDS-drug composites were found to have sustained release profiles. - Graphical abstract: Seven new drug intercalates of hydroxy double salts (HDSs) have been prepared and characterised. The intercalation mechanisms have been explored, and the drug release properties of the HDS/drug composites quantified. Display Omitted.

  8. Hydroxy double salts loaded with bioactive ions: Synthesis, intercalation mechanisms, and functional performance

    Science.gov (United States)

    Y. A. Kaassis, Abdessamad; Xu, Si-Min; Guan, Shanyue; Evans, David G.; Wei, Min; Williams, Gareth R.

    2016-06-01

    The intercalation of the anions of diclofenac (Dic), naproxen (Nap), and valproic acid (Val) into three hydroxy double salts (HDSs) has been explored in this work. Experiments were performed with [Co1.2Zn3.8(OH)8](NO3)2·2H2O (CoZn-NO3), [Ni2Zn3(OH)8](NO3)2·2H2O (NiZn-NO3) and [Zn5(OH)8](NO3)2·2H2O (Zn-NO3). It proved possible to intercalate diclofenac and naproxen into all three HDSs. In contrast, Val could be intercalated into CoZn-NO3 but when it was reacted with Zn-NO3 the HDS structure was destroyed, and the product comprised ZnO. Successful intercalation was verified by X-ray diffraction, IR spectroscopy, and elemental microanalysis. Molecular dynamics simulations showed the Dic and Nap ions to arrange themselves in an "X" shape in the interlayer space, forming a bilayer. Val was found to adopt a position with its aliphatic groups parallel to the HDS layer, again in a bilayer. In situ time resolved X-ray diffraction experiments revealed that intercalation of Dic and Nap into CoZn-NO3 and Zn-NO3 is mechanistically complex, with a number of intermediate phases observed. In contrast, the intercalation of all three guests into NiZn-NO3 and of Val into CoZn-NO3 are simple one step reactions proceeding directly from the starting material to the product. The HDS-drug composites were found to have sustained release profiles.

  9. Synthesis and physical properties of new layered double hydroxides based on ionic liquids: Application to a polylactide matrix

    KAUST Repository

    Livi, Sébastien

    2012-12-01

    Ionic liquids based on tetraalkylphosphonium salts combined with different anions (decanoate and dodecylsulfonate) have been used as intercalating agents of layered double hydroxides (LDHs) by ion exchange. The synthesized phosphonium-treated LDHs display a dramatically improved thermal degradation and a significant increase in the interlayer distance as confirmed by thermogravimetric analysis (TGA) and X-ray Diffraction (XRD), respectively. To highlight the effect of thermostable ionic liquids, a very low amount of LDHs has been introduced within a polylactide (PLA) matrix and PLA/LDHs nanocomposites have been processed in melt by twin-screw extrusion. Then, transmission electron microscopy (TEM) analysis has been used to investigate the influence of ILs on the different morphologies of these nanocomposites. Even though the thermal stability of PLA matrix decreased, an excellent stiffness-toughness compromise has been obtained. © 2012 Elsevier Inc.

  10. Synthesising methods of layered double hydroxides and its use in the fabrication of dye Sensitised solar cell (DSSC): A short review

    Science.gov (United States)

    George, Giphin; Saravanakumar, M. P.

    2017-11-01

    The layered double hydroxides (LDH) which are anionic clay substances comprising of stacked cationic layers and interlayer anions. The cationic sheets contain octahedral structure consisting the divalent and trivalent ions in the center and hydroxyl bunches in the corners, gathered by three bonding with the neighbouring octahedra on every side of the layer. The ratio between the quantity of cations and OH‑ ions is 2:1, so a positive charge shows up on the layer because of the presence of trivalent cations. The interlayer space gives the compensation anions and water molecules, assuring a balanced out layered structure. The LDH materials were successfully synthesised from magnesium, aluminium, zinc and chromium chloride salts utilizing the co-precipitation technique. A Zn-Al LDH was researched as a potential sorbent material. This article reviews the recent advances in the preparation and intercalation of layered double hydroxides and its application in the fabrication of Dye Sensitized Solar Cell (DSSC).

  11. Colorful and transparent poly(vinyl alcohol) composite films filled with layered zinc hydroxide salts, intercalated with anionic orange azo dyes (methyl orange and orange II)

    International Nuclear Information System (INIS)

    Neves da Silva, Marlon Luiz; Marangoni, Rafael; Cursino, Ana Cristina Trindade; Schreiner, Wido Herwig; Wypych, Fernando

    2012-01-01

    Highlights: ► Zinc hydroxide salts were successfully intercalated with anionic orange azo dyes. ► The anionic dye was co-intercalated with hydrated chloride anions. ► The orange materials were used as fillers for poly(vinyl alcohol). ► Transparent, homogeneous, colorful PVA films were obtained by wet casting. ► Some composites stored at lower humidity exhibited improved mechanical properties. - Abstract: Layered zinc hydroxide salts (zinc LHS) were intercalated with anionic orange azo dyes, namely methyl orange (MO) and orange II (OII), and co-intercalated with hydrated chloride anions. After characterization by X-ray diffraction (XRD), thermal analysis (TGA/DTA), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS), the materials were used as fillers for poly(vinyl alcohol) (PVA). Colorful transparent films were obtained by wet casting, revealing good dispersion of the material into the polymer. In the case of zinc LHS/OII, PVA was intercalated between the zinc LHS layers. Evaluation of the mechanical properties of the PVA composite films revealed that the layered colorful materials were able to increase the mechanical properties of the PVA films only when the films were stored under lower relative humidity. As expected, films with higher water content displayed reduced tensile strength and modulus because of the plasticizing effect of water. As for the films stored at 43% relative humidity, more pronounced improvement of modulus was observed for 1 and 4% zinc LHS/OII, and enhanced tensile strength was achieved for 0.5 and 1% zinc LHS/OII. This effect can be attributed to better dispersion of the layered filler and its better adhesion to the PVA matrix.

  12. Removal of boron species by layered double hydroxides: a review.

    Science.gov (United States)

    Theiss, Frederick L; Ayoko, Godwin A; Frost, Ray L

    2013-07-15

    Boron, which is an essential element for plants, is toxic to humans and animals at high concentrations. Layered double hydroxides (LDHs) and thermally activated LDHs have shown good uptake of a range of boron species in laboratory scale experiments when compared to current available methods, which are for the most part ineffective or prohibitively expensive. LDHs were able to remove anions from water by anion exchange, the reformation (or memory) effect and direct precipitation. The main mechanism of boron uptake appeared to be anion exchange, which was confirmed by powder X-ray diffraction (XRD) measurements. Solution pH appeared to have little effect on boron sorption while thermal activation did not always significantly improve boron uptake. In addition, perpetration of numerous LDHs with varying boron anions in the interlayer region by direct co-precipitation and anion exchange have been reported by a number of groups. The composition and orientation of the interlayer boron ions could be identified with reasonable certainty by applying a number of characterisation techniques including: powder XRD, nuclear magnetic resonance spectroscopy (NMR), X-ray photoelectron spectroscopy (XPS) and infrared (IR) spectroscopy. There is still considerable scope for future research on the application of LDHs for the removal of boron contaminants. Copyright © 2013 Elsevier Inc. All rights reserved.

  13. Silica@layered double hydroxide core-shell hybrid materials.

    Science.gov (United States)

    Kwok, Wing L J; Crivoi, Dana-Georgiana; Chen, Chunping; Buffet, Jean-Charles; O'Hare, Dermot

    2017-12-19

    A series of silica@layered double hydroxides (SiO 2 @Mg 2 Al-CO 3 -AMO-LDHs) have been synthesised by in situ precipitation of Mg 2 Al-CO 3 -LDH at room temperature in the presence of amorphous spherical silica particles (∼500 nm). We have systematically investigated a number of synthetic parameters in order to evaluate their effects on the composition, morphological and physical properties of the isolated materials. Syntheses carried out at moderate stirring speeds (e.g. 500 rpm) were found to promote the formation of vertically aligned LDH platelets with respect to the silica surface. Addition rates of the metal solutions slower than 0.43 mmol h -1 were found to create a thicker LDH shell consisting of vertically aligned LDH platelets. When the metal solutions were added rapidly (0.86 mmol h -1 ), we observed that for both slow and fast stirring speeds the synthesised core-shell materials had thin LDH shells and the majority of the LDH precipitated independent of the silica, forming unbound "free" LDH.

  14. Acid Green 1 removal from wastewater by layered double hydroxides

    Science.gov (United States)

    Elkhattabi, El Hassan; Lakraimi, Mohamed; Berraho, Moha; Legrouri, Ahmed; Hammal, Radouan; El Gaini, Layla

    2018-03-01

    The paper presents the removal of Acid Green 1 (AG1) from aqueous solutions by [Zn-Al-Cl]-layered double hydroxides (LDHs). The LDH was prepared by coprecipitation at constant pH. The affinity of this material for AG1 was studied as a function of contact time, pH of the solution, LDH dose and AG1/LDH mass ratio. It was found that 32 h are enough to reach the equilibrium with a maximum retention at pH 8 for an LDH dose of 100 mg and with an AG1/LDH mass ratio higher than 2. The adsorption isotherm is of L-type, as described by the Langmuir model. The results demonstrate that AG1 retention on LDHs occurs by adsorption on external surface when AG1/LDH mass ratio is equal or lower than 2 and by both adsorption and interlayer ion exchange for ratios higher than 2. A mechanism for the AG1 removal has been confirmed by X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric-differential thermal analyses and scanning electron microscopy.

  15. Layered double hydroxide nanoparticles in gene and drug delivery.

    Science.gov (United States)

    Ladewig, Katharina; Xu, Zhi Ping; Lu, Gao Qing Max

    2009-09-01

    Layered double hydroxides (LDHs) have been known for many decades as catalyst and ceramic precursors, traps for anionic pollutants, catalysts and additives for polymers, but their successful synthesis on the nanometer scale a few years ago opened up a whole new field for their application in nanomedicine. The delivery of drugs and other therapeutic/bioactive molecules (e.g., peptides, proteins, nucleic acids) to mammalian cells is an area of research that is of tremendous importance to medicine and provides manifold applications for any new developments in the area of nanotechnology. Among the many different nanoparticles that have been shown to facilitate gene and/or drug delivery, LDH nanoparticles have attracted particular attention owing to their many desirable properties. This review aims to report recent progress in gene and drug delivery using LDH nanoparticles. It summarizes the advantages and disadvantages of using LDH nanoparticles as carriers for nucleic acids and drugs against the general background of bottlenecks that are encountered by cellular delivery systems. It describes further the models that have been proposed for the internalization of LDH nanoparticles into cells so far and discusses the intracellular fate of the particles and their cargo. The authors offer some remarks on how this field of research will progress in the near future and which challenges need to be overcome before LDH nanoparticles can be used in a clinical setting.

  16. Drug delivery system for an anticancer agent, chlorogenate-Zn/Al-layered double hydroxide nanohybrid synthesised using direct co-precipitation and ion exchange methods

    Energy Technology Data Exchange (ETDEWEB)

    Barahuie, Farahnaz [Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Hussein, Mohd Zobir, E-mail: mzobir@putra.upm.edu.my [Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Arulselvan, Palanisamy [Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Fakurazi, Sharida [Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Department of Human Anatomy, Faculty of Medicine and Health Sciences, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Zainal, Zulkarnain [Materials Synthesis and Characterization Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia)

    2014-09-15

    A nano-structured drug-inorganic clay hybrid involving an active anticancer compound, which is chlorogenic acid (CA) intercalated into Zn/Al-layered double hydroxide, has been assembled via ion-exchange and co-precipitation methods to form a nanohybrid CZAE (a chlorogenic acid-Zn/Al nanohybrid synthesised using an ion-exchange method) and CZAC (a chlorogenic acid-Zn/Al nanohybrid synthesised using a direct method), respectively. The X-ray diffraction (XRD) results confirmed that the CA-LDH had a hybrid structure in which the anionic chlorogenate is arranged between the interlayers as a horizontal monolayer at 90 and 20° angles from the x axis for CZAE and CZAC, respectively. Both nanohybrids have the properties of mesoporous materials. The high loading percentage of chlorogenic acid (approximately 43.2% for CZAE and 45.3% for CZAC) with basal spacings of 11.7 and 12.6 Å for CZAE and CZAC, respectively, corroborates the successful intercalation of chlorogenic acid into the interlayer gallery of layered double hydroxides. Free chlorogenic acid and the synthesised nanocomposites (CZAE, CZAC) were assessed for their cytotoxicity against various cancer cells. The Fourier transform infrared data supported the formation of both nanohybrids, and a thermal analysis showed that the nanohybrids are more thermally stable than their counterparts. The chlorogenate shows a sustained release, and the release rate of chlorogenate from CZAE and CZAC nanohybrids at pH 7.4 is remarkably lower than that at pH 4.8 due to their different release mechanisms. The release rate of chlorogenate from both nanohybrids can be described as pseudo-second order. The present investigation revealed the potential of the nanohybrids to enhance the in vitro anti-tumour effect of chlorogenic acid in liver and lung cancer cells in vitro. - Highlights: • We intercalated chlorogenic into Zn/Al-layered double hydroxide by ion-exchange and coprecipitation methods. • The two methods gave nanocomposites

  17. Polymethyl methacrylate and polystyrene with layered double hydroxide nano composites: In situ synthesis, morphology and thermal properties; Nanocompositos de polimetacrilato de metila e poliestireno com hidroxido duplo lamelar: sintese in situ, morfologia e propriedades termicas

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2011-07-01

    Over the past decade, polymer nanocomposites have attracted interest, both in industry and in academia, because they often exhibit remarkable improvement in their properties when compared with pure polymer or conventional micro and macro-composites using low levels of reinforcements. In this work polymethyl methacrylate and polystyrene reinforced with layered double hydroxide, which was intercalated with sodium dodecyl sulfate were synthesized by in situ bulk polymerization. The nanocomposites were characterized and compared by X-ray diffraction, thermogravimetric analysis and flammability test. The X-ray diffraction demonstrated that synthesized nanocomposites showed a high global dispersion of layered double hydroxide, suggesting exfoliated morphology. The result of thermogravimetric analysis and flammability test for synthesized polystyrene/ layered double hydroxide nanocomposite presented a significant improvement in thermal stability and flammability property when compared with pure polymer. (author)

  18. Layered double hydroxide catalyst for the conversion of crude vegetable oils to a sustainable biofuel

    Science.gov (United States)

    Mollaeian, Keyvan

    Over the last two decades, the U.S. has developed the production of biodiesel, a mixture of fatty acid methyl esters, using chiefly vegetable oils as feedstocks. However, there is much concern about the availability of high-quality vegetable oils for longterm biodiesel production. Problems have also risen due to the production of glycerol, an unwanted byproduct, as well as the need for process wash water. Therefore, this study was initiated to produce not only fatty acid methyl esters (FAMEs) but also fatty acid glycerol carbonates (FAGCs) by replacing methanol with dimethyl carbonate (DMC). The process would have no unnecessary byproducts and would be a simplified process compared to traditional biodiesel. In addition, this altering of the methylating agent could convert triglycerides, free fatty acids, and phospholipids to a sustainable biofuel. In this project, Mg-Al Layered Double Hydroxide (LDH) was optimized by calcination in different temperature varied from 250°C to 450°C. The gallery between layers was increased by intercalating sodium dodecylsulfate (SDS). During catalyst preparation, the pH was controlled ~10. In our experiment, triazabicyclodecene (TBD) was attached with trimethoxysilane (3GPS) as a coupling agent, and N-cetyl-N,N,N-trimethylammonium bromide (CTAB) was added to remove SDS from the catalyst. The catalyst was characterized by XRD, FTIR, and Raman spectroscopy. The effect of the heterogeneous catalyst on the conversion of canola oil, corn oil, and free fatty acids was investigated. To analyze the conversion of lipid oils to biofuel an in situ Raman spectroscopic method was developed. Catalyst synthesis methods and a proposed mechanism for converting triglycerides and free fatty acids to biofuel will be presented.

  19. Processing and characterization of polystyrene nanocomposites based on CoAl layered double hydroxide

    Directory of Open Access Journals (Sweden)

    Kelothu Suresh

    2016-09-01

    Full Text Available The present work deals with the development of polystyrene (PS nanocomposites through solvent blending technique with diverse contents of modified CoAl layered double hydroxide (LDH. The prepared PS as well as PS/CoAl LDH (1–7 wt.% nanocomposites were characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, Fourier transform infrared spectroscopy (FTIR, rheological analysis, thermogravimetric analysis (TGA and differential scanning calorimetry (DSC. The XRD results suggested the formation of exfoliated structure, while TEM images clearly indicated the intercalated morphology of PS nanocomposites at higher loading. The presence of various functional groups in the CoAl LDH and PS/CoAl LDH nanocomposites was verified by FTIR analysis. TGA data confirmed that the thermal stability of PS composites was enhanced significantly as compared to pristine PS. While considering 15% weight loss as a reference point, it was found that the thermal degradation (Td temperature increased up to 28.5 °C for PS nanocomposites prepared with 7 wt.% CoAl LDH loading over pristine PS. All the nanocomposite samples displayed superior glass transition temperature (Tg, in which PS nanocomposites containing 7 wt.% LDH showed about 5.5 °C higher Tg over pristine PS. In addition, the kinetics for thermal degradation of the composites was studied using Coats-Redfern method. The Criado method was ultimately used to evaluate the decomposition reaction mechanism of the nanocomposites. The complex viscosity and rheological muduli of nanocomposites were found to be higher than that of pristine PS when the frequency increased from 0.01 to 100 s−1.

  20. Layered Double Hydroxides as Effective Adsorbents for U(VI and Toxic Heavy Metals Removal from Aqueous Media

    Directory of Open Access Journals (Sweden)

    G. N. Pshinko

    2013-01-01

    Full Text Available Capacities of different synthesized Zn,Al-hydrotalcite-like adsorbents, including the initial carbonate [Zn4Al2(OH12]·CO3·8H2O and its forms intercalated with chelating agents (ethylenediaminetetraacetic acid (EDTA, diethylenetriaminepentaacetic acid (DTPA, and hexamethylenediaminetetraacetic acid (HMDTA and heat-treated form Zn4Al2O7, to adsorb uranium(VI and ions of toxic heavy metals have been compared. Metal sorption capacities of hydrotalcite-like adsorbents have been shown to correlate with the stability of their complexes with the mentioned chelating agents in a solution. The synthesized layered double hydroxides (LDHs containing chelating agents in the interlayer space are rather efficient for sorption purification of aqueous media free from U(VI irrespective of its forms of natural abundance (including water-soluble bi- and tricarbonate forms and from heavy metal ions. [Zn4Al2(OH12]·EDTA·nH2O is recommended for practical application as one of the most efficient and inexpensive synthetic adsorbents designed for recovery of both cationic and particularly important anionic forms of U(VI and other heavy metals from aqueous media. Carbonate forms of LDHs turned out to be most efficient for recovery of Cu(II from aqueous media with pH0≥7 owing to precipitation of Cu(II basic carbonates and Cu(II hydroxides. Chromate ions are efficiently adsorbed from water only by calcinated forms of LDHs.

  1. Formation and rejoining of deoxyribonucleic acid double-strand breaks induced in isolated cell nuclei by antineoplastic intercalating agents.

    Science.gov (United States)

    Pommier, Y; Schwartz, R E; Kohn, K W; Zwelling, L A

    1984-07-03

    The biochemical characteristics of the formation and disappearance of intercalator-induced DNA double-strand breaks (DSB) were studied in nuclei from mouse leukemia L1210 cells by using filter elution methodology [Bradley, M. O., & Kohn, K.W. (1979) Nucleic Acids Res. 7, 793-804]. The three intercalators used were 4'-(9-acridinylamino)-methanesulfon-m-anisidide (m-AMSA), 5-iminodaunorubicin (5-ID), and ellipticine. These compounds differ in that they produced predominantly DNA single-strand breaks (SSB) (m-AMSA) or predominantly DNA double-strand breaks (ellipticine) or a mixture of both SSB and DSB (5-ID) in whole cells. In isolated nuclei, each intercalator produced DSB at a frequency comparable to that which is produced in whole cells. Moreover, these DNA breaks reversed within 30 min after drug removal. It thus appeared that neither ATP nor other nucleotides were necessary for intercalator-dependent DNA nicking-closing reactions. The formation of the intercalator-induced DSB was reduced at ice temperature. Break formation was also reduced in the absence of magnesium, at a pH above 6.4 and at NaCl concentrations above 200 mM. In the presence of ATP and ATP analogues, the intercalator-induced cleavage was enhanced. These results suggest that the intercalator-induced DSB are enzymatically mediated and that the enzymes involved in these reactions can catalyze DNA double-strand cleavage and rejoining in the absence of ATP, although the occupancy of an ATP binding site might convert the enzyme to a form more reactive to intercalators. Three inhibitors of DNA topoisomerase II--novobiocin, nalidixic acid, and norfloxacin--reduced the formation of DNA strand breaks.(ABSTRACT TRUNCATED AT 250 WORDS)

  2. Thermal decomposition of Co–Al layered double hydroxide ...

    Indian Academy of Sciences (India)

    Administrator

    In this, paper, we study the thermal decomposition of the Co–Al–. CO. 2. 3. –. LDH by in situ variable temperature powder X-ray diffraction (VTPXRD), and follow the structural changes taking place in the LDH prior to the decomposition reac- tion. We report the formation of a precursor hydroxide phase having a topochemical ...

  3. Design and fabrication of enhanced corrosion resistance Zn-Al layered double hydroxides films based anion-exchange mechanism on magnesium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Meng; Yan, Luchun; Ling, Hao; Diao, Yupeng; Pang, Xiaolu; Wang, Yanlin; Gao, Kewei, E-mail: kwgao@yahoo.com

    2017-05-15

    Highlights: • Zn-Al LDHs film loaded nitrate anions has been fabricated on a magnesium alloy substrate via a facile hydrothermal crystallization method. • The Zn-Al-Cl LDHs and Zn-Al-VO{sub x} LDHs film were obtained based on anion-exchange mechanism. • The Zn-Al-Cl LDHs and Zn-Al-VO{sub x} LDHs film could effectively protect magnesium alloy. - Abstract: Layered double hydroxides (LDHs) with brucite-like layer structure and the facile exchangeability of intercalated anions had attracted tremendous interest in many fields because of their great importance for both fundamental studies and practical applications. Herein zinc-aluminum layered double hydroxides (Zn-Al LDHs) films intercalated with nitrate anions on the magnesium alloy substrate were designed and fabricated via a facile hydrothermal crystallization method. In order to obtain better corrosion resistance, chloride and vanadate anions were intercalated into the LDHs interlayers via the anion-exchange reaction. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electronic microscopy (SEM) were used to examine structure, composition and morphology of the Zn-Al-NO{sub 3} LDHs, Zn-Al-Cl LDHs and Zn-Al-VO{sub x} LDHs films. The corrosion resistance of the Zn-Al LDHs with different anion films was estimated by the electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization measurement. EIS and polarization curves measurements revealed that the magnesium alloy could be effectively protected by the Zn-Al-Cl LDHs and Zn-Al-VO{sub x} LDHs films due to the blocking effect of chloride anions and the control-release ability of vanadate anions.

  4. Mg/Al Ordering in Layered Double Hydroxides Revealed by Multinuclear NMR Spectroscopy

    DEFF Research Database (Denmark)

    Nielsen, Ulla Gro; Grey, Clare P.; Sideris, Paul J.

    2008-01-01

    The anion- exchange ability of layered double hydroxides ( LDHs) has been exploited to create materials for use in catalysis, drug delivery, and environmental remediation. The specific cation arrangements in the hydroxide layers of hydrotalcite- like LDHs, of general formula Mg1-x2+Alx3+OH2(Anion...... and aluminum distribution. These data, in combination with H-1-Al-27 double- resonance and Mg-25 triple- quantum MAS NMR data, show that the cations are fully ordered for magnesium: aluminum ratios of 2:1 and that at lower aluminum content, a nonrandom distribution of cations persists, with no Al3+-Al3+ close...

  5. Synthesis of Zn–Fe layered double hydroxides via an oxidation process and structural analysis of products

    Energy Technology Data Exchange (ETDEWEB)

    Morimoto, Kazuya, E-mail: kazuya.morimoto@aist.go.jp [Institute for Geo-Resources and Environment, National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Higashi, Tsukuba, Ibaraki 305-8567 (Japan); Tamura, Kenji [Environmental Remediation Materials Unit, National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Anraku, Sohtaro [Graduate School of Engineering, Hokkaido University, Kita 13 Nishi 8, Kita-ku, Sapporo 060-8628 (Japan); Sato, Tsutomu [Faculty of Engineering, Hokkaido University, Kita 13 Nishi 8, Kita-ku, Sapporo 060-8628 (Japan); Suzuki, Masaya [Institute for Geo-Resources and Environment, National Institute of Advanced Industrial Science and Technology (AIST), 1-1-1 Higashi, Tsukuba, Ibaraki 305-8567 (Japan); Yamada, Hirohisa [Environmental Remediation Materials Unit, National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan)

    2015-08-15

    The synthesis of Zn–Fe(III) layered double hydroxides was attempted, employing different pathways using either Fe(II) or Fe(III) species together with Zn as the initial reagents. The product derived from the synthesis employing Fe(II) was found to transition to a Zn–Fe(III) layered double hydroxides phase following oxidation process. In contrast, the product obtained with Fe(III) did not contain a layered double hydroxides phase, but rather consisted of simonkolleite and hydrous ferric oxide. It was determined that the valency of the Fe reagent used in the initial synthesis affected the generation of the layered double hydroxides phase. Fe(II) species have ionic radii and electronegativities similar to those of Zn, and therefore are more likely to form trioctahedral hydroxide layers with Zn species. - Graphical abstract: The synthesis of Zn–Fe(III) layered double hydroxides was attempted, employing different pathways using either Fe(II) or Fe(III) species together with Zn as the initial reagents. - Highlights: • Iron valency affected the generation of Zn–Fe layered double hydroxides. • Zn–Fe layered double hydroxides were successfully synthesized using Fe(II). • Fe(II) species were likely to form trioctahedral hydroxide layers with Zn species.

  6. Formation of Layered Double Hydroxides on Alumina Surface in Aqueous Solutions Containing Divalent Metal Cations

    Czech Academy of Sciences Publication Activity Database

    Kovanda, F.; Mašátová, P.; Novotná, P.; Jirátová, Květa

    2009-01-01

    Roč. 57, č. 4 (2009), s. 425-432 ISSN 0009-8604 R&D Projects: GA ČR GA104/07/1400 Institutional research plan: CEZ:AV0Z40720504 Keywords : deposition * layered double hydroxides * supported mixed oxides Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.431, year: 2009

  7. Facile preparation of layered double hydroxide/MoS{sub 2}/poly(vinyl alcohol) composites

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Keqing, E-mail: zhoukq@cug.edu.cn [Faculty of Engineering, China University of Geosciences (Wuhan), 388 Lumo Road, Wuhan, Hubei, 430074 (China); Hu, Yixin [Department of Chemistry, Lanzhou University, Lanzhou 730000 (China); Liu, Jiajia [State Key Laboratory of Fire Science, University of Science and Technology of China, 96 Jinzhai Road, Hefei, Anhui, 230026 (China); Gui, Zhou, E-mail: zgui@ustc.edu.cn [State Key Laboratory of Fire Science, University of Science and Technology of China, 96 Jinzhai Road, Hefei, Anhui, 230026 (China); Jiang, Saihua [School of Mechanical and Automotive Engineering, South China University of Technology, Wushan Road 381, Guangzhou, 510641 (China); Tang, Gang [School of Architecture and Civil Engineering, Anhui University of Technology, 59 Hudong Road, Ma' anshan, Anhui, 243002 (China)

    2016-08-01

    In present study, the layered double hydroxide/MoS{sub 2} hybrids are facilely synthesized by self-assembly of exfoliated MoS{sub 2} nanosheets and layered double hydroxide nanoplates via electrostatic interaction, with the aim of combining their physical and chemical functionalities to form a promising nanofiller for flame retardancy in polymer composites. The structure and morphology of the layered double hydroxide/MoS{sub 2} hybrids are probed by X-ray diffraction and transmission electron microscopy. Subsequently, the hybrids are incorporated into poly (vinyl alcohol) to serve as reinforcements. The flame retardant efficiency of MoS{sub 2} nanosheets in poly (vinyl alcohol) is significantly enhanced after the incorporation of layered double hydroxide nanoplates, which can be explained by the forming of a compact and uniform char during combustion. - Highlights: • The LDH/MoS{sub 2} hybrids were facilely synthesized by self-assembly method. • The flame retardant efficiency of LDH/MoS{sub 2} hybrids in PVA was significantly enhanced. • It is a promising strategy for improving the flame retardant efficiency of MoS{sub 2}.

  8. Anomalous impact strength for layered double hydroxide-palmitate/poly(e-caprolactone) nanocomposites

    CSIR Research Space (South Africa)

    Moyo, Lumbidzani

    2014-11-01

    Full Text Available is needed in order to transfer this potential into reality, particularly for short-term packaging applications. In this context, layered double hydroxide modified with palmitic acid (LDH-palmitate), was used as a nanoadditive to enhance the mechanical...

  9. Migration of nanosized layered double hydroxide platelets from polylactide nanocomposite films

    DEFF Research Database (Denmark)

    Schmidt, Bjørn; Katiyar, Vimal; Plackett, David

    2011-01-01

    Melt-extruded L-polylactide (PLA) nanocomposite films were prepared from commercially available PLA and laurate-modified Mg–Al layered double hydroxide (LDH-C12). Three films were tested for total migration as well as specific migration of LDH, tin, laurate and low molecular weight PLA oligomers...

  10. Hydrothermal Synthesis and Characterization of 3R Polytypes of Mg-Al Layered Double Hydroxides

    NARCIS (Netherlands)

    Budhysutanto, W.N.

    2010-01-01

    Layered Double Hydroxides (LDH) is a unique group of clays that have an anionic exchange capability. This research explored the hydrothermal method as an alternative method to synthesize Mg-Al LDH. It is a simple and more environmentally friendly compared to the conventional method of

  11. Coagulation Behavior of Graphene Oxide on Nanocrystallined Mg/Al Layered Double Hydroxides: Batch Experimental and Theoretical Calculation Study.

    Science.gov (United States)

    Zou, Yidong; Wang, Xiangxue; Ai, Yuejie; Liu, Yunhai; Li, Jiaxing; Ji, Yongfei; Wang, Xiangke

    2016-04-05

    Graphene oxide (GO) has attracted considerable attention because of its remarkable enhanced adsorption and multifunctional properties. However, the toxic properties of GO nanosheets released into the environment could lead to the instability of biological system. In aqueous phase, GO may interact with fine mineral particles, such as chloridion intercalated nanocrystallined Mg/Al layered double hydroxides (LDH-Cl) and nanocrystallined Mg/Al LDHs (LDH-CO3), which are considered as coagulant molecules for the coagulation and removal of GO from aqueous solutions. Herein the coagulation of GO on LDHs were studied as a function of solution pH, ionic strength, contact time, temperature and coagulant concentration. The presence of LDH-Cl and LDH-CO3 improved the coagulation of GO in solution efficiently, which was mainly attributed to the surface oxygen-containing functional groups of LDH-Cl and LDH-CO3 occupying the binding sites of GO. The coagulation of GO by LDH-Cl and LDH-CO3 was strongly dependent on pH and ionic strength. Results of theoretical DFT calculations indicated that the coagulation of GO on LDHs was energetically favored by electrostatic interactions and hydrogen bonds, which was further evidenced by FTIR and XPS analysis. By integrating the experimental results, it was clear that LDH-Cl could be potentially used as a cost-effective coagulant for the elimination of GO from aqueous solutions, which could efficiently decrease the potential toxicity of GO in the natural environment.

  12. Mechanical and Morphological Properties of Poly-3-hydroxybutyrate/Poly(butyleneadipate-co-terephthalate/Layered Double Hydroxide Nanocomposites

    Directory of Open Access Journals (Sweden)

    Yen Leng Pak

    2013-01-01

    Full Text Available Nanocomposites of poly-3-hydroxybutyrate/poly(butyleneadipate-co-terephthalate/layered double hydroxide (PHB/PBAT/LDH were prepared from a binary blend of PHB/PBAT and stearate-Zn3Al LDH via a solution casting method using chloroform as solvent in this study. The pristine Zn3Al LDH was synthesized from nitrate salts solution at pH 7 by using coprecipitation technique and then was modified by stearate anions surfactant via ion exchange reaction. As a result, the basal spacing of the LDH was increased from 8.77 to 24.94 Å after the modification. Intercalated nanocomposites were formed due to the presence of diffraction peak in XRD diffractograms. The infrared spectrum of stearate-Zn3Al LDH exhibited the existence of stearate anions in the synthesized Zn3Al LDH. Mechanical properties with 2 wt% stearate-Zn3Al LDH loading nanocomposites showed 56 wt% improvements in elongation at break compared to those of the blend.

  13. Layered double hydroxides as fillers in poly(l-lactide nanocomposites, obtained by in situ bulk polymerization

    Directory of Open Access Journals (Sweden)

    Telma Nogueira

    Full Text Available Abstract In this study in situ bulk polymerization of L-lactide filled with layered double hydroxides (LDH was investigated. Four different LDHs intercalated with two different organic anions (salicylate and sebacate were synthesized and characterized. After characterization, these synthetic layered compounds were used as fillers in poly(L-lactide (PLLA nanocomposites with two different fillers’s loadings (1 wt% and 2 wt%. PLLA and PLLA nanocomposites were evaluated by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, ultraviolet and visible spectroscopy, thermogravimetric analysis (TGA, dynamical mechanical analysis (DMA, flexural testing and differential scanning calorimetry (DSC. The results demonstrated that, compared to PLLA, the nanocomposite containing 1 wt% of Zn/Al salicylate transmitted less UVA and UVB light, while keeping a similar transparency in the visible region. Thermogravimetric analysis revealed that the nanocomposite with 1 wt% of Zn/Al salicylate exhibited the highest thermal stability. In general the flexural and dynamical mechanical properties were reduced in compassion to neat PLLA. DSC results, demonstrated that, compared to PLLA, all the nanocomposites exhibited lower glass transition temperature and melting temperature values.

  14. Removal of indigo carmine dye from water to Mg-Al-CO(3)-calcined layered double hydroxides.

    Science.gov (United States)

    El Gaini, L; Lakraimi, M; Sebbar, E; Meghea, A; Bakasse, M

    2009-01-30

    Layered double hydroxides (LDHs) calcined, denoted as CLDHs, have been shown to recover their original layered structure in the presence of appropriate anions. In the light of this so-called "memory effect", the removal of indigo carmine (IC), an anionic dye, from aqueous solution by calcined Mg-Al-CO(3) LDHs was investigated in batch mode. We looked at the influence of pH values, dye-adsorbent contact time, initial dye concentration and various temperatures of heating of LDHs on the decolorization rate of IC. The adsorption isotherms, described by Freundlich model are L-type. The characterization of the solids CLDHs, both fresh and after removal of IC, by X-ray diffraction and infrared spectroscopy shows that the IC adsorption on CLDHs is enhanced by reconstruction of a matrix hydrotalcite intercaled by the dye, and the intercalation of the organic ion was clearly evidenced by the net increase in the basal spacing from 0.76 nm for [Mg-Al-CO(3)] to 2.13 nm for the organic derivative.

  15. Removal of indigo carmine dye from water to Mg-Al-CO3-calcined layered double hydroxides

    International Nuclear Information System (INIS)

    El Gaini, L.; Lakraimi, M.; Sebbar, E.; Meghea, A.; Bakasse, M.

    2009-01-01

    Layered double hydroxides (LDHs) calcined, denoted as CLDHs, have been shown to recover their original layered structure in the presence of appropriate anions. In the light of this so-called 'memory effect', the removal of indigo carmine (IC), an anionic dye, from aqueous solution by calcined Mg-Al-CO 3 LDHs was investigated in batch mode. We looked at the influence of pH values, dye-adsorbent contact time, initial dye concentration and various temperatures of heating of LDHs on the decolorization rate of IC. The adsorption isotherms, described by Freundlich model are L-type. The characterization of the solids CLDHs, both fresh and after removal of IC, by X-ray diffraction and infrared spectroscopy shows that the IC adsorption on CLDHs is enhanced by reconstruction of a matrix hydrotalcite intercaled by the dye, and the intercalation of the organic ion was clearly evidenced by the net increase in the basal spacing from 0.76 nm for [Mg-Al-CO 3 ] to 2.13 nm for the organic derivative

  16. Removal of indigo carmine dye from water to Mg-Al-CO{sub 3}-calcined layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    El Gaini, L. [Faculty of Science, University Chouaib Doukkali, 24000 El Jadida (Morocco); Lakraimi, M. [ENS Ecole Normale Superieure, 40000 Marrakech (Morocco); Sebbar, E. [Faculty of Science, University Chouaib Doukkali, 24000 El Jadida (Morocco); Meghea, A. [University POLITEHNICA of Bucharest (Romania); Bakasse, M. [Faculty of Science, University Chouaib Doukkali, 24000 El Jadida (Morocco)], E-mail: bakassem@yahoo.fr

    2009-01-30

    Layered double hydroxides (LDHs) calcined, denoted as CLDHs, have been shown to recover their original layered structure in the presence of appropriate anions. In the light of this so-called 'memory effect', the removal of indigo carmine (IC), an anionic dye, from aqueous solution by calcined Mg-Al-CO{sub 3} LDHs was investigated in batch mode. We looked at the influence of pH values, dye-adsorbent contact time, initial dye concentration and various temperatures of heating of LDHs on the decolorization rate of IC. The adsorption isotherms, described by Freundlich model are L-type. The characterization of the solids CLDHs, both fresh and after removal of IC, by X-ray diffraction and infrared spectroscopy shows that the IC adsorption on CLDHs is enhanced by reconstruction of a matrix hydrotalcite intercaled by the dye, and the intercalation of the organic ion was clearly evidenced by the net increase in the basal spacing from 0.76 nm for [Mg-Al-CO{sub 3}] to 2.13 nm for the organic derivative.

  17. Degradation of l-polylactide during melt processing with layered double hydroxides

    DEFF Research Database (Denmark)

    Gerds, Nathalie; Katiyar, Vimal; Koch, Christian Bender

    2012-01-01

    PLA was melt compounded in small-scale batches with two forms of laurate-modified magnesium–aluminum layered double hydroxide (Mg-Al-LDH-C12), the corresponding carbonate form (Mg-Al-LDH-CO3) and a series of other additives. Various methods were then adopted to characterize the resulting compounds...... in an effort to gain greater insights into PLA degradation during melt processing. PLA molecular weight reduction was found to vary according to the type of LDH additive. It is considered that the degree of particle dispersion and LDH exfoliation, and hence the accessibility of the hydroxide layer surfaces...

  18. The effect of magnesium hydroxide, hydromagnesite and layered double hydroxide on the heat stability and fire performance of plasticized poly(vinyl chloride)

    CSIR Research Space (South Africa)

    Molefe, DM

    2015-09-01

    Full Text Available , FJWJ (Johan) Labuschagne, Walter W Focke, Isbé van der Westhuizen and Osei Ofosu. Magnesium hydroxide derivatives as fire retardants for plasticized PVC. Journal of Fire Sciences November 2015 vol. 33 no. 6 493-510 doi: 10.1177/0734904115612501 http...://jfs.sagepub.com/content/33/6/493.abstract The effect of magnesium hydroxide, hydromagnesite and layered double hydroxide on the heat stability and fire performance of plasticized PVC Dan Matlhomola Molefe1, FJWJ (Johan) Labuschagne2, Walter W Focke2,*, Isbé van der...

  19. Mechanical and thermal properties of polypropylene and layered double hydroxides nanocomposites; Propriedades mecanicas e termicas de nanocompositos de polipropileno e hidroxidos duplos lamelares

    Energy Technology Data Exchange (ETDEWEB)

    Duarte de Farias, A.M.; Fraga, M.A.; Oliveira, R.B.; Oliveira, M.G., E-mail: marcia.oliveira@int.gov.b [Instituto Nacional de Tecnologia (INT), Rio de Janeiro, RJ (Brazil)

    2010-07-01

    The recent interest in polymer nanocomposites involving layered double hydroxides (LDH) is due to improved thermal stability, flame resistance, mechanical and barrier properties. The LDHs are structurally described as the stacking of layers with positively charged hydrated anions intercalated between these lamellae. In this paper, polypropylene nanocomposites with Mg / Al-HDL unmodified and modified with sodium dodecyl sulfate (DS) were prepared in the internal mixing chamber equipped with roller rotors and heated to 190 deg C. The nanocomposites were injected molded and then morphology, mechanical and thermal properties were evaluated by X-ray diffraction, tensile tests and DSC, respectively. The results revealed that both LDH and LDH-DS reached a good degree of dispersion in the PP matrix, resulting in increased stiffness, but reduced capacity for deformation and toughness of nanocomposites. The crystallinity of the nanocomposites was higher compared to the PP matrix. (author)

  20. Gold Nanoparticles on Layered Double Hydroxide Nanosheets and Its Electrocatalysis for Glucose Oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Hye Ran; Lee, Jong Hyeon [The Catholic University of Korea, Bucheon (Korea, Republic of); Cho, Se Hee; Ji, Hong Geun [H and A PharmaChem, Bucheon (Korea, Republic of)

    2016-03-15

    We developed a new way to form the well-defined nanocomposite of Au NPs and exfoliated LDH nanosheet by in situ chemical reduction with NaBH{sub 4}. The optical and structural studies indicate that the Au NPs are highly dispersed and immobilized on the surface of LDH nanosheets. The Au/LDH nanosheet exhibited an excellent electrocatalysis toward glucose oxidation reaction. The results strongly demonstrate that the nanoscopic natures and dense positive charges of LDH nanosheet effectively stabilized the Au NPs to maintain their inherent properties during the synthesis and the electrocatalysis. The use of the double hydroxide nanosheets as nanoscopic support materials for the transition-metal NPs will dramatically improve their functionalities in heterogeneous catalysis. Recently, two-dimensional nanosheet of exfoliated layered double hydroxide (LDH) has emerged as a new type of solid support to immobilize the diverse metal NPs because of the large metal hydroxide area, good biochemical stability, and highly charged positive potential of 1- to 2-nm thick LDH layers. LDHs consist of a continuous stack of positively charged metal hydroxide layers with counter anions and water molecules placed in interlayer spaces.

  1. Drug delivery system for an anticancer agent, chlorogenate-Zn/Al-layered double hydroxide nanohybrid synthesised using direct co-precipitation and ion exchange methods

    Science.gov (United States)

    Barahuie, Farahnaz; Hussein, Mohd Zobir; Arulselvan, Palanisamy; Fakurazi, Sharida; Zainal, Zulkarnain

    2014-09-01

    A nano-structured drug-inorganic clay hybrid involving an active anticancer compound, which is chlorogenic acid (CA) intercalated into Zn/Al-layered double hydroxide, has been assembled via ion-exchange and co-precipitation methods to form a nanohybrid CZAE (a chlorogenic acid-Zn/Al nanohybrid synthesised using an ion-exchange method) and CZAC (a chlorogenic acid-Zn/Al nanohybrid synthesised using a direct method), respectively. The X-ray diffraction (XRD) results confirmed that the CA-LDH had a hybrid structure in which the anionic chlorogenate is arranged between the interlayers as a horizontal monolayer at 90 and 20° angles from the x axis for CZAE and CZAC, respectively. Both nanohybrids have the properties of mesoporous materials. The high loading percentage of chlorogenic acid (approximately 43.2% for CZAE and 45.3% for CZAC) with basal spacings of 11.7 and 12.6 Å for CZAE and CZAC, respectively, corroborates the successful intercalation of chlorogenic acid into the interlayer gallery of layered double hydroxides. Free chlorogenic acid and the synthesised nanocomposites (CZAE, CZAC) were assessed for their cytotoxicity against various cancer cells. The Fourier transform infrared data supported the formation of both nanohybrids, and a thermal analysis showed that the nanohybrids are more thermally stable than their counterparts. The chlorogenate shows a sustained release, and the release rate of chlorogenate from CZAE and CZAC nanohybrids at pH 7.4 is remarkably lower than that at pH 4.8 due to their different release mechanisms. The release rate of chlorogenate from both nanohybrids can be described as pseudo-second order. The present investigation revealed the potential of the nanohybrids to enhance the in vitro anti-tumour effect of chlorogenic acid in liver and lung cancer cells in vitro.

  2. Self-healing Li-Al layered double hydroxide conversion coating modified with aspartic acid for 6N01 Al alloy

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Caixia; Luo, Xiaohu; Pan, Xinyu; Liao, Liying; Wu, Xiaosong; Liu, Yali, E-mail: yaliliu@hnu.edu.cn

    2017-02-01

    Highlights: • A self-healing chrome-free Li-Al layered double hydroxide conversion coating modified with Aspartic acid was prepared. • One-step conversion coating formed by simple immersion in a conversion solution for a short time and a low temperature. • The conversion coating had excellent corrosion resistance. • The possible mechanism via exchange/self-assembly of the conversion coating was proposed in this paper. - Abstract: A self-healing Li-Al layered double hydroxide conversion coating (LCC) modified with aspartic acid (ALCC) was prepared on 6N01 Al alloy for corrosion protection. Scanning electron microscopy (SEM) showed that a compact thin film has been successfully formed on the alloy. X-ray diffraction (XRD) and FT-IR spectra proved that species of aspartic acid anions were successfully intercalated into LCC. Potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and neutral salt spray (NSS) testing showed that the resultant ALCC could provide effective corrosion protection for the Al alloy. During immersion of the ALCC-coated alloy in 3.5% NaCl solution, new film was formed in the area of artificially introduced scratch, indicating its self-healing capability. XPS results demonstrated that Cl- anions exchange partial Asp anions according to the change content of element on conversion coating. From the above results, the possible mechanism via exchange/self-assembly was proposed to illustrate the phenomenon of self-healing.

  3. Study of 2,4-dichlorophenoxyacetic acid (2,4-D) removal by Cu-Fe-layered double hydroxide from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Nejati, Kamellia, E-mail: k_nejati@pnu.ac.ir; Davary, Soheila; Saati, Marziye

    2013-09-01

    The hydrotalcite-like compound of Cu-Fe-layered double hydroxide was studied as a potential adsorbent of herbicide 2,4-dichlorophenoxyacetic acid (2,4-D). The nanoparticles of Cu-Fe layered double hydroxide were prepared by Cu/Fe molar ratio of 2:1 using a coprecipitation method at pH 8.5 and characterized by the X-ray powder diffraction (XRD), the Fourier transform infrared spectroscopy (FT-IR), the thermal gravimetric analysis (TGA) and the elemental analysis. The size and morphology of nanoparticles were examined by the transmission electron microscopy (TEM). The adsorption experiments on LDH, on the other hand, were conducted in three different procedures, namely, time-dependent, pH-dependent and temperature-dependent. Characterization of the adsorption products by the XRD method indicates that the intercalation of 2,4-D between the LDH layers has not occurred and the surface adsorption had taken place. The adsorption kinetic was tested for pseudo-first-order, pseudo-second-order, Elovich and Intra-particle diffusion kinetic models and the rate constants were calculated. The equilibrium adsorption data were described by Langmuir and Freundlich equations. It was observed that, the Langmuir isotherm slightly better fitted to the experimental data rather than that of Freundlich. In the adsorption experiments, the Gibbs free energy values, ΔG°, the enthalpy, ΔH°, and the entropy, ΔS° were also determined.

  4. Anion-exchange membranes derived from quaternized polysulfone and exfoliated layered double hydroxide for fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Wan; Liang, Na; Peng, Pai; Qu, Rong; Chen, Dongzhi; Zhang, Hongwei, E-mail: hanqiujiang@163.com

    2017-02-15

    Layered double hydroxides (LDH) are prepared by controlling urea assisted homogeneous precipitation conditions. Morphology and crystallinity of LDHs are confirmed by X-ray diffraction and scanning electron microscope. After LDHs are incorporated into quaternized polysulfone membranes, transmission electron microscope is used to observe the exfoliated morphology of LDH sheets in the membranes. The properties of the nanocomposite membranes, including water uptake, swelling ratio, mechanical property and ionic conductivity are investigated. The nanocomposite membrane containing 5% LDH sheets shows more balanced performances, exhibiting an ionic conductivity of 2.36×10{sup −2} S cm{sup −1} at 60 °C. - Graphical abstract: Anion-exchange membrane based on quaternized polysulfone and exfoliated layered double hydroxide is optically transparent and has good ionic properties.

  5. Synthesis and carbon dioxide sorption of layered double hydroxide/silica foam nanocomposites with hierarchical mesostructure

    KAUST Repository

    Fu, Liling

    2014-03-05

    Layered double hydroxides (LDHs) with a hierarchical mesostructure are successfully synthesized on mesoporous silica foams by simple impregnation and hydrothermal treatment. The as-synthesized LDH/silica foam nanocomposites show well-defined mesostructures with high surface areas, large pore volumes, and mesopores of 6-7 nm. The nanocomposites act as carbon dioxide (CO2) sorbents under simulated flue gas conditions. They also exhibit significantly enhanced CO2 capacities under high-pressure conditions and high CO2/N2 and CO2/CH4 selectivities. Respect the hierarchy: Hierarchical mesoporous layered double hydroxide (LDH) nanocomposites with high surface areas and large pore volumes are synthesized by controlled hydrothermal growth of LDH precursors on a mesoporous silica foam. The as-synthesized nanocomposites exhibit a significantly enhanced capacity and selectivity towards carbon dioxide, making them very promising candidates for carbon dioxide (CO2) separation applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Functionalized layered double hydroxide-based epoxy nanocomposites with improved flame retardancy and mechanical properties

    OpenAIRE

    Ehsan Naderi Kalali; Xin Wanga; De-Yi Wang

    2015-01-01

    Functionalized layered double hydroxides (LDHs) based on a multi-modifier system composed of hydroxypropyl-sulfobutyl-beta-cyclodextrin sodium (sCD), dodecylbenzenesulfonate (DBS) and taurine (T) have been designed and fabricated in this paper, aiming at developing high performance fire retardant epoxy nanocomposites. In this multi-modifier system, sCD was utilized to improve the char yield, DBS was used to enlarge the inter-layer distance of LDH and T was used to enhance the interaction betw...

  7. Mixed oxides obtained from Co and Mn containing layered double hydroxides: Preparation, characterization, and catalytic properties

    Czech Academy of Sciences Publication Activity Database

    Kovanda, F.; Rojka, T.; Dobešová, J.; Machovič, V.; Bezdička, Petr; Obalová, L.; Jirátová, Květa; Grygar, Tomáš

    2006-01-01

    Roč. 179, č. 3 (2006), s. 812-823 ISSN 0022-4596 R&D Projects: GA ČR(CZ) GA104/04/2116; GA ČR(CZ) GA106/05/0366 Institutional research plan: CEZ:AV0Z40320502; CEZ:AV0Z40720504 Keywords : layered double hydroxides * hydrotalcite-like compounds * thermal decomposition Subject RIV: CA - Inorganic Chemistry Impact factor: 2.107, year: 2006

  8. Magnetic behavior of Mg-Al-Zn-Fe mixed oxides from precursors layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Oliva, M.I., E-mail: marcosivanoliva@gmail.com [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, M. Allende y H. de la Torre Ciudad Universitaria, 5000 Cordoba (Argentina); IFFAM AF (CONICET - FaMAF UNC), M. Allende y H. de la Torre Ciudad Universitaria, 5000 Cordoba (Argentina); Heredia, A. [CITeQ - Facultad R. Cordoba, Universidad Tecnologica Nacional Maestro Lopez esq. Cruz Roja Argentina, CP 5016 Cordoba (Argentina); Zandalazini, C.I. [Centro Laser de Ciencias Moleculares. INFIQC-FCQ-Grupo de Ciencia de Materiales-FaMAF-Universidad Nacional de Cordoba, Ciudad Universitaria, CP5000 Cordoba, Argentina CONICET (Argentina); Crivello, M. [CITeQ - Facultad R. Cordoba, Universidad Tecnologica Nacional Maestro Lopez esq. Cruz Roja Argentina, CP 5016 Cordoba (Argentina); Corchero, E. [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, M. Allende y H. de la Torre Ciudad Universitaria, 5000 Cordoba (Argentina)

    2012-08-15

    Mixed oxides of Mg-Al-Zn-Fe were obtained by calcination of layered double hydroxides (LDH) prepared by coprecipitation reaction with hydrothermal treatment. The structural characterization of precursors and oxides was carried out by X rays diffraction, showing increases of ZnO phase with the increase of the zinc content. Magnetic behavior was studied by vibrating sample magnetometer (VSM) and by a superconducting quantum interference device (SQUID) showing both paramagnetic and super paramagnetic behavior depending on both particles size and composition.

  9. Evaluation of layered zinc hydroxide nitrate and zinc/nickel double hydroxide salts in the removal of chromate ions from solutions

    Energy Technology Data Exchange (ETDEWEB)

    Bortolaz de Oliveira, Henrique; Wypych, Fernando, E-mail: wypych@ufpr.br

    2016-11-15

    Layered zinc hydroxide nitrate (ZnHN) and Zn/Ni layered double hydroxide salts were synthesized and used to remove chromate ions from solutions at pH 8.0. The materials were characterized by many instrumental techniques before and after chromate ion removal. ZnHN decomposed after contact with the chromate solution, whereas the layered structure of Zn/Ni hydroxide nitrate (Zn/NiHN) and Zn/Ni hydroxide acetate (Zn/NiHA) remained their layers intact after the topotactic anionic exchange reaction, only changing the basal distances. ZnHN, Zn/NiHN, and Zn/NiHA removed 210.1, 144.8, and 170.1 mg of CrO{sub 4}{sup 2−}/g of material, respectively. Although the removal values obtained for Zn/NiHN and Zn/NiHA were smaller than the values predicted for the ideal formulas of the solids (194.3 and 192.4 mg of CrO{sub 4}{sup 2−}/g of material, respectively), the measured capacities were higher than the values achieved with many materials reported in the literature. Kinetic experiments showed the removal reaction was fast. To facilitate the solid/liquid separation process after chromium removal, Zn/Ni layered double hydroxide salts with magnetic supports were also synthesized, and their ability to remove chromate was evaluated. - Highlights: • Zinc hydroxide nitrate and Zn/Ni hydroxide nitrate or acetate were synthesized. • The interlayer anions were replaced by chromate anions at pH=8.0. • Only Zn/Ni hydroxide nitrate or acetate have the structure preserved after exchange. • Fast exchange reaction and high capacity of chromate removal were observed. • Magnetic materials were obtained to facilitate the solids removal the from solutions.

  10. Ciprofloxacin-intercalated Zinc Layered Hydroxides Hybrid Material: Synthesis and in Vitro Release Profiles of an Antibiotic Compound

    International Nuclear Information System (INIS)

    Mohd Zobir Hussein; Mohd Zobir Hussein; Stanslas, J.; Abdul Halim Abdullah

    2011-01-01

    The intriguing anion exchange properties of layered hydroxides salts, combined with its high layer charge density have provided strong motivations for the potential use of the inorganic layered host material in drug delivery applications. Ciprofloxacin (CFX), a wide spectrum antibiotic has been anion exchanged with nitrate of zinc hydroxide nitrate (ZHN), which belongs to the LHS family, resulted in the expansion of the basal spacing from 9.92 Amstrom of ZHN to 21.5 Angstrom of ZCFX, the obtained hybrid material. Other characterizations, such as Fourier transform infra red spectroscopy (FTIR), CHNS analysis and TGA/ DTG have further corroborated this finding. Electron microscopy study reveals the plate-like structure of the nano hybrid material. The in vitro release of CFX was performed in phosphate saline buffer at pH 7.4 and it behaves in a slow and sustained release profile over a period of 72 hours. This study suggests that ZHN, which demonstrates a controlled release behavior, could be a potential host material in the drug delivery applications. (author)

  11. Hidróxidos duplos lamelares: nanopartículas inorgânicas para armazenamento e liberação de espécies de interesse biológico e terapêutico Layered double hydroxides: inorganic nanoparticles for storage and release of species of biological and therapeutic interest

    Directory of Open Access Journals (Sweden)

    Vanessa R. R. Cunha

    2010-01-01

    Full Text Available Studies about the inorganic nanoparticles applying for non-viral release of biological and therapeutic species have been intensified nowadays. This work reviews the preparation strategies and application of layered double hydroxides (LDH as carriers for storing, carrying and control delivery of intercalated species as drugs and DNA for gene therapy. LDH show low toxicity, biocompatibility, high anion exchange capacity, surface sites for functionalization, and a suitable equilibrium between chemical stability and biodegradability. LDH can increase the intercalated species stability and promote its sub-cellular uptake for biomedical purposes. Concerning the healthy field, LDH have been evaluated for clinical diagnosis as a biosensor component.

  12. Radiation induced topotactic [2 + 2] dimerisation of acrylate derivatives among the layers of a CaFe layered double hydroxide followed by IR spectroscopy

    Science.gov (United States)

    Srankó, D. F.; Canton, S.; Enghdahl, A.; Muráth, Sz.; Kukovecz, Á.; Kónya, Z.; Sipiczki, M.; Sipos, P.; Pálinkó, I.

    2013-07-01

    Various acrylates [E-phenylpropenoate, E-3(4‧-nitrophenyl)propenoate, E-3(2‧,5‧-difluorphenyl)propenoate, E-3(2‧-thienyl)propenoate, E-3(4‧-imidazolyl)propenoate or E-2,3-dimethylpropenoate] were successfully intercalated into Ca(II)Fe(III) layered double hydroxide (CaFe-LDH) verified by a range of instrumental methods. The possible arrangements for the organic anions were suggested on the basis of basal spacing data, layer thickness and the dimensions of the quantum chemically optimised structures of the acrylate ions. Using the acrylate-CaFe-LDHs as reactant-filled nanoreactors, photoinitiated topotactic [2 + 2] cyclisation reactions followed by IR spectroscopy could be performed with many representatives [E-phenylpropenoate-, E-3(4‧-nitrophenyl)propenoate-, E-3(2‧,5‧-difluorphenyl)propenoate- or E-3(2‧-thienyl)propenoate-CaFe-LDHs] resulting in cyclobutane derivatives within the layers of the host material indicating that there were domains where the intercalated anions were in close proximity to each other and in proper arrangement for the reaction to occur.

  13. Cadmium-Aluminum Layered Double Hydroxide Microspheres for Photocatalytic CO2Reduction

    KAUST Repository

    Saliba, Daniel

    2016-03-30

    We report the synthesis of cadmium-aluminum layered double hydroxide (CdAl LDH) using the reaction-diffusion framework. As the hydroxide anions diffuse into an agar gel matrix containing the mixture of aluminum and cadmium salts at a given ratio, they react to give the LDH. The LDH self-assembles inside the pores of the gel matrix into a unique spherical-porous shaped microstructure. The internal and external morphologies of the particles are studied by electron microscopy and tomography revealing interconnected channels and a high surface area. This material is shown to exhibit a promising performance in the photoreduction of carbon dioxide using solar light. Moreover, the palladium-decorated version shows a significant improvement in its reduction potential at room temperature. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. A facile mechanochemical approach to synthesize Zn-Al layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Qu, Jun, E-mail: forsjun@whut.edu.cn [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); He, Xiaoman; Chen, Min; Huang, Pengwu [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); Zhang, Qiwu, E-mail: zhangqw@whut.edu.cn [School of Resources and Environmental Engineering, Wuhan University of Technology, Luoshi Road 122, Wuhan, Hubei 430070 (China); Liu, Xinzhong [College of Ecological Environment and Urban Construction, Fujian University of Technology, Fuzhou 350118 (China)

    2017-06-15

    In this study, a mechanochemical route to synthesize Zn-Al layered double hydroxide (LDH) was introduced, in which Zn basic carbonate and Al hydroxide were first dry milled into an activated state and then agitated in water to obtain the final products. The as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Thermogravimetry (TG) and Scanning electron microscopy (SEM). The products possessed a high crystallinity of Zn–Al LDH phase without any other impurities, proving a facile and effective preparation of Zn–Al LDH by using non-heating mechanochemical approach. - Highlights: • A non-heating mechanochemical route to synthesize Zn-Al LDH. • The products possessed high crystalline Zn-Al LDH phase. • No emission of other impurities or wastewater.

  15. High pressure measurement of the uniaxial stress of host layers on intercalants and staging transformation of intercalation compounds

    CERN Document Server

    Park, T R; Kim, H; Min, P

    2002-01-01

    A layered double-hydroxide intercalation compound was synthesized to measure the uniaxial stress the host layers exert on the intercalants. To measure the uniaxial stress, we employed the photoluminescence (PL) from the intercalated species, the Sm ion complex, as it is sensitive to the deformation of the intercalants. Of the many PL peaks the Sm ion complex produces, the one that is independent of the counter-cation environment was chosen for the measurement since the Sm ion complexes are placed under a different electrostatic environment after intercalation. The peak position of the PL was redshifted linearly with increasing hydrostatic pressure on the intercalated sample. Using this pressure-induced redshifting rate and the PL difference at ambient pressure between the pre-intercalation and the intercalated ions, we found that, in the absence of external pressure, the uniaxial stress exerted on the samarium ion complexes by the host layers was about 13.9 GPa at room temperature. Time-resolved PL data also ...

  16. Review of the synthesis of layered double hydroxides: a thermodynamic approach

    Directory of Open Access Journals (Sweden)

    Bravo-Suárez Juan J.

    2004-01-01

    Full Text Available The synthesis of layered double hydroxides (LDHs by hydrothermal-LDH reconstruction and coprecipitation methods is reviewed using a thermodynamic approach. A mixture model was used for the estimation of the thermodynamics of formation of LDHs. The synthesis and solubility of LDHs are discussed in terms of standard molar Gibbs free energy change of reaction. Data for numerous divalent and trivalent metals as well as for some monovalent and tetravalent metals that may be part of the LDH structure have been compiled. Good agreement is found between theoretical and experimental data. Diagrams and tables for the prediction of possible new LDH materials are provided.

  17. Retention of heavy metals on layered double hydroxides thin films deposited by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Vlad, A., E-mail: angela.vlad@gmail.com [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., 76900 Bucharest-Magurele (Romania); Birjega, R.; Matei, A.; Luculescu, C.; Mitu, B.; Dinescu, M. [National Institute for Lasers, Plasma and Radiation Physics, 409 Atomistilor Str., 76900 Bucharest-Magurele (Romania); Zavoianu, R.; Pavel, O.D. [University of Bucharest, Faculty of Chemistry, Department of Chemical Technology and Catalysis, 4-12 Regina Elisabeta Bd., Bucharest (Romania)

    2014-05-01

    Heavy metals are toxic and hazardous pollutants in the environment due to their nonbiodegradability and persistence, which can pose serious threats to living organisms. The ability of Mg–Al based layered double hydroxides (LDHs) thin films to retain heavy metals from aqueous solutions at different concentrations is a novel topic with prospects of attractive applications, such as detection of heavy metals. We report on the ability of a series of Mg–Al based layered double hydroxides thin films to detect Ni and Co cations in aqueous solutions. Uptake of heavy metals ions such as Ni{sup 2+}, Co{sup 2+} from aqueous solutions was studied as function of contact time at a standard metal ion concentration. The LDHs thin films were deposited using pulsed laser deposition (PLD). The different adsorption mechanisms were studied in connection with different heavy metals used as probe cations. X-ray diffraction, atomic force microscopy, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy, Fourier transform infra-red spectroscopy were the techniques used for the investigation of as deposited and after heavy metals retention thin films.

  18. A study of thermally activated Mg–Fe layered double hydroxides as potential environmental catalysts

    Directory of Open Access Journals (Sweden)

    MILICA S. HADNAĐEV-KOSTIĆ

    2010-09-01

    Full Text Available Layered double hydroxides (LDHs and mixed oxides derived after thermal decomposition of LDHs with different Mg–Fe contents were investigated. These materials were chosen because of the possibility to tailor their various properties, such as ion-exchange capability, redox and acid–base and surface area. Layered double hydroxides, [Mg1-xFex(OH2](CO3x/2×mH2O (where x presents the content of trivalent ions, x = M(III/(M(II + M(III were synthesized using the low supersaturation precipitation method. The influence of different Mg/Fe ratios on the structure and surface properties of the LDH and derived mixed oxides was investigated in correlation to their catalytic properties in the chosen test reaction (Fischer–Tropsch synthesis. It was determined that the presence of active sites in the mixed oxides is influenced by the structural properties of the initial LDH and by the presence of additional Fe phases. Furthermore, a synthesis outside the optimal range for the synthesis of single phase LDHs leads to the formation of metastable, multiphase systems with specific characteristics and active sites.

  19. Chloride adsorption by calcined layered double hydroxides in hardened Portland cement paste

    KAUST Repository

    Yoon, Seyoon

    2014-06-01

    This study investigated the feasibility of using calcined layered double hydroxides (CLDHs) to prevent chloride-induced deterioration in reinforced concrete. CLDHs not only adsorbed chloride ions in aqueous solution with a memory effect but also had a much higher binding capacity than the original layered double hydroxides (LDHs) in the cement matrix. We investigated this adsorption in hardened cement paste in batch cultures to determine adsorption isotherms. The measured and theoretical binding capacities (153 mg g -1 and 257 mg g-1, respectively) of the CLDHs were comparable to the theoretical capacity of Friedel\\'s salt (2 mol mol-1 or 121 mg g-1), which belongs to the LDH family among cementitious phases. We simulated chloride adsorption by CLDHs through the cement matrix using the Fickian model and compared the simulation result to the X-ray fluorescence (XRF) chlorine map. Based on our results, it is proposed that the adsorption process is governed by the chloride transport through the cement matrix; this process differs from that in an aqueous solution. X-ray diffraction (XRD) analysis showed that the CLDH rebuilds the layered structure in a cementitious environment, thereby demonstrating the feasibility of applying CLDHs to the cement and concrete industries. © 2014 Published by Elsevier B.V. All rights reserved.

  20. Preparation and properties of blends composed of lignosulfonated layered double hydroxide/plasticized starch and thermoplastics.

    Science.gov (United States)

    Privas, Edwige; Leroux, Fabrice; Navard, Patrick

    2013-07-01

    Layered double hydroxide prepared with lignosulfonate (LDH/LS) can be easily dispersed down to the nanometric scale in thermoplastic starch, at concentration of 1 up to 4 wt% of LDH/LS. They can thus be used as a bio-based reinforcing agent of thermoplastic starch. Incorporation of LDH/LS in starch must be done using LDH/LS slurry instead of powder on order to avoid secondary particles aggregation, the water of the paste being used as the starch plasticizer. This reinforced starch was used for preparing a starch-polyolefine composite. LDH/LS-starch nanocomposites were mixed in a random terpolymer of ethylene, butyl acrylate (6%) and maleic anhydride (3%) at concentrations of 20 wt% and 40 wt%. With a 20% loading of (1 wt% LDH/LS in thermoplastic starch), the ternary copolymer is partially bio-based while keeping nearly its original processability and mechanical properties and improving oxygen barrier properties. The use of layered double hydroxides is also removing most odours linked to the lignin phase. Copyright © 2013 Elsevier Ltd. All rights reserved.

  1. Mg/Al ordering in layered double hydroxides revealed by multinuclear NMR spectroscopy.

    Science.gov (United States)

    Sideris, Paul J; Nielsen, Ulla Gro; Gan, Zhehong; Grey, Clare P

    2008-07-04

    The anion-exchange ability of layered double hydroxides (LDHs) has been exploited to create materials for use in catalysis, drug delivery, and environmental remediation. The specific cation arrangements in the hydroxide layers of hydrotalcite-like LDHs, of general formula Mg2+(1-x)Al3+(x)OH2(Anion(n-)(x/n)).yH2O, have, however, remained elusive, and their elucidation could enhance the functional optimization of these materials. We applied rapid (60 kilohertz) magic angle spinning (MAS) to obtain high-resolution hydrogen-1 nuclear magnetic resonance (1H NMR) spectra and characterize the magnesium and aluminum distribution. These data, in combination with 1H-27Al double-resonance and 25Mg triple-quantum MAS NMR data, show that the cations are fully ordered for magnesium:aluminum ratios of 2:1 and that at lower aluminum content, a nonrandom distribution of cations persists, with no Al3+-Al3+ close contacts. The application of rapid MAS NMR methods to investigate proton distributions in a wide range of materials is readily envisaged.

  2. Anionic clay as the drug delivery vehicle: tumor targeting function of layered double hydroxide-methotrexate nanohybrid in C33A orthotopic cervical cancer model

    Directory of Open Access Journals (Sweden)

    Choi G

    2016-01-01

    Full Text Available Goeun Choi,1 Huiyan Piao,1 Zeid A Alothman,2 Ajayan Vinu,3 Chae-Ok Yun,4 Jin-Ho Choy1 1Center for Intelligent Nano-Bio Materials, Department of Chemistry and Nano Science, Ewha Womans University, Seoul, Korea; 2Advanced Materials Research Chair, Chemistry Department, College of Science, King Saud University, Riyadh, Saudi Arabia; 3Future Industries Institute, University of South Australia, Mawson Lakes, SA, Australia; 4Department of Bioengineering, College of Engineering, Hanyang University, Seoul, Korea Abstract: Methotrexate (MTX, an anticancer agent, was successfully intercalated into the anionic clay, layered double hydroxides to form a new nanohybrid drug. The coprecipitation and subsequent hydrothermal method were used to prepare chemically, structurally, and morphologically well-defined two-dimensional drug-clay nanohybrid. The resulting two-dimensional drug-clay nanohybrid showed excellent colloidal stability not only in deionized water but also in an electrolyte solution of Dulbecco’s Modified Eagle’s Medium with 10% fetal bovine serum, in which the average particle size in colloid and the polydispersity index were determined to be around 100 and 0.250 nm, respectively. The targeting property of the nanohybrid drug was confirmed by evaluating the tumor-to-blood and tumor-to-liver ratios of the MTX with anionic clay carrier, and these ratios were compared to those of free MTX in the C33A orthotopic cervical cancer model. The biodistribution studies indicated that the mice treated with the former showed 3.5-fold higher tumor-to-liver ratio and fivefold higher tumor-to-blood ratio of MTX than those treated with the latter at 30 minutes postinjection. Keywords: anionic clay, biodistribution, cervical cancer, colloidal stability, layered double hydroxide, methotrexate 

  3. Preparation of hydroxide ion conductive KOH–layered double hydroxide electrolytes for an all-solid-state iron–air secondary battery

    Directory of Open Access Journals (Sweden)

    Taku Tsuneishi

    2014-06-01

    Full Text Available Anion conductive solid electrolytes based on Mg–Al layered double hydroxide (LDH were prepared for application in an all-solid-state Fe–air battery. The ionic conductivity and the conducting ion species were evaluated from impedance and electromotive force measurements. The ion conductivity of LDH was markedly enhanced upon addition of KOH. The electromotive force in a water vapor concentration cell was similar to that of an anion-conducting polymer membrane. The KOH–LDH obtained was used as a hydroxide ion conductive electrolyte for all-solid-state Fe–air batteries. The cell performance of the Fe–air batteries was examined using a mixture of KOH–LDH and iron-oxide-supported carbon as the negative electrode.

  4. Synthesis of nanocomposite coating based on TiO2/ZnAl layer double hydroxides

    International Nuclear Information System (INIS)

    Jovanov, V.; Rudic, O.; Ranogajec, J.; Fidanchevska, E.

    2017-01-01

    The aim of this investigation was the synthesis of nanocomposite coatings based on Zn-Al layered double hydroxides (Zn-Al LDH) and TiO2. The Zn-Al LDH material, which acted as the catalyst support of the active TiO2 component (in the content of 3 and 10 wt. %), was synthesized by a low super saturation co-precipitation method. The interaction between the Zn-Al LDH and the active TiO2 component was accomplished by using vacuum evaporation prior to the mechanical activation and only by mechanical activation. The final suspension based on Zn-Al LDH and 10wt. % TiO2, impregnated only by mechanical activation, showed the optimal characteristics from the aspect of particle size distribution and XRD analysis. These properties had a positive effect on the functional properties of the coatings (photocatalytic activity and self-cleaning efficiency) after the water rinsing procedure. [es

  5. Poly I-lactide-layered double hydroxide nanocomposites via in situ polymerization of I-lactide

    DEFF Research Database (Denmark)

    Katiyar, Vimal; Gerds, N.; Koch, C.B.

    2010-01-01

    The use of clay nanofillers offers a potential route to improved barrier properties in polylactide films. Magnesium–aluminium layered double hydroxides (LDHs) are interesting in this respect and we therefore explored synthesis of PLA-LDH nanocomposites by ring-opening polymerization. This method...... is attractive because it should ensure good dispersion of LDH in the polymer. The effect of adding either LDH carbonate (LDH-CO3) or laurate-modified LDH (LDH-C12) was investigated. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy revealed that exfoliated nanocomposites were...... weight was significantly reduced when in-situ polymerization was conducted in the presence of the LDHs and we suggest that chain termination via LDH surface hydroxyl groups and/or metal-catalyzed degradation could be responsible....

  6. Layered-Double-Hydroxide Nanosheets as Efficient Visible-Light-Driven Photocatalysts for Dinitrogen Fixation.

    Science.gov (United States)

    Zhao, Yufei; Zhao, Yunxuan; Waterhouse, Geoffrey I N; Zheng, Lirong; Cao, Xingzong; Teng, Fei; Wu, Li-Zhu; Tung, Chen-Ho; O'Hare, Dermot; Zhang, Tierui

    2017-11-01

    Semiconductor photocatalysis attracts widespread interest in water splitting, CO 2 reduction, and N 2 fixation. N 2 reduction to NH 3 is essential to the chemical industry and to the Earth's nitrogen cycle. Industrially, NH 3 is synthesized by the Haber-Bosch process under extreme conditions (400-500 °C, 200-250 bar), stimulating research into the development of sustainable technologies for NH 3 production. Herein, this study demonstrates that ultrathin layered-double-hydroxide (LDH) photocatalysts, in particular CuCr-LDH nanosheets, possess remarkable photocatalytic activity for the photoreduction of N 2 to NH 3 in water at 25 °C under visible-light irradiation. The excellent activity can be attributed to the severely distorted structure and compressive strain in the LDH nanosheets, which significantly enhances N 2 chemisorption and thereby promotes NH 3 formation. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Silver Orthophosphate Immobilized on Flaky Layered Double Hydroxides as the Visible-Light-Driven Photocatalysts

    Directory of Open Access Journals (Sweden)

    Xianlu Cui

    2012-01-01

    Full Text Available Flaky layered double hydroxide (FLDH was prepared by the reconstruction of its oxide in alkali solution. The composites with FLDH/Ag3PO4 mass ratios at 1.6 : 1 and 3 : 1 were fabricated by the coprecipitation method. The powders were characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscope, and UV-vis diffuse reflectance spectroscopy. The results indicated that the well-distributed Ag3PO4 in a fine crystallite size was formed on the surface of FLDH. The photocatalytic activities of the Ag3PO4 immobilized on FLDH were significantly enhanced for the degradation of acid red G under visible light irradiation compared to bare Ag3PO4. The composite with the FLDH/Ag3PO4 mass ratio of 3 : 1 showed a higher photocatalytic efficiency.

  8. Synthesis of Co–Al layered double hydroxide nanoclusters as reduction nanocatalyst in aqueous media

    Directory of Open Access Journals (Sweden)

    Daisuke Kino

    2017-12-01

    Full Text Available Layered double hydroxides (LDHs have attracted attention as green materials due to their catalytic ability in benign aqueous solvents. We here demonstrate the synthesis of colloidal Co–Al LDH nanoclusters with an average size of <10 nm via a facile liquid-phase reaction for the enhancement of the catalytic activity. To the best of our knowledge, the present LDH is the smallest Co–Al LDH with an extremely large surface area and stability in an aqueous solvent, forming a stable and concentrated colloidal solution as high as 40 g/L. We investigated the formation mechanism, and the catalytic activity of Co–Al LDH nanoclusters. The Co–Al LDH nanoclusters showed 47 times higher rate of the reduction of dye molecules in the aqueous media than standard Co–Al LDH particles with a micrometer size. LDH nanoclusters demonstrated here are promising green nanocatalysts for the aqueous reaction processes.

  9. Fatigue Properties of Layered Double Hydroxides Modified Asphalt and Its Mixture

    Directory of Open Access Journals (Sweden)

    Xing Liu

    2014-01-01

    Full Text Available This study investigated the influence of layered double hydroxides (LDHs on the fatigue properties of asphalt mixture. In this paper, different aging levels (thin film oven test (TFOT and ultraviolet radiation aging (UV aging for short of bitumen modified with various mass ratios of the LDHs were investigated. The TFOT and UV aging process were used to simulate short-term field thermal-oxidative aging and long-term field light UV aging of bitumen, respectively. The influences of LDHs on the fatigue properties of LDHs were evaluated by dynamic shear rheometer (DSR and indirect tensile fatigue test. Results indicated that the introduction of LDHs could change the fatigue properties of bitumen under a stress control mode. The mixture with modified bitumen showed better fatigue resistance than the mixture with base bitumen. The results illustrated that the LDHs would be alternative modifiers used in the bitumen to improve the lifetime of asphalt pavements.

  10. Interactions Between Biological Cells and Layered Double Hydroxides: Towards Functional Materials.

    Science.gov (United States)

    Forano, Claude; Bruna, Felipe; Mousty, Christine; Prevot, Vanessa

    2018-03-08

    This review highlights the current research on the interactions between biological cells and Layered Double Hydroxides (LDH). The as-prepared biohybrid materials appear extremely attractive in diverse fields of application relating to health care, environment and energy production. We describe how thanks to the main features of biological cells and LDH layers, various strategies of assemblies can be carried out for constructing smart biofunctional materials. The interactions between the two components are described with a peculiar attention to the adsorption, biocompatibilization, LDH layer internalization, antifouling and antimicrobial properties. The most significant achievements including authors' results, involving biological cells and LDH assemblies in waste water treatment, bioremediation and bioenergy generation are specifically addressed. © 2018 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Structural characterisation of aluminium layered double hydroxides by (27)Al solid-state NMR.

    Science.gov (United States)

    Vyalikh, Anastasia; Massiot, Dominique; Scheler, Ulrich

    2009-09-01

    (27)Al solid-state NMR has been applied to study the local structure of pristine and chemically modified aluminium layered double hydroxides (LDH). The pristine LDH only shows six-fold coordinated, octahedral, aluminium, while the calcined and subsequently surfactant treated LDH sample shows a significant fraction of four-fold coordinated tetrahedral aluminium. The co-existence of two types of octahedral sites with different quadrupolar parameters is clearly observed in both samples. Quadrupolar coupling constants and isotropic chemical shifts have been measured from the (27)Al triple-quantum MAS NMR allowing to fit the (27)Al MAS spectra and quantify the different species in the samples. The quantitative analysis reveals that 30% of the aluminium is in four-fold coordination in the surfactant-modified LDH. We show that this chemical modification retains the two types of AlO(6) sites with a decreased intensity of the site showing the lowest quadrupolar coupling constant.

  12. Tunable Properties of Exfoliated Polyvinylalcohol Nanocomposites by In Situ Coprecipitation of Layered Double Hydroxides

    Science.gov (United States)

    Liu, Jiajia; Yuen, Richard K. K.; Hu, Yuan

    2017-10-01

    Poly(vinyl alcohol) (PVA) nanocomposites were prepared by a “one step” method based on the coprecipitation of layered double hydroxide (LDH) nanosheets in the polymer aqueous solution. The morphology, fire resistance properties, mechanical and optical properties of the PVA/LDH nanocomposites were studied. The LDH nanosheets were homogeneously dispersed in the PVA matrix as indicated by X-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) characterization. Meanwhile, the peak of heat release rate (pHRR) and total heat release (THR) were decreased by 58% and 28%, respectively. Storage modulus at 30 °C was increased, and the transmittance of more than 90% at the visible region was obtained upon addition of 5 wt% LDH.

  13. Layered double hydroxide materials coated carbon electrode: New challenge to future electrochemical power devices

    Science.gov (United States)

    Djebbi, Mohamed Amine; Braiek, Mohamed; Namour, Philippe; Ben Haj Amara, Abdesslem; Jaffrezic-Renault, Nicole

    2016-11-01

    Layered double hydroxides (LDHs) have been widely used in the past years due to their unique physicochemical properties and promising applications in electroanalytical chemistry. The present paper is going to focus exclusively on magnesium-aluminum and zinc-aluminum layered double hydroxides (MgAl & ZnAl LDHs) in order to investigate the property and structure of active cation sites located within the layer structure. The MgAl and ZnAl LDH nanosheets were prepared by the constant pH co-precipitation method and uniformly supported on carbon-based electrode materials to fabricate an LDH electrode. Characterization by powder x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy revealed the LDH form and well-crystallized materials. Wetting surface properties (hydrophilicity and hydrophobicity) of both prepared LDHs were recorded by contact angle measurement show hydrophilic character and basic property. The electrochemical performance of these hybrid materials was investigated by mainly cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry techniques to identify the oxidation/reduction processes at the electrode/electrolyte interface and the effect of the divalent metal cations in total reactivity. The hierarchy of the modified electrode proves that the electronic conductivity of the bulk material is considerably dependent on the divalent cation and affects the limiting parameter of the overall redox process. However, MgAl LDH shows better performance than ZnAl LDH, due to the presence of magnesium cations in the layers. Following the structural, morphological and electrochemical behavior studies of both synthesized LDHs, the prepared LDH modified electrodes were tested through microbial fuel cell configuration, revealing a remarkable, potential new pathway for high-performance and cost-effective electrode use in electrochemical power devices.

  14. Mixed oxides derived from layered double hydroxides as novel catalysts for phenol photodegradation

    Science.gov (United States)

    Puscasu, C. M.; Carja, G.; Mureseanu, M.; Zaharia, C.

    2017-08-01

    The removal of organic pollutants is nowadays a very challenging aspect of the environmental research. There are strong interests to develop novel semiconducting photocatalysts able to efficiently promote advanced oxidation reactions. The development of photocatalysts based on the mixtures of mixed oxides derived from layered double hydroxides (LDHs) - a family of naturally occurring anionic clays - might offer novel environmental-friendly solutions for the cost effective removal of organic pollutants. This work presents ZnO/ZnAl2O4, ZnO/Zn2TiO4 and ZnO/ZnCr2O4 as novel photocatalytic formulations for phenol degradation under UV irradiation. They were obtained by the controlled thermal treatment of the layered double hydroxides matrices (LDHs), as precursors materials, type ZnM-LDH (M = Al3+, Cr3+ or Ti4+). The LDHs were synthesized by the co-precipitation method at a constant pH. Controlled calcination at 650°C gives rise to solutions of mixed metal oxides. The structural and nanoarchitectonics characteristics of the studied catalysts were described by: XRD, SEM/TEM and TG/DTG techniques. Results show that in the photocatalytic process of the phenol degradation from aqueous solutions, ZnO/ZnCr2O4 and ZnO/ZnAl2O4 showed the best performance degrading ∼98% of phenol after 3.5 hs and 5 hs, respectively; while ZnO/Zn2TiO4 has degraded almost 80 % after 7.5 hs of UV irradiation. These results open new opportunities in the development of new cost effective photoresponsive formulations able to facilitate the photo-degradation of the organic pollution as “green” solution for removal of dangerous pollutants.

  15. Enhanced electrochemical performance of CoAl-layered double hydroxide nanosheet arrays coated by platinum films

    International Nuclear Information System (INIS)

    Cheng, J.P.; Fang, J.H.; Li, M.; Zhang, W.F.; Liu, F.; Zhang, X.B.

    2013-01-01

    Graphical abstract: Schematic illustration for the electron transport between the current collector and the active CoAl LDH arrays, where the yellow arrows indicate the high resistance of CoAl LDH, while the green arrows present the high conductivity of Pt films on LDH. -- Highlights: •CoAl layered double hydroxide nanosheet arrays are synthesized by hydrothermal method. •Pt films coated on surface of CoAl nanosheets facilitate fast electron transport. •CoAl LDH nanosheets coated with Pt film for 5 min have an excellent performance. -- Abstract: Three-dimensional network of cobalt and aluminum layered double hydroxide (LDH) nanosheets was synthesized on nickel foam by a simple hydrothermal method. The CoAl-LDH nonosheets were subsequently coated by ion sputtering with thin layers of Pt films to facilitate fast electron transport between current collector and the CoAl-LDH active materials. The optimal thickness of the Pt film acquiring the best performance was identified by applying various sputtering time in controlled experiments. The supercapacitor built by the CoAl-LDH nanosheets coated with Pt film sputtered for 5 min has a high specific capacitance (734.4 F g −1 at 3 A g −1 ), excellent rate capability as well as cycling stability. Moreover, it showed a long life of 77% retention after 6000 cycles and its general morphology was preserved after the test. The synergetic affect of conductive layer of Pt films and CoAl-LDH on the improvement of electrochemical properties was discussed and this would provide a useful clue in designing novel and effective electrode materials for supercapacitors

  16. Synthesis of Zn/Co/Fe-layered double hydroxide nanowires with controllable morphology in a water-in-oil microemulsion

    International Nuclear Information System (INIS)

    Wu Hongyu; Jiao Qingze; Zhao Yun; Huang Silu; Li Xuefei; Liu Hongbo; Zhou Mingji

    2010-01-01

    The Zn/Co/Fe-layered double hydroxide nanowires were synthesized via a reverse microemulsion method by using cetyltrimethyl ammonium bromide (CTAB) /n-hexane/n-hexanol/water as Soft-Template. ZnSO 4 , CoSO 4 , Fe 2 (SO 4 ) 3 and urea were used as raw materials. The influence of reaction temperature, time, urea concentration and Cn (molar ratio of cetyltrimethyl ammonium bromide to water) on the structure and morphology of Zn/Co/Fe-layered double hydroxides was investigated. The samples were characterized using Transmission Electron Microscopy (TEM), Inductively Coupled Plasma (ICP), X-ray Diffraction (XRD) and Infrared Absorption Spectrum (IR). The results indicate that higher temperature is beneficial to the formation of layered double hydroxides, but particles apart from nanowires could be produced if temperature is up to 120 deg. C. By varying the temperature, reaction time, urea concentration and Cn, we got the optimum conditions of synthesizing uniform Zn/Co/Fe-layered double hydroxide nanowires: 100 deg. C, more than 12 h, Cn: 30-33, urea concentration: 0.3 M.

  17. How the Method of Synthesis Governs the Local and Global Structure of Zinc Aluminum Layered Double Hydroxides

    DEFF Research Database (Denmark)

    Puschparaj, Suraj S. C.; Forano, Claude; Prevot, Vanessa

    2015-01-01

    Seven zinc aluminum layered double hydroxides (ZnAl LDHs), [Zn1-xAlx (OH)2Ax,nH2O] A = NO3-, Cl- or CO32-, prepared by the urea and co-precipitation synthesis methods were investigated to determine how synthesis parameters (pH, metal ion concentration and post synthesis treatment) affect the local...

  18. Synthesis of Zn/Co/Fe-layered double hydroxide nanowires with controllable morphology in a water-in-oil microemulsion

    Energy Technology Data Exchange (ETDEWEB)

    Wu Hongyu; Jiao Qingze [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing, 100081 (China); Zhao Yun, E-mail: zhaoyun@bit.edu.cn [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing, 100081 (China); Huang Silu; Li Xuefei; Liu Hongbo; Zhou Mingji [School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing, 100081 (China)

    2010-02-15

    The Zn/Co/Fe-layered double hydroxide nanowires were synthesized via a reverse microemulsion method by using cetyltrimethyl ammonium bromide (CTAB) /n-hexane/n-hexanol/water as Soft-Template. ZnSO{sub 4}, CoSO{sub 4}, Fe{sub 2}(SO{sub 4}){sub 3} and urea were used as raw materials. The influence of reaction temperature, time, urea concentration and Cn (molar ratio of cetyltrimethyl ammonium bromide to water) on the structure and morphology of Zn/Co/Fe-layered double hydroxides was investigated. The samples were characterized using Transmission Electron Microscopy (TEM), Inductively Coupled Plasma (ICP), X-ray Diffraction (XRD) and Infrared Absorption Spectrum (IR). The results indicate that higher temperature is beneficial to the formation of layered double hydroxides, but particles apart from nanowires could be produced if temperature is up to 120 deg. C. By varying the temperature, reaction time, urea concentration and Cn, we got the optimum conditions of synthesizing uniform Zn/Co/Fe-layered double hydroxide nanowires: 100 deg. C, more than 12 h, Cn: 30-33, urea concentration: 0.3 M.

  19. Structural Differentiation between Layered Single (Ni) and Double Metal Hydroxides (Ni–Al LDHs) Using Wavelet Transformation

    Energy Technology Data Exchange (ETDEWEB)

    Siebecker, Matthew G. [University of Delaware, Delaware Environmental Institute; Sparks, Donald L. [University of Delaware, Delaware Environmental Institute

    2017-09-07

    Layered double hydroxides (LDHs) are anionic clays important in disciplines such as environmental chemistry, geochemistry, and materials science. Developments in signal processing of extended X-ray absorption fine structure (EXAFS) data, such as wavelet transformation (WT), have been used to identify transition metals and Al present in the hydroxide sheets of LDHs. The WT plots of LDHs should be distinct from those of isostructural single metal hydroxides. However, no direct comparison of these minerals appears in the literature using WT. This work systematically analyzes a suite of Ni-rich mineral standards, including Ni–Al LDHs, single metal Ni hydroxides, and Ni-rich silicates using WT. The results illustrate that the WT plots for α-Ni(OH)2 and Ni–Al LDHs are often indistinguishable from each other, with similar two-component plots for the different mineral types. This demonstrates that the WT of the first metal shell often cannot be used to differentiate an LDH from a single metal hydroxide. Interlayer anions adsorbed to the hydroxide sheet of α-Ni(OH)2 affect the EXAFS spectra and are not visible in the FT but are clearly resolved and discrete in the WT.

  20. DOUBLE-SHELL TANK (DST) HYDROXIDE DEPLETION MODEL FOR CARBON DIOXIDE ABSORPTION

    International Nuclear Information System (INIS)

    OGDEN DM; KIRCH NW

    2007-01-01

    This document generates a supernatant hydroxide ion depletion model based on mechanistic principles. The carbon dioxide absorption mechanistic model is developed in this report. The report also benchmarks the model against historical tank supernatant hydroxide data and vapor space carbon dioxide data. A comparison of the newly generated mechanistic model with previously applied empirical hydroxide depletion equations is also performed

  1. DOUBLE SHELL TANK (DST) HYDROXIDE DEPLETION MODEL FOR CARBON DIOXIDE ABSORPTION

    Energy Technology Data Exchange (ETDEWEB)

    OGDEN DM; KIRCH NW

    2007-10-31

    This document generates a supernatant hydroxide ion depletion model based on mechanistic principles. The carbon dioxide absorption mechanistic model is developed in this report. The report also benchmarks the model against historical tank supernatant hydroxide data and vapor space carbon dioxide data. A comparison of the newly generated mechanistic model with previously applied empirical hydroxide depletion equations is also performed.

  2. Use of calcined layered double hydroxides for the removal of color and organic matter from textile effluents: kinetic, equilibrium and recycling studies

    Directory of Open Access Journals (Sweden)

    T. P. F. Teixeira

    2014-03-01

    Full Text Available This paper presents data for the synthesis and characterization of layer double hydroxides (LDH and their use for color and chemical oxygen demand (COD removal from effluents generated by a textile industry. Adsorption studies with raw and biologically treated (activated sludge textile effluent showed that the pseudo-second order model best fitted the experimental data, leading to adsorption coefficients of 39.1 and 102.9 mgCOD/gLDH for raw and treated effluents, respectively. The best conditions for color and COD removal were obtained at lower values of temperature and pH (25 °C and pH 7 and, in these conditions, an LDH dose of 10 g/L resulted in color removal efficiencies of 56% for samples of raw and 66% for samples of treated effluent. Recycling studies indicated that the reuse of thermally treated LDH led to a progressive loss in the removal efficiencies of COD and color. The reduction was more pronounced with samples of the raw textile effluent. LDH characterization performed before and after each adsorption and regeneration experiment showed that there was no intercalation of dye molecules in the interlayer region of the LDH, indicating that COD and color removal might be due to the adsorption of organic molecules onto the LDH surface.

  3. Anionic clay as the drug delivery vehicle: tumor targeting function of layered double hydroxide-methotrexate nanohybrid in C33A orthotopic cervical cancer model.

    Science.gov (United States)

    Choi, Goeun; Piao, Huiyan; Alothman, Zeid A; Vinu, Ajayan; Yun, Chae-Ok; Choy, Jin-Ho

    2016-01-01

    Methotrexate (MTX), an anticancer agent, was successfully intercalated into the anionic clay, layered double hydroxides to form a new nanohybrid drug. The coprecipitation and subsequent hydrothermal method were used to prepare chemically, structurally, and morphologically well-defined two-dimensional drug-clay nanohybrid. The resulting two-dimensional drug-clay nanohybrid showed excellent colloidal stability not only in deionized water but also in an electrolyte solution of Dulbecco's Modified Eagle's Medium with 10% fetal bovine serum, in which the average particle size in colloid and the polydispersity index were determined to be around 100 and 0.250 nm, respectively. The targeting property of the nanohybrid drug was confirmed by evaluating the tumor-to-blood and tumor-to-liver ratios of the MTX with anionic clay carrier, and these ratios were compared to those of free MTX in the C33A orthotopic cervical cancer model. The biodistribution studies indicated that the mice treated with the former showed 3.5-fold higher tumor-to-liver ratio and fivefold higher tumor-to-blood ratio of MTX than those treated with the latter at 30 minutes postinjection.

  4. 8-Hydroxypyrene-1,3,6-trisulphonate and octanesulphonate co-assembled layered double hydroxide and its controllable solid-state luminescence by hydrothermal synthesis

    Science.gov (United States)

    Dang, Sile; Yan, Dongpeng; Lu, Jun

    2012-01-01

    8-Hydroxy-pyrene-1,3,6-trisulphonate (HPTS) and octanesulphonate (OS) have been co-intercalated into the ZnAl layered double hydroxide (LDH) host by a hydrothermal co-precipitation method, with samples denoted as HPTS (x%)-OS/Zn2Al-LDH (x stands for the molar percentage content of HPTS with respect to total amount of HPTS and OS). The structure and chemical compositions of the as-prepared compounds were characterized by X-ray diffraction (XRD) and elemental analysis. The steady-state and time-decay fluorescent studies show that HPTS (2%)-OS/Zn2Al-LDH has the optimal luminous emission and the longest fluorescent lifetime. Moreover, these samples exhibit controllable dual fluorescence between the blue and green regions upon changing the interlayer HPTS content, external pH values, and host-guest interaction, illustrating that these organic-inorganic samples have potential application in the field of tunable solid luminescent materials.

  5. Layered double hydroxide materials coated carbon electrode: New challenge to future electrochemical power devices

    International Nuclear Information System (INIS)

    Djebbi, Mohamed Amine; Braiek, Mohamed; Namour, Philippe; Ben Haj Amara, Abdesslem; Jaffrezic-Renault, Nicole

    2016-01-01

    Highlights: • MgAl and ZnAl LDH nanosheets were chemically synthesized and deposited over carbon electrode materials. • Catalytic performance of both LDHs was investigated for Fe(II) reduction reaction. • Satisfactory results have been achieved with the MgAl LDH material. • MgAl and ZnAl LDH modified carbon felt were applied in MFC as an efficient anode catalyst. • The LDH-modified anode significantly increased power performance of MFC. - Abstract: Layered double hydroxides (LDHs) have been widely used in the past years due to their unique physicochemical properties and promising applications in electroanalytical chemistry. The present paper is going to focus exclusively on magnesium-aluminum and zinc-aluminum layered double hydroxides (MgAl & ZnAl LDHs) in order to investigate the property and structure of active cation sites located within the layer structure. The MgAl and ZnAl LDH nanosheets were prepared by the constant pH co-precipitation method and uniformly supported on carbon-based electrode materials to fabricate an LDH electrode. Characterization by powder x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy revealed the LDH form and well-crystallized materials. Wetting surface properties (hydrophilicity and hydrophobicity) of both prepared LDHs were recorded by contact angle measurement show hydrophilic character and basic property. The electrochemical performance of these hybrid materials was investigated by mainly cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry techniques to identify the oxidation/reduction processes at the electrode/electrolyte interface and the effect of the divalent metal cations in total reactivity. The hierarchy of the modified electrode proves that the electronic conductivity of the bulk material is considerably dependent on the divalent cation and affects the limiting parameter of the overall redox process. However

  6. Layered double hydroxide materials coated carbon electrode: New challenge to future electrochemical power devices

    Energy Technology Data Exchange (ETDEWEB)

    Djebbi, Mohamed Amine, E-mail: mohamed.djebbi@etu.univ-lyon1.fr [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Braiek, Mohamed [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Namour, Philippe [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France); Irstea, 5 rue de la Doua, 69100 Villeurbanne (France); Ben Haj Amara, Abdesslem [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Jaffrezic-Renault, Nicole [Institut des Sciences Analytiques UMR CNRS 5280, Université Claude Bernard-Lyon 1, 5 rue de la Doua, 69100 Villeurbanne (France)

    2016-11-15

    Highlights: • MgAl and ZnAl LDH nanosheets were chemically synthesized and deposited over carbon electrode materials. • Catalytic performance of both LDHs was investigated for Fe(II) reduction reaction. • Satisfactory results have been achieved with the MgAl LDH material. • MgAl and ZnAl LDH modified carbon felt were applied in MFC as an efficient anode catalyst. • The LDH-modified anode significantly increased power performance of MFC. - Abstract: Layered double hydroxides (LDHs) have been widely used in the past years due to their unique physicochemical properties and promising applications in electroanalytical chemistry. The present paper is going to focus exclusively on magnesium-aluminum and zinc-aluminum layered double hydroxides (MgAl & ZnAl LDHs) in order to investigate the property and structure of active cation sites located within the layer structure. The MgAl and ZnAl LDH nanosheets were prepared by the constant pH co-precipitation method and uniformly supported on carbon-based electrode materials to fabricate an LDH electrode. Characterization by powder x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy revealed the LDH form and well-crystallized materials. Wetting surface properties (hydrophilicity and hydrophobicity) of both prepared LDHs were recorded by contact angle measurement show hydrophilic character and basic property. The electrochemical performance of these hybrid materials was investigated by mainly cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry techniques to identify the oxidation/reduction processes at the electrode/electrolyte interface and the effect of the divalent metal cations in total reactivity. The hierarchy of the modified electrode proves that the electronic conductivity of the bulk material is considerably dependent on the divalent cation and affects the limiting parameter of the overall redox process. However

  7. The importance of proper crystal-chemical and geometrical reasoning demonstrated using layered single and double hydroxides

    International Nuclear Information System (INIS)

    Richardson, Ian G.

    2013-01-01

    The importance and utility of proper crystal-chemical and geometrical reasoning in structural studies is demonstrated through the consideration of layered single and double hydroxides. New yet fundamental information is provided and it is evident that the crystal chemistry of the double hydroxide phases is much more straightforward than is apparent from the literature. Atomistic modelling techniques and Rietveld refinement of X-ray powder diffraction data are widely used but often result in crystal structures that are not realistic, presumably because the authors neglect to check the crystal-chemical plausibility of their structure. The purpose of this paper is to reinforce the importance and utility of proper crystal-chemical and geometrical reasoning in structural studies. It is achieved by using such reasoning to generate new yet fundamental information about layered double hydroxides (LDH), a large, much-studied family of compounds. LDH phases are derived from layered single hydroxides by the substitution of a fraction (x) of the divalent cations by trivalent. Equations are derived that enable calculation of x from the a parameter of the unit cell and vice versa, which can be expected to be of widespread utility as a sanity test for extant and future structure determinations and computer simulation studies. The phase at x = 0 is shown to be an α form of divalent metal hydroxide rather than the β polymorph. Crystal-chemically sensible model structures are provided for β-Zn(OH) 2 and Ni- and Mg-based carbonate LDH phases that have any trivalent cation and any value of x, including x = 0 [i.e. for α-M(OH) 2 ·mH 2 O phases

  8. Adsorption performance of magnesium/aluminum layered double hydroxide nanoparticles for metronidazole from aqueous s

    Directory of Open Access Journals (Sweden)

    Mohammad Noori Sepehr

    2017-07-01

    Full Text Available Magnesium/aluminum layered double hydroxide (LDH nanoparticles were synthesized by hydrolyzing urea and used to remove metronidazole (MN from aqueous solution. The surface morphology images of the LDH nanoparticles showed that the adsorbent surface consisted of hexagonal nanosheets with a diameter of 200–1000 nm. The MN removal efficiency was strongly dependent on the solution pH ranging from 3 to 9. The addition of nitrate, sulfate, and carbonate did not remarkably affect MN adsorption, while hardness slightly improved MN removal efficiency. The adsorption isotherm data could be well described using the Sips equation. The analysis of kinetic data showed that the adsorption of MN onto LDH closely followed the Avrami model and that several kinetic processes may control the rate of sorption. The adsorption process was non-spontaneous and exothermic in nature. The maximum Langmuir adsorption capacity was 62.804 mg/g, demonstrating that LDH is an efficient adsorbent that can be used for the removal of MN compounds.

  9. Kinetic Evaluation of Lipid Oils Conversion to Biofuel Using Layered Double Hydroxide Doped with Triazabicyclodece Catalyst

    Science.gov (United States)

    Nato Lopez, Frank D.

    Worldwide, there is an ever increasing need for sustainable, renewable fuels that will accommodate the rapidly increasing energy demand and provide independence from fossil fuels. The search for a sustainable alternative to petroleum based fuels has been a great challenge to the scientific community; therefore, great efforts are being made to overcome the fossil fuels dependence by exploring the prominent field of biofuels (bioethanol and biodiesel). Traditional biodiesel is produced from feedstocks such as vegetable oils and animal fats by converting the triglycerides with methanol in the presence of a homogeneous catalyst to produce fatty acid methyl esters (FAMEs). However, drawbacks of this process are the undesired glycerol byproduct and post reaction processing, including separation from reaction mixture, that results in high costs factors. In the present work, the reaction kinetics of a glycerol-free biodiesel method is studied. This method consists of the transesterification of a vegetable oil (i.e. canola oil) using dimethyl carbonate (DMC) as an alternative methylating agent in presence of layered double hydroxides doped with triazabicyclodecene catalyst (a basic organocatalyst). Furthermore, is theorized that this heterogeneous catalyst (TBD/LDH) simultaneously converts both FFAs and triglycerides due to acid sites formed by Al3+ active sites of the LDH structure. Additionally, the versatility of the Raman in situ technique was used as quantitative analysis tool to monitor the reaction kinetics and collect real time data.

  10. Treatment with coated layer double hydroxide clays decreases the toxicity of copper-contaminated water.

    Science.gov (United States)

    Blake, Deanne; Nar, Mangesh; D'Souza, Nandika Anne; Glenn, J Brad; Klaine, Stephen J; Roberts, Aaron P

    2014-05-01

    Copper is a common pollutant found in watersheds that exerts toxic effects on both invertebrates and vertebrates. Layer double hydroxide (LDH) clays are able to adsorb a wide range of contaminants through ion-exchange mechanisms. Coating LDH clays with various materials alters the aggregation of clay particles into the nano-size range, thus increasing relative surface area and offering great potential for contaminant remediation. The goal of this study was to determine if treatment with coated LDH clays decreases the toxicity of copper-containing solutions to Daphnia magna. Four LDH clays with different coatings used to alter hydrophobicity were as follows: used: Na(+) montmorillonite, Zn-Al LDH-nitrate, Zn-Al LDH-stearate, and Zn-Al LDH-carbonate. It was determined that coated LDH clays decreased copper toxicity by decreasing bioavailability and that smaller aggregate sizes decreased bioavailability the most. 96 h LC50 values increased by as much as 4.2 times with the treatment of the solutions with 100 mg/L LDH clay. Copper analysis of the clay and solutions indicated that the clays work by decreasing copper bioavailability by way of a binding mechanism. Coated LDH clays hold promise as a small-scale remediation tool or as an innovative tool for toxicity identification and evaluation characterization of metals.

  11. Structure and conductive properties of poly(ethylene oxide)/layered double hydroxide nanocomposite polymer electrolytes

    International Nuclear Information System (INIS)

    Liao, C.-S.; Ye, W.-B.

    2004-01-01

    The oligo(ethylene oxide) modified layered double hydroxide (LDH) prepared by template method was added as a nanoscale nucleating agent into poly(ethylene oxide) (PEO) to form PEO/OLDH nanocomposite electrolytes. The effects of OLDH addition on morphology and conductivities of nanocomposite electrolytes were studied using wide-angle X-ray diffractometer, polarized optical microscopy, differential scanning calorimetry and ionic conductivity measurement. The results show that the exfoliated morphology of nanocomposites is formed due to the surface modification of LDH layers with PEO matrix compatible oligo(ethylene oxide)s. The nanoscale dispersed OLDH layers inhibit the crystal growth of PEO crystallites and result in a plenty amount of intercrystalline grain boundary within PEO/OLDH nanocomposites. The ionic conductivities of nanocomposite electrolytes are enhanced by three orders of magnitude compared to the pure PEO polymer electrolytes at ambient temperature. It can be attributed to the ease transport of Li + along intercrystalline amorphous phase. This novel nanocomposite electrolytes system with high conductivities will be benefited to fabricate the thin-film type of Li-polymer secondary battery

  12. New Insights into CO2 Adsorption on Layered Double Hydroxide (LDH)-Based Nanomaterials

    Science.gov (United States)

    Tang, Nian; He, Tingyu; Liu, Jie; Li, Li; Shi, Han; Cen, Wanglai; Ye, Zhixiang

    2018-02-01

    The interlamellar spacing of layered double hydroxides (LDHs) was enlarged by dodecyl sulfonate ions firstly, and then, (3-aminopropyl)triethoxysilane (APS) was chemically grafted (APS/LDHs). The structural characteristics and thermal stability of these prepared samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), reflectance Fourier transform infrared spectrometer (FTIR), thermogravimetric analysis (TG), and elemental analysis (EA) respectively. The CO2 adsorption performance was investigated adopting TG and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). The results presented that the CO2 adsorption capacity on APS/LDHs was as high as 90 mg/g and showed no obvious reduction during a five cyclic adsorption-desorption test, indicating its superior performance stability. The DRIFTS results showed that both carbamates and weakly bounded CO2 species were generated on APS/LDHs. The weakly adsorbed species was due to the different local chemical environment for CO2 capture provided by the surface moieties of LDHs like free silanol and hydrogen bonds.

  13. Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

    Science.gov (United States)

    Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

    2017-12-01

    The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

  14. Recent progress in layered double hydroxide based materials for electrochemical capacitors: design, synthesis and performance.

    Science.gov (United States)

    Zhao, Mingming; Zhao, Qunxing; Li, Bing; Xue, Huaiguo; Pang, Huan; Chen, Changyun

    2017-10-19

    As representative two-dimensional (2D) materials, layered double hydroxides (LDHs) have received increasing attention in electrochemical energy storage and conversion because of the facile tunability between their composition and morphology. The high dispersion of active species in layered arrays, the simple exfoliation into monolayer nanosheets and chemical modification offer the LDHs an opportunity as active electrode materials in electrochemical capacitors (ECs). LDHs are favourable in providing large specific surface areas, good transport features as well as attractive physicochemical properties. In this review, our purpose is to provide a detailed summary of recent developments in the synthesis and electrochemical performance of the LDHs. Their composites with carbon (carbon quantum dots, carbon black, carbon nanotubes/nanofibers, graphene/graphene oxides), metals (nickel, platinum, silver), metal oxides (TiO 2 , Co 3 O 4 , CuO, MnO 2 , Fe 3 O 4 ), metal sulfides/phosphides (CoS, NiCo 2 S 4 , NiP), MOFs (MOF derivatives) and polymers (PEDOT:PSS, PPy (polypyrrole), P(NIPAM-co-SPMA) and PET) are also discussed in this review. The relationship between structures and electrochemical properties as well as the associated charge-storage mechanisms is discussed. Moreover, challenges and prospects of the LDHs for high-performance ECs are presented. This review sheds light on the sustainable development of ECs with LDH based electrode materials.

  15. Recovery of Lithium from Geothermal Brine with Lithium-Aluminum Layered Double Hydroxide Chloride Sorbents.

    Science.gov (United States)

    Paranthaman, Mariappan Parans; Li, Ling; Luo, Jiaqi; Hoke, Thomas; Ucar, Huseyin; Moyer, Bruce A; Harrison, Stephen

    2017-11-21

    We report a three-stage bench-scale column extraction process to selectively extract lithium chloride from geothermal brine. The goal of this research is to develop materials and processing technologies to improve the economics of lithium extraction and production from naturally occurring geothermal and other brines for energy storage applications. A novel sorbent, lithium aluminum layered double hydroxide chloride (LDH), is synthesized and characterized with X-ray powder diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), and thermogravimetric analysis. Each cycle of the column extraction process consists of three steps: (1) loading the sorbent with lithium chloride from brine; (2) intermediate washing to remove unwanted ions; (3) final washing for unloading the lithium chloride ions. Our experimental analysis of eluate vs feed concentrations of Li and competing ions demonstrates that our optimized sorbents can achieve a recovery efficiency of ∼91% and possess excellent Li apparent selectivity of 47.8 compared to Na ions and 212 compared to K ions, respectively in the brine. The present work demonstrates that LDH is an effective sorbent for selective extraction of lithium from brines, thus offering the possibility of effective application of lithium salts in lithium-ion batteries leading to a fundamental shift in the lithium supply chain.

  16. Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

    Directory of Open Access Journals (Sweden)

    Chia-Hsuan Lin

    2017-12-01

    Full Text Available The synthesis and optical properties of Mg-Al layered double hydroxide (LDH precursor powders were investigated using X-ray diffraction (XRD, Fourier transform-infrared (FT-IR spectroscopy, transmission electron microscopy (TEM, selected area electron diffraction (SAED, high-resolution TEM (HRTEM, UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363–1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH2](CO30.083·(H2O0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

  17. Thermokinetic study of the rehydration process of a calcined MgAl-layered double hydroxide.

    Science.gov (United States)

    Pfeiffer, Heriberto; Lima, Enrique; Lara, Víctor; Valente, Jaime S

    2010-03-16

    The rehydration process of a calcined MgAl-layered double hydroxide (LDH) with a Mg/Al molar ratio of 3 was systematically analyzed at different temperatures and relative humidity. Qualitative and quantitative experiments were done. In the first set of samples, the temperature or the relative humidity was varied, fixing the second variable. Both adsorption and absorption phenomena were present; absorption process was associated to the LDH regeneration. Of course, in all cases the LDH regeneration was confirmed by other techniques such as TGA, solid state NMR, and SAXS. In the second set of experiments, a kinetic analysis was performed, the results allowed to obtain different activation enthalpies for the LDH regeneration as a function of the relative humidity. The activation enthalpies varied from 137.6 to 83.3 kJ/mol as a function of the relative humidity (50 and 80%, respectively). All these experiments showed that LDH regeneration is highly dependent on the temperature and relative humidity.

  18. RECONSTRUCTION OF CALCINED Zn -Al LAYERED DOUBLE HYDROXIDES DURING TETRACYCLINE ADSORPSION

    Directory of Open Access Journals (Sweden)

    G. M. Starukh

    2015-12-01

    Full Text Available Zn-Al mixed oxides containing ZnO different degree crystallinity were obtained by calcinations of Zn-Al layered double hydroxides (LDHs. The reconstruction of calcined Zn-Al LDHs has been performed under stirring in aqueous suspensions. The assynthesized LDHs, its decomposition products, as well as the reconstructed solids upon hydration were characterized by XRD, N2adsorption, differential and thermal gravimetric analysis. It was found that the ability of Zn-Al LDHs to recover a layered structure under the hydration of mixed oxides depends on the degree of ZnO crystallinity. The partial reconstruction of Zn-Al layered structure occurs in tetracycline solutions irrespective to the degree of ZnO crystallinity in calcined LDHs. Calcined Zn-Al LDHs demonstrate the higher adsorption capacity to tetracycline in comparison with as-prepared Zn-Al LDHs. The adsorption of TC on calcined and uncalcined ZnAl LDHs occurs on the centers of one particular type. It is suggested that surface complexation of the A-ring ligand of TC with Al-OH centers takes place.

  19. The Adsorption of Dextranase onto Mg/Fe-Layered Double Hydroxide: Insight into the Immobilization

    Directory of Open Access Journals (Sweden)

    Yi Ding

    2018-03-01

    Full Text Available We report the adsorption of dextranase on a Mg/Fe-layered double hydroxide (Mg/Fe-LDH. We focused the effects of different buffers, pH, and amino acids. The Mg/Fe-LDH was synthesized, and adsorption experiments were performed to investigate the effects. The maximum adsorption occurred in pH 7.0 4-(2-hydroxyethyl-1-piperazineethanesulfonic acid (HEPES buffer, and the maximum dextranase adsorption uptake was 1.38 mg/g (416.67 U/mg; histidine and phenylalanine could affect the adsorption. A histidine tag could be added to the protein to increase the adsorption significantly. The performance features and mechanism were investigated with X-ray diffraction patterns (XRD and Fourier transform infrared spectra (FTIR. The protein could affect the crystal structure of LDH, and the enzyme was adsorbed on the LDH surface. The main interactions between the protein and LDH were electrostatic and hydrophobic. Histidine and phenylalanine could significantly affect the adsorption. The hexagonal morphology of LDH was not affected after adsorption.

  20. Layered double hydroxides functionalized with anionic surfactant: Direct electrochemistry and electrocatalysis of hemoglobin

    International Nuclear Information System (INIS)

    Li Maoguo; Chen Shuihong; Ni Fang; Wang Yinling; Wang Lun

    2008-01-01

    Direct electrochemistry of hemoglobin (Hb), which was immobilized on the glass carbon electrode (GCE) modified with Zn-Al layered double hydroxide (LDH) functionalized with sodium dodecylsulfonate (SDS), was investigated. The resulting electrode (Hb/LDH-SDS/GCE) gave a well-defined redox couple for HbFe(III)/Fe(II) with a formal potential of about -0.34 V (vs. AgCl/Ag) in pH 7.0 buffer. The electron-transfer rate constant was estimated to be 2.6 s -1 . The Hb/LDH-SDS/GCE exhibited a remarkable electrocatalytic activity for the reduction of hydrogen peroxide (H 2 O 2 ). The low calculated apparent Michaelis-Menten constant (K M app ) was 456 μM. Based on the high catalytic activity of Hb immobilized on LDH-SDS modified electrode to the reduction of H 2 O 2 , LDH functionalized with SDS is expected to have widely potential applications for development of new biosensors and biocatalysis

  1. Synthesis of Fluorinated Graphene/CoAl-Layered Double Hydroxide Composites as Electrode Materials for Supercapacitors.

    Science.gov (United States)

    Peng, Weijun; Li, Hongqiang; Song, Shaoxian

    2017-02-15

    CoAl-layered double hydroxide/fluorinated graphene (CoAl-LDH/FGN) composites were fabricated via a two-step hydrothermal method. The synthesized CoAl-LDH/FGN composites have been characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and electrochemical measurements. The results indicated that the fluorinated carbon with various configuration forms were grafted onto the framework of graphene, and the C-F bond configuration and fluorine content could be tuned by the fluorination time. Most of semi-ionic C-F bonds were formed at an appropriate fluorination time and, then, converted into fluorine rich surface groups (such as CF 2 , CF 3 , etc.) which were electrochemically inactive as the fluorination time prolonged. Moreover, the CoAl-LDH/FGN composites prepared at the optimal fluorination time exhibited the highest specific capacitance (1222 F/g at 1 A/g), the best rate capability, and the most stable capacitance retention, which offered great promise as electrode materials for supercapacitors.

  2. Synergistic Effect of Cobalt and Iron in Layered Double Hydroxide Catalysts for the Oxygen Evolution Reaction.

    Science.gov (United States)

    Yang, Fengkai; Sliozberg, Kirill; Sinev, Ilya; Antoni, Hendrik; Bähr, Alexander; Ollegott, Kevin; Xia, Wei; Masa, Justus; Grünert, Wolfgang; Cuenya, Beatriz Roldan; Schuhmann, Wolfgang; Muhler, Martin

    2017-01-10

    Co-based layered double hydroxide (LDH) catalysts with Fe and Al contents in the range of 15 to 45 at % were synthesized by an efficient coprecipitation method. In these catalysts, Fe 3+ or Al 3+ ions play an essential role as trivalent species to stabilize the LDH structure. The obtained catalysts were characterized by a comprehensive combination of surface- and bulk-sensitive techniques and were evaluated for the oxygen evolution reaction (OER) on rotating disk electrodes. The OER activity decreased upon increasing the Al content for the Co- and Al-based LDH catalysts, whereas a synergistic effect in Co- and Fe-based LDHs was observed, which resulted in an optimal Fe content of 35 at %. This catalyst was spray-coated on Ni foam electrodes and showed very good stability in a flow-through cell with a potential of approximately 1.53 V at 10 mA cm -2 in 1 m KOH for at least 48 h. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Acid-etched layered double hydroxides with rich defects for enhancing the oxygen evolution reaction.

    Science.gov (United States)

    Zhou, Peng; Wang, Yanyong; Xie, Chao; Chen, Chen; Liu, Hanwen; Chen, Ru; Huo, Jia; Wang, Shuangyin

    2017-08-22

    Water splitting is promising for energy storage and conversion, but the sluggish oxygen evolution reaction (OER) hinders its wide application. The search for efficient and low-cost electrocatalysts for oxygen evolution has been pursued owing to their significance for green energy generation and storage. Layered Double Hydroxide (LDH) based materials are promising for the OER to improve this weakness. However, the wide application of LDHs is limited by their electronic properties and active sites. Here we report a simple and promising method to improve the OER catalytic activity via an acid-base reaction, which resulted in an exfoliation process and multiple defects including Co, Fe and O vacancies. The acid etched LDHs exhibit better oxygen evolution performance than the pristine LDHs under alkaline conditions with a small Tafel slope and good durability. The acid etching improves the electronic structure and provides more active sites, which results in significant enhancement of OER activity. This work will open up a novel and inexpensive way to improve the catalytic performance in an alkaline substance.

  4. Comparative study of the coprecipitation methods for the preparation of Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Crepaldi Eduardo L.

    2000-01-01

    Full Text Available Coprecipitation is the method most frequently applied to prepare Layered Double Hydroxides (LDHs. Two variations of this method can be used, depending on the pH control conditions during the precipitation step. In one case the pH values are allowed to vary while in the other they are kept constant throughout coprecipitation. Although research groups have their preferences, no systematic comparison of the two variations of the coprecipitation method is available in the literature. On this basis, the objective of the present study was to compare the properties of LDHs prepared using the two forms of pH control in the coprecipitation method. The results showed that even though coprecipitation is easier to perform under conditions of variable pH values, materials with more interesting properties, from the point of view of technological applications, are obtained at constant pH. Higher crystallinity, smaller particle size, higher specific surface area and higher average pore diameter were found for materials obtained by coprecipitation at constant pH, when compared to the materials obtained at variable pH.

  5. The Adsorption of Dextranase onto Mg/Fe-Layered Double Hydroxide: Insight into the Immobilization

    Science.gov (United States)

    Ding, Yi; Liu, Le; Fang, Yaowei; Zhang, Xu; Lyu, Mingsheng; Wang, Shujun

    2018-01-01

    We report the adsorption of dextranase on a Mg/Fe-layered double hydroxide (Mg/Fe-LDH). We focused the effects of different buffers, pH, and amino acids. The Mg/Fe-LDH was synthesized, and adsorption experiments were performed to investigate the effects. The maximum adsorption occurred in pH 7.0 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES) buffer, and the maximum dextranase adsorption uptake was 1.38 mg/g (416.67 U/mg); histidine and phenylalanine could affect the adsorption. A histidine tag could be added to the protein to increase the adsorption significantly. The performance features and mechanism were investigated with X-ray diffraction patterns (XRD) and Fourier transform infrared spectra (FTIR). The protein could affect the crystal structure of LDH, and the enzyme was adsorbed on the LDH surface. The main interactions between the protein and LDH were electrostatic and hydrophobic. Histidine and phenylalanine could significantly affect the adsorption. The hexagonal morphology of LDH was not affected after adsorption. PMID:29562655

  6. Uptake of chloride ion from aqueous solution by calcined layered double hydroxides: equilibrium and kinetic studies.

    Science.gov (United States)

    Lv, Liang; He, Jing; Wei, Min; Evans, D G; Duan, Xue

    2006-02-01

    Layered double hydroxides (LDH) calcined within a certain temperature range (denoted as CLDH) have been shown to recover their original layered structure in the presence of appropriate anions. In the light of this so-called "memory effect", uptake of chloride ion from aqueous solution by calcined MgAl-CO3 LDH was investigated in batch mode. The equilibrium isotherm showed that the uptake of chloride ion by CLDH was consistent with the Langmuir and Freundlich equations and that the Langmuir model gave a better fit to the experimental data than the Freundlich model. The maximum uptake capacity of CLDH for chloride ion was 149.5 mg/g, close to the stoichiometric uptake (168 mg/g). The influence of varying pH of solution, initial chloride concentration, adsorbent quantity, and temperature on the kinetics of chloride removal has also been explored. Four kinetic models were used to fit the experimental data, and it was found that the pseudo-second-order kinetics model could be used to describe the uptake process satisfactorily. The calculated value of Ea was found to be 56.8 kJ/mol, which suggests that the process of uptake of chloride ion is controlled by the rate of reaction of chloride ion with the CLDH rather than diffusion. A mechanism for removal of chloride ion has been confirmed by X-ray diffraction, FT-IR spectroscopy and TG-MS measurements.

  7. Defect-Rich Ultrathin Cobalt-Iron Layered Double Hydroxide for Electrochemical Overall Water Splitting.

    Science.gov (United States)

    Liu, Peng Fei; Yang, Shuang; Zhang, Bo; Yang, Hua Gui

    2016-12-21

    Efficient and durable electrocatalysts from earth-abundant elements play a vital role in the key renewable energy technologies including overall water splitting and hydrogen fuel cells. Here, generally used CoFe based layered double hydroxides (LDHs) were first delaminated and exfoliated in the DMF-ethanol solvent (CoFe LDH-F), with enhancement both in oxygen evolution reaction (OER) and hydrogen evolution reaction (HER). The exfoliation process creates more coordinatively unsaturated metals and improves the intrinsic electronic conductivity, which is important in water electrolyzer reactions. In the basic solution, the CoFe LDH-F catalyst outperforms the commercial iridium dioxide (IrO 2 ) electrocatalyst in activity and stability for OER and approaches the performance of platinum (Pt) for HER. The bifunctional electrocatalysts can be further used for overall water splitting, with a current density of ∼10 mA/cm 2 at the applied voltage of 1.63 V for long-term electrolysis test, rivalling the performance of Pt and IrO 2 combination as benchmarks. Our findings demonstrate the promising catalytic activity of LDHs for scale-up alkaline water splitting.

  8. Starch Biocatalyst Based on α-Amylase-Mg/Al-Layered Double Hydroxide Nanohybrids.

    Science.gov (United States)

    Bruna, Felipe; Pereira, Marita G; Polizeli, Maria de Lourdes T M; Valim, João B

    2015-08-26

    The design of new biocatalysts through the immobilization of enzymes, improving their stability and reuse, plays a major role in the development of sustainable methodologies toward the so-called green chemistry. In this work, α-amylase (AAM) biocatalyst based on Mg3Al-layered double-hydroxide (LDH) matrix was successfully developed with the adsorption method. The adsorption process was studied and optimized as a function of time and enzyme concentration. The biocatalyst was characterized, and the mechanism of interaction between AAM and LDH, as well as the immobilization effects on the catalytic activity, was elucidated. The adsorption process was fast and irreversible, thus yielding a stable biohybrid material. The immobilized AAM partially retained its enzymatic activity, and the biocatalyst rapidly hydrolyzed starch in an aqueous solution with enhanced efficiency at intermediate loading values of ca. 50 mg/g of AAM/LDH. Multiple attachments through electrostatic interactions affected the conformation of the immobilized enzyme on the LDH surface. The biocatalyst was successfully stored in its dry form, retaining 100% of its catalytic activity. The results reveal the potential usefulness of a LDH compound as a support of α-amylase for the hydrolysis of starch that may be applied in industrial and pharmaceutical processes as a simple, environmentally friendly, and low-cost biocatalyst.

  9. Universal biomimetic preparation and immobilization of layered double hydroxide films and adsorption behavior

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Wei; Zhang, Wenpeng; Chen, Zilin

    2017-01-15

    Highlights: • An in situ method is developed for immobilization of nanoscale LDHs. • The universal method can be applied on multiple substrates. • The homogeneous LDHs film can be synthesis and immobilized in one step. • The LDHs film showed good adsorption performance towards anionic compounds. - Abstract: Preparation and immobilization of layered double hydroxides (LDHs) film onto multiple substrates is important and challenging in functional materials fields by date. In this work, a simple and universal polydopamine (PD)-based layer-by-layer assembly strategy was developed for the immobilization of LDHs film onto surfaces such as polypropylene chip, glass slides and metal coins. The surface of substrates was firstly modified by polydopamine functionalization, and then LDHs film was synthesized via urea method and directly immobilized on the PD layer by in situ growing strategy in one step. The PD layer as well as the final LDHs film was characterized by energy dispersive X-ray spectroscopy, scanning electron microscope, infrared spectroscopy, X-ray diffraction pattern and X-ray photoelectron spectra. It has been demonstrated the formation of the dense and homogeneous nanoscaled LDHs film with 400 nm thickness. Adsorption behavior of the fabricated NiAl-LDHs film toward anionic dyes and pharmaceuticals was further assessed. To demonstrate their extensive application, fast and high efficient adsorption of anionic dyes and pharmaceuticals was achieved by NiAl-LDHs-modified polypropylene centrifugal tube.

  10. Study on the adsorption of DNA on the layered double hydroxides (LDHs)

    Science.gov (United States)

    Li, Bin; Wu, Pingxiao; Ruan, Bo; Liu, Paiyu; Zhu, Nengwu

    2014-03-01

    Four kinds of layered double hydroxides (LDHs) were prepared by chemical coprecipitation method and used as DNA adsorbents. Multiple characterization tools such as power X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and Standard electronic modules (SEM) were employed to characterize the LDHs. By examining the effect of initial concentration, solution pH, adsorption experiments were carried out to investigate the adsorption capacities of LDHs for DNA. The results revealed that the LDHs with Mg/Al = 3 had higher ability on adsorbing the DNA and were not affected by pH values. The LDHs exhibited excellent adsorption properties and completely adsorbed DNA within 2 h. The adsorption equilibrium data were fitted to the Langmuir and Freundlich models, showing that the Langmuir model which represented monolayer adsorption had better correlation with the adsorption linear equation. In addition, Circular dichroism (CD) spectrum, UV-vis spectorscopy and agarose gel electrophoresis revealed the integrity of DNA structure, suggesting that there had no damage on the DNA structure during the adsorption process.

  11. Immobilization of layered double hydroxides in the fluidic system for nanoextraction of specific DNA molecules

    Science.gov (United States)

    Chen, Jem-Kun; Chan, Chia-Hao; Chang, Feng-Chih

    2008-02-01

    The purpose of this study was to immobilize inorganic layered double hydroxides (LDHs) on the poly(methylmethacrylate) substrate as the media to extract the specific DNA molecules through fluidic system to enhance the efficiency of extract specific DNA molecules from extremely low concentration in sample solution. LDH immobilized through solvent swelling and plasma treatment on the polymer surface captured the specific DNA molecules lysed from Escherichia coli (E. coli) cells as the target DNA molecules with 2×10-4g/l of concentration in sample solution mixed biomacromolecules lysed from human blood. The encapsulated DNA molecules released through dissolving of LDHs by slight acid (pH=4-5) solution then amplified by polymerase chain reaction (PCR) process through the primers for E. coli cells. The DNA molecules amplified by PCR process were characterized by gel electrophoresis to recognize the existence of E. coli cells. The results show that immobilized LDHs could be regarded as the specific DNA detector for rapid disease diagnosis through fluidic system.

  12. MgAl-Layered Double Hydroxide Solid Base Catalysts for Henry Reaction: A Green Protocol

    Directory of Open Access Journals (Sweden)

    Magda H. Abdellattif

    2018-03-01

    Full Text Available A series of MgAl-layered double hydroxide (MgAl-HT, the calcined form at 500 °C (MgAlOx, and the rehydrated one at 25 °C (MgAl-HT-RH were synthesized. Physicochemical properties of the catalysts were characterized by X-ray diffraction (XRD and scanning electron microscopy (SEM. Surface area of the as-synthesized, calcined, and rehydrated catalysts was determined by N2 physisorption at −196 °C. CO2 temperature-programmed desorption (CO2-TPD was applied to determine the basic sites of catalysts. The catalytic test reaction was carried out using benzaldehyde and their derivatives with nitromethane and their derivatives. The Henry products (1–15 were obtained in a very good yield using MgAl-HT-RH catalyst either by conventional method at 90 °C in liquid phase or under microwave irradiation method. The mesoporous structure and basic nature of the rehydrated solid catalyst were responsible for its superior catalytic efficiency. The robust nature was determined by using the same catalyst five times, where the product % yield was almost unchanged significantly.

  13. Ionic elastomers based on carboxylated nitrile rubber (XNBR and magnesium aluminum layered double hydroxide (hydrotalcite

    Directory of Open Access Journals (Sweden)

    A. Laskowska

    2014-06-01

    Full Text Available The presence of carboxyl groups in carboxylated nitrile butadiene rubber (XNBR allows it to be cured with different agents. This study considers the effect of crosslinking of XNBR by magnesium aluminum layered double hydroxide (MgAl-LDH, known also as hydrotalcite (HT, on rheometric, mechano-dynamical and barrier properties. Results of XNBR/HT composites containing various HT loadings without conventional curatives are compared with XNBR compound crosslinked with commonly used zinc oxide. Hydrotalcite acts as an effective crosslinking agent for XNBR, as is particularly evident from rheometric and Fourier transform infrared spectroscopy (FTIR studies. The existence of ionic crosslinks was also detected by dynamic mechanical analysis (DMA of the resulting composites. DMA studies revealed that the XNBR/HT composites exhibited two transitions – one occurring at low temperature is associated to the Tg of elastomer and the second at high temperature corresponds to the ionic transition temperature Ti. Simultaneous application of HT as a curing agent and a filler may deliver not only environmentally friendly, zinc oxide-free rubber product but also ionic elastomer composite with excellent mechanical, barrier and transparent properties.

  14. Equilibrium and Thermodynamic Studies of Anionic Dyes Removal by an Anionic Clay-Layered Double Hydroxide

    International Nuclear Information System (INIS)

    Kantasamy, N.; Siti Mariam Sumari

    2016-01-01

    Adsorption isotherm describes the interaction of adsorbates with adsorbent in equilibrium. Equilibrium data was examined using Langmuir and Freundlich isotherm models. Thermodynamic studies were used to evaluate the thermodynamic parameters; heat of enthalpy change (ΔH degree), Gibbs free energy change (ΔG degree) and heat of entropy change (ΔSdegree) in order to gain information regarding the nature of adsorption (exothermic or endothermic). Four reactive dyes of anionic type, Acid Blue 29 (AB29), Reactive Black 5 (RB5), Reactive Orange 16 (RO16) and Reactive Red 120 (RR120) were used to obtain equilibrium isotherms at 25, 35, 45 and 55 degree Celsius. Based on Giles' classification, the isotherm produced were of L2-type, indicating strong dye affinity towards the adsorbent, and with weak competition with the solvent molecules for active adsorption sites. Equilibrium data fitted both Langmuir and Freundlich isotherm models with high correlation coefficient (R 2 > 0.91) indicating the possibility of both homogeneity and heterogeneous nature of adsorption. The negative values of ΔGdegree indicate the adsorption processes were spontaneous and feasible. The negative values of ΔHdegree lie between -20 to -75 kJ/ mol, suggesting these processes were exothermic and physical in nature. The negative values of ΔSdegree are indication of decreased disorder and randomness of spontaneous adsorption of reactive dyes on layered double hydroxide as adsorbent. (author)

  15. Novel route for layered double hydroxides preparation by enzymatic decomposition of urea

    Science.gov (United States)

    Vial, S.; Prevot, V.; Forano, C.

    2006-05-01

    This study presents a new route for the preparation of a series of layered double hydroxide materials with controlled textural properties. It concerns the biogenesis of hydrotalcite like phases by Jack bean urease through the enzymatic decomposition process of urea. Different conditions of LDH biogenesis are investigated (urease activity, urea concentration). A comparative study with the precipitation method based on the thermal decomposition of urea (90 °C) is conducted in order to asses the effect of the various urea hydrolysis conditions (kinetic, temperature) and the presence of enzyme in the reaction medium on the structural and textural properties of the as prepared LDH materials. Mechanisms of formation of the LDH phases for both synthesis processes are discussed on basis of their pH control. The PXRD and SEM analysis of samples prepared by the thermal process evidence higher crystallinity and greater particle sizes than LDH obtained in mild biogenic conditions. In the latter case, presence of urease or effect of some M(II) metals may inhibit the crystallization.

  16. Fluorescent vancomycin and terephthalate comodified europium-doped layered double hydroxides nanoparticles: synthesis and application for bacteria labelling

    Science.gov (United States)

    Sun, Jianchao; Fan, Hai; Wang, Nan; Ai, Shiyun

    2014-09-01

    Vancomycin (Van)- and terephthalate (TA)-comodified europium-doped layered double hydroxides (Van-TA-Eu-LDHs) nanoparticles were successfully prepared by a two-step method, in which, TA acted as a sensitizer to enhance the fluorescent property and Van was modified on the surface of LDH to act as an affinity reagent to bacteria. The obtained products were characterized by X-ray diffraction, transmission electron microscope and fluorescent spectroscopy. The results demonstrated that the prepared Van- and TA-comodified europium-doped layered double hydroxides (Van-TA-Eu-LDHs) nanoparticles with diameter of 50 nm in size showed highly efficient fluorescent property. Furthermore, due to the high affinity of Van to bacteria, the prepared Van-TA-Eu-LDHs nanoparticles showed efficient bacteria labelling by fluorescent property. The prepared nanoparticles may have wide applications in the biological fields, such as biomolecular labelling and cell imaging.

  17. Total Oxidation of Ethanol over Layered Double Hydroxide-Related Mixed Oxide Catalysts: Effect of Cation Composition.

    Czech Academy of Sciences Publication Activity Database

    Jirátová, Květa; Kovanda, F.; Ludvíková, Jana; Balabánová, Jana; Klempa, Jan

    2016-01-01

    Roč. 277, NOV 15 (2016), s. 61-67 ISSN 0920-5861. [Czech-Italian- Spanish Conference on Molecular Sieves and Catalysis /16./. Amantea, 14.06.2015-17.06.2015] R&D Projects: GA ČR GA14-13750S Institutional support: RVO:67985858 Keywords : layered double hydroxides * transition metal oxides * vox oxidation Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 4.636, year: 2016

  18. Total Oxidation of Ethanol over Layered Double Hydroxide-Related Mixed Oxide Catalysts: Effect of Cation Composition.

    Czech Academy of Sciences Publication Activity Database

    Jirátová, Květa; Kovanda, F.; Ludvíková, Jana; Balabánová, Jana; Klempa, Jan

    2016-01-01

    Roč. 277, NOV 15 (2016), s. 61-67 ISSN 0920-5861. [Czech-Italian-Spanish Conference on Molecular Sieves and Catalysis /16./. Amantea, 14.06.2015-17.06.2015] R&D Projects: GA ČR GA14-13750S Institutional support: RVO:67985858 Keywords : layered double hydroxides * transition metal oxides * vox oxidation Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 4.636, year: 2016

  19. Supported Layered Double Hydroxide-Related Mixed Oxides and Their Application in the Total Oxidation of Volatile Organic Compounds

    Czech Academy of Sciences Publication Activity Database

    Kovanda, F.; Jirátová, Květa

    2011-01-01

    Roč. 53, č. 2 (2011), s. 305-316 ISSN 0169-1317 R&D Projects: GA ČR GAP106/10/1762; GA ČR GA106/09/1664 Institutional research plan: CEZ:AV0Z40720504 Keywords : layered double hydroxides * hydrothermal reaction * mixed oxides Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 2.474, year: 2011

  20. The application of layered double hydroxide clay (LDH)-poly(lactide-co-glycolic acid) (PLGA) film composites for the controlled release of antibiotics

    DEFF Research Database (Denmark)

    Chakraborti, Michelle; Jackson, John K.; Plackett, David

    2012-01-01

    bone cement, used in orthopedics, release very little drug. The purpose of this study was to investigate the use of nanoparticulates composed of layered double hydroxide clays to bind various antibiotics and release them in a controlled manner. Mg–Al (carbonate) layered double hydroxides were...... and quantitation of the unbound fraction by UV/Vis absorbance or HPLC analysis. Drug release from layered double hydroxide clay/drug complexes dispersed in polymeric films was measured by incubation in phosphate-buffered saline (pH 7.4) at 37 °C using absorbance or HPLC analysis. Antimicrobial activity of drug....../clay complexes in poly(lactic-co-glycolic acid) films resulted in a reduced burst phase of release and a slow continuous release for many weeks with effective antimicrobial amounts of VAN and SF released at later time points. Layered double hydroxide clays may be useful for controlled release applications...

  1. Selectivity of layered double hydroxides and their derivative mixed metal oxides as sorbents of hydrogen sulfide.

    Science.gov (United States)

    Othman, Mohamed A; Zahid, Waleed M; Abasaeed, Ahmed E

    2013-06-15

    In the context of finding high efficient sorbent materials for removing hydrogen sulfide (H2S) from air stream, a screening study was performed to find the best combination of metals for the synthesis of layered double hydroxides (LDHs) and their derivative mixed metal oxides. Based on selectivity of 998 natural mineral species of sulfur-containing compounds, Cu(2+), Ni(2+) and Zn(2+) were selected as divalent metals, and Fe(3+), Al(3+) and Cr(3+) as trivalent metals to synthesis the LDHs sorbents. 10 LDHs materials and their calcined mixed metal oxides, Ni(0.66)Al(0.34), Cu(0.35)Ni(0.32)Al(0.33), Zn(0.66)Al(0.34), Cu(0.36)Zn(0.32)Al(0.32), Ni(0.64)Fe(0.36), Cu(0.35)Ni(0.31)Fe(0.34), Ni(0.66)Cr(0.34), Cu(0.35)Ni(0.31)Cr(0.34), Zn(0.66)Cr(0.34), Cu(0.33)Zn(0.32)Cr(0.35) were synthesized, characterized chemically and physically, and then tested using breakthrough test to determine their sulfur uptake. Ni(0.64)Fe(0.36) mixed metal oxides was found to have the best uptake of hydrogen sulfide (136 mg H₂S/g). Regeneration of spent Ni(0.64)Fe(0.36) mixed metal oxides was studied using two different mixture solutions, NaCl/NaOH and acetate-buffer/NaCl/NaOH. The latter mixture successfully desorbed the sulfur from the Ni0.64Fe0.36 sorbent for 2 cycles of regeneration/sorption. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Tribological Behavior of NiAl-Layered Double Hydroxide Nanoplatelets as Oil-Based Lubricant Additives.

    Science.gov (United States)

    Wang, Hongdong; Liu, Yuhong; Liu, Wenrui; Wang, Rong; Wen, Jianguo; Sheng, Huaping; Peng, Jinfang; Erdemir, Ali; Luo, Jianbin

    2017-09-13

    Layered double hydroxides (LDHs) are a class of naturally occurring inorganic minerals that are composed of divalent and trivalent metal cations. In this study, three different sized NiAl-LDH nanoplatelets were synthesized by varying crystallization time during the microemulsification process. The layered structure and three-dimensional size of nanoplatelets were confirmed by transmission electron microscopy (TEM) and atomic force microscopy (AFM). As lubricant additives, their tribological properties in base oil were evaluated by use of a ball-on-disk reciprocating tribometer under three different loads: 50, 100, and 150 N (which created peak Hertz pressures of 1.74, 2.16, and 2.47 GPa). Under contact pressures of up 2.16 GPa, not only did the coefficient of friction (COF) decrease by about 10% after nano-LDHs were added but also the wear performance improved substantially. These improvements resulted from a protective tribolayer formation on the contact interface, as revealed by detailed surface and structure analytical studies. In particular, cross-sectional TEM images revealed that the larger size nanoplatelets (NiAl-24h), rather than the smaller ones (NiAl-6h) showed the best and most stable tribological performance. This was mainly because of their higher degree of crystallinity, which in turn resulted in the formation of a tribofilm with far superior mechanical properties during sliding. Owing to the simple synthetic method and superior tribological properties as oil-based additives, nano-LDHs hold great potential for use in demanding industrial applications in the future.

  3. Porphyrins intercalated in Zn/Al and Mg/Al layered double hydroxides: properties and structural arrangement

    Czech Academy of Sciences Publication Activity Database

    Káfuňková, Eva; Taviot-Guého, Ch.; Bezdička, Petr; Klementová, Mariana; Kovář, P.; Kubát, Pavel; Mosinger, Jiří; Pospíšil, M.; Lang, Kamil

    2010-01-01

    Roč. 22, č. 8 (2010), s. 2481-2490 ISSN 0897-4756 R&D Projects: GA ČR GA203/07/1424; GA ČR GAP207/10/1447 Institutional research plan: CEZ:AV0Z40320502; CEZ:AV0Z40400503 Keywords : hydrotalcite-like compounds * molecular-dynamic simulations * photophysical properties Subject RIV: CA - Inorganic Chemistry Impact factor: 6.400, year: 2010

  4. Antituberculosis nanodelivery system with controlled-release properties based on para-amino salicylate–zinc aluminum-layered double-hydroxide nanocomposites

    Directory of Open Access Journals (Sweden)

    Saifullah B

    2013-11-01

    Full Text Available Bullo Saifullah,1 Mohd Zobir Hussein,1 Samer Hasan Hussein-Al-Ali,2 Palanisamy Arulselvan,3 Sharida Fakurazi3,41Materials Synthesis and Characterization Laboratory, 2Laboratory of Molecular Biomedicine, 3Laboratory of Vaccines and Immunotherapeutics, 4Department of Human Anatomy, Universiti Putra Malaysia, Serdang, Selangor, MalaysiaAbstract: We report the intercalation and characterization of para-amino salicylic acid (PASA into zinc/aluminum-layered double hydroxides (ZLDHs by two methods, direct and indirect, to form nanocomposites: PASA nanocomposite prepared by a direct method (PASA-D and PASA nanocomposite prepared by an indirect method (PASA-I. Powder X-ray diffraction, Fourier-transform infrared spectroscopy, and thermogravimetric analysis revealed that the PASA drugs were accommodated within the ZLDH interlayers. The anions of the drug were accommodated as an alternate monolayer (along the long-axis orientation between ZLDH interlayers. Drug loading was estimated to be 22.8% and 16.6% for PASA-D and PASA-I, respectively. The in vitro release properties of the drug were investigated in physiological simulated phosphate-buffered saline solution of pH 7.4 and 4.8. The release followed the pseudo-second-order model for both nanocomposites. Cell viability (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyltetrazolium bromide [MTT] assays was assessed against normal human lung fibroblast MRC-5 and 3T3 mouse fibroblast cells at 24, 48, and 72 hours. The results showed that the nanocomposite formulations did not possess any cytotoxicity, at least up to 72 hours.Keywords: drug-delivery system, slow-release nanocarrier, tuberculosis, biocompatible nanocomposites

  5. Synthesis of linear alkylbenzene sulphonate intercalated iron(II) iron(III) hydroxide sulphate (green rust) and adsorption of carbon tetrachloride

    DEFF Research Database (Denmark)

    Ayala Luis, Karina Barbara; Kaldor, D.K.; Bender Koch, Christian

    2007-01-01

    Green rusts, GRs, can act as both sorbents and reductants towards selected pollutants. Organo-GRs are expected to combine these properties with a high affinity for hydrophobic substances. A novel organo-GR, GRLAS, was synthesized by incorporating a mixture of linear alkylbenzenesulphonates (LAS...... was well ordered, although a mixture of surfactant was used for intercalation. The basal spacings of the GRLAS and the kinetics of the ion-exchange process were dependent on the initial surfactant loading; basal spacings of ~2.85 nm were obtained at The ratio LAS solution concentrations >10 mM. LASadsorbed...

  6. Monodisperse embedded nanoparticles derived from an atomic metal-dispersed precursor of layered double hydroxide for architectured carbon nanotube formation

    DEFF Research Database (Denmark)

    Tian, Gui-Li; Zhao, Meng-Qiang; Zhang, Bingsen

    2014-01-01

    understood. Herein, the preparation of metal NPs with tunable areal density from layered double hydroxide (LDH) precursors in which the metal cations were pre-dispersed at an atomic scale was explored. Large quantities of mesopores induced by the Kirkendall effect were formed on the as-calcined layered...... double oxide (LDO) flakes. The O atoms bonded with Fe3+ cations were easy to be extracted at a temperature higher than 750 degrees C, which greatly increased the mobility of Fe. Consequently, coalescence of the reduced Fe atoms into large NPs enhanced the Kirkendall effect, leading to the formation....... When the areal density was increased from 0.039 to 0.55, and to 2.1 x 10(15) m(-2), the Fe NPs embedded on the LDO flakes exhibited good catalytic performance for the growth of entangled carbon nanotubes (CNTs), aligned CNTs, and double helical CNTs, respectively. This work provides not only new...

  7. Calcined Ni-Al Layered Double Hydroxide as Catalyst for Total Oxidation of VOC: Effect of Precursor Crystallinity.

    Czech Academy of Sciences Publication Activity Database

    Mikulová, Zuzana; Čuba, Pavel; Balabánová, Jana; Rojka, T.; Kovanda, F.; Jirátová, Květa

    2007-01-01

    Roč. 61, 2 (2007) , s. 103-109 ISSN 0366-6352. [International Conference of Slovak Society of Chemical Engineering /33./. Matliare, 26.05.2006-30.05.2006] R&D Projects: GA ČR(CZ) GA104/04/2116; GA ČR(CZ) GD203/03/H140 Institutional research plan: CEZ:AV0Z40720504 Keywords : layered double hydroxide * mixed oxide * hydrothermal treatment Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 0.367, year: 2007

  8. Adsorption of phosphate in hydrocalumite-like layered double hydroxides: a comparison between memory effect and ion exchange processes

    International Nuclear Information System (INIS)

    Bernardo, M.P.; Moreira, F.K.V.; Ribeiro, C.

    2016-01-01

    Phosphorus is an essential element for agriculture, but the excessive use of this element has caused severe damages to the environment. Layered double hydroxide (LDHs) are excellent candidates to remove PO 4 3- anions through adsorption process. In this work, the phosphate adsorption on hydrocalumite-like (Ca-Al) LDHs was evaluated over the ion exchange and memory effect processes. X-ray diffraction measurements revealed formation of analogous crystalline phases from both process as the phosphate concentration was increased. However, the phosphate quantity adsorbed varied according to the process used. The ion exchange route is the most efficient process to remove phosphate from aqueous medium. (author)

  9. Palladium on Layered Double Hydroxide: A Heterogeneous System for the Enol Phosphate Carbon-Oxygen Bond Activation in Aqueous Media

    Directory of Open Access Journals (Sweden)

    Jaqueline D. Senra

    2017-01-01

    Full Text Available In this work, a new catalytic approach for the C-O activation of enol phosphates based on a palladium supported on layered double hydroxide was developed. In this case, two different ketene aminal phosphates were used as models to study the synthesis of α-phenyl enecarbamates N-Boc/CBz under the Suzuki-Miyaura conditions. The use of an ortho-bromoaniline as precursor allowed the synthesis of the 2-phenyl indole through an arylation/Heck cyclization. Catalyst reusability enabled the synthesis of the heterocycle in moderate yields for four consecutive runs.

  10. Intercalation reactions into graphite: a two-dimensional chemistry; Les reactions d'intercalation dans le graphite. Une chimie bidimensionnelle

    Energy Technology Data Exchange (ETDEWEB)

    Herold, C. [Nancy-1 Univ. Henri Poincare, Lab. de Chimie du Solide Mineral-UMR 7555, 54 (France); Lagrange, Ph. [Ecole Europeenne d' Ingenieurs en Genie des Materiaux, Institut National Polytechnique de Lorraine, 54 - Nancy (France)

    2006-03-15

    The lamellar structure of graphite and its oxidizing and reducing double nature lead this material to accommodate in its Van der Waals's gaps numerous and largely various chemical species, necessarily oxidizing or reducing. Thus the graphite intercalation compounds contain graphene planes, systematically reduced or oxidized. An overview on the graphite intercalation chemistry with electron donor species is presented in this paper: alkali, alkaline-earth metals, lanthanides, metallic alloys, ionic compounds like alkaline halides, chalcogenides and hydroxides. The crystal chemistry of these compounds brings the 'memory' out, that possess the intercalated sheets of the 3D structure of the initial species. Lastly, several of their electronic properties are given. (authors)

  11. Direct growth of cobalt aluminum double hydroxides on graphene nanosheets and the capacitive properties of the resulting composites

    International Nuclear Information System (INIS)

    Kim, Yuna; Kim, Seok

    2015-01-01

    We synthesized graphene nanosheets (GNs)/cobalt aluminum (CoAl) double hydroxide composites through a layer-by-layer deposition process while varying the concentration of the graphene precursor used. The CoAl layered double hydroxide particles were uniformly distributed on the surfaces of the graphene layers and effectively prevented the agglomeration of the GNs, resulting in a higher reactive surface area and easier ion transport. We employed X-ray diffraction analysis, energy-dispersive X-ray spectroscopy, field-emission scanning electron microscopy, and field-emission transmission electron microscopy to investigate the microstructures and morphologies of the composites. In addition, cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge/discharge measurements were performed to analyze the electrochemical behaviors of the composites. The as-prepared composites showed desirable electrochemical characteristics, including high specific capacitances, low resistances, and high cycling stabilities. In particular, the composite formed by optimizing the GNs/CoAl ratio (the electrolyte used was a 6 M aqueous KOH solution) exhibited the maximum specific capacitance, which was 974 F g −1

  12. Non-enzymatic acetylcholine sensor based on Ni–Al layered double hydroxides/ordered mesoporous carbon

    International Nuclear Information System (INIS)

    Ju Jian; Bai Jing; Bo Xiangjie; Guo Liping

    2012-01-01

    Highlights: ► Nanostructured Ni–Al layered double hydroxides supported on ordered mesoporous carbon. ► A non-enzymatic amperometric sensor for acetylcholine. ► High sensitivity, wide linear range, and low limit of detection for acetylcholine. - Abstract: In this work, a novel non-enzymatic acetylcholine (ACh) sensor was constructed based on electrodepoition of Ni–Al layered double hydroxides (Ni–Al LDHs) on ordered mesoporous carbon (OMC) modified glassy carbon (GC) electrode. The obtained Ni–Al LDHs/OMC nanocomposite was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and electrochemical methods. A novel non-enzymatic acetylcholine (ACh) sensor based on Ni–Al LDHs/OMC was developed. Compared with the pristine OMC and Ni–Al LDHs modified electrodes, Ni–Al LDHs/OMC displayed higher electrocatalytic activity toward ACh and gave a wide concentration interval of 2–4922 μM and a low limit of detection (42 nM, R = 0.999), which is better than some reports in the literatures. The sensor also exhibited long-term stability and remarkable antifouling property. The excellent electrocatalysis for ACh can be attributed to the combination of the unique properties of Ni–Al LDHs nanoparticles and the ordered mesostructure of OMCs matrix.

  13. Electro-oxidation nitrite based on copper calcined layered double hydroxide and gold nanoparticles modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Cui Lin; Meng Xiaomeng; Xu Minrong; Shang Kun; Ai Shiyun; Liu Yinping

    2011-01-01

    Highlights: → A nitrite sensor fabricated based on copper calcined layered double hydroxides and gold nanoparticles modified electrode. → This sensor exhibited excellent electrocatalytic oxidation to nitrite. → This nitrite sensor exhibited very good analytical performance with low cost, convenient preparation and rapid detection. - Abstract: In this paper, a novel nitrite sensor was constructed based on electrodeposition of gold nanoparticles (AuNPs) on a copper calcined layered double hydroxide (Cu-CLDH) modified glassy carbon electrode. Electrochemical experiments showed that AuNPs/CLDH composite film exhibited excellent electrocatalytic oxidation activity with nitrite due to the synergistic effect of the Cu-CLDH with AuNPs. The fabricated sensor exhibited excellent performance for nitrite detection within a wide concentration interval of 1-191 μM and with a detection limit of 0.5 μM. The superior electrocatalytic response to nitrite was mainly attributed to the large surface area, minimized diffusion resistance, and enhanced electron transfer of the Cu-CLDH and AuNPs composition film. This platform offers a novel route for nitrite sensing with wide analytical applications and will supply the practical applications for a variety of simple, robust, and easy-to-manufacture analytical approaches in the future.

  14. New type ternary NiAlCe layered double hydroxide photocatalyst for efficient visible-light photoreduction of CO2 into CH4

    Science.gov (United States)

    Li, Ji; (Bill Yang, Y. J.

    2018-02-01

    New type of ternary NiAlCe layered double hydroxide photocatalyst was synthesized by a simple hydrothermal reaction. The obtained photocatalyst shows efficient visible-light activity for CO2 reduction to CH4. We have investigated the optimal Ce content in the catalyst and analyzed the mechanism by materials characterization. Additionally, a novel alkali etching method was used to construct the porous structure. The effect of the porosity and morphologies on the activity is investigated. It is found that the ternary NiAlCe layered double hydroxide photocatalyst with porosity showing the best photocatalytic activity among all the samples. Based on the characterization and first principle calculation, the detailed photocatalytic mechanism of the ternary NiAlCe layered double hydroxide photocatalyst is deduced.

  15. Intercalation compounds involving inorganic layered structures

    Directory of Open Access Journals (Sweden)

    CONSTANTINO VERA R. L.

    2000-01-01

    Full Text Available Two-dimensional inorganic networks can shown intracrystalline reactivity, i.e., simple ions, large species as Keggin ions, organic species, coordination compounds or organometallics can be incorporated in the interlayer region. The host-guest interaction usually causes changes in their chemical, catalytic, electronic and optical properties. The isolation of materials with interesting properties and making use of soft chemistry routes have given rise the possibility of industrial and technological applications of these compounds. We have been using several synthetic approaches to intercalate porphyrins and phthalocyanines into inorganic materials: smectite clays, layered double hydroxides and layered niobates. The isolated materials have been characterized by elemental and thermal analysis, X-ray diffraction, surface area measurements, scanning electronic microscopy, electronic and resonance Raman spectroscopies and EPR. The degree of layer stacking and the charge density of the matrices as well their acid-base nature were considered in our studies on the interaction between the macrocycles and inorganic hosts.

  16. Porphyrin-layered double hydroxide/polymer composites as novel ecological photoactive surfaces

    Czech Academy of Sciences Publication Activity Database

    Káfuňková, Eva; Lang, Kamil; Kubát, Pavel; Klementová, Mariana; Mosinger, Jiří; Šlouf, Miroslav; Troutier-Thuilliez, A. L.; Leroux, F.; Verney, V.; Taviot-Guého, Ch.

    2010-01-01

    Roč. 20, č. 42 (2010), s. 9423-9432 ISSN 0959-9428 R&D Projects: GA ČR GAP207/10/1447 Institutional research plan: CEZ:AV0Z40320502; CEZ:AV0Z40400503; CEZ:AV0Z40500505 Keywords : porphyrins * nanoparticles * hydroxide/polymer composites Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 5.101, year: 2010

  17. Synthesis and characterization of carboxymethyl cellulose/layered double hydroxide nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Yadollahi, Mehdi; Namazi, Hassan, E-mail: namazi@tabrizu.ac.ir [University of Tabriz, Research Laboratory of Dendrimers and Nanopolymers, Faculty of Chemistry (Iran, Islamic Republic of)

    2013-04-15

    In this study, coprecipitation method was employed for intercalation of carboxy methyl cellulose (CMC) into hydrotalcite-like anionic clays (Mg/Al and Ni/Al). The synthesized nanocomposites were characterized using FTIR, XRD, TEM, and Thermo gravimetric analysis. Furthermore, their swelling behavior was studied at various pH values. The intercalation of Carboxymethyl cellulose polymeric chains into LDH sheets was confirmed by FTIR spectroscopy and XRD analysis. The d-values are 1.73 nm for the Mg-Al-CMC-LDH and 2.23 nm for the Ni-Al-CMC-LDH, supporting a multilayer arrangement of CMC into the LDH interlayer space. Thermo gravimetric analysis showed a better thermal resistance of CMC in the presence of LDH sheets, especially for Mg-Al-CMC-LDH. The obtained nanocomposites revealed a pH dependent swelling behavior. The swelling of the prepared nanocomposites increased slowly with increasing pH from 2 to 10. However, their swelling ratio increased sharply in the pH values above 10.

  18. Double-blind, randomized, placebo-controlled trial of the use of topical 10% potassium hydroxide solution in the treatment of molluscum contagiosum.

    Science.gov (United States)

    Short, Katherine A; Fuller, L Claire; Higgins, Elisabeth M

    2006-01-01

    Molluscum contagiosum is a common viral infection of the skin that frequently affects children. Lesions take between 6 and 18 months to resolve spontaneously and are a source of great embarrassment to both caretakers and children, often affecting attendance at school and limiting social activity. Treatment options to date have been poorly tolerated by children but recent studies have suggested that potassium hydroxide may be beneficial. This double-blind, randomized, placebo-controlled study compared 10% potassium hydroxide with placebo (normal saline). Twenty patients, aged 2 to 12 years, were recruited. Parents applied a solution twice daily to lesional skin until signs of inflammation appeared. Children were examined by the same observer on days 0, 15, 30, 60, and 90. Seventy percent of children receiving topical potassium hydroxide cleared, compared with 20% in the placebo group. Further dosing studies are required to identify whether weaker concentrations of potassium hydroxide are as efficacious, with less irritancy.

  19. Layered double hydroxide-enhanced luminescence in a Fenton-like system for selective sensing of cobalt in Hela cells

    Science.gov (United States)

    Yu, Mei; Yuan, Zhiqin; Lu, Chao

    2017-09-01

    This work presented a facile and eco-friendly method for the determination of cobalt ions (Co(II)) in living cells based on layered double hydroxides (Mg-Al CO3-LDHs) enhanced chemiluminescence (CL) emission of a Co(II)-hydrogen peroxide-sodium hydroxide system. The enhanced CL emission was attributed to the large specific surface area of Mg-Al CO3-LDHs, which facilitates the generation of an excited-stated intermediate. The proposed method displayed high selectivity toward Co(II) over other metal ions. Under the optimal conditions, the increased CL intensity showed a linear response versus Co(II) concentration in the range of 5.0-1000 nM with a detection limit of 3.7 nM (S/N = 3). The relative standard deviation for nine repeated measurements of 100 nM Co(II) was 3.2%. Furthermore, the proposed method was successfully applied to detect Co(II) in living cell samples, and the results were agreed with those obtained by the standard ICP-MS method.

  20. Advanced oxidation of rhodamine B with hydrogen peroxide over ZnCr layered double hydroxide catalysts

    Directory of Open Access Journals (Sweden)

    Nguyen Tien Thao

    2017-09-01

    Full Text Available Zn/Cr layered zinc hydroxide materials with different molar ratios of Cr/Zn have been synthesized through the coprecipitation method at pH of 9.0–9.5. At high Cr/Zn molar ratios of 0.5/1–1/3, the materials possess some layered structure with carbonate anions between the interlayer galleries. The catalysts present uniform particle sizes and quite high surface area. An isomorphous substitution of Zn2+ by Cr3+ in the brucite-like sheets makes the layered Cr-doped zinc hydroxides potential catalysts for efficient oxidation of rhodamine B with H2O2 solution. The experimental results indicated that the intra-lattice Cr3+ ions are more active than Cr2O3 components in the oxidative removal of rhodamine B. The degradation efficiency is dependent on the intra lattice Cr3+ contents and reaction variables. The Cr/Zn LDH gave a high decolorization (99% of rhodamine B at near neutral pH and room temperature.

  1. Precursor preparation for Ca-Al layered double hydroxide to remove hexavalent chromium coexisting with calcium and magnesium chlorides

    Energy Technology Data Exchange (ETDEWEB)

    Zhong, Lihua; He, Xiaoman; Qu, Jun; Li, Xuewei; Lei, Zhiwu; Zhang, Qiwu [School of Resources and Environment Engineering, Wuhan University of Technology, Wuhan 430070 (China); Liu, Xinzhong [College of Ecological Environment and Urban Construction, Fujian University of Technology, Fuzhou 350118 (China)

    2017-01-15

    Al(OH){sub 3} and Ca(OH){sub 2} powders are co-ground to prepare a precursor which hydrates into a layered double hydroxide (LDH) phase by agitation in aqueous solution with target hexavalent chromium (Cr(VI)) at room temperature, to achieve an obvious improvement in removal efficiency of Cr(VI) through an easy incorporation into the structure. Although the prepared precursor transforms into LDH phases also when agitated in the solutions of calcium and magnesium chlorides, it incorporates Cr(VI) preferentially to the chloride salts when they coexist. The adsorption isotherm and kinetic studies show that the phenomena occurring on the Al-Ca precursor fit a pseudo-second-order kinetics with a Langmuir adsorption capacity of 59.45 mg/g. Besides, characterizations of the prepared precursor and the samples after adsorption are also performed by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Transmission electron microscope (TEM) to understand the reason of the preferential incorporation of Cr(VI) to the coexisting chloride salts during the LDH phase formation. - Graphical abstract: Activated Ca-Al hydroxides (C{sub 3}A) transformed into Ca-Al-OH compound when agitated in water. Ca-Al precursor (C{sub 3}A) was agitated in a hexavalent chromium (Cr(VI)) solution to form Al-Ca-CrO{sub 4} LDH product. Ca-Al-CrO{sub 4} LDH phase occurred preferentially to Ca-Al-MCl{sub 2} LDH phases in the solutions of calcium and magnesium chlorides, it incorporates Cr(VI) preferentially to the chloride salts when they coexist. - Highlights: • Activated Ca-Al hydroxides transformed into LDH when agitated in water with some inorganic substances. • Hexavalent Cr was incorporated in the LDH structure at high adsorption capacity. • Ca-Al-Cr LDH phase occurred preferentially to Ca-Al-MCl{sub 2} LDH phases with coexistence. • The prepared Ca-Al hydroxides had high performance as adsorbent even with high salinity of the solution.

  2. Improvement of pharmacokinetic and antitumor activity of layered double hydroxide nanoparticles by coating with PEGylated phospholipid membrane.

    Science.gov (United States)

    Yan, Mina; Zhang, Zhaoguo; Cui, Shengmiao; Lei, Ming; Zeng, Ke; Liao, Yunhui; Chu, Weijing; Deng, Yihui; Zhao, Chunshun

    2014-01-01

    Layered double hydroxide (LDH) has attracted considerable attention as a drug carrier. However, because of its poor in vivo behavior, polyethylene glycolylated (PEGylated) phospholipid must be used as a coformer to produce self-assembled core-shell nanoparticles. In the present study, we prepared a PEGylated phospholipid-coated LDH (PLDH) (PEG-PLDH) delivery system. The PEG-PLDH nanoparticles had an average size of 133.2 nm. Their core-shell structure was confirmed by transmission electron microscopy and X-ray photoelectron spectroscopy. In vitro liposome-cell-association and cytotoxicity experiments demonstrated its ability to be internalized by cells. In vivo studies showed that PEGylated phospholipid membranes greatly reduced the blood clearance rate of LDH nanoparticles. PEG-PLDH nanoparticles demonstrated a good control of tumor growth and increased the survival rate of mice. These results suggest that PEG-PLDH nanoparticles can be a useful drug delivery system for cancer therapy.

  3. The preparation of layered double hydroxide wrapped carbon nanotubes and their application as a flame retardant for polypropylene

    International Nuclear Information System (INIS)

    Du Baoxian; Fang Zhengping

    2010-01-01

    Carbon nanotubes (CNTs) wrapped with layered double hydroxide (LDH-w-CNTs) were facilely obtained through in situ introduction of CNTs into the hydrothermal reaction system of LDH, with the goal of combining their unique physical and chemical characteristics to meet new advanced applications. Morphological observations indicated that LDH lamellae enwrapped the surface of CNTs and the wrapping degree was dependent on the functionalization of CNTs. ζ-potential measurements showed that the interaction between the positive charge of LDH and the negative charge of CNTs was the main driving force of the wrapping process. Both hybrids led to a reduction in the peak heat release rate (PHRR) of polypropylene, indicating that they could confer better flame retardancy on polypropylene with respect to LDH and CNTs.

  4. Electrochemical oxidation of 4-chloro phenol over a carbon paste electrode modified with Zn Al layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez F, D.; Palomar P, M.; Licona S, T. de J.; Romero R, M. [Universidad Autonoma Metropolitana, Unidad Azcapotzalco, Departamento de Materiales, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D. F. (Mexico); Valente, Jaime S., E-mail: mepp@correo.azc.uam.mx [Instituto Mexicano del Petroleo, Eje Central No. 152, 07730 Mexico D. F. (Mexico)

    2014-07-01

    A study is presented on the electrochemical oxidation of 4-chloro phenol (4cp) in aqueous solution using a bare carbon paste electrode, Cpe, and another one that was modified with Zn Al layered double hydroxides (Cpe/Zn Al-LDH). The electro-oxidation was effected at ph values ranging from 3 up to 11. It was found through cyclic voltammetry that this process was irreversible, namely, there were no reduction peaks, and that depending on the nature of the electrode, the anodic current was limited either by adsorption (Cpe) or diffusion (Cpe/Zn Al-LDH). The energy required and the oxidation reaction rate depended on the ph and on the nature of the electrode, such that the greater rates were obtained when the Cpe/Zn Al-LDH electrode and acid ph were used. The Zn Al-LDH was characterized by means of X-ray diffraction. (Author)

  5. Microstructural modification of NiAl layered double hydroxide electrodes by adding graphene nanosheets and their capacitative property

    International Nuclear Information System (INIS)

    Kim, Yuna; Kim, Seok

    2015-01-01

    NiAl layered double hydroxide (LDH) composite electrodes containing various contents of graphene nanosheets (GNS) were prepared by a hydrothermal method. The microstructure and morphological properties were examined by FE-SEM, FE-TEM, XRD, and FTIR. Electrochemical analysis was also carried out by cyclic voltammetry, impedance, and cycle life measurement. The as-prepared composite that contained 500 mg of graphene (denoted as NiAl/G-50) achieved the highest specific capacitance of 1147 F/g among the various NiAl LDH/GNS composites. Besides, the NiAl LDH/GNS composite exhibited the lower diffusion resistance, improved rate capability, and good cyclic stability (83% of initial capacitance after 2000 cycles). Considering the morphological data and the improved capacitative properties together, we concluded the synthesized NiAl LDH/GNS composites would be a promising electrode material for supercapacitors

  6. Microstructural modification of NiAl layered double hydroxide electrodes by adding graphene nanosheets and their capacitative property

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Yuna; Kim, Seok [School of Chemical and Biomolecular Engineering, Pusan National University, Busan (Korea, Republic of)

    2015-02-15

    NiAl layered double hydroxide (LDH) composite electrodes containing various contents of graphene nanosheets (GNS) were prepared by a hydrothermal method. The microstructure and morphological properties were examined by FE-SEM, FE-TEM, XRD, and FTIR. Electrochemical analysis was also carried out by cyclic voltammetry, impedance, and cycle life measurement. The as-prepared composite that contained 500 mg of graphene (denoted as NiAl/G-50) achieved the highest specific capacitance of 1147 F/g among the various NiAl LDH/GNS composites. Besides, the NiAl LDH/GNS composite exhibited the lower diffusion resistance, improved rate capability, and good cyclic stability (83% of initial capacitance after 2000 cycles). Considering the morphological data and the improved capacitative properties together, we concluded the synthesized NiAl LDH/GNS composites would be a promising electrode material for supercapacitors.

  7. Mg-Cu-Al layered double hydroxides based catalysts for the reduction of nitrates in aqueous solutions

    Directory of Open Access Journals (Sweden)

    Vulić Tatjana J.

    2010-01-01

    Full Text Available The secondary waste and bacterial contamination in physico-chemical and biological separation processes used today for nitrate removal from ground water make novel catalytic technologies that convert nitrates to unharmful gaseous nitrogen, very attractive for scientific research. The Mg-Cu-Al layered double hydroxide (LDH based catalysts with different Mg/Al ratio were investigated in water denitrification reaction in the presence of hydrogen and with solely copper as an active phase. Since LDHs have ion exchange properties and their derived mixed oxides possess memory effect (restoration of layered structure after thermal decomposition, their adsorption capacity for nitrates was also measured in the same model system. All studied samples showed nitrate removal from 23% to 62% following the decrease in Al content, as well as the substantial adsorption capacity ranging from 18% to 38%. These results underlie the necessity to take into account the effects of the adsorption in all future investigations.

  8. Synthesis and Properties of Layered Organic-inorganic Hybrid Material: Zn-Al Layered Double Hydroxide-dioctyl Sulfosuccinate Nanocomposite

    International Nuclear Information System (INIS)

    Mohd Zobir bin Hussein; Tan Kim Hwa

    2000-01-01

    A layered organic-inorganic hybrid nanocomposite was prepared by using a surfactant, dioctyl sulphosuccinate (DSS) as a guest in Zn-Al layered double hydroxide (LDH) inorganic host by a self-assembly technique. The Zn-Al ratio of the mother liquor was kept constant at 4 at the beginning of the synthesis. Powder X-ray diffractogram shows that the basal spacing of the Zn-Al LDH with sulphate as the intergallery anion (ZASUL) expanded from 11.0 to 26.3 A to accommodate the DSS surfactant anion for the formation of the Zn-Al LDH-DSS layered organic-inorganic hybrid nanocomposite (ZADON). It was also found that the BET surface area reduced by about 90%, from 22.5 to 2.2 m 2 /g, for ZASUL and ZADON, respectively if 0.1 M DSS was used for the synthesis of the latter

  9. Recent Advances in Stimuli-Responsive Photofunctional Materials Based on Accommodation of Chromophore into Layered Double Hydroxide Nanogallery

    Directory of Open Access Journals (Sweden)

    Wu Li

    2013-01-01

    Full Text Available The assembly of photofunctional molecules into host matrices has become an important strategy to achieve tunable fluorescence and to develop intelligent materials. The stimuli-responsive photofunctional materials based on chromophores-assembled layered double hydroxides (LDHs have received much attention from both academic and industry fields as a result of their advantages, such as high photo/thermal stability, easy processing, and well reversibility, which can construct new types of smart luminescent nanomaterials (e.g., ultrathin film and nanocomposite for sensor and switch applications. In this paper, external environmental stimuli have mainly involved physical (such as temperature, pressure, light, and electricity and chemical factors (such as pH and metal ion; recent progress on the LDH-based organic-inorganic stimuli-responsive materials has been summarized. Moreover, perspectives on further development of these materials are also discussed.

  10. Prolate spheroidal hematite particles equatorially belt with drug-carrying layered double hydroxide disks: Ring Nebula-like nanocomposites

    Directory of Open Access Journals (Sweden)

    Nedim Ay Ahmet

    2011-01-01

    Full Text Available Abstract A new nanocomposite architecture is reported which combines prolate spheroidal hematite nanoparticles with drug-carrying layered double hydroxide [LDH] disks in a single structure. Spindle-shaped hematite nanoparticles with average length of 225 nm and width of 75 nm were obtained by thermal decomposition of hydrothermally synthesized hematite. The particles were first coated with Mg-Al-NO3-LDH shell and then subjected to anion exchange with salicylate ions. The resulting bio-nanohybrid displayed a close structural resemblance to that of the Ring Nebula. Scanning electron microscope and transmission electron microscopy images showed that the LDH disks are stacked around the equatorial part of the ellipsoid extending along the main axis. This geometry possesses great structural tunability as the composition of the LDH and the nature of the interlayer region can be tailored and lead to novel applications in areas ranging from functional materials to medicine by encapsulating various guest molecules.

  11. Layered double hydroxides based ion exchange extraction for high sensitive analysis of non-steroidal anti-inflammatory drugs.

    Science.gov (United States)

    Zhou, Wei; Wang, Chenlu; Liu, Yikun; Zhang, Wenpeng; Chen, Zilin

    2017-09-15

    Layered double hydroxides (LDHs) are ideal sorbents for solid phase extraction (SPE) because of the excellent ion exchange capacity and high specific surface area. However, difficult elution of the analytes from the LDHs is a problem due to the strong ionic interaction between anions and LDHs. High concentrated NaOH solution is employed to elute the sample, but it not suitable for analyzing by HPLC. To solve this problem, a simple acid-base neutralization method was proposed after elution, and then the neutral samples were directly injected to HPLC for analysis. Nickel-aluminum layered double hydroxides (NiAl-LDHs) were synthesized by co-precipitation method and packed into a micro pipette tip for the extraction of three non-steroidal anti-inflammatory drugs (NSAIDs) including ketoprofen, naproxen and flurbiprofen from aqueous samples. After optimization of the experimental parameters such as the concentration of the NaOH, sample pH, sampling rate and sample volume, excellent extraction efficiency towards three NSAIDs was obtained with high enrichment factors of 28-32. A NiAl-LDHs based SPE-HPLC method was developed for quantitative analysis of NSAIDs, and the method showed low limits of detection (0.002-0.1ng/mL), good linearity (R 2 ≥0.9995) and good reproducibility (intraday RSD≤4.37%). The developed method was also applied to the analysis of three NSAIDs in spiked human plasma and rat plasma after oral administration, which demonstrated the practicality of the proposed method. Copyright © 2017. Published by Elsevier B.V.

  12. Applications vs properties of Mg-Al Layered Double Hydroxides provided by their syntheses methods: alkoxide and alkoxide-free sol-gel syntheses and hydrothermal precipitation

    NARCIS (Netherlands)

    Chubar, N.; Gerda, V.; Megantari, O.; Mičušík, M.; Omastova, M.; Heister, K.; Man, P.; Fraissard, J.

    2013-01-01

    A tremendous number of studies have examined layered double hydroxides (LDH) for their technological applications in the ion exchange removal of toxic ions, recovery of valuable substances, catalysis, CO2 capture, as a layered host for storage/delivery of biologically active molecules, additives to

  13. A unique growth mechanism of donut-shaped Mg–Al layered double hydroxides crystals revealed by AFM and STEM–EDX

    NARCIS (Netherlands)

    Budhysutanto, W.N.; Van Den Bruele, F.J.; Rossenaar, B.D.; Van Agterveld, D.; Van Enckevort, W.J.P.; Kramer, H.J.M.

    2010-01-01

    Donut-like crystals of Mg–Al layered double hydroxides (LDH) are synthesized using a hydrothermal method with microwave heating. This morphology provides enlargement of the specific surface area of the {h k 0} faces, needed for adsorption application. The growth mechanism for donut-shaped crystals

  14. {1H}/{2H} and {1H}/{17O} nuclear quadrupole double-resonance study of several hydroxide compounds. II. The water molecule

    Science.gov (United States)

    Poplett, Ian J. F.

    Using the technique of double resonance with coupled multiplets at 77 K and room temperature, 17O double-resonance signals were detected from the H 2O molecules in a number of hydrates of the alkali metal and alkaline earth metal hydroxides at natural abundance. The deuteron double-resonance signals were measured in deuterated samples at 77 K using double resonance by level crossing. The correlations between the 17O and 2H quadrupole coupling constants and the hydrogen bond strength are discussed. The 17O DRCM results for BeSO 4 · 4H 2O are included.

  15. Composition and structure of an iron-bearing, layered double hydroxide (LDH) - Green rust sodium sulphate

    DEFF Research Database (Denmark)

    Christiansen, B. C.; Balic-Zunic, T.; Petit, P. O.

    2009-01-01

    Mixed-valent Fe(II),Fe(III)-layered hydroxide, known as green rust, was synthesized from slightly basic, sodium sulphate solutions in an oxygen-free glove box. Solution conditions were monitored with pH and Eh electrodes and optimized to ensure a pure sulphate green-rust phase. The solid...... was characterised using Mossbauer spectroscopy, X-ray diffraction, scanning electron microscopy and atomic force microscopy. The composition of the solution from which the green rust precipitated was established by mass and absorption spectroscopy. The sulphate form of green rust is composed of brucite-like layers......(III)(3)(SO4)(2)(OH)(18)center dot 12H(2)O, space group P-3, a = 9.528(6) angstrom, c = 10.968(8) angstrom and Z = 1. Green rust sodium sulphate, GR(Na,SO4) crystallizes in thin, hexagonal plates. Particles range from less than 50 nm to 2 mu m in diameter and are 40 nm thick or less. The material is redox...

  16. Aluminum Hydroxide and Magnesium Hydroxide

    Science.gov (United States)

    Aluminum Hydroxide, Magnesium Hydroxide are antacids used together to relieve heartburn, acid indigestion, and upset stomach. They ... They combine with stomach acid and neutralize it. Aluminum Hydroxide, Magnesium Hydroxide are available without a prescription. ...

  17. Superhydrophobic ZnAl double hydroxide nanostructures and ZnO films on Al and glass substrates

    Energy Technology Data Exchange (ETDEWEB)

    De, Debasis, E-mail: debasis.de@bcrec.ac.in [Electronics and Instrumentation Engineering Department, Dr. B C Roy Engineering College, Durgapur, West Bengal 713206 (India); Sarkar, D.K. [Centre Universitaire de Recherche sur l' Aluminium (CURAL), L' Université du Québec à Chicoutimi, 555 Blvd. Université, Chicoutimi, Saguenay, Québec G7H 2B1 (Canada)

    2017-01-01

    Superhydrophobic nanostructured ZnAl: layered double hydroxides (LDHs) and ZnO films have been fabricated on Al and glass substrates, respectively, by a simple and cost effective chemical bath deposition technique. Randomly oriented hexagonal patterned of ZnAl: LDHs thin nanoplates are clearly observed on Al-substrate in the scanning electron microscopic images. The average size of these hexagonal plates is ∼4 μm side and ∼30 nm of thickness. While on the glass substrate, a oriented hexagonal patterned ZnO nanorods (height ∼5 μm and 1 μm diameter) are observed and each rod is further decorated throughout the top few nanometers with several nanosteps. At the top of the nanorod, a perfectly hexagonal patterned ZnO surface with ∼250 nm sides is observed. The tendency to form hexagonal morphological features is due to the hexagonal crystal structure of ZnO confirmed from X-ray diffraction patterns and transmission electron microscopy image. The ZnAl: LDHs and/or ZnO coated substrates have been passivated by using stearic acid (SA) molecules. Infrared spectra of passivated ZnAl: LDHs coated substrates confirm the presence of SA. X-ray diffraction pattern also corroborates the results of infrared spectrum. The contact angle of the as prepared samples is zero. The superhydrophobicity is achieved by observing contact angle of ∼161° with a hysteresis of ∼4° for Al-substrate. On the glass substrate, a higher contact angle of ∼168° with a lower hysteresis of ∼3° is observed. A lower surface roughness of ∼4.93 μm is measured on ZnAl: LDHs surface layer on the Al substrate as compare to a higher surface roughness of 6.87 μm measured on ZnO layer on glass substrate. The superhydrophobicity of passivated nanostructured films on two different substrates is observed due to high surface roughness and low surface energy. - Highlights: • ZnAl: layered double hydroxides (LDHs) nanoplates are fabricated on Al substrate. • ZnO nanorods are fabricated on

  18. Anticancer Drug-Incorporated Layered Double Hydroxide Nanohybrids and Their Enhanced Anticancer Therapeutic Efficacy in Combination Cancer Treatment

    Directory of Open Access Journals (Sweden)

    Tae-Hyun Kim

    2014-01-01

    Full Text Available Objective. Layered double hydroxide (LDH nanoparticles have been studied as cellular delivery carriers for anionic anticancer agents. As MTX and 5-FU are clinically utilized anticancer drugs in combination therapy, we aimed to enhance the therapeutic performance with the help of LDH nanoparticles. Method. Anticancer drugs, MTX and 5-FU, and their combination, were incorporated into LDH by reconstruction method. Simply, LDHs were thermally pretreated at 400°C, and then reacted with drug solution to simultaneously form drug-incorporated LDH. Thus prepared MTX/LDH (ML, 5-FU/LDH (FL, and (MTX + 5-FU/LDH (MFL nanohybrids were characterized by X-ray diffractometer, scanning electron microscopy, infrared spectroscopy, thermal analysis, zeta potential measurement, dynamic light scattering, and so forth. The nanohybrids were administrated to the human cervical adenocarcinoma, HeLa cells, in concentration-dependent manner, comparing with drug itself to verify the enhanced therapeutic efficacy. Conclusion. All the nanohybrids successfully accommodated intended drug molecules in their house-of-card-like structures during reconstruction reaction. It was found that the anticancer efficacy of MFL nanohybrid was higher than other nanohybrids, free drugs, or their mixtures, which means the multidrug-incorporated LDH nanohybrids could be potential drug delivery carriers for efficient cancer treatment via combination therapy.

  19. Single-Atom Au/NiFe Layered Double Hydroxide Electrocatalyst: Probing the Origin of Activity for Oxygen Evolution Reaction.

    Science.gov (United States)

    Zhang, Jingfang; Liu, Jieyu; Xi, Lifei; Yu, Yifu; Chen, Ning; Sun, Shuhui; Wang, Weichao; Lange, Kathrin M; Zhang, Bin

    2018-03-21

    A fundamental understanding of the origin of oxygen evolution reaction (OER) activity of transition-metal-based electrocatalysts, especially for single precious metal atoms supported on layered double hydroxides (LDHs), is highly required for the design of efficient electrocatalysts toward further energy conversion technologies. Here, we aim toward single-atom Au supported on NiFe LDH ( s Au/NiFe LDH) to clarify the activity origin of LDHs system and a 6-fold OER activity enhancement by 0.4 wt % s Au decoration. Combining with theoretical calculations, the active behavior of NiFe LDH results from the in situ generated NiFe oxyhydroxide from LDH during the OER process. With the presence of s Au, s Au/NiFe LDH possesses an overpotential of 0.21 V in contrast to the calculated result (0.18 V). We ascribe the excellent OER activity of s Au/NiFe LDH to the charge redistribution of active Fe as well as its surrounding atoms causing by the neighboring s Au on NiFe oxyhydroxide stabilized by interfacial CO 3 2- and H 2 O interfacing with LDH.

  20. Two-Dimensional Layered Double Hydroxides for Reactions of Methanation and Methane Reforming in C1 Chemistry.

    Science.gov (United States)

    Li, Panpan; Yu, Feng; Altaf, Naveed; Zhu, Mingyuan; Li, Jiangbing; Dai, Bin; Wang, Qiang

    2018-01-31

    CH₄ as the paramount ingredient of natural gas plays an eminent role in C1 chemistry. CH₄ catalytically converted to syngas is a significant route to transmute methane into high value-added chemicals. Moreover, the CO/CO₂ methanation reaction is one of the potent technologies for CO₂ valorization and the coal-derived natural gas production process. Due to the high thermal stability and high extent of dispersion of metallic particles, two-dimensional mixed metal oxides through calcined layered double hydroxides (LDHs) precursors are considered as the suitable supports or catalysts for both the reaction of methanation and methane reforming. The LDHs displayed compositional flexibility, small crystal sizes, high surface area and excellent basic properties. In this paper, we review previous works of LDHs applied in the reaction of both methanation and methane reforming, focus on the LDH-derived catalysts, which exhibit better catalytic performance and thermal stability than conventional catalysts prepared by impregnation method and also discuss the anti-coke ability and anti-sintering ability of LDH-derived catalysts. We believe that LDH-derived catalysts are promising materials in the heterogeneous catalytic field and provide new insight for the design of advance LDH-derived catalysts worthy of future research.

  1. Reduced graphene oxide modified NiFe-calcinated layered double hydroxides for enhanced photocatalytic removal of methylene blue

    Science.gov (United States)

    Zhao, Guoqing; Li, Caifeng; Wu, Xia; Yu, Jingang; Jiang, Xinyu; Hu, Wenjihao; Jiao, Feipeng

    2018-03-01

    Calcined layered double hydroxides (CLDH) are one of the remarkable photocatalysts passionately studied for photodecolorization of organic dyes. NiFe-CLDH was successfully modified by reduced graphene oxide (RGO) through a facile in situ crystallization technique. The obtained RGO/NiFe-CLDH composites were fully characterized by powder X-ray diffraction (XRD), Scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared (FT-IR), and UV-vis diffuse reflectance spectroscopy (DRS). The results analysis indicated that RGO sheets could work as base course to prompt the growth of LDH crystallites and NiFe-LDH lamellar crystal promiscuously distributed on the sheets with a strong interplay between each other. The photocatalytic performance of RGO/NiFe-CLDH composites toward decolorization of methylene blue tightly depended on the mass fraction of RGO and calcinated temperature. At the RGO weight loading of 1%, calcination temperature of 500 °C, the photocatalytic degradation efficiency of RGO/NiFe-CLDH composites reached 93.0% within 5.0 h. The enhanced activity of RGO/NiFe-CLDH composites may be due to the concerted catalysis effect between two constituents of as-prepared composites.

  2. Vertically Aligned FeOOH/NiFe Layered Double Hydroxides Electrode for Highly Efficient Oxygen Evolution Reaction.

    Science.gov (United States)

    Chi, Jun; Yu, Hongmei; Qin, Bowen; Fu, Li; Jia, Jia; Yi, Baolian; Shao, Zhigang

    2017-01-11

    Employing a low-cost and highly efficient electrocatalyst to replace Ir-based catalysts for oxygen evolution reaction (OER) has drawn increasing interest in renewable energy storage. In this work, a vertically aligned FeOOH/NiFe layered double hydroxides (LDHs) nanosheets supported on Ni foam (VA FeOOH/NiFe LDHs-NF) is prepared as a highly effective OER electrode in alkaline electrolyte. The VA FeOOH/NiFe LDHs-NF represents nanosheet arrays on nickel foam with some interspace among them. The vertically aligned and interlayer-structured architecture is binder-free and contributes to facile strain relaxation, relieving the exfoliation of the catalysts layer caused by the oxygen evolution process. The as-prepared electrode shows current densities of 10 and 500 mA cm -2 at overpotentials of 208 and 288 mV, and good stability in a half-cell electrolyzer. Besides, the alkaline polymer electrolyte water electrolyzer (APEWE) with this electrode showed 1.71 V at 200 mA cm -2 , and 2.041 V at 500 mA cm -2 , exhibiting the corresponding energy efficiency of 86.0% and 72.0% (based on the lower heating value of hydrogen), which is better than the typical commercial alkaline water electrolyzer.

  3. Environmental Benign Synthesis of Lithium Silicates and Mg-Al Layered Double Hydroxide from Vermiculite Mineral for CO2 Capture

    Directory of Open Access Journals (Sweden)

    Yu Zhang

    2017-04-01

    Full Text Available This research introduces a completely new environmental benign synthesis route for obtaining two kinds of inter-mediate and high temperature CO2 sorbents, Mg-Al layered double hydroxide (LDH and Li4SiO4, from vermiculite. The mineral vermiculite was leached with acid, from which the obtained SiO2 was used for the synthesis of Li4SiO4 and the leaching waste water was used for the synthesis of Mg-Al LDH. Therefore, no waste was produced during the whole process. Both Li4SiO4 and Mg-Al LDH sorbents were carefully characterized using XRD, SEM, and BET analyses. The CO2 capturing performance of these two sorbents was comprehensively evaluated. The influence of the Li/Si ratio, calcination temperature, calcination time, and sorption temperature on the CO2 sorption capacity of Li4SiO4, and the sorption temperature on the CO2 sorption capacity of LDH, were investigated. The optimal leaching acid concentration for vermiculite and the CO2 sorption/desorption cycling performance of both the Li4SiO4 and Mg-Al LDH sorbents were determined. In sum, this demonstrated a unique and environment-friendly scheme for obtaining two CO2 sorbents from cheap raw materials, and this idea is applicable to the efficient utilization of other minerals.

  4. Interstratified nanohybrid assembled by alternating cationic layered double hydroxide nanosheets and anionic layered titanate nanosheets with superior photocatalytic activity

    International Nuclear Information System (INIS)

    Lin, Bizhou; Sun, Ping; Zhou, Yi; Jiang, Shaofeng; Gao, Bifen; Chen, Yilin

    2014-01-01

    Graphical abstract: - Highlights: • Two kinds of nanosheets are well arranged in a layer-by-layer alternating fashion. • Effective interfacial heterojunction and high specific surface were observed. • Interstratified nanohybrid exhibits a superior photocatalytic activity. - Abstract: Oppositely charged 2D inorganic nanosheets of ZnAl-layered double hydroxide and layered titanate were successfully assembled into an interstratified nanohybrid through simply mixing the corresponding nanosheet suspensions. Powder X-ray diffraction and high-resolution transmission electron microscope clearly revealed that the component nanosheets in the as-obtained nanohybrid ZnAl–Ti 3 O 7 retain the 2D sheet skeletons of the pristine materials and that the two kinds of nanosheets are well arranged in a layer-by-layer alternating fashion with a basal spacing of about 1.3 nm, coincident with the thickness summation of the two component nanosheets. The effective interfacial heterojunction between them and the high specific surface area resulted in that the nanohybrid exhibits a superior photocatalytic activity in the degradation of methylene blue with a reaction constant k of 2.81 × 10 −2 min −1 , which is about 9 and 4 times higher than its precursors H 2 Ti 3 O 7 and ZnAl-LDH, respectively. Based on UV–vis, XPS and photoelectrochemical measurements, a proposed photoexcitation model was provided to understand its photocatalytic behavior

  5. Effect of rare Earth ions on the properties of composites composed of ethylene vinyl acetate copolymer and layered double hydroxides.

    Directory of Open Access Journals (Sweden)

    Lili Wang

    Full Text Available BACKGROUND: The study on the rare earth (RE-doped layered double hydroxides (LDHs has received considerable attention due to their potential applications in catalysts. However, the use of RE-doped LDHs as polymer halogen-free flame retardants was seldom investigated. Furthermore, the effect of rare earth elements on the hydrophobicity of LDHs materials and the compatibility of LDHs/polymer composite has seldom been reported. METHODOLOGY/PRINCIPAL FINDINGS: The stearate sodium surface modified Ni-containing LDHs and RE-doped Ni-containing LDHs were rapidly synthesized by a coprecipitation method coupled with the microwave hydrothermal treatment. The influences of trace amounts of rare earth ions La, Ce and Nd on the amount of water molecules, the crystallinity, the morphology, the hydrophobicity of modified Ni-containing LDHs and the adsorption of modifier in the surface of LDHs were investigated by TGA, XRD, TEM, contact angle and IR, respectively. Moreover, the effects of the rare earth ions on the interfacial compatibility, the flame retardancy and the mechanical properties of ethylene vinyl acetate copolymer (EVA/LDHs composites were also explored in detail. CONCLUSIONS/SIGNIFICANCE: S-Ni₀.₁MgAl-La displayed more uniform dispersion and better interfacial compatibility in EVA matrix compared with other LDHs. Furthermore, the S-Ni₀.₁MgAl-La/EVA composite showed the best fire retardancy and mechanical properties in all composites.

  6. Novel layered double hydroxides-hydroxyapatite/gelatin bone tissue engineering scaffolds: Fabrication, characterization, and in vivo study.

    Science.gov (United States)

    Fayyazbakhsh, Fateme; Solati-Hashjin, Mehran; Keshtkar, Abbas; Shokrgozar, Mohammad Ali; Dehghan, Mohammad Mehdi; Larijani, Bagher

    2017-07-01

    Developing porous biodegradable scaffolds through simple methods is one of the main approaches of bone tissue engineering (BTE). In this work, a novel BTE composite containing layered double hydroxides (LDH), hydroxyapatite (HA) and gelatin (GEL) was fabricated using co-precipitation and solvent-casting methods. Physiochemical characterizations showed that the chemical composition and microstructure of the scaffolds were similar to the natural spongy bone. Interconnected macropores ranging over 100 to 600μm were observed for both scaffolds while the porosity of 90±0.12% and 92.11±0.15%, as well as, Young's modulus of 19.8±0.41 and 12.5±0.35GPa were reported for LDH/GEL and LDH-HA/GEL scaffolds, respectively. The scaffolds were degraded in deionized water after a month. The SEM images revealed that between two scaffolds, the LDH-HA/GEL with needle-like secondary HA crystals showed better bioactivity. According to the alkaline phosphatase activity and Alizarin red staining results, LDH-HA/GEL scaffolds demonstrated better bone-specific activities comparing to LDH/Gel scaffold as well as control sample (Pbone formation (Pbone regeneration. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Two-Dimensional Layered Double Hydroxides for Reactions of Methanation and Methane Reforming in C1 Chemistry

    Directory of Open Access Journals (Sweden)

    Panpan Li

    2018-01-01

    Full Text Available CH4 as the paramount ingredient of natural gas plays an eminent role in C1 chemistry. CH4 catalytically converted to syngas is a significant route to transmute methane into high value-added chemicals. Moreover, the CO/CO2 methanation reaction is one of the potent technologies for CO2 valorization and the coal-derived natural gas production process. Due to the high thermal stability and high extent of dispersion of metallic particles, two-dimensional mixed metal oxides through calcined layered double hydroxides (LDHs precursors are considered as the suitable supports or catalysts for both the reaction of methanation and methane reforming. The LDHs displayed compositional flexibility, small crystal sizes, high surface area and excellent basic properties. In this paper, we review previous works of LDHs applied in the reaction of both methanation and methane reforming, focus on the LDH-derived catalysts, which exhibit better catalytic performance and thermal stability than conventional catalysts prepared by impregnation method and also discuss the anti-coke ability and anti-sintering ability of LDH-derived catalysts. We believe that LDH-derived catalysts are promising materials in the heterogeneous catalytic field and provide new insight for the design of advance LDH-derived catalysts worthy of future research.

  8. Layered Double Hydroxide Nanoplatelets with Excellent Tribological Properties under High Contact Pressure as Water-Based Lubricant Additives

    Science.gov (United States)

    Wang, Hongdong; Liu, Yuhong; Chen, Zhe; Wu, Bibo; Xu, Sailong; Luo, Jianbin

    2016-01-01

    High efficient and sustainable utilization of water-based lubricant is essential for saving energy. In this paper, a kind of layered double hydroxide (LDH) nanoplatelets is synthesized and well dispersed in water due to the surface modification with oleylamine. The excellent tribological properties of the oleylamine-modified Ni-Al LDH (NiAl-LDH/OAm) nanoplatelets as water-based lubricant additives are evaluated by the tribological tests in an aqueous environment. The modified LDH nanoplatelets are found to not only reduce the friction but also enhance the wear resistance, compared with the water-based cutting fluid and lubricants containing other particle additives. By adding 0.5 wt% LDH nanoplatelets, under 1.5 GPa initial contact pressure, the friction coefficient, scar diameter, depth and width of the wear track dramatically decrease by 83.1%, 43.2%, 88.5% and 59.5%, respectively. It is considered that the sufficiently small size and the excellent dispersion of NiAl-LDH/OAm nanoplatelets in water are the key factors, so as to make them enter the contact area, form a lubricating film and prevent direct collision of asperity peaks. Our investigations demonstrate that the LDH nanoplatelet as a water-based lubricant additive has a great potential value in industrial application. PMID:26951794

  9. DFT-Based Simulation and Experimental Validation of the Topotactic Transformation of MgAl Layered Double Hydroxides.

    Science.gov (United States)

    Zhang, Shi-Tong; Dou, Yibo; Zhou, Junyao; Pu, Min; Yan, Hong; Wei, Min; Evans, David G; Duan, Xue

    2016-09-05

    The thermal topotactic transformation mechanism of MgAl layered double hydroxides (LDHs) is investigated by a combined theoretical and experimental study. Thermogravimetric differential thermal analysis (TG-DTA) results reveal that the LDH phase undergoes four key endothermic events at 230, 330, 450, and 800 °C. DFT calculations show that the LDH decomposes into CO2 and residual O atoms via a monodentate intermediate at 330 °C. At 450 °C, the metal cations almost maintain their original distribution within the LDH(001) facet during the thermal dehydration process, but migrate substantially along the c-axis direction perpendicular to the (001) facet; this indicates that the metal arrangement/dispersion in the LDH matrix is maintained two-dimensionally. A complete collapse of the layered structure occurs at 800 °C, which results in a totally disordered cation distribution and many holes in the final product. The structures of the simulated intermediates are highly consistent with the observed in situ powder XRD data for the MgAl LDH sample calcined at the corresponding temperatures. Understanding the structural topotactic transformation process of LDHs would provide helpful information for the design and preparation of metal/metal oxides functional materials derived from LDH precursors. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Synergistic effect between strongly coupled CoAl layered double hydroxides and graphene for the electrocatalytic reduction of oxygen

    International Nuclear Information System (INIS)

    Wang, Yinling; Wang, Zhangcui; Wu, Xiaoqin; Liu, Xiaowang; Li, Maoguo

    2016-01-01

    Highlights: • CoAl-LDHs were synthesized on the surface of graphene oxide in situ. • The oxygen reduction reaction activity of the catalyst was investigated. • The synergistic effect between CoAl-LDHs and rGO is discussed in detail. • The roles of Co 2+ in the LDHs were clarified. - Abstract: Precious metal-free electrocatalysts with high efficiency and durability for the oxygen reduction reaction (ORR) are strongly desired in the field of energy technology. Herein, the CoAl layered double hydroxides (CoAl-LDHs)/reduced graphene oxide (rGO) composites were successfully prepared by growing CoAl-LDHs on the surface of GO in situ via coprecipitation and subsequently hydrothermal treatment. The structure, composition, morphology and ORR catalytic activity of the CoAl-LDHs/rGO composites were investigated as a function of mass ratios of CoAl-LDHs and GO. The results show that there is an optimum mass ratio of CoAl-LDHs and GO (w CoAl-LDHs :w GO = 1:5) for the ORR catalytic activity, where the electron transfer number for ORR at the CoAl-LDHs/rGO composites reaches to 3.5, closing to the full four-electron process. The synergistic effect between CoAl-LDHs and rGO is discussed in detail and the discussion is instructive for the construction of the better transition metal oxides/carbon composite-based ORR catalysts.

  11. Two-Dimensional Layered Double Hydroxide Derived from Vermiculite Waste Water Supported Highly Dispersed Ni Nanoparticles for CO Methanation

    Directory of Open Access Journals (Sweden)

    Panpan Li

    2017-03-01

    Full Text Available Expanded multilayered vermiculite (VMT was successfully used as catalyst support and Ni/VMT synthesized by microwave irradiation assisted synthesis (MIAS exhibited excellent performance in our previous work. We also developed a two-dimensional porous SiO2 nanomesh (2D VMT-SiO2 by mixed-acid etching of VMT. Compared with three-dimensional (3D MCM-41, 2D VMT-SiO2 as a catalyst support provided a superior position for implantation of NiO species and the as-obtained catalyst exhibited excellent performance. In this paper, we successfully synthesized a layered double hydroxide (LDH using the spent liquor after mixed-acid etching of VMT, which mainly contained Mg2+ and Al3+. The as-calcined layered double oxide (LDO was used as a catalyst support for CO methanation. Compared with Ni/MgAl-LDO, Ni/VMT-LDO had smaller active component particles; therefore, in this study, it exhibited excellent catalytic performance over the whole temperature range of 250–500 °C. Ni/VMT-LDO achieved the best activity with 87.88% CO conversion, 89.97% CH4 selectivity, and 12.47 × 10−2·s−1 turn over frequency (TOF at 400 °C under a gas hourly space velocity of 20,000 mL/g/h. This study demonstrated that VMT-LDO as a catalyst support provided an efficient way to develop high-performance catalysts for synthetic natural gas (SNG from syngas.

  12. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides: an in situ X-ray powder diffraction study

    DEFF Research Database (Denmark)

    Johnsen, Rune; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO3 CoAl-Cl CoAl-CO3, CoAl-Cl CoAl-NO3 and CoAl-CO3 CoAl-SO4. The XRPD data show that the CoAl-CO3 CoAl-Cl process...

  13. Local environment and composition of magnesium gallium layered double hydroxides determined from solid-state 1H and 71Ga NMR spectroscopy

    DEFF Research Database (Denmark)

    Boisen Staal, Line; Lipton, Andrew S.; Zorin, Vadim

    2014-01-01

    Ordering of gallium(III) in a series of magnesium gallium (MgGa) layered double hydroxides (LDHs), [Mg1−xGax(OH)2(NO3)x·yH2O] was investigated using solid-state 1H and 71Ga NMR spectroscopy as well as powder X-ray diffraction. Three different proton environments from Mg3single bondOH, Mg2Gasingle...

  14. Self-Assembly of Single-Layer CoAl-Layered Double Hydroxide Nanosheets on 3D Graphene Network Used as Highly Efficient Electrocatalyst for Oxygen Evolution Reaction.

    Science.gov (United States)

    Ping, Jianfeng; Wang, Yixian; Lu, Qipeng; Chen, Bo; Chen, Junze; Huang, Ying; Ma, Qinglang; Tan, Chaoliang; Yang, Jian; Cao, Xiehong; Wang, Zhijuan; Wu, Jian; Ying, Yibin; Zhang, Hua

    2016-09-01

    A non-noble metal based 3D porous electrocatalyst is prepared by self-assembly of the liquid-exfoliated single-layer CoAl-layered double hydroxide nanosheets (CoAl-NSs) onto 3D graphene network, which exhibits higher catalytic activity and better stability for electrochemical oxygen evolution reaction compared to the commercial IrO2 nanoparticle-based 3D porous electrocatalyst. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Ionic liquids as surfactants for layered double hydroxide fillers: effect on the final properties of poly(butylene adipate-co-terephthalate)

    Czech Academy of Sciences Publication Activity Database

    Livi, S.; Lins, L. C.; Peter, Jakub; Beneš, Hynek; Kredatusová, Jana; Donato, R. K.; Pruvost, S.

    2017-01-01

    Roč. 7, č. 10 (2017), s. 1-16, č. článku 297. ISSN 2079-4991 R&D Projects: GA ČR(CZ) GA17-08273S Institutional support: RVO:61389013 Keywords : ionic liquids * poly(butylene adipate-co-terephthalate) * layered double hydroxide Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 3.553, year: 2016

  16. Nickel–cobalt layered double hydroxide ultrathin nanoflakes decorated on graphene sheets with a 3D nanonetwork structure as supercapacitive materials

    International Nuclear Information System (INIS)

    Yan, Tao; Li, Ruiyi; Li, Zaijun

    2014-01-01

    Graphical abstract: The microwave heating reflux approach was developed for the fabrication of nickel–cobalt layered double hydroxide ultrathin nanoflakes decorated on graphene sheets, in which ammonia and ethanol were used as the precipitator and medium for the synthesis. The obtained composite shows a 3D flowerclusters morphology with nanonetwork structure and largely enhanced supercapacitive performance. - Highlights: • The paper reported the microwave synthesis of nickel–cobalt layered double hydroxide/graphene composite. • The novel synthesis method is rapid, green, efficient and can be well used to the mass production. • The as-synthesized composite offers a 3D flowerclusters morphology with nanonetwork structure. • The composite offers excellent supercapacitive performance. • This study provides a promising route to design and synthesis of advanced graphene-based materials with the superiorities of time-saving and cost-effective characteristics. - Abstract: The study reported a novel microwave heating reflux method for the fabrication of nickel–cobalt layered double hydroxide ultrathin nanoflakes decorated on graphene sheets (GS/NiCo-LDH). Ammonia and ethanol were employed as precipitant and reaction medium for the synthesis, respectively. The resulting GS/NiCo-LDH offers a 3D flowerclusters morphology with nanonetwork structure. Due to the greatly enhanced rate of electron transfer and mass transport, the GS/NiCo-LDH electrode exhibits excellent supercapacitive performances. The maximum specific capacitance was found to be 1980.7 F g −1 at the current density of 1 A g −1 . The specific capacitance can remain 1274.7 F g −1 at the current density of 15 A g −1 and it has an increase of about 2.9% after 1500 cycles. Moreover, the study also provides a promising approach for the design and synthesis of metallic double hydroxides/graphene hybrid materials with time-saving and cost-effective characteristics, which can be potentially applied

  17. Development of efficient electrocatalysts via molecular hybridization of NiMn layered double hydroxide nanosheets and graphene

    Science.gov (United States)

    Ma, Wei; Ma, Renzhi; Wu, Jinghua; Sun, Pengzhan; Liu, Xiaohe; Zhou, Kechao; Sasaki, Takayoshi

    2016-05-01

    Ni2+Mn3+ layered double hydroxide (LDH) nanoplatelets have been hydrothermally synthesized in a homogeneous precipitation of mixed Ni2+/Mn2+ salts at a molar ratio of 2 : 1 via the hydrolysis of hexamethylenetetramine (HMT) and in situ oxidation with H2O2. After anion-exchange, NiMn LDH was exfoliated into unilamellar nanosheets. Subsequent flocculation of NiMn LDH nanosheets with (reduced) graphene oxide (GO/rGO) into superlattice composites was achieved and further tested as electrocatalysts for oxygen evolution reaction (OER). The face-to-face heteroassembly of NiMn LDH nanosheets with conductive rGO at an alternating sequence resulted in a small overpotential of 0.26 V and a Tafel slope of 46 mV per decade, which is much superior to as-exfoliated nanosheets. The analyses of electrochemical activity surface area (ECSA) and impedance spectra clearly indicated that the superlattice structure was ideal in facilitating the migration/transfer of the charge and reactants, revealing the electrochemical energetics and mechanism behind the synergistic effect arising from molecular hybridization. The proof of concept toward total water splitting using the newly developed hybrid electrocatalyst was demonstrated by an electrolysis cell powered by a single AA battery.Ni2+Mn3+ layered double hydroxide (LDH) nanoplatelets have been hydrothermally synthesized in a homogeneous precipitation of mixed Ni2+/Mn2+ salts at a molar ratio of 2 : 1 via the hydrolysis of hexamethylenetetramine (HMT) and in situ oxidation with H2O2. After anion-exchange, NiMn LDH was exfoliated into unilamellar nanosheets. Subsequent flocculation of NiMn LDH nanosheets with (reduced) graphene oxide (GO/rGO) into superlattice composites was achieved and further tested as electrocatalysts for oxygen evolution reaction (OER). The face-to-face heteroassembly of NiMn LDH nanosheets with conductive rGO at an alternating sequence resulted in a small overpotential of 0.26 V and a Tafel slope of 46 mV per decade

  18. Layered double hydroxide nanoparticles promote self-renewal of mouse embryonic stem cells through the PI3K signaling pathway

    Science.gov (United States)

    Wu, Youjun; Zhu, Rongrong; Zhou, Yang; Zhang, Jun; Wang, Wenrui; Sun, Xiaoyu; Wu, Xianzheng; Cheng, Liming; Zhang, Jing; Wang, Shilong

    2015-06-01

    Embryonic stem cells (ESCs) hold great potential for regenerative medicine due to their two unique characteristics: self-renewal and pluripotency. Several groups of nanoparticles have shown promising applications in directing the stem cell fate. Herein, we investigated the cellular effects of layered double hydroxide nanoparticles (LDH NPs) on mouse ESCs (mESCs) and the associated molecular mechanisms. Mg-Al-LDH NPs with an average diameter of ~100 nm were prepared by hydrothermal methods. To determine the influences of LDH NPs on mESCs, cellular cytotoxicity, self-renewal, differentiation potential, and the possible signaling pathways were explored. Evaluation of cell viability, lactate dehydrogenase release, ROS generation and apoptosis demonstrated the low cytotoxicity of LDH NPs. The alkaline phosphatase activity and the expression of pluripotency genes in mESCs were examined, which indicated that exposure to LDH NPs could support self-renewal and inhibit spontaneous differentiation of mESCs under feeder-free culture conditions. The self-renewal promotion was further proved to be independent of the leukemia inhibitory factor (LIF). Furthermore, cells treated with LDH NPs maintained the potential to differentiate into all three germ layers both in vitro and in vivo through formation of embryoid bodies and teratomas. In addition, we observed that LDH NPs initiated the activation of the PI3K/Akt pathway, while treatment with the PI3K inhibitor LY294002 could block the effects of LDH NPs on mESCs. The results confirmed that the promotion of self-renewal by LDH NPs was associated with activation of the PI3K/Akt signaling pathway. Altogether, our studies identified a new role of LDH NPs in maintaining self-renewal of mouse ES cells which could potentially be applied in stem cell research.Embryonic stem cells (ESCs) hold great potential for regenerative medicine due to their two unique characteristics: self-renewal and pluripotency. Several groups of nanoparticles

  19. In-syringe extraction using dissolvable layered double hydroxide-polymer sponges templated from hierarchically porous coordination polymers.

    Science.gov (United States)

    Ghani, Milad; Frizzarin, Rejane M; Maya, Fernando; Cerdà, Víctor

    2016-07-01

    Herein we report the use of cobalt porous coordination polymers (PCP) as intermediates to prepare advanced extraction media based on layered double hydroxides (LDH) supported on melamine polymer foam. The obtained dissolvable Ni-Co LDH composite sponges can be molded and used as sorbent for the in-syringe solid-phase extraction (SPE) of phenolic acids from fruit juices. The proposed sorbent is obtained due to the surfactant-assisted self-assembly of Co(II)/imidazolate PCPs on commercially available melamine foam, followed by the in situ conversion of the PCP into the final dissolvable LDH coating. Advantageous features for SPE are obtained by using PCPs with hierarchical porosity (HPCPs). The LDH-sponge prepared using intermediate HPCPs (HLDH-sponge) is placed in the headspace of a glass syringe, enabling flow-through extraction followed by analyte elution by the dissolution of the LDH coating in acidic conditions. Three phenolic acids (gallic acid, p-hydroxybenzoic acid and caffeic acid) were extracted and quantified using high performance liquid chromatography. Using a 5mL sample volume, the obtained detection limits were 0.15-0.35μgL(-1). The proposed method for the preparation of HLDH-sponges showed a good reproducibility as observed from the intra- and inter-day RSD's, which were <10% for all analytes. The batch-to-batch reproducibility for three different batches of HLDH-sponges was 10.6-11.2%. Enrichment factors of 15-21 were obtained. The HLDH-sponges were applied satisfactorily to the determination of phenolic acids in natural and commercial fruit juices, obtaining relative recoveries among 89.7-95.3%. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Improvement of the crystallinity and photocatalytic property of zinc oxide as calcination product of Zn–Al layered double hydroxide

    International Nuclear Information System (INIS)

    Ahmed, Abdullah Ahmed Ali; Talib, Zainal Abidin; Hussein, Mohd Zobir bin; Zakaria, Azmi

    2012-01-01

    Highlights: ► ZnO phase and ZnAl 2 O 4 spinel can be formed as Zn–Al–NO 3 –LDH calcination products. ► The crystallinity of ZnO phase increased with an increase of calcination temperature. ► The optical band gaps of ZnO were improved with an increase in temperature. ► The oxygen vacancies in ZnO and ZnAl 2 O 4 generated the ESR signals. - Abstract: Zinc oxide with different degrees of crystallinity can be formed as Zn–Al-layered double hydroxide (Zn–Al–NO 3 –LDH) calcination products. ZnAl 2 O 4 spinel is also formed in a range of calcination temperatures from 600 to 1000 °C from the LDH. X-ray diffraction patterns showed that the crystallinity of the ZnO phase increased as calcination temperatures increased. The LDH structure was fully collapsed at and above 400 °C. The photocatalytic activity was determined by UV–VIS–NIR diffuse reflectance spectroscopy. The band gap of the calcined samples increased as the calcination temperature increased. Electron spin resonance (ESR) spectra of the fresh and calcined LDH at room temperature demonstrated that oxygen vacancies in the ZnO and ZnAl 2 O 4 were responsible for the generation of ESR signals. One BET specific surface area increased from 1 m 2 /g for the LDH to a maximum at 400 °C (43 m 2 /g) and decreased thereafter down to 6 m 2 /g at 1000 °C.

  1. Synthesis, characterization and magnetic behavior of Mg–Fe–Al mixed oxides based on layered double hydroxide

    Energy Technology Data Exchange (ETDEWEB)

    Heredia, Angélica C., E-mail: angelicacheredia@gmail.com [Universidad Tecnológica Nacional, Facultad Regional Córdoba-CITeQ, Maestro López esq. Cruz Roja Argentina, Ciudad Universitaria, 5016 Córdoba (Argentina); Oliva, Marcos I. [IFEG, Universidad Nacional de Córdoba, Córdoba (Argentina); CONICET (Argentina); Agú, Ulises [Universidad Tecnológica Nacional, Facultad Regional Córdoba-CITeQ, Maestro López esq. Cruz Roja Argentina, Ciudad Universitaria, 5016 Córdoba (Argentina); CONICET (Argentina); Zandalazini, Carlos I. [CONICET (Argentina); INFIQC, FCQ Universidad Nacional de Córdoba, Córdoba (Argentina); Marchetti, Sergio G. [CINDECA, UNLP, Buenos Aires (Argentina); Herrero, Eduardo R.; Crivello, Mónica E. [Universidad Tecnológica Nacional, Facultad Regional Córdoba-CITeQ, Maestro López esq. Cruz Roja Argentina, Ciudad Universitaria, 5016 Córdoba (Argentina)

    2013-09-15

    In the present work, Mg–Al–Fe layered double hydroxides were prepared by coprecipitation reaction with hydrothermal treatment. The characterization of precursors and their corresponding calcinated products (mixed oxides) were carried out by X ray diffraction, X-ray photoelectron spectroscopy (XPS), termogravimetric analysis and differential scanning calorimetry, diffuse reflectance UV–vis spectroscopy, specific surface area, Mössbauaer and magnetic properties. The Fe{sup 3+} species were observed in tetrahedrally and octahedrally coordination in brucite layered. The XPS analysis shows that the Fe{sup 3+} ions can be found in two coordination environments (tetrahedral and octahedral) as mixed oxides, and as spinel-structure. Oxides show a decrease in the specific surface areas when the iron loading is increased. The magnetic and Mössbauaer response show that MgAlFe mixed oxides are different behaviours such as different population ratios of ferromagnetic, weak-ferromagnetic, paramagnetic and superparamagnetic phases. The better crystallization of spinel structure with increased temperature, is correlated with the improved magnetic properties. - Highlights: • Mg–Al–Fe were successfully prepared by coprecipitation with hydrothermal treatment. • MgO, α-Fe{sub 2}O{sub 3,} MgFe{sub 2}O{sub 4} were detected by XRD in the calcined samples. • The Fe{sup 3+} is in tetrahedral and octahedral coordination in the brucite layered. • The specific surface area is directly related with the iron content. • The magnetic properties and MgFe{sub 2}O{sub 4} improve with increasing calcination temperature.

  2. Investigation of γ-(2,3-Epoxypropoxypropyltrimethoxy Silane Surface Modified Layered Double Hydroxides Improving UV Ageing Resistance of Asphalt

    Directory of Open Access Journals (Sweden)

    Canlin Zhang

    2017-01-01

    Full Text Available γ-(2,3-Epoxypropoxypropyltrimethoxy silane surface modified layered double hydroxides (KH560-LDHs were prepared and used to improve the ultraviolet ageing resistance of asphalt. The results of X-ray photoelectron spectrometry (XPS indicated that KH560 has been successfully grafted onto the surface of LDHs. The agglomeration of LDHs particles notably reduced after KH560 surface modification according to scanning electron microscopy (SEM, which implied that the KH560 surface modification was helpful to promote the dispersibility of LDHs in asphalt. Then, the influence of KH560-LDHs and LDHs on the physical and rheological properties of asphalt before and after UV ageing was thoroughly investigated. The storage stability test showed that the difference in softening point (ΔS of LDHs modified asphalt decreased from 0.6 °C to 0.2 °C at an LDHs content of 1% after KH560 surface modification, and the tendency became more pronounced with the increase of LDH content, indicating that KH560 surface modification could improve the stability of LDHs in asphalt. After UV ageing, the viscous modulus (G’’ of asphalt significantly reduced, and correspondingly, the elastic modulus (G’ and rutting factor (G*/sin δ rapidly increased. Moreover, the asphaltene increased and the amount of “bee-like” structures of the asphalt decreased. Compared with LDHs, KH560-LDHs obviously restrained performance deterioration of the asphalt, and helped to relieve the variation of the chemical compositions and morphology of asphalt, which suggested that the improvement of KH560-LDHs on UV ageing resistance of asphalt was superior to LDHs.

  3. Effect of added zinc on the properties of cobalt-containing ceramic pigments prepared from layered double hydroxides

    Science.gov (United States)

    Pérez-Bernal, M. E.; Ruano-Casero, R. J.; Rives, V.

    2009-09-01

    Layered double hydroxides (LDHs) with the hydrotalcite-type structure containing Co and Al, or Zn, Co and Al in the brucite-like layers and carbonate in the interlayer have been prepared by coprecipitation. The Zn/Co molar ratio was kept to 1 in all samples, while the divalent/trivalent molar ratio was varied from 2/1 to 1/2. The samples have been characterised by element chemical analysis, powder X-ray diffraction, differential thermal and thermogravimetric analysis, temperature-programmed reduction and FT-IR spectroscopy. A single hydrotalcite-like phase is formed for samples with molar ratio 2/1, which crystallinity decreases as the Al content is increased, developing small amounts of diaspore and dawsonite and probably an additional amorphous phase. Calcination at 1200 °C in air led to formation of spinels; a small amount of NaAlO 2 was observed in the Al-rich samples, which was removed by washing. The nature of the spinels formed (containing Co II, Co III, Al III and Zn II) strongly depends on the cations molar ratio in the starting materials and the calcination treatment, leading to a partial oxidation of Co II species to Co III ones. Colour properties ( L* a* b*) of the original and calcined solids have been measured. While the original samples show a pink colour (lighter for the series containing Zn), the calcined Co,Al samples show a dark blue colour and the Zn,Co,Al ones a green colour. Changes due to the different molar ratios within a given calcined series are less evident than between samples with the same composition in different series. These calcined materials could be usable as ceramic pigments.

  4. Topotactic Synthesis of Porous Cobalt Ferrite Platelets from a Layered Double Hydroxide Precursor and Their Application in Oxidation Catalysis.

    Science.gov (United States)

    Ortega, Klaus Friedel; Anke, Sven; Salamon, Soma; Özcan, Fatih; Heese, Justus; Andronescu, Corina; Landers, Joachim; Wende, Heiko; Schuhmann, Wolfgang; Muhler, Martin; Lunkenbein, Thomas; Behrens, Malte

    2017-09-12

    Monocrystalline, yet porous mosaic platelets of cobalt ferrite, CoFe 2 O 4 , can be synthesized from a layered double hydroxide (LDH) precursor by thermal decomposition. Using an equimolar mixture of Fe 2+ , Co 2+ , and Fe 3+ during co-precipitation, a mixture of LDH, (Fe II Co II ) 2/3 Fe III 1/3 (OH) 2 (CO 3 ) 1/6 ⋅m H 2 O, and the target spinel CoFe 2 O 4 can be obtained in the precursor. During calcination, the remaining Fe II fraction of the LDH is oxidized to Fe III leading to an overall Co 2+ :Fe 3+ ratio of 1:2 as required for spinel crystallization. This pre-adjustment of the spinel composition in the LDH precursor suggests a topotactic crystallization of cobalt ferrite and yields phase pure spinel in unusual anisotropic platelet morphology. The preferred topotactic relationship in most particles is [111] Spinel ∥[001] LDH . Due to the anion decomposition, holes are formed throughout the quasi monocrystalline platelets. This synthesis approach can be used for different ferrites and the unique microstructure leads to unusual chemical properties as shown by the application of the ex-LDH cobalt ferrite as catalyst in the selective oxidation of 2-propanol. Compared to commercial cobalt ferrite, which mainly catalyzes the oxidative dehydrogenation to acetone, the main reaction over the novel ex-LDH cobalt is dehydration to propene. Moreover, the oxygen evolution reaction (OER) activity of the ex-LDH catalyst was markedly higher compared to the commercial material. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. EXAFS and FTIR studies of selenite and selenate sorption by alkoxide-free sol–gel generated Mg–Al–CO 3 layered double hydroxide with very labile interlayer anions

    KAUST Repository

    Chubar, Natalia

    2014-08-08

    © the Partner Organisations 2014. Current research on Layered Double Hydroxides (LDHs, also known as hydrotalcites, HTs) is predominantly focused on their intercalations, but the industrial application of LDHs for anion exchange adsorption has not yet been achieved. It was recently recognized that, to develop LDH applications, these materials should be produced using methods other than direct co-precipitation. Mg-Al-CO3LDH produced using an alkoxide-free sol-gel synthesis showed exceptional removal properties for aqueous selenium species. Se K-edge EXAFS/XANES and FTIR studies (supporting the data by XRD patterns) were performed to explain the unusual adsorptive performance of Mg-Al LDH by revealing the molecular-level mechanism of HSeO3 -, SeO4 2-and {HSeO3 -+ SeO4 2-} uptake at pH 5, 7 and 8.5. The role of inner-sphere complexation (exhibited by inorganic adsorbents with good performance) in adsorption of both selenium aqueous species was not confirmed. However, Mg-Al LDH fully met the other expectations regarding the involvement of the interlayer anions. The interlayer carbonate (due to its favorable speciation and generous HT hydration) gave a "second breath" to selenite sorption and was the only mechanism that controlled the removal of Se(vi). Because inner sphere complexation was the leading mechanism for selenite removal, ion exchange via surface OH-and interlayer CO3 2-species was the only mechanism for selenate removal; both of these species were easily bound to Mg-Al LDH (on its surface and gently parked into the interlayer forming a multilayer without violation of the structure of Mg-Al-CO3LDH). This work provides the first theoretical explanation of why it is more difficult to sorb selenate than selenite and which material should be used for this purpose. This journal is

  6. A ratiometric fluorescence sensor for Be{sup 2+} based on Beryllon II/layered double hydroxide ultrathin films

    Energy Technology Data Exchange (ETDEWEB)

    Ji Xiaolan; Shi Wenying; Zhang Shitong [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Wei Min, E-mail: weimin@mail.buct.edu.cn [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Evans, David G.; Duan Xue [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China)

    2012-05-30

    Graphical abstract: This paper reports the fabrication of Beryllon II/layered double hydroxide ultrathin films via the layer-by-layer assembly technique, which can be used as a ratiometric fluorescence chemosensor for Be{sup 2+} with good repeatability, high stability and excellent selectivity. Highlights: Black-Right-Pointing-Pointer A ratiometric fluorescence sensor for Be{sup 2+} was fabricated by LBL method. Black-Right-Pointing-Pointer The chemosensor shows a broad linear response range and a low detection limit. Black-Right-Pointing-Pointer The sensor exhibits a high stability and excellent selectivity toward Be{sup 2+}. Black-Right-Pointing-Pointer The chemosensor can be easily regenerated and reused. - Abstract: A ratiometric fluorescence sensor for Be{sup 2+} has been fabricated via alternate assembly of 2-(3,6-disulfo-8-hydroxynaphthylazo)-1,8-dihydroxynaphthalene-3, 6-disulfonate (Beryllon II) and MgAl-LDH nanosheets on quartz substrates using the layer-by-layer (LBL) deposition technique. UV-vis absorption and the fluorescence emission spectroscopy indicate a stepwise and regular growth of the Beryllon II/LDH UTFs upon increasing deposition cycle. The film of Beryllon II/LDH possesses a periodic layered structure perpendicular to the substrate revealed by X-ray diffraction and scanning electron microscopy. Atomic force microscopy images show that the film surface is continuous and uniform. The Beryllon II/LDH UTFs display ratiometric fluorescence response for Be{sup 2+} with a linear response range in 1.0 Multiplication-Sign 10{sup -7}-1.9 Multiplication-Sign 10{sup -6} mol L{sup -1} and a detection limit of 4.2 Multiplication-Sign 10{sup -9} mol L{sup -1}. Furthermore, the ratiometric sensor exhibits good repeatability, high stability (thermal, storage and mechanical) as well as excellent selectivity toward Be{sup 2+}. XPS and Raman measurements demonstrate that the specific response of the sensor is attributed to the coordination between Be{sup 2

  7. Formation of Zn-rich phyllosilicate, Zn-layered double hydroxide and hydrozincite in contaminated calcareous soils

    Energy Technology Data Exchange (ETDEWEB)

    Jacquat, Olivier; Voegelin, Andreas; Villard, Andre; Marcus, Matthew A.; Kretzschmar, Ruben

    2007-10-15

    Recent studies demonstrated that Zn-phyllosilicate- and Zn-layered double hydroxide-type (Zn-LDH) precipitates may form in contaminated soils. However, the influence of soil properties and Zn content on the quantity and type of precipitate forming has not been studied in detail so far. In this work, we determined the speciation of Zn in six carbonate-rich surface soils (pH 6.2 to 7.5) contaminated by aqueous Zn in the runoff from galvanized power line towers (1322 to 30090 mg/kg Zn). Based on 12 bulk and 23 microfocused extended X-ray absorption fine structure (EXAFS) spectra, the number, type and proportion of Zn species were derived using principal component analysis, target testing, and linear combination fitting. Nearly pure Zn-rich phyllosilicate and Zn-LDH were identified at different locations within a single soil horizon, suggesting that the local availabilities of Al and Si controlled the type of precipitate forming. Hydrozincite was identified on the surfaces of limestone particles that were not in direct contact with the soil clay matrix. With increasing Zn loading of the soils, the percentage of precipitated Zn increased from {approx}20% to {approx}80%, while the precipitate type shifted from Zn-phyllosilicate and/or Zn-LDH at the lowest studied soil Zn contents over predominantly Zn-LDH at intermediate loadings to hydrozincite in extremely contaminated soils. These trends were in agreement with the solubility of Zn in equilibrium with these phases. Sequential extractions showed that large fractions of soil Zn ({approx}30% to {approx}80%) as well as of synthetic Zn-kerolite, Zn-LDH, and hydrozincite spiked into uncontaminated soil were readily extracted by 1 M NH{sub 4}NO{sub 3} followed by 1 M NH{sub 4}-acetate at pH 6.0. Even though the formation of Zn precipitates allows for the retention of Zn in excess to the adsorption capacity of calcareous soils, the long-term immobilization potential of these precipitates is limited.

  8. Precipitation of the rare earth double sodium and rare earths from the sulfuric liquor and the conversion into rare earth hydroxides through meta ethic reaction

    International Nuclear Information System (INIS)

    Abreu, Renata D.; Oliveira, Ester F.; Brito, Walter de; Morais, Carlos A.

    2007-01-01

    This work presents the purification study of the rare earths through precipitation of rare earth and sodium (Na TR (SO 4 ) 2 . x H 2 O)) double sulfate and his conversion to rare earths hydroxide TR(OH) 3 by meta ethic reaction through the addition of sodium hydroxide solution to the solid double sulfate. The study used the sulfuric liquor as rare earth sample, generated in the chemical processing of the monazite with sulfuric acid by the Industrias Nucleares do Brasil - INB, Brazil, after the thorium and uranium extraction. The work investigated the influence of the main variables involved in the precipitation of Na TR(SO 4 ) 2 .xH 2 O and in the conversion for the TR(OH) 3 , as follows: type and excess of the precipitation agent, temperature and time reaction. The obtained solid composites were characterized by X-ray diffraction, infrared and chemical analysis. The double sulfate diffractogram indicated the Na TR(SO 4 ) 2 mono-hydrated. The characterization of the metatese products has shown that, for obtaining the complete conversion of NaTR(SO 4 ) 2 .H 2 O into TR(OH) 3 , the reaction must be hot processed (∼70 deg C) and with small excess of Na OH (≤ 5 percent). (author)

  9. Synthesis of Mesoporous Silica@Co–Al Layered Double Hydroxide Spheres: Layer-by-Layer Method and Their Effects on the Flame Retardancy of Epoxy Resins

    OpenAIRE

    Jiang, Shu-Dong; Bai, Zhi-Man; Tang, Gang; Song, Lei; Stec, Anna A; Hull, T Richard; Hu, Yuan; Hu, Wei-Zhao

    2014-01-01

    Hierarchical mesoporous silica@Co–Al layered double hydroxide (m-SiO2@Co–Al LDH) spheres were prepared through a layer-by-layer assembly process, in order to integrate their excellent physical and chemical functionalities. TEM results depicted that, due to the electrostatic potential difference between m-SiO2 and Co–Al LDH, the synthetic m-SiO2@Co–Al LDH hybrids exhibited that m-SiO2 spheres were packaged by the Co–Al LDH nanosheets. Subsequently, the m-SiO2@Co–Al LDH spheres were incorporate...

  10. Magnesium Hydroxide

    Science.gov (United States)

    Magnesium hydroxide is used on a short-term basis to treat constipation.This medication is sometimes prescribed ... Magnesium hydroxide come as a tablet and liquid to take by mouth. It usually is taken as ...

  11. Aluminum Hydroxide

    Science.gov (United States)

    Aluminum hydroxide is used for the relief of heartburn, sour stomach, and peptic ulcer pain and to ... Aluminum hydroxide comes as a capsule, a tablet, and an oral liquid and suspension. The dose and ...

  12. Keggin type polyoxometalate H4[αSiW12O40].nH2O as intercalant for hydrotalcite

    Directory of Open Access Journals (Sweden)

    Neza Rahayu Palapa

    2017-06-01

    Full Text Available The synthesis of hydrotalcite and polyoxometalate H4[αSiW12O40].nH2O with the ratio (2:1, (1:1, (1:2 and (1:3 has been done. The product of intercalation was characterized using FT-IR spectrophotometer, XRD, and TG-DTA. Polyoxometalate H4[αSiW12O40].nH2O intercalated layered double hydroxide was optimised to use as adsorbent Congo red dye. Characterization using FT-IR was not showing the optimal insertion process. The result using XRD characterization was showed successful of polyoxometalate H4[αSiW12O40].nH2O inserted layered double hydroxide with a ratio (1:1 which the basal spacing was expanded from 7,8 Ȧ to 9,81 Ȧ. Furthermore, the thermal analysis was performed using TG-DTA. The result show that the decomposition of polyoxometalate H4[αSiW12O40].nH2O intercalated  hydrotalcite with ratio (1:1 was occured at 80oC to 400oC with a loss of OH in the layer at 150oC to 220oC, and then the decomposition of the compound polyoxometalate H4[αSiW12O40].nH2O at 350oC to 420oC. Keywords: Hydrotalcite, Layered Double Hydroxide, Polyoxometalate, Intercalation

  13. Lubrication performance and mechanisms of Mg/Al-, Zn/Al-, and Zn/Mg/Al-layered double hydroxide nanoparticles as lubricant additives

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shuo [School of Materials Science and Technology, China University of Geosciences (Beijing), 29 Xueyuan Road, Haidian Distract, Beijing 100083 (China); Nanoprobe Laboratory for Bio- & Nanotechnology and Biomimetics (NLBB), The Ohio State University, 201 W. 19th Avenue Columbus, OH 43210-1142 (United States); Bhushan, Bharat, E-mail: bhushan.2@osu.edu [Nanoprobe Laboratory for Bio- & Nanotechnology and Biomimetics (NLBB), The Ohio State University, 201 W. 19th Avenue Columbus, OH 43210-1142 (United States)

    2016-08-15

    Highlights: • Mg/Al-, Zn/Al- and Zn/Mg/Al-layered double hydroxide were synthesized. • Mg/Al-LDH had superior tribological performance compared to other LDHs. • The best thermal stability of Mg/Al-LDH was responsible for its friction property. - Abstract: Solid lubricant particles are commonly used as oil additives for low friction and wear. Mg/Al-, Zn/Al-, and Zn/Mg/Al-layered double hydroxides (LDH) were synthesized by coprecipitation method. The benefits of LDH nanoparticles are that they can be synthesized using chemical methods where size and shape can be controlled, and can be modified organically to allow dispersal in fluids. The LDH nanoparticles were characterized by X-ray diffraction, scanning electron microscope, thermogravimetry, and differential scanning calorimetry. A pin-on-disk friction and wear tester was used for evaluating the friction and wear properties of LDH nanoparticles as lubricant additives. LDH nanoparticles have friction-reducing and anti-wear properties compared to oil without LDHs. Mg/Al-LDH has the best lubrication, possibly due to better thermal stability in severe conditions.

  14. Hierarchical Ni-Co layered double hydroxide nanosheets on functionalized 3D-RGO films for high energy density asymmetric supercapacitor

    Science.gov (United States)

    Jiang, Liyang; Sui, Yanwei; Qi, Jiqiu; Chang, Yuan; He, Yezeng; Meng, Qingkun; Wei, Fuxiang; Sun, Zhi; Jin, Yunxue

    2017-12-01

    In this paper, ultrathin reduced graphene oxide films on nickel foam were fabricated via a facile dip-coating method combined with thermal reduction. Hierarchical Ni-Co layered double hydroxide nanosheets with network structure were electrodeposited on the ultrathin reduced graphene oxide films in a simple three-electrode system. The thickness of Ni-Co layered double hydroxide nanosheets can be controlled through adjusting the deposition temperature. The as-prepared electrode exhibited excellent electrochemical performance with specific capacitance of 1454.2 F g-1 at a current density of 1 A g-1. An asymmetric supercapacitor device was designed with the as-prepared composites as positive electrode material and Nitrogen-doped reduced graphene oxide as negative electrode material. This device could be operated in a working voltage range of 0-1.8 V in 1 M KOH aqueous electrolyte, delivering a high energy density of 56.4 W h kg-1 at a power density of 882.5 W kg-1. One supercapacitor can power two LEDs with rated voltage of 1.8-2.0 V. After 10,000 consecutive charge-discharge tests at 10 A g-1, this asymmetric supercapacitor revealed an excellent cycle life with 98.3% specific capacitance retention. These excellent electrochemical performances make it become one of most promising candidates for high energy supercapacitor device.

  15. Synthesis and Enhanced Corrosion Protection Performance of Reduced Graphene Oxide Nanosheet/ZnAl Layered Double Hydroxide Composite Films by Hydrothermal Continuous Flow Method.

    Science.gov (United States)

    Luo, Xiaohu; Yuan, Song; Pan, Xinyu; Zhang, Caixia; Du, Shuo; Liu, Yali

    2017-05-31

    Prevention of water, oxygen, and chloride ions contained in hydrotalcite interlayers from diffusing through the layered double hydroxides (LDH) is of crucial importance in corrosion protection. In this work, a hybrid composed of reduced graphene oxide (RGO) nanosheets/Zn 2+ /Al 3+ layered double hydroxide (RGO/ZnAl-LDH) composite films on the surface of 6N01 aluminum (Al) alloy was successfully synthesized by a novel and facile hydrothermal continuous flow method, which enabled direct growth of the composite on the surface of the Al alloy substrate. The structure and morphology of the RGO/ZnAl-LDH composite films were fully characterized. Based on electrochemical measurements in a NaCl solution, the RGO/ZnAl-LDH composite film significantly enhanced the corrosion protection, as compared with the ZnAl-LDH film. The RGO/ZnAl-LDH composite film could maintain an outstanding corrosion resistance after 7 days immersion in a high concentration of NaCl solution (i.e., 5.0 wt %). The enhanced corrosion resistance was attributed to the barrier effect on diffusion of water, oxygen, and chloride ions by the RGO contained in the RGO/ZnAl-LDH composite films.

  16. Self-assembly of exfoliated layered double hydroxide and graphene nanosheets for electrochemical energy storage in zinc/nickel secondary batteries

    Science.gov (United States)

    Long, Jun; Yang, Zhanhong; Huang, Jianhang; Zeng, Xiao

    2017-08-01

    In this work, the Zn-Al layered double hydroxide (Zn-Al LDH) is exfoliated. Ambient temperature ion exchange and chemical exfoliation route have been developed to synthesize the exfoliated layered double hydroxide/graphene compounds (Exfoliated LDH/G). The as-prepared Exfoliated LDH/G nanocomposites demonstrate no obvious impurity and good morphology, being characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). Here we intensively study the electrochemical performances of Exfoliated LDH/G and pure LDH electrodes for Zn-Ni secondary battery. It was found that the as-prepared Exfoliated LDH/G here exhibits higher and wide discharge voltage plateaus due to the well electrical conductivity and lower self-corrosion, which could promote charge-transfer of the exfoliated LDH. The preliminary results show that the Exfoliated LDH/G displays superior Zn-Ni secondary battery performance with outstanding reversible capacity, prominent cyclic performance (343 mA h g-1 after 1200 cycles at 1 C), highlighting the practicability of the self-assembly Exfoliated LDH/G for maximum anodic utilization of exfoliated LDH for power storage in Zn-Ni secondary battery.

  17. Lubrication performance and mechanisms of Mg/Al-, Zn/Al-, and Zn/Mg/Al-layered double hydroxide nanoparticles as lubricant additives

    International Nuclear Information System (INIS)

    Li, Shuo; Bhushan, Bharat

    2016-01-01

    Highlights: • Mg/Al-, Zn/Al- and Zn/Mg/Al-layered double hydroxide were synthesized. • Mg/Al-LDH had superior tribological performance compared to other LDHs. • The best thermal stability of Mg/Al-LDH was responsible for its friction property. - Abstract: Solid lubricant particles are commonly used as oil additives for low friction and wear. Mg/Al-, Zn/Al-, and Zn/Mg/Al-layered double hydroxides (LDH) were synthesized by coprecipitation method. The benefits of LDH nanoparticles are that they can be synthesized using chemical methods where size and shape can be controlled, and can be modified organically to allow dispersal in fluids. The LDH nanoparticles were characterized by X-ray diffraction, scanning electron microscope, thermogravimetry, and differential scanning calorimetry. A pin-on-disk friction and wear tester was used for evaluating the friction and wear properties of LDH nanoparticles as lubricant additives. LDH nanoparticles have friction-reducing and anti-wear properties compared to oil without LDHs. Mg/Al-LDH has the best lubrication, possibly due to better thermal stability in severe conditions.

  18. The influence of the UV irradiation intensity on photocatalytic activity of ZnAl layered double hydroxides and derived mixed oxides

    Directory of Open Access Journals (Sweden)

    Hadnađev-Kostić Milica S.

    2012-01-01

    Full Text Available Layered double hydroxides (LDHs have been studied to a great extent as environmental-friendly complex materials that can be used as photocatalysts or photocatalyst supports. ZnAl layered double hydroxides and their derived mixed oxides were chosen for the investigation of photocatalytic performances in correlation with the UV intensities measured in the South Pannonia region. Low supersaturation coprecipitation method was used for the ZnAl LDH synthesis. For the characterization of LDH and thermal treated samples powder X-ray diffraction (XRD, scanning electron microscopy (SEM, electron dispersive spectroscopy (EDS, nitrogen adsorption-desorption were used. The decomposition of azodye, methylene blue was chosen as photocatalytic test reaction. The study showed that the ZnAl mixed oxide obtained by thermal decomposition of ZnAl LDH has stable activity in the broader UV light irradiation range characterizing the selected region. Photocatalytic activity could be mainly attributed to the ZnO phase, detected both in LDH and thermally treated samples. The study showed that the ZnAl mixed oxide obtained by the calcination of ZnAl LDH has a stable activity within the measured UV light irradiation range; whereas the parent ZnAl LDH catalyst did not perform satisfactory when low UV irradiation intensity is implied.

  19. Compósitos de poli(álcool vinílico contendo hidroxissais lamelares de zinco, intercalados com corantes aniônicos azo (tropaeolina 0 e tropaeolina 00 Poly(vinyl alcohol composites containing layered hydroxide salts, intercalated with anionic azo dyes (tropaeolin 0 and tropaeolin 0

    Directory of Open Access Journals (Sweden)

    Marlon Luiz Neves da Silva

    2013-01-01

    Full Text Available Hidroxissais lamelares de zinco foram intercalados com corantes aniônicos azo, obtendo-se pigmentos de coloração laranja. Os materiais foram caracterizados por difração de raios X (XRD, espectroscopia vibracional na região do infravermelho com transformada de Fourier (FTIR, análise térmica (TGA/DTA/DSC e espectroscopia fotoeletrônica de raios X (XPS. Após caracterização, os pigmentos lamelares foram dispersos em uma matriz de poli(álcool vinílico - PVA, em concentrações variáveis, em relação à massa de PVA. Filmes homogêneos, transparentes e coloridos foram obtidos pelo método de "casting" úmido e mantidos em dessecador em umidade controlada de 65 % por uma semana e avaliados quanto às suas propriedades mecânicas. Devido às diferentes polaridades dos ânions intercalados, diferentes comportamentos foram observados para os pigmentos quando utilizados como cargas em PVA. Esse trabalho abre uma frente de pesquisas na utilização de hidroxissais lamelares intercalados com corantes aniônicos, como cargas alternativas em materiais compósitos poliméricos.Layered zinc hydroxide salts were intercalated with anionic azo dyes, obtaining orange pigments. The materials were characterized by X-ray diffraction (XRD, Fourier Transform Infrared spectroscopy (FTIR, thermal analysis (TGA/DTA/DSC and X-ray photoelectron spectroscopy (XPS. After characterization, the layered pigments were dispersed into a matrix of poly(vinyl alcohol - PVA, in variable concentrations, in relation to the PVA mass. Homogeneous, transparent and colorful films were obtained by wet casting method and kept in a desiccator at 65% of humidity for one week and evaluated in relation to their mechanical properties. Owing to the different intercalated anions polarities, different behaviors were observed for both pigments when used as fillers in PVA. This work opens a research front in the utilization of layered hydroxide salt intercalated with anionic dyes, as

  20. Hierarchical Ni-Co layered double hydroxide nanosheets entrapped on conductive textile fibers: a cost-effective and flexible electrode for high-performance pseudocapacitors

    Science.gov (United States)

    Nagaraju, Goli; Raju, G. Seeta Rama; Ko, Yeong Hwan; Yu, Jae Su

    2015-12-01

    Hierarchical three-dimensional (3D) porous nanonetworks of nickel-cobalt layered double hydroxide (Ni-Co LDH) nanosheets (NSs) are grown and decorated on flexible conductive textile substrate (CTs) via a simple two-electrode system based electrochemical deposition (ED) method. By applying a proper external cathodic voltage of -1.2 V for 15 min, the Ni-Co LDH NSs are densely deposited over the entire surface of the CTs with good adhesion. The flexible Ni-Co LDH NSs on CTs (Ni-Co LDH NSs/CTs) architecture with high porosity facilitates enhanced electrochemical performance in 1 M KOH electrolyte solution. The effect of growth concentration and external cathodic voltage on the electrochemical properties of Ni-Co LDH NSs/CTs is also investigated. The Ni10Co5 LDH NSs/CTs electrode exhibits a high specific capacitance of 2105 F g-1 at a current density of 2 A g-1 as well as an excellent cyclic stability as a pseudocapacitive electrode due to the advantageous properties of 3D interconnected porous frameworks of Ni10Co5 LDH NSs/CTs. This facile fabrication of bimetallic hydroxide nanostructures on CTs can provide a promising electrode for low-cost energy storage device applications.Hierarchical three-dimensional (3D) porous nanonetworks of nickel-cobalt layered double hydroxide (Ni-Co LDH) nanosheets (NSs) are grown and decorated on flexible conductive textile substrate (CTs) via a simple two-electrode system based electrochemical deposition (ED) method. By applying a proper external cathodic voltage of -1.2 V for 15 min, the Ni-Co LDH NSs are densely deposited over the entire surface of the CTs with good adhesion. The flexible Ni-Co LDH NSs on CTs (Ni-Co LDH NSs/CTs) architecture with high porosity facilitates enhanced electrochemical performance in 1 M KOH electrolyte solution. The effect of growth concentration and external cathodic voltage on the electrochemical properties of Ni-Co LDH NSs/CTs is also investigated. The Ni10Co5 LDH NSs/CTs electrode exhibits a high

  1. Superb adsorption capacity of hierarchical calcined Ni/Mg/Al layered double hydroxides for Congo red and Cr(VI) ions

    Energy Technology Data Exchange (ETDEWEB)

    Lei, Chunsheng [State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); College of Environmental & Safety Engineering, Changzhou University, Changzhou 213164 (China); Zhu, Xiaofeng [College of Environmental & Safety Engineering, Changzhou University, Changzhou 213164 (China); Zhu, Bicheng; Jiang, Chuanjia; Le, Yao [State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Yu, Jiaguo, E-mail: jiaguoyu@yahoo.com [State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Department of Physics, Faculty of Science, King Abdulaziz University, Jeddah 21589 (Saudi Arabia)

    2017-01-05

    Highlights: • Ni/Mg/Al layered double hydroxides (NMA-LDHs) synthesized. • NMA-LDHs with hierarchically hollow microsphere structure. • Calcined NMA-LDHs have large adsorption capacities for CR and Cr(VI) ions. - Abstract: The preparation of hierarchical porous materials as catalysts and sorbents has attracted much attention in the field of environmental pollution control. Herein, Ni/Mg/Al layered double hydroxides (NMA-LDHs) hierarchical flower-like hollow microspheres were synthesized by a hydrothermal method. After the NMA-LDHs was calcined at 600 °C, NMA-LDHs transformed into Ni/Mg/Al layered double oxides (NMA-LDOs), which maintained the hierarchical flower-like hollow structure. The crystal phase, morphology, and microstructure of the as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy elemental mapping, Fourier transform infrared spectroscopy, and nitrogen adsorption−desorption methods. Both the calcined and non-calcined NMA-LDHs were examined for their performance to remove Congo red (CR) and hexavalent chromium (Cr(VI)) ions in aqueous solution. The maximum monolayer adsorption capacities of CR and Cr(VI) ions over the NMA-LDOs sample were 1250 and 103.4 mg/g at 30 °C, respectively. Thermodynamic studies indicated that the adsorption process was endothermic in nature. In addition, the addition of coexisting anions negatively influenced the adsorption capacity of Cr(VI) ions, in the following order: CO{sub 3}{sup 2−} > SO{sub 4}{sup 2−} > H{sub 2}PO{sub 4}{sup −} > Cl{sup −}. This work will provide new insight into the design and fabrication of advanced adsorption materials for water pollutant removal.

  2. New insights into the intercalation chemistry of Al(OH)3.

    Science.gov (United States)

    Williams, Gareth R; Moorhouse, Saul J; Prior, Timothy J; Fogg, Andrew M; Rees, Nicholas H; O'Hare, Dermot

    2011-06-14

    This paper reports a number of recent developments in the intercalation chemistry of Al(OH)(3). From Rietveld refinement and solid-state NMR, it has been possible to develop a structural model for the recently reported [M(II)Al(4)(OH)(12)](NO(3))(2)·yH(2)O family of layered double hydroxides (LDHs). The M(2+) cations occupy half of the octahedral holes in the Al(OH)(3) layers, and it is thought that there is complete ordering of the metal ions while the interlayer nitrate anions are highly disordered. Filling the remainder of the octahedral holes in the layers proved impossible. While the intercalation of Li salts into Al(OH)(3) is facile, it was found that the intercalation of M(II) salts is much more capricious. Only with Co, Ni, Cu, and Zn nitrates and Zn sulfate were phase-pure LDHs produced. In other cases, there is either no reaction or a phase believed to be an LDH forms concomitantly with impurity phases. Reacting Al(OH)(3) with mixtures of M(II) salts can lead to the production of three-metal M(II)-M(II)'-Al LDHs, but it is necessary to control precisely the starting ratios of the two M(II) salts in the reaction gel because Al(OH)(3) displays selective intercalation of M nitrate (Li > Ni > Co ≈ Zn). The three-metal M(II)-M(II)'-Al LDHs exhibit facile ion exchange intercalation, which has been investigated in the first energy dispersive X-ray diffraction study of a chemical reaction system performed on Beamline I12 of the Diamond Light Source.

  3. Hydroxide catalysts for lignin depolymerization

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg T; Biddy, Mary J.; Kruger, Jacob S.; Chmely, Stephen C.; Sturgeon, Matthew

    2017-10-17

    Solid base catalysts and their use for the base-catalyzed depolymerization (BCD) of lignin to compounds such as aromatics are presented herein. Exemplary catalysts include layered double hydroxides (LDHs) as recyclable, heterogeneous catalysts for BCD of lignin.

  4. Hydroxide catalysts for lignin depolymerization

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg T.; Biddy, Mary J.; Chmely, Stephen C.; Sturgeon, Matthew

    2017-04-25

    Solid base catalysts and their use for the base-catalyzed depolymerization (BCD) of lignin to compounds such as aromatics are presented herein. Exemplary catalysts include layered double hydroxides (LDHs) as recyclable, heterogeneous catalysts for BCD of lignin.

  5. Pulse electrodeposition of CoFe thin films covered with layered double hydroxides as a fast route to prepare enhanced catalysts for oxygen evolution reaction

    Science.gov (United States)

    Sakita, Alan M. P.; Noce, Rodrigo Della; Vallés, Elisa; Benedetti, Assis V.

    2018-03-01

    A novel, ultra-fast, and one-step method for obtaining an effective catalyst for oxygen evolution reaction is proposed. The procedure consists in direct electrodeposition, in a free-nitrate bath, of CoFe alloy films covered with layered double hydroxides (LDH), by potentiostatic mode, in continuous or pulsed regime. The catalyst is directly formed on glassy carbon substrates. The best-prepared catalyst material reveals a mixed morphology with granular and dendritic CoFe alloy covered with a sponge of CoFe-LDH containing a Cl interlayer. An overpotential of η10 mA = 286 mV, with a Tafel slope of 48 mV dec-1, is obtained for the OER which displays the enhanced properties of the catalyst. These improved results demonstrate the competitiveness and efficacy of our proposal for the production of OER catalysts.

  6. Enhanced activity of CaFeMg layered double hydroxides-supported gold nanodendrites for the electrochemical evolution of oxygen and hydrogen in alkaline media

    Science.gov (United States)

    Havakeshian, Elaheh; Salavati, Hossein; Taei, Masoumeh; Hasheminasab, Fatemeh; Seddighi, Mohadeseh

    2018-02-01

    In this study, Au was electrodeposited on a support of CaFeMg layered double hydroxide and then, its catalytic activity was investigated for oxygen evolution reaction (OER) and hydrogen evolution reaction (HER). Field emission scanning electron microscopy images showed that a uniform porous film of aggregated nano-particles of the LDH has been decorated with Au nanodendrite-like structures (AuNDs@LDH). The results obtained from polarization curves, Tafel plots and electrochemical impedance spectroscopy showed that the AuNDs@LDH exhibits lower overpotential, higher current density, faster kinetics and enhanced stability for both of the OER and HER, in comparison with the single AuNPs and LDH catalysts.

  7. Layered double hydroxides for preparing CoMn{sub 2}O{sub 4} nanoparticles as anodes of lithium ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Xu; Ma, Jingjing; Yuan, Ruo, E-mail: yuanruo@swu.edu.cn; Yang, Xia, E-mail: xiayang2@swu.edu.cn

    2017-06-15

    In the field of lithium-ion batteries, CoMn{sub 2}O{sub 4} as an anode material has attracted a wide attention because it inherited the splendid electrochemical performances of Mn and Co-based metal oxides. Compared to graphite, Co-based oxides have a higher capacity which is about twice of the graphite. Moreover, Mn-based oxides have lower operating voltages and manganese exists abundantly in nature. Layered double hydroxides (LDHs), similar with brucite structure, were used as precursor for CoMn{sub 2}O{sub 4} nanoparticles in this work. Under high temperature process, the LDHs decomposed to CoMn{sub 2}O{sub 4} nanoparticles. When evaluated as anode materials for lithium ion batteries, the CoMn{sub 2}O{sub 4} nanoparticles behaved good electrochemical performance with the discharge and charge capacity of 733 mAh g{sup -1} and 721 mAh g{sup -1} at current density of 200 mA g{sup -1} after 100 cycles. This method for preparing CoMn{sub 2}O{sub 4} nanoparticles is easy, which may provide a way for synthesis of other bimetallic oxides and anodes of lithium ion batteries. - Highlights: • Layered double hydroxides were employed as precursors to synthesize CoMn{sub 2}O{sub 4}. • The CoMn{sub 2}O{sub 4} nanoparticles behaved good electrochemical performance. • This study provides a guideline for preparing bimetallic oxides.

  8. Ag-loaded MgSrFe-layered double hydroxide/chitosan composite scaffold with enhanced osteogenic and antibacterial property for bone engineering tissue.

    Science.gov (United States)

    Cao, Dandan; Xu, Zhengliang; Chen, Yixuan; Ke, Qinfei; Zhang, Changqing; Guo, Yaping

    2018-02-01

    Bone tissue engineering scaffolds for the reconstruction of large bone defects should simultaneously promote osteogenic differentiation and avoid postoperative infection. Herein, we develop, for the first time, Ag-loaded MgSrFe-layered double hydroxide/chitosan (Ag-MgSrFe/CS) composite scaffold. This scaffold exhibits three-dimensional interconnected macroporous structure with a pore size of 100-300 μm. The layered double hydroxide nanoplates in the Ag-MgSrFe/CS show lateral sizes of 200-400 nm and thicknesses of ∼50 nm, and the Ag nanoparticles with particle sizes of ∼20 nm are uniformly dispersed on the scaffold surfaces. Human bone marrow-derived mesenchymal stem cells (hBMSCs) present good adhesion, spreading, and proliferation on the Ag-MgSrFe/CS composite scaffold, suggesting that the Ag and Sr elements in the composite scaffold have no toxicity to hBMSCs. When compared with MgFe/CS composite scaffold, the Ag-MgSrFe/CS composite scaffold has better osteogenic property. The released Sr 2+ ions from the composite scaffold enhance the alkaline phosphatase activity of hBMSCs, promote the extracellular matrix mineralization, and increase the expression levels of osteogenic-related RUNX2 and BMP-2. Moreover, the Ag-MgSrFe/CS composite scaffold possesses good antibacterial property because the Ag nanoparticles in the composite scaffold effectively prevent biofilm formation against S. aureus. Hence, the Ag-MgSrFe/CS composite scaffold with excellent osteoinductivity and antibacterial property has a great potential for bone tissue engineering. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 863-873, 2018. © 2017 Wiley Periodicals, Inc.

  9. Síntese e caracterização de hidróxidos duplos a partir da lama vermelha Synthesis and characterization of layered double hydroxides from red mud

    Directory of Open Access Journals (Sweden)

    M. V. P. O. Cunha

    2011-03-01

    testar esses materiais como adsorventes de metais pesados.Bauxite refinery residues, commonly known as "red mud", have been shown to be capable of binding trace metals such as copper, cadmium, zinc, chromium, nickel and lead under suitable conditions. Neutralization of red mud is necessary because red muds are typically highly caustic, with a reaction pH of about 13. Much research has been carried out on utilization of red mud because it contains a lot of valuable components. Although utilization of the red mud as building material and as an absorbent is attractive because the red mud is used in bulk, nothing can be done without discarding valuable components such as titanium, zirconium and the main iron. Hydrotalcite-synthesis connected with recycling of alkali-solution is a prospective way for effective use of the solution under the strong demand for the environmental protection in the world. The hydrotalcite-like compounds, precipitated during neutralization, also remove oxy-anions of transition metals through a combination of intercalation and adsorption of the anionic species on the external surfaces. Layered double hydroxides (LDHs have been investigated for many years as host materials for a range of anion exchange intercalation reactions. The lamellar structure of LDHs can be used for the controlled addition or removal of a variety of species, both organic and inorganic. This is achieved through their ability to adjust the separation of the hydroxide layers, and the reactivity of the interlayer region. The resultant material adsorbs anions when placed in solution and reverts to the hydrotalcite structure. Significant advances have been made recently on the characterization of these materials, including structural studies on the mechanism of intercalation. The aim of this work was the synthesis and characterizations of LDHs from red mud that will be tested as adsorbent material for heavy metals.

  10. Closing the Phosphorus Loop by Recovering Phosphorus From Waste Streams With Layered Double Hydroxide Nanocomposites and Converting the Product into an Efficient Fertilizer

    Science.gov (United States)

    Yan, H.; Shih, K.

    2015-12-01

    Phosphorus (P) recovery has been frequently discussed in recent decades due to the uncertain availability and uneven distribution of global phosphate rock reserves. Sorption technology is increasingly considered as a reliable, efficient and environmentally friendly P removal method from aqueous solution. In this study, a series of Mg-Al-based layered double hydroxide nanocomposites and their corresponding calcined products were fabricated and applied as phosphate adsorbents. The prepared samples were with average size at ~50 nm and self-assembled into larger particles in irregular shapes. The results of batch adsorption experiments demonstrated that calcination significantly enhanced the adsorption ability of LDHs for phosphorus, and the maximum adsorption capacity of calcined Mg-Al-LDH was as high as 100.7 mg-P/g. Furthermore, incorporation of Zr4+ and La3+ into LDH materials increases the sorption selectivity as well as sorption amount of phosphorus in LDHs, which was confirmed by experiments operated in synthetic human urine. For the first time ammonia (NH4OH) and potassium hydroxide (KOH) solutions were employed to desorb the P-loaded LDH. Identification of solids derived from two eluting solutions showed that struvite (MgNH4PO4•6H2O, MAP) was precipitated in ammonia solution while most phosphate was desorbed into liquid phase in KOH system without crystallization of potassium struvite (MgKPO4•6H2O) due to its higher solubility. Quantitative X-ray diffraction technique was used to determine struvite contents in obtained solids and the results revealed that ~ 30% of adsorbed P was transferred into struvite form in the sample extracted by 0.5M NH4OH. Leaching tests suggested that the phosphorus releasing kinetics of ammonia treated LDH was comparable to that of pure struvite product, indicating that postsorption Mg-Al-LDH desorbed with ammonia could serve as a slow-releasing fertilizer in agriculture (see Figure 1).

  11. Variable Charge and Electrical Double Layer of Mineral-Water Interfaces: Silver Halides versus Metal (Hydr)Oxides

    NARCIS (Netherlands)

    Hiemstra, T.

    2012-01-01

    Classically, silver (Ag) halides have been used to understand thermodynamic principles of the charging process and the corresponding development of the electrical double layer (EDL). A mechanistic approach to the processes on the molecular level has not yet been carried out using advanced surface

  12. Efficient removal of dyes by a novel magnetic Fe{sub 3}O{sub 4}/ZnCr-layered double hydroxide adsorbent from heavy metal wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Dan; Li, Yang; Zhang, Jia [School of Environmental and Chemical Engineering, Shanghai University, No. 99 Shangda Road, Shanghai 200444 (China); Li, Wenhui [Department of Chemistry, East China University of Science and Technology, 130 Meilong Road, Shanghai 200237 (China); Zhou, Jizhi; Shao, Li [School of Environmental and Chemical Engineering, Shanghai University, No. 99 Shangda Road, Shanghai 200444 (China); Qian, Guangren, E-mail: grqian@shu.edu.cn [School of Environmental and Chemical Engineering, Shanghai University, No. 99 Shangda Road, Shanghai 200444 (China)

    2012-12-15

    Graphical abstract: To purify heavy metal wastewater (pickling waste liquor (PWL{sub A} and PWL{sub B}) and electroplating wastewater (EPW{sub C} and EPW{sub D})), a novel magnetic Fe{sub 3}O{sub 4}/ZnCr-LDH material was formed via two-step microwave hydrothermal method (Step 1 and Step 2) and applicable for organic dyes wastewater treatment. Highlights: Black-Right-Pointing-Pointer Fe{sub 3}O{sub 4}/ZnCr-layered double hydroxide adsorbent was produced from wastewater. Black-Right-Pointing-Pointer RSM was successfully applied to the optimization of the preparation conditions. Black-Right-Pointing-Pointer The maximum adsorption capacity of MO was found to be 240.16 mg/g. Black-Right-Pointing-Pointer The MO adsorption mechanism on MFLA was certified. Black-Right-Pointing-Pointer MFLA could be recycled after catalytic regeneration by the oxidation technology. - Abstract: A novel magnetic Fe{sub 3}O{sub 4}/ZnCr-layered double hydroxide adsorbent was produced from electroplating wastewater and pickling waste liquor via a two-step microwave hydrothermal method. Adsorption of methyl orange (MO) from water was studied using this material. The effects of three variables have been investigated by a single-factor method. The response surface methodology (RSM) based on Box-Behnken design was successfully applied to the optimization of the preparation conditions. The maximum adsorption capacity of MO was found to be 240.16 mg/g, indicating that this material may be an effective adsorbent. It was shown that 99% of heavy metal ions (Fe{sup 2+}, Fe{sup 3+}, Cr{sup 3+}, and Zn{sup 2+}) can be effectively removed into precipitates and released far less in the adsorption process. In addition, this material with adsorbed dye can be easily separated by a magnetic field and recycled after catalytic regeneration with advanced oxidation technology. Meanwhile, kinetic models, FTIR spectra and X-ray diffraction pattern were applied to the experimental data to examine uptake mechanism. The

  13. ZnO-Layered Double Hydroxide@Graphitic Carbon Nitride Composite for Consecutive Adsorption and Photodegradation of Dyes under UV and Visible Lights

    Science.gov (United States)

    Zhang, Luhong; Li, Li; Sun, Xiaoming; Liu, Peng; Yang, Dongfang; Zhao, Xiusong

    2016-01-01

    In this work, a ZnO-layered double hydroxide@graphitic carbon nitride composite (ZnO-LDH@C3N4) was synthesized via co-precipitation method with solvothermal treatment. The structure and morphology of ZnO-LDH@C3N4 composite were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopes/transmission electron microscopes (SEM/TEM), N2 adsorption/desorption, ultraviolet visible diffuse reflectance spectroscopy (UV-Vis-DRS), photoluminescence spectrometer (PL) and electrochemical impedance spectroscopy (EIS). The adsorption and photocatalytic properties of ZnO-LDH@C3N4 composite towards the organic dyes: Orange II sodium salt (OrgII, an anionic azo dye) and methylene blue (MB, a cationic azo dye) were investigated. Compared to ZnO-LDH and g-C3N4, the ZnO-LDH@C3N4 composite displayed an excellent performance in both adsorption and photocatalytic degradation of the organic dyes. Moreover, a combination of ZnO-LDH and g-C3N4 significantly improved the photocatalytic performance of ZnO-LDH and g-C3N4 under visible-light irradiation. The adsorption and photocatalytic mechanism were also investigated. PMID:28774047

  14. ZnO-Layered Double Hydroxide@Graphitic Carbon Nitride Composite for Consecutive Adsorption and Photodegradation of Dyes under UV and Visible Lights

    Directory of Open Access Journals (Sweden)

    Luhong Zhang

    2016-11-01

    Full Text Available In this work, a ZnO-layered double hydroxide@graphitic carbon nitride composite (ZnO-LDH@C3N4 was synthesized via co-precipitation method with solvothermal treatment. The structure and morphology of ZnO-LDH@C3N4 composite were characterized using X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR, scanning electron microscopes/transmission electron microscopes (SEM/TEM, N2 adsorption/desorption, ultraviolet visible diffuse reflectance spectroscopy (UV-Vis-DRS, photoluminescence spectrometer (PL and electrochemical impedance spectroscopy (EIS. The adsorption and photocatalytic properties of ZnO-LDH@C3N4 composite towards the organic dyes: Orange II sodium salt (OrgII, an anionic azo dye and methylene blue (MB, a cationic azo dye were investigated. Compared to ZnO-LDH and g-C3N4, the ZnO-LDH@C3N4 composite displayed an excellent performance in both adsorption and photocatalytic degradation of the organic dyes. Moreover, a combination of ZnO-LDH and g-C3N4 significantly improved the photocatalytic performance of ZnO-LDH and g-C3N4 under visible-light irradiation. The adsorption and photocatalytic mechanism were also investigated.

  15. Ultrasonically assisted solvothermal synthesis of novel Ni/Al layered double hydroxide for capturing of Cd(II) from contaminated water

    Science.gov (United States)

    Rahmanian, Omid; Maleki, Mohammad Hassan; Dinari, Mohammad

    2017-11-01

    A novel adsorbent of nickel aluminum layered double hydroxide (Ni/Al-LDH) was prepared through the precipitation of metal nitrates by ultrasonically assisted solvothermal method. The surface morphology, chemical structure and thermal properties of this compound were examined by X-ray diffraction (XRD), Fourier Transform Infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) techniques. The XRD, TEM and FE-SEM results established that the synthesized LDH have a well-ordered layer structure with good crystalline nature. Then it was applied to remove excessive Cd(II) ions from water and the effects of contact time, pH and adsorbent dose were examined at initial Cd(II) concentration of 10 mg/L. Results show that the time required to reach equilibrium was fast (40 min) and working pH solution was neutral (pH 7). Langmuir and Freundlich model of adsorption isotherms were explored; the results show that the Freundlich model was better fitted than that Langmuir model. This results predicting a multilayer adsorption of Cd(II) on LDH. The equilibrium kinetic adsorption data were fixed to the pseudo-second order kinetic equation.

  16. Multifunctional organic–inorganic hybrid nanoparticles and nanosheets based on chitosan derivative and layered double hydroxide: cellular uptake mechanism and application for topical ocular drug delivery

    Science.gov (United States)

    Chi, Huibo; Gu, Yan; Xu, Tingting; Cao, Feng

    2017-01-01

    To study the cellular uptake mechanism of multifunctional organic–inorganic hybrid nanoparticles and nanosheets, new chitosan–glutathione–valine–valine-layered double hydroxide (CG-VV-LDH) nanosheets with active targeting to peptide transporter-1 (PepT-1) were prepared, characterized and further compared with CG-VV-LDH nanoparticles. Both organic–inorganic hybrid nanoparticles and nanosheets showed a sustained release in vitro and prolonged precorneal retention time in vivo, but CG-VV-LDH nanoparticles showed superior permeability in the isolated cornea of rabbits than CG-VV-LDH nanosheets. Furthermore, results of cellular uptake on human corneal epithelial primary cells (HCEpiC) and retinal pigment epithelial (ARPE-19) cells indicated that both clathrin-mediated endocytosis and active transport of PepT-1 are involved in the internalization of CG-VV-LDH nanoparticles and CG-VV-LDH nanosheets. In summary, the CG-VV-LDH nanoparticle may be a promising carrier as a topical ocular drug delivery system for the treatment of ocular diseases of mid-posterior segments, while the CG-VV-LDH nanosheet may be suitable for the treatment of ocular surface diseases. PMID:28280329

  17. Selective extraction by dissolvable (nitriloacetic acid-nickel)-layered double hydroxide coupled with reaction with potassium thiocyanate for sensitive detection of iron(III).

    Science.gov (United States)

    Tang, Sheng; Chang, Yuepeng; Shen, Wei; Lee, Hian Kee

    2016-07-01

    A highly selective method has been proposed for the determination of iron cation (Fe(3+)). (Nitriloacetic acid-nickel)-layered double hydroxide ((NTA-Ni)-LDH) was successfully synthesized and used as dissolvable sorbent in dispersive solid-phase extraction to pre-concentrate and separate Fe(3+) from aqueous phase. Since Fe(3+) has a larger formation constant with NTA compared to Ni(2+), subsequently ion exchange occurred when (NTA-Ni)-LDH was added to the sample solution. The resultant (NTA-Fe)-LDH sol was isolated and transferred in an acidic medium containing potassium thiocyanate (KSCN). Since (NTA-Fe)-LDH could be dissolved in acidic conditions, Fe(3+)was released and reacted with SCN(-) to form an Fe-SCN complex. The resulting product was measured by ultraviolet-visible spectrometry for quantitative detection of Fe(3+). Extraction factors, including sample pH, reaction pH, extraction temperature, extraction time, reaction time and concentration of KSCN were optimized. This method achieved a low limit of detection of 15.2nM and a good linear range from 0.05 to 50μM (r(2)=0.9937). A nearly 18-fold enhancement of signal intensity was achieved after selective extraction. The optimized conditions were validated by applying the method to determine Fe(3+) in seawater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Efficient Flame-Retardant and Smoke-Suppression Properties of Mg-Al-Layered Double-Hydroxide Nanostructures on Wood Substrate.

    Science.gov (United States)

    Guo, Bingtuo; Liu, Yongzhuang; Zhang, Qi; Wang, Fengqiang; Wang, Qingwen; Liu, Yixing; Li, Jian; Yu, Haipeng

    2017-07-12

    Improving the flame retardancy of wood is an imperative yet highly challenging step in the application of wood in densely populated spaces. In this study, Mg-Al-layered double-hydroxide (LDH) coating was successfully fabricated on a wood substrate to confer flame-retardant and smoke-suppression properties. The chemical compositions and bonding states characterized by energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy confirmed the coating constituents of Mg-Al LDH. The coating evenly covered the sample wood surfaces and provided both mechanical enhancement and flame-retardancy effects. The limiting oxygen index of the Mg-Al LDH-coated wood increased to 39.1% from 18.9% in the untreated wood. CONE calorimetry testing revealed a 58% reduction in total smoke production and a 41% reduction in maximum smoke production ratio in the Mg-Al LDH-coated wood compared to the untreated wood; the peak heat release rate and total heat release were also reduced by 49% and 40%, respectively. The Mg-Al LDH coating is essentially hydrophilic, but simple surface modification by fluoroalkyl silane could make it superhydrophobic, with a water contact angle of 152° and a sliding angle of 8.6°. The results of this study altogether suggest that Mg-Al LDH coating is a feasible and highly effective approach to nanoconstructing wood materials with favorable flame-retardant and smoke-suppression properties.

  19. The use of dissolvable layered double hydroxide components in an in situ solid-phase extraction for chromatographic determination of tetracyclines in water and milk samples.

    Science.gov (United States)

    Phiroonsoontorn, Nattaphorn; Sansuk, Sira; Santaladchaiyakit, Yanawath; Srijaranai, Supalax

    2017-10-13

    This research presents a simple and green in situ solid phase extraction (is-SPE) combined with high-performance liquid chromatography (HPLC) for the simultaneous analysis of tetracyclines (TCs) including tetracycline, oxytetracycline, and chlortetracycline. In is-SPE, TCs were efficiently extracted through the precipitation formation of dissolvable layered double hydroxides (LDHs) by mixing the LDH components such as magnesium and aluminum ions (both in metal chloride salts) thoroughly in an alkaline sample solution. After the centrifugation, the precipitate was completely dissolved with trifluoroacetic acid to release the enriched TCs, and then analyzed by HPLC. Under optimized conditions, this method gave good enrichment factors (EFs) of 41-93 with low limits of detection (LODs) of 0.7-6μg/L and limits of quantitation (LOQs) of 3-15μg/L. Also, the proposed method was successfully applied for the determination of TCs in water and milk samples with the recoveries ranging from 81.7-108.1% for water and 55.7-88.7% for milk. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Thermal Analysis and Flame-Retarded Mechanism of Composites Composed of Ethylene Vinyl Acetate and Layered Double Hydroxides Containing Transition Metals (Mn, Co, Cu, Zn

    Directory of Open Access Journals (Sweden)

    Lili Wang

    2016-05-01

    Full Text Available The effects of transition metals on the hydrophobicity of nano–structured layered double hydroxides (LDHs and the compatibility of LDHs/ethylene vinyl acetate (EVA composites have seldom been reported. NiMgAl–LDHs slightly surface–modified with stearate and doped with transition metal cations (Mn2+, Co2+, Cu2+, Zn2+ are investigated. Compared to the pure EVA, not only were the maximal degradation–rate temperatures (Tmax of the ethylene–based chains enhanced, but also the smoke production rate (SPR and the production rate of CO (COP were sharply decreased for all the composites. Most importantly, a new flame retardant mechanism was found, namely the peak heat release rate (pk-HRR time, which directly depends on the peak production rate of CO2 (pk-CO2 time for EVA and all composites by cone calorimeter test. Moreover, the Mn–doped LDH S–NiMgAl–Mn shows more uniform dispersion and better interfacial compatibility in the EVA matrix. The cone calorimetric residue of S–NiMgAl–Mn/EVA has the intumescent char layer and the compact metal oxide layer. Therefore, S–NiMgAl–Mn/EVA shows the lowest pk-HRR and the longest pk-HRR time among all the composites.

  1. Nickel-cobalt layered double hydroxide anchored zinc oxide nanowires grown on carbon fiber cloth for high-performance flexible pseudocapacitive energy storage devices

    KAUST Repository

    Shakir, Imran

    2014-05-01

    Nickel-cobalt layered double hydroxide (Ni-Co LDH) nanoflakes-ZnO nanowires hybrid array has been directly synthesized on a carbon cloth substrate by a facile cost-effective two-step hydrothermal route. As electrode materials for flexible pseudocapacitors, Ni-Co LDH nanoflakes-ZnO nanowires hybrid array exhibits a significantly enhanced specific capacitance of 1927 Fg-1, which is a ∼1.8 time greater than pristine Ni-Co LDH nanoflakes. The synthesized Ni-Co LDH nanoflakes-ZnO nanowires hybrid array shows a maximum energy density of 45.55 Whkg-1 at a power density of 46.15 kWkg -1, which is 35% higher than the pristine Ni-Co LDH nanoflakes electrode. Moreover, Ni-Co LDH nanoflakes-ZnO nanowires hybrid array exhibit excellent excellent rate capability (80.3% capacity retention at 30 Ag -1) and cycling stability (only 3.98% loss after 3000 cycles), due to the significantly improved faradaic redox reaction. © 2014 Elsevier Ltd.

  2. Graphene-oxide-supported CuAl and CoAl layered double hydroxides as enhanced catalysts for carbon-carbon coupling via Ullmann reaction

    Science.gov (United States)

    Ahmed, Nesreen S.; Menzel, Robert; Wang, Yifan; Garcia-Gallastegui, Ainara; Bawaked, Salem M.; Obaid, Abdullah Y.; Basahel, Sulaiman N.; Mokhtar, Mohamed

    2017-02-01

    Two efficient catalyst based on CuAl and CoAl layered double hydroxides (LDHs) supported on graphene oxide (GO) for the carbon-carbon coupling (Classic Ullmann Homocoupling Reaction) are reported. The pure and hybrid materials were synthesised by direct precipitation of the LDH nanoparticles onto GO, followed by a chemical, structural and physical characterisation by electron microscopy, X-ray diffraction (XRD), thermogravimetric analysis (TGA), surface area measurements and X-ray photoelectron spectroscopy (XPS). The GO-supported and unsupported CuAl-LDH and CoAl-LDH hybrids were tested over the Classic Ullman Homocoupling Reaction of iodobenzene. In the current study CuAl- and CoAl-LDHs have shown excellent yields (91% and 98%, respectively) at very short reaction times (25 min). GO provides a light-weight, charge complementary and two-dimensional material that interacts effectively with the 2D LDHs, in turn enhancing the stability of LDH. After 5 re-use cycles, the catalytic activity of the LDH/GO hybrid is up to 2 times higher than for the unsupported LDH.

  3. Determination of Iodate in Food, Environmental, and Biological Samples after Solid-Phase Extraction with Ni-Al-Zr Ternary Layered Double Hydroxide as a Nanosorbent

    Directory of Open Access Journals (Sweden)

    Hossein Abdolmohammad-Zadeh

    2012-01-01

    Full Text Available Nanostructured nickel-aluminum-zirconium ternary layered double hydroxide was successfully applied as a solid-phase extraction sorbent for the separation and pre-concentration of trace levels of iodate in food, environmental and biological samples. An indirect method was used for monitoring of the extracted iodate ions. The method is based on the reaction of the iodate with iodide in acidic solution to produce iodine, which can be spectrophotometrically monitored at 352 nm. The absorbance is directly proportional to the concentration of iodate in the sample. The effect of several parameters such as pH, sample flow rate, amount of nanosorbent, elution conditions, sample volume, and coexisting ions on the recovery was investigated. In the optimum experimental conditions, the limit of detection (3s and enrichment factor were 0.12 μg mL−1 and 20, respectively. The calibration graph using the preconcentration system was linear in the range of 0.2–2.8 μg mL−1 with a correlation coefficient of 0.998. In order to validate the presented method, a certified reference material, NIST SRM 1549, was also analyzed.

  4. Conformal Coating of Cobalt-Nickel Layered Double Hydroxides Nanoflakes on Carbon Fibers for High-performance Electrochemical Energy Storage Supercapacitor Devices

    KAUST Repository

    Warsi, Muhammad Farooq

    2014-07-01

    High specific capacitance coupled with the ease of large scale production is two desirable characteristics of a potential pseudo-supercapacitor material. In the current study, the uniform and conformal coating of nickel-cobalt layered double hydroxides (CoNi0.5LDH,) nanoflakes on fibrous carbon (FC) cloth has been achieved through cost-effective and scalable chemical precipitation method, followed by a simple heat treatment step. The conformally coated CoNi0.5LDH/FC electrode showed 1.5 times greater specific capacitance compared to the electrodes prepared by conventional non-conformal (drop casting) method of depositing CoNi0.5LDH powder on the carbon microfibers (1938 Fg-1 vs 1292 Fg-1). Further comparison of conformally and non-conformally coated CoNi0.5LDH electrodes showed the rate capability of 79%: 43% capacity retention at 50 Ag-1 and cycling stability 4.6%: 27.9% loss after 3000 cycles respectively. The superior performance of the conformally coated CoNi0.5LDH is mainly due to the reduced internal resistance and fast ionic mobility between electrodes as compared to non-conformally coated electrodes which is evidenced by EIS and CV studies. © 2014 Elsevier Ltd.

  5. Facile synthesis of core-shell nanostructured hollow carbon nanospheres@nickel cobalt double hydroxides as high-performance electrode materials for supercapacitors.

    Science.gov (United States)

    Xu, Juan; Ma, Chaojie; Cao, Jianyu; Chen, Zhidong

    2017-03-07

    Core-shell nanostructured hollow carbon nanospheres@nickel cobalt double hydroxides (HCNs@NiCo-LDH) were fabricated using a facile hydrothermal method and investigated as high-performance electrode materials for supercapacitors. HCNs were acquired by a successive polymerization, carbonization and etching process, which was subsequently wrapped by ultrathin NiCo-LDH nanosheets. The HCNs@NiCo-LDH electrode achieved a high specific capacitance (2558 F g -1 at 1 A g -1 ) and outstanding rate capability with 74.9% capacitance retention after a 20-fold increase in current density. Capacitances of 2405, 2310, 2168, 2006 and 1916 F g -1 can be achieved at rates of 3, 5, 10, 15 and 20 A g -1 , respectively, which are much higher than the specific capacitances of most reported carbon loaded NiCo-LDH. Specifically, the assembled HCNs@NiCo-LDH//graphene asymmetric supercapacitor displayed distinguished capacitive behaviors with a prominent specific capacitance of 172.8 F g -1 and eminent cycling stability with 93.5% capacitance retention after 3000 cycles. These remarkable electrochemical properties indicate that the unique HCNs@NiCo-LDH core-shell electrode is highly promising for application in energy storage fields.

  6. ZnO-Layered Double Hydroxide@Graphitic Carbon Nitride Composite for Consecutive Adsorption and Photodegradation of Dyes under UV and Visible Lights.

    Science.gov (United States)

    Zhang, Luhong; Li, Li; Sun, Xiaoming; Liu, Peng; Yang, Dongfang; Zhao, Xiusong

    2016-11-15

    In this work, a ZnO-layered double hydroxide@graphitic carbon nitride composite (ZnO-LDH@C₃N₄) was synthesized via co-precipitation method with solvothermal treatment. The structure and morphology of ZnO-LDH@C₃N₄ composite were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopes/transmission electron microscopes (SEM/TEM), N₂ adsorption/desorption, ultraviolet visible diffuse reflectance spectroscopy (UV-Vis-DRS), photoluminescence spectrometer (PL) and electrochemical impedance spectroscopy (EIS). The adsorption and photocatalytic properties of ZnO-LDH@C₃N₄ composite towards the organic dyes: Orange II sodium salt (OrgII, an anionic azo dye) and methylene blue (MB, a cationic azo dye) were investigated. Compared to ZnO-LDH and g-C₃N₄, the ZnO-LDH@C₃N₄ composite displayed an excellent performance in both adsorption and photocatalytic degradation of the organic dyes. Moreover, a combination of ZnO-LDH and g-C₃N₄ significantly improved the photocatalytic performance of ZnO-LDH and g-C₃N₄ under visible-light irradiation. The adsorption and photocatalytic mechanism were also investigated.

  7. Visible-light-responsive photocatalysts toward water oxidation based on NiTi-layered double hydroxide/reduced graphene oxide composite materials.

    Science.gov (United States)

    Li, Bei; Zhao, Yufei; Zhang, Shitong; Gao, Wa; Wei, Min

    2013-10-23

    A visible-light responsive photocatalyst was fabricated by anchoring NiTi-layered double hydroxide (NiTi-LDH) nanosheets to the surface of reduced graphene oxide sheets (RGO) via an in situ growth method; the resulting NiTi-LDH/RGO composite displays excellent photocatalytic activity toward water splitting into oxygen with a rate of 1.968 mmol g(-1) h(-1) and a quantum efficiency as high as 61.2% at 500 nm, which is among the most effective visible-light photocatalysts. XRD patterns and SEM images indicate that the NiTi-LDH nanosheets (diameter: 100-200 nm) are highly dispersed on the surface of RGO. UV-vis absorption spectroscopy exhibits that the introduction of RGO enhances the visible-light absorption range of photocatalysts, which is further verified by the largely decreased band gap (∼1.78 eV) studied by cyclic voltammetry measurements. Moreover, photoluminescence (PL) measurements indicate a more efficient separation of electron-hole pairs; electron spin resonance (ESR) and Raman scattering spectroscopy confirm the electrons transfer from NiTi-LDH nanosheets to RGO, accounting for the largely enhanced carrier mobility and the resulting photocatalytic activity in comparison with pristine NiTi-LDH material. Therefore, this work demonstrates a facile approach for the fabrication of visible-light responsive NiTi-LDH/RGO composite photocatalysts, which can be used as a promising candidate in solar energy conversion and environmental science.

  8. Carbon quantum dots/layered double hydroxide hybrid for fast and efficient decontamination of Cd(II): The adsorption kinetics and isotherms

    Science.gov (United States)

    Rahmanian, Omid; Dinari, Mohammad; Abdolmaleki, Mahmood Karimi

    2018-01-01

    Novel carbon quantum dots/zinc aluminum layered double hydroxide (CQD/ZnAl-LDH) composite was prepared through the precipitation of metal nitrates in the presence of CQD by a facile and simple method and further applied to remove excessive Cd(II) ions from water. The chemical composition and morphology of the CQDs/ZnAl-LDH hybrid was investigated by Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and Energy-dispersive X-ray spectroscopy. Batch studies were done to evaluate the effects of the adsorption of Cd(II) by CQDs/ZnAl-LDH to optimize the major parameters such as pH, contact time, and initial concentration. The maximum uptake capacity of Cd(II) on CQDs/ZnAl-LDH was only 12.60 mg/g at 20 min due to the available exterior sites on the adsorbent. The adsorption kinetics and isotherms of Cd(II) on CQDs/ZnAl-LDH were also investigated. The experimental data indicated that the adsorption kinetics and adsorption isotherms of Cd(II) on CQDs/ZnAl-LDH were well-fitted by the pseudo-second-order kinetic model and the Freundlich isotherm model, respectively.

  9. Enhancement of photocatalytic degradation of dimethyl phthalate with nano-TiO2 immobilized onto hydrophobic layered double hydroxides: a mechanism study.

    Science.gov (United States)

    Huang, Zhujian; Wu, Pingxiao; Lu, Yonghong; Wang, Xiaorong; Zhu, Nengwu; Dang, Zhi

    2013-02-15

    The organic layered double hydroxides (LHDs)/TiO(2) composites with various mass ratios were prepared by the reconstruction of mixed metal oxides to photodegrade dimethyl phthalate (DMP). The physicochemical properties of the obtained products were analyzed by X-ray diffraction (XRD) spectra, X-ray photoelectron spectra (XPS), UV-vis diffuse reflectance spectroscope and scanning electron microscope (SEM). The results showed that the TiO(2) particles and the organic LDHs were combined together through chemical bonds, and TiO(2) particles were well distributed on the surface of the interconnecting organic LDHs nano-flakes. According to the experimental results of adsorptive and photodegradation of DMP, the organic LDHs with flaky structure could effectively adsorb the DMP molecules and the adsorption isotherm by the composites modeled well with the Langmuir equation. The enrichment of DMP onto the composites and the external hydroxyl groups of the composites produce a synergistic effect leading to greatly enhance the rate of DMP photocatalytic degradation by the obtained composites. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Removal of indigo carmine and green bezanyl-F2B from water using calcined and uncalcined Zn/Al + Fe layered double hydroxide

    Directory of Open Access Journals (Sweden)

    Hassiba Bessaha

    2017-06-01

    Full Text Available Layered double hydroxide Zn/(Al + Fe with a molar ratio of 3:(0.85 + 0.15, designated as ZAF-HT, was synthetized by co-precipitation. Its calcined product CZAF was obtained by heat treatment of ZAF-HT at 500°C. The calcined and uncalcined materials were used to remove the acid dyes indigo carmine (IC and green bezanyl-F2B (F2B from water in batch mode. The synthetized materials were characterized by X-ray diffraction, scanning electron microscopy, Brunauer–Emmett–Teller analysis, Fourier transform infra-red spectroscopy and thermogravimetric/differential thermal analysis. The sorption kinetic data fitted a pseudo-second-order model. The adsorbed amounts of the calcined material were much larger than ZAF-HT. The maximum adsorption capacity of CZAF was found to be 617.3 mg g−1 for IC and 1,501.4 mg g−1 for F2B. The isotherms showed that the removal of IC and F2B by ZAF-HT and CZAF could be described by a Langmuir model. The thermodynamic parameters were also calculated. The negative values of standard free energy ΔG° indicate the spontaneity of sorption process. The reuse of CZAF was studied for both dyes and the calcined material showed a good stability for four thermal cycles.

  11. Characteristics of selective fluoride adsorption by biocarbon-Mg/Al layered double hydroxides composites from protein solutions: kinetics and equilibrium isotherms study.

    Science.gov (United States)

    Ma, Wei; Lv, Tengfei; Song, Xiaoyan; Cheng, Zihong; Duan, Shibo; Xin, Gang; Liu, Fujun; Pan, Decong

    2014-03-15

    In the study, two novel applied biocarbon-Mg/Al layered double hydroxides composites (CPLDH and CPLDH-Ca) were successfully prepared and characterized by TEM, ICP-AES, XFS, EDS, FTIR, XRD, BET and pHpzc. The fluoride removal efficiency (RF) and protein recovery ratio (RP) of the adsorbents were studied in protein systems of lysozyme (LSZ) and bovine serum albumin (BSA). The results showed that the CPLDH-Ca presented remarkable performance for selective fluoride removal from protein solution. It reached the maximum RF of 92.1% and 94.8% at the CPLDH-Ca dose of 2.0g/L in LSZ and BSA system, respectively. The RP in both systems of LSZ and BSA were more than 90%. Additionally, the RP of CPLDH-Ca increased with the increase of ionic strengths, and it almost can be 100% with more than 93% RF. Fluoride adsorption by the CPLDH-Ca with different initial fluoride concentrations was found to obey the mixed surface reaction and diffusion controlled adsorption kinetic model, and the overall reaction rate is probably controlled by intra-particle diffusion, boundary layer diffusion and reaction process. The adsorption isotherms of fluoride in BSA system fit the Langmuir-Freundlich model well. The BSA has synergistic effect on fluoride adsorption and the degree increased with the increase of the initial BSA concentration. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. In vivo pharmacological evaluation and efficacy study of methotrexate-encapsulated polymer-coated layered double hydroxide nanoparticles for possible application in the treatment of osteosarcoma.

    Science.gov (United States)

    Ray, Sayantan; Saha, Suman; Sa, Biswanath; Chakraborty, Jui

    2017-04-01

    Considering the existing drawbacks of methotrexate (MTX) with respect to its solubility and toxicity, we incorporated it in a nanoceramic matrix, Mg-Al-layered double hydroxide (LDH) to form LDH-MTX nanoparticles, and the same was in turn encapsulated in a nontoxic and biodegradable polymer, poly (D,L-lactide-co-glycolide) (PLGA), to arrest the initial burst release and dose-dumping-related toxicity, already reported by our group. Our present study was designed to evaluate the pharmacokinetics, tissue distribution, survival rate of the test animals, and antitumor efficacy of the PLGA-LDH-MTX nanoparticles and its counterpart without LDH, PLGA-MTX nanoparticles compared with bare MTX. The median lethal dose (LD 50 ) of the former was higher, compared with bare MTX, using Balb/c nude mice, indicating it to be completely safe for use. Also, a comparative pharmacokinetic and antitumour efficacy study using MTX, PLGA-MTX, and PLGA-LDH-MTX nanoparticles in osteosarcoma-induced Balb/c nude mice in vivo demonstrated superiority of PLGA-LDH-MTX as compared to PLGA-MTX and bare MTX. The results suggest that PLGA-LDH-MTX nanoparticles might exhibit potential advantages over the present-day chemotherapy over bare MTX, for the possibility of treatment of osteosarcoma.

  13. Engineering one-dimensional and two-dimensional birnessite manganese dioxides on nickel foam-supported cobalt–aluminum layered double hydroxides for advanced binder-free supercapacitors

    KAUST Repository

    Hao, Xiaodong

    2014-11-19

    © The Royal Society of Chemistry. We report a facile decoration of the hierarchical nickel foam-supported CoAl layered double hydroxides (CoAl LDHs) with MnO2 nanowires and nanosheets by a chemical bath method and a hydrothermal approach for high-performance supercapacitors. We demonstrate that owing to the sophisticated configuration of binder-free LDH@MnO2 on the conductive Ni foam (NF), the designed NF/LDH@MnO2 nanowire composites exhibit a highly boosted specific capacitance of 1837.8 F g-1 at a current density of 1 A g-1, a good rate capability, and an excellent cycling stability (91.8% retention after 5000 cycles). By applying the hierarchical NF/LDH@MnO2 nanowires as the positive electrode and activated microwave exfoliated graphite oxide activated graphene as the negative electrode, the fabricated asymmetric supercapacitor produces an energy density of 34.2 Wh kg-1 with a maximum power density of 9 kW kg-1. Such strategies with controllable assembly capability could open up a new and facile avenue in fabricating advanced binder-free energy storage electrodes. This journal is

  14. Transesterification of edible, non-edible and used cooking oils for biodiesel production using calcined layered double hydroxides as reusable base catalysts.

    Science.gov (United States)

    Sankaranarayanan, Sivashunmugam; Antonyraj, Churchil A; Kannan, S

    2012-04-01

    Fatty acid methyl esters (FAME) were produced from edible, non-edible and used cooking oils with different fatty acid contents by transesterification with methanol using calcined layered double hydroxides (LDHs) as solid base catalysts. Among the catalysts, calcined CaAl2-LDH (hydrocalumite) showed the highest activity with >90% yield of FAME using low methanol:oil molar ratio (<6:1) at 65 °C in 5 h. The activity of the catalyst was attributed to its high basicity as supported by Hammett studies and CO(2)-TPD measurements. The catalyst was successfully reused in up to four cycles. Some of the properties such as density, viscosity, neutralization number and glycerol content of the obtained biodiesel matched well with the standard DIN values. It is concluded that a scalable heterogeneously catalyzed process for production of biodiesel in high yields from a wide variety of triglyceride oils including used oils is possible using optimized conditions. Copyright © 2012 Elsevier Ltd. All rights reserved.

  15. Stacking Faults and Polytypes for Layered Double Hydroxides: What Can We Learn from Simulated and Experimental X-ray Powder Diffraction Data?

    Science.gov (United States)

    Sławiński, Wojciech A; Sjåstad, Anja Olafsen; Fjellvåg, Helmer

    2016-12-19

    Layered double hydroxides (LDH) are a broad group of widely studied materials. The layered character of those materials and their high flexibility for accommodating different metals and anions make them technologically interesting. The general formula for the LDH compound is [M 1-x II M x III (OH) 2 ][A n- ] x/n ·mH 2 O, where M II is a divalent metal cation which can be substituted by M III trivalent cation, and A n- is a charge compensating anion located between positively charged layers. In this paper we present a comprehensive study on possible structural disorder in LDH. We show how X-ray powder diffraction (XRPD) can be used to reveal important features of the LDH crystal structure such as stacking faults, random interlayer shifts, anion-molecule orientation, crystal water content, distribution of interlayer distances, and also LDH slab thickness. All calculations were performed using the Discus package, which gives a better flexibility in defining stacking fault sequences, simulating and refining XRPD patterns, relative to DIFFaX, DIFFaX+, and FAULTS. Finally, we show how the modeling can be applied to two LDH samples: Ni 0.67 Cr 0.33 (OH) 2 (CO 3 ) 0.16 ·mH 2 O (3D structure) and Mg 0.67 Al 0.33 (OH) 2 (NO 3 ) 0.33 (2D layered structure).

  16. Synthesis of mesoporous silica@Co-Al layered double hydroxide spheres: layer-by-layer method and their effects on the flame retardancy of epoxy resins.

    Science.gov (United States)

    Jiang, Shu-Dong; Bai, Zhi-Man; Tang, Gang; Song, Lei; Stec, Anna A; Hull, T Richard; Hu, Yuan; Hu, Wei-Zhao

    2014-08-27

    Hierarchical mesoporous silica@Co-Al layered double hydroxide (m-SiO2@Co-Al LDH) spheres were prepared through a layer-by-layer assembly process, in order to integrate their excellent physical and chemical functionalities. TEM results depicted that, due to the electrostatic potential difference between m-SiO2 and Co-Al LDH, the synthetic m-SiO2@Co-Al LDH hybrids exhibited that m-SiO2 spheres were packaged by the Co-Al LDH nanosheets. Subsequently, the m-SiO2@Co-Al LDH spheres were incorporated into epoxy resin (EP) to prepare specimens for investigation of their flame-retardant performance. Cone results indicated that m-SiO2@Co-Al LDH incorporated obviously improved fire retardant of EP. A plausible mechanism of fire retardant was hypothesized based on the analyses of thermal conductivity, char residues, and pyrolysis fragments. Labyrinth effect of m-SiO2 and formation of graphitized carbon char catalyzed by Co-Al LDH play pivotal roles in the flame retardance enhancement.

  17. Superb adsorption capacity of hierarchical calcined Ni/Mg/Al layered double hydroxides for Congo red and Cr(VI) ions.

    Science.gov (United States)

    Lei, Chunsheng; Zhu, Xiaofeng; Zhu, Bicheng; Jiang, Chuanjia; Le, Yao; Yu, Jiaguo

    2017-01-05

    The preparation of hierarchical porous materials as catalysts and sorbents has attracted much attention in the field of environmental pollution control. Herein, Ni/Mg/Al layered double hydroxides (NMA-LDHs) hierarchical flower-like hollow microspheres were synthesized by a hydrothermal method. After the NMA-LDHs was calcined at 600°C, NMA-LDHs transformed into Ni/Mg/Al layered double oxides (NMA-LDOs), which maintained the hierarchical flower-like hollow structure. The crystal phase, morphology, and microstructure of the as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy elemental mapping, Fourier transform infrared spectroscopy, and nitrogen adsorption-desorption methods. Both the calcined and non-calcined NMA-LDHs were examined for their performance to remove Congo red (CR) and hexavalent chromium (Cr(VI)) ions in aqueous solution. The maximum monolayer adsorption capacities of CR and Cr(VI) ions over the NMA-LDOs sample were 1250 and 103.4mg/g at 30°C, respectively. Thermodynamic studies indicated that the adsorption process was endothermic in nature. In addition, the addition of coexisting anions negatively influenced the adsorption capacity of Cr(VI) ions, in the following order: CO 3 2- >SO 4 2- >H 2 PO 4 - >Cl - . This work will provide new insight into the design and fabrication of advanced adsorption materials for water pollutant removal. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Three-dimensional electrode of Ni/Co layered double hydroxides@NiCo2S4@graphene@Ni foam for supercapacitors with outstanding electrochemical performance

    International Nuclear Information System (INIS)

    Tao, Yan; Ruiyi, Li; Lin, Zhou; Chenyang, Ma; Zaijun, Li

    2015-01-01

    We reported a new strategy for fabricating three-dimensiona electrode of Ni/Co layered double hydroxide@NiCo 2 S 4 @graphene@Ni foam for supercapacitors. The resulting 3D electrode offers a jungle-like architecture. The unique structure creates ultra fast electron transfer and electrolyte transport as well as the maximum utilization rate of the space and the surface. The electrode exhibits a prominent advantage of high specific capacitance, high-current capacitive behaviour and cycle stability. - Highlights: • The study developed a new strategy for fabricating 3D electrode of Ni/Co-LDH@NiCo 2 S 4 @G. • The as-prepared 3D electrode offers a jungle-like architecture. • The unique structure creates an efficient conduction network and high mass loading. • The electrode achieves significantly synergetic effect among different materials. • The electrode exhibits an excellent electrochemical performance for supercapacitors. - ABSTRACT: Great challenge for the fabrication of free-standing three-dimensional electrode still remains to simultaneously achieve high specific capacitance, rate performance and cycle stability. The paper reprted a new three-dimensional (3D) electrode of Ni/Co layered double hydroxide@NiCo 2 S 4 @graphene@Ni foam (Ni/Co-LDH@NiCo 2 S 4 @G) for supercapacitors. The as-prepared 3D electrode offers an unique architecture, which create an efficient conduction network and maximum utilization of space and interface. The graphene acts as well-knit and conductive skin coated on the skeleton of Ni foam for growing NiCo 2 S 4 . The conductive NiCo 2 S 4 array serves as bridge between Ni/Co-LDH and graphene, leading to ultrafast electron transfer and electrolyte transport. A slew of splits and holes existing in the NiCo 2 S 4 array play one role as the ion-reservoir to contain host of electrolyte ions. To evaluate the feasibility of 3D electrode’s application in supercapacitors, the electrochemical performance was investigated by using the three

  19. Multifunctional organic–inorganic hybrid nanoparticles and nanosheets based on chitosan derivative and layered double hydroxide: cellular uptake mechanism and application for topical ocular drug delivery

    Directory of Open Access Journals (Sweden)

    Chi H

    2017-02-01

    Full Text Available Huibo Chi,1,2,* Yan Gu,1,* Tingting Xu,1 Feng Cao1 1Department of Pharmaceutics, School of Pharmacy, China Pharmaceutical University, Nanjing, 2State Key Laboratory of Drug Delivery Technology and Pharmacokinetics, Tianjin Institute of Pharmaceutical Research Co., Ltd., Tianjin, People’s Republic of China *These authors contributed equally to this work Abstract: To study the cellular uptake mechanism of multifunctional organic–inorganic hybrid nanoparticles and nanosheets, new chitosan–glutathione–valine–valine-layered double hydroxide (CG-VV-LDH nanosheets with active targeting to peptide transporter-1 (PepT-1 were prepared, characterized and further compared with CG-VV-LDH nanoparticles. Both organic–inorganic hybrid nanoparticles and nanosheets showed a sustained release in vitro and prolonged precorneal retention time in vivo, but CG-VV-LDH nanoparticles showed superior permeability in the isolated cornea of rabbits than CG-VV-LDH nanosheets. Furthermore, results of cellular uptake on human corneal epithelial primary cells (HCEpiC and retinal pigment epithelial (ARPE-19 cells indicated that both clathrin-mediated endocytosis and active transport of PepT-1 are involved in the internalization of CG-VV-LDH nanoparticles and CG-VV-LDH nanosheets. In summary, the CG-VV-LDH nanoparticle may be a promising carrier as a topical ocular drug delivery system for the treatment of ocular diseases of mid-posterior segments, while the CG-VV-LDH nanosheet may be suitable for the treatment of ocular surface diseases. Keywords: LDH nanoparticles, LDH nanosheets, ocular drug delivery, human corneal epithelial primary cell, retinal pigment cell, ARPE-19, active targeting

  20. Mesoporous layer-by-layer ordered nanohybrids of layered double hydroxide and layered metal oxide: highly active visible light photocatalysts with improved chemical stability.

    Science.gov (United States)

    Gunjakar, Jayavant L; Kim, Tae Woo; Kim, Hyo Na; Kim, In Young; Hwang, Seong-Ju

    2011-09-28

    Mesoporous layer-by-layer ordered nanohybrids highly active for visible light-induced O(2) generation are synthesized by self-assembly between oppositely charged 2D nanosheets of Zn-Cr-layered double hydroxide (Zn-Cr-LDH) and layered titanium oxide. The layer-by-layer ordering of two kinds of 2D nanosheets is evidenced by powder X-ray diffraction and cross-sectional high resolution-transmission electron microscopy. Upon the interstratification process, the original in-plane atomic arrangements and electronic structures of the component nanosheets remain intact. The obtained heterolayered nanohybrids show a strong absorption of visible light and a remarkably depressed photoluminescence signal, indicating an effective electronic coupling between the two component nanosheets. The self-assembly between 2D inorganic nanosheets leads to the formation of highly porous stacking structure, whose porosity is controllable by changing the ratio of layered titanate/Zn-Cr-LDH. The resultant heterolayered nanohybrids are fairly active for visible light-induced O(2) generation with a rate of ∼1.18 mmol h(-1) g(-1), which is higher than the O(2) production rate (∼0.67 mmol h(-1) g(-1)) by the pristine Zn-Cr-LDH material, that is, one of the most effective visible light photocatalysts for O(2) production, under the same experimental condition. This result highlights an excellent functionality of the Zn-Cr-LDH-layered titanate nanohybrids as efficient visible light active photocatalysts. Of prime interest is that the chemical stability of the Zn-Cr-LDH is significantly improved upon the hybridization, a result of the protection of the LDH lattice by highly stable titanate layer. The present findings clearly demonstrate that the layer-by-layer-ordered assembly between inorganic 2D nanosheets is quite effective not only in improving the photocatalytic activity of the component semiconductors but also in synthesizing novel porous LDH-based hybrid materials with improved chemical

  1. Applications versus properties of Mg–Al layered double hydroxides provided by their syntheses methods: Alkoxide and alkoxide-free sol–gel syntheses and hydrothermal precipitation

    KAUST Repository

    Chubar, Natalia

    2013-12-01

    A tremendous number of studies have examined layered double hydroxides (LDH) for their technological applications in the ion exchange removal of toxic ions, recovery of valuable substances, catalysis, CO2 capture, as a layered host for storage/delivery of biologically active molecules, additives to plastics and building materials, and other functions. Numerous publications always conclude that the materials (prepared, as a rule, using the oldest synthesis method) are very promising for each investigated application; however, the main chemical industries producing these materials advertise them mainly (or only) as plastic additives. The authors performed extensive research using many of the appropriate methods to compare the structure, surface and adsorptive properties of three Mg-Al LHDs produced by advanced synthesis methods. One industrial sample (by Sasol, Germany) prepared by the alkoxide sol-gel method and two novel Mg-Al LDHs synthesised in-house by alkoxide-free sol-gel and hydrothermal precipitation approaches were investigated. Reasons for the very different adsorptive selectivity of the three LDHs towards arsenate, selenate, phosphate, arsenite and selenite have been provided, highlighting the role of speciation of the interlayer carbonate, aluminium, magnesium, interlayer hydration and moisture content in the adsorptive selectivity towards each toxic anion. This work is the first report presenting the regularities of the LDHs structure, surface and anion exchange properties as a function of their syntheses method. It establishes the links to potential technological applications of each investigated LDH and explains the necessary properties required to make the technological application cost-effective and efficient. The paper might accelerate industrial applications of these advanced materials. © 2013 Elsevier B.V.

  2. Fe(II)–Al(III) layered double hydroxides prepared by ultrasound-assisted co-precipitation method for the reduction of bromate

    International Nuclear Information System (INIS)

    Zhong, Yu; Yang, Qi; Luo, Kun; Wu, Xiuqiong; Li, Xiaoming; Liu, Yang; Tang, Wangwang; Zeng, Guangming; Peng, Bo

    2013-01-01

    Highlights: ► Fe(II)–Al(III) LDHs were synthesized by ultrasound-assisted co-precipitation method. ► The Fe–Al (30 min) exhibited highly reduction reactivity on bromate. ► Pseudo-first-order model described the experimental data well. ► The mechanisms of bromate removal were proposed. -- Abstract: Bromate is recognized as an oxyhalide disinfection byproduct in drinking water. In this paper, Fe(II)–Al(III) layered double hydroxides (Fe–Al LDHs) prepared by the ultrasound-assisted co-precipitation method were used for the reduction of bromate in solution. The Fe–Al LDHs particles were characterized by X-ray diffractometer, scanning electron microscopy and thermogravimetry–differential scanning calorimetry. It was found that ultrasound irradiation assistance promoted the formation of the hydrotalcite-like phase and then improved the removal efficiency of bromate. In addition, the effects of solid-to-solution ratio, contact time, initial bromate concentration, initial pH, coexisting anions on the bromate removal were investigated. The results showed the bromate with an initial concentration of 1.56 μmol/L could be completely removed from solution by Fe–Al LDHs within 120 min. When the initial bromate concentration was 7.81 μmol/L, the Fe–Al LDHs with irradiation time of 30 min exhibited the optimum removal efficiency and the bromate removal capacity (q e ) was 6.80 μmol/g. In addition, the appearance of sulfate and production of bromide were observed simultaneously in this process, which suggested that ion-exchange between sulfate and bromate, and the reduction of bromate to bromide by Fe 2+ were the main mechanisms responsible for the bromate removal by Fe–Al LDHs

  3. Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

    Science.gov (United States)

    Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

    2013-11-15

    A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Effect of calcium hydroxide and double and triple antibiotic pastes on the bond strength of epoxy resin-based sealer to root canal dentin.

    Science.gov (United States)

    Akcay, Merve; Arslan, Hakan; Topcuoglu, Hüseyin Sinan; Tuncay, Oznur

    2014-10-01

    The aim of this study was to evaluate the effects of calcium hydroxide (CH) and triple (TAP) and double (DAP) antibiotic pastes on the bond strength of an epoxy resin-based sealer (AH Plus Jet; Dentsply DeTrey, Konstanz, Germany) to the root canal dentin. Sixty-four single-rooted human mandibular premolars were decoronated and prepared using the rotary system to size 40. The specimens were randomly divided into a control group (without intracanal dressing) and 3 experimental groups that received an intracanal dressing with either CH, DAP, or TAP (n = 16). The intracanal dressing was removed by rinsing with 10 mL 17% EDTA followed by 10 mL 2.5% sodium hypochlorite. The root canals were then obturated with gutta-percha and AH Plus Jet sealer. A push-out test was used to measure the bond strength between the root canal dentin and the sealer. The data were analyzed using 2-way analysis of variance and Tukey post hoc tests to detect the effect of the independent variables (intracanal medicaments and root canal thirds) and their interactions on the push-out bond strength of the root canal filling material to the root dentin (P = .05). The push-out bond strength values were significantly affected by the intracanal medicaments (P .05). In the middle and apical third, the bond strength of the TAP group was higher than those of the CH and DAP groups (P < .05). The DAP and CH did not affect the bond strength of the epoxy resin-based sealer. Additionally, the TAP improved the bond strength of the epoxy resin-based sealer in the middle and apical thirds. Copyright © 2014 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

  5. Photocatalytic Conversion of Carbon Dioxide Using Zn–Cu–Ga Layered Double Hydroxides Assembled with Cu Phthalocyanine: Cu in Contact with Gaseous Reactant is Needed for Methanol Generation

    Directory of Open Access Journals (Sweden)

    Kawamura Shogo

    2015-09-01

    Full Text Available Photocatalytic conversion of CO2 into fuels is an attractive option in terms of both reducing the increased concentration of atmospheric CO2 as well as generating renewable hydrocarbon fuels. It is necessary to investigate good catalysts for CO2 conversion and to clarify the mechanism irradiated by natural light. Layered Double Hydroxides (LDH have been attracting attention for CO2 photoreduction with the expectation of sorption capacity for CO2 in the layered space and tunable semiconductor properties as a result of the choice of metal cations. This study first clarifies the effects of Cu doping to LDH comprising Zn and Al or Ga. Cu could be incorporated in the cationic layers of LDH as divalent metal cations and/or interlayer anions as Cu(OH42−. The formation rates of methanol and CO were optimized for [Zn1.5Cu1.5Ga(OH8]+2Cu(OH42−·mH2O at a total rate of 560 nmol h−1 gcat−1 irradiated by UV–visible light. Cu phthalocyanine tetrasulfonate hydrate (CuPcTs4− and silver were effective as promoters of LDH for CO2 photoreduction. Especially, the total formation rate using CuPcTs-[Zn3Ga(OH8]+2CO32−·mH2O irradiated by visible light was 73% of that irradiated by UV–visible light. The promotion was based on HOMO–LUMO excitation of CuPcTs4− by visible light. The LUMO was distributed on N atoms of pyrrole rings bound to central Cu2+ ions. The photogenerated electrons diffused to the Cu site would photoreduce CO2 progressively in a similar way to inlayer and interlayer Cu sites in the LDH in this study.

  6. Biochar pyrolyzed from MgAl-layered double hydroxides pre-coated ramie biomass (Boehmeria nivea (L.) Gaud.): Characterization and application for crystal violet removal.

    Science.gov (United States)

    Tan, Xiao-Fei; Liu, Yun-Guo; Gu, Yan-Ling; Liu, Shao-Bo; Zeng, Guang-Ming; Cai, Xiaoxi; Hu, Xin-Jiang; Wang, Hui; Liu, Si-Mian; Jiang, Lu-Hua

    2016-12-15

    A novel biochar/MgAl-layered double hydroxides composite (CB-LDH) was prepared for the removal of crystal violet from aqueous solution by pyrolyzing MgAl-LDH pre-coated ramie stem (Boehmeria nivea (L.) Gaud.). Pyrolysis played dual role for both converting biomass into biochar and calcining MgAl-LDH during the pyrolysis process. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray analysis (EDS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) and zeta potential analysis were used to characterize the CB-LDH. The results of characterization suggested that the calcined LDH was successfully synthesized and coated on biochar. The resulted CB-LDH had higher total pore volume and more functional groups than the pristine biochar. Adsorption experimental data fitted well with the pseudo-second order kinetics model and the Freundlich isotherm model. The rate-controlled step was controlled by film-diffusion initially and then followed by intra-particle diffusion. Thermodynamic analysis showed that the adsorption of crystal violet was a spontaneous and endothermic process. The higher pH and temperature of the solution enhanced the adsorption performance. CB-LDH could also have excellent ability for the removal of crystal violet from the actual industrial wastewater and groundwater with high ionic strength. LDH adsorption, electrostatic attraction, pore-filling, π-π interaction and hydrogen bond might be the main mechanisms for crystal violet adsorption on CB-LDH. The results of this study indicated that CB-LDH is a sustainable and green adsorbent with high performance for crystal violet contaminated wastewater treatment and groundwater remediation. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. Investigation of γ-(2,3-Epoxypropoxy)propyltrimethoxy Silane Surface Modified Layered Double Hydroxides Improving UV Ageing Resistance of Asphalt

    Science.gov (United States)

    Zhang, Canlin; Yu, Jianying; Xue, Lihui; Sun, Yubin

    2017-01-01

    γ-(2,3-Epoxypropoxy)propyltrimethoxy silane surface modified layered double hydroxides (KH560-LDHs) were prepared and used to improve the ultraviolet ageing resistance of asphalt. The results of X-ray photoelectron spectrometry (XPS) indicated that KH560 has been successfully grafted onto the surface of LDHs. The agglomeration of LDHs particles notably reduced after KH560 surface modification according to scanning electron microscopy (SEM), which implied that the KH560 surface modification was helpful to promote the dispersibility of LDHs in asphalt. Then, the influence of KH560-LDHs and LDHs on the physical and rheological properties of asphalt before and after UV ageing was thoroughly investigated. The storage stability test showed that the difference in softening point (ΔS) of LDHs modified asphalt decreased from 0.6 °C to 0.2 °C at an LDHs content of 1% after KH560 surface modification, and the tendency became more pronounced with the increase of LDH content, indicating that KH560 surface modification could improve the stability of LDHs in asphalt. After UV ageing, the viscous modulus (G’’) of asphalt significantly reduced, and correspondingly, the elastic modulus (G’) and rutting factor (G*/sin δ) rapidly increased. Moreover, the asphaltene increased and the amount of “bee-like” structures of the asphalt decreased. Compared with LDHs, KH560-LDHs obviously restrained performance deterioration of the asphalt, and helped to relieve the variation of the chemical compositions and morphology of asphalt, which suggested that the improvement of KH560-LDHs on UV ageing resistance of asphalt was superior to LDHs. PMID:28772438

  8. Bifunctional sensor of pentachlorophenol and copper ions based on nanostructured hybrid films of humic acid and exfoliated layered double hydroxide via a facile layer-by-layer assembly

    International Nuclear Information System (INIS)

    Yuan, Shuang; Peng, Dinghua; Hu, Xianluo; Gong, Jingming

    2013-01-01

    Graphical abstract: -- Highlights: •A new highly sensitive bifunctional electrochemical sensor developed. •As-prepared sensor fabricated by alternate assembly of HA and exfoliated LDH nanosheets. •Such a newly designed sensor combining the individual properties of HA and LDH nanosheets. •Simultaneous determination of pentachlorophenol and copper ions achieved. •Practical applications demonstrated in water samples. -- Abstract: A new, highly sensitive bifunctional electrochemical sensor for the simultaneous determination of pentachlorophenol (PCP) and copper ions (Cu 2+ ) has been developed, where organic–inorganic hybrid ultrathin films were fabricated by alternate assembly of humic acid (HA) and exfoliated Mg–Al-layered double hydroxide (LDH) nanosheets onto ITO substrates via a layer-by-layer (LBL) approach. The multilayer films were then characterized by means of UV–vis spectrometry, scanning electron microscopy (SEM), and atomic force microscope (AFM). These films were found to have a relatively smooth surface with almost equal amounts of HA incorporated in each cycle. Its electrochemical performance was systematically investigated. Our results demonstrate that such a newly designed (LDH/HA) n multilayer films, combining the individual properties of HA (dual recognition ability for organic herbicides and metal ions) together with LDH nanosheets (a rigid inorganic matrix), can be applied to the simultaneous analysis of PCP and Cu(II) without interference from each other. The LBL assembled nanoarchitectures were further investigated by X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (IR), which provides insight for bifunctional sensing behavior. Under the optimized conditions, the detection limit was found to be as low as 0.4 nM PCP, well below the guideline value of PCP in drinking water (3.7 nM) set by the United States Environmental Protection Agency (U.S. EPA), and 2.0 nM Cu 2+ , much below the guideline value (2.0 mg L −1

  9. Synthesis of functionalized MgAl-layered double hydroxides via modified mussel inspired chemistry and their application in organic dye adsorption.

    Science.gov (United States)

    Zhao, Jiao; Huang, Qiang; Liu, Meiying; Dai, Yanfeng; Chen, Junyu; Huang, Hongye; Wen, Yuanqing; Zhu, Xiaoli; Zhang, Xiaoyong; Wei, Yen

    2017-11-01

    In this paper, a novel strategy for the preparation of poly(levodopa) functionalized MgAl-layered double hydroxide (PDOPA-f-LDH) was developed based on the modified mussel inspired chemistry. The utilization of PDOPA-f-LDH for the removal of methylene blue (MB) from aqueous solution was also examined. Taken advantage of the self-polymerization of levodopa (DOPA) in alkaline solution and the strong affinity of catechol groups to the substrate surface, the LDH was covered homogeneously by a layer of polymer coating of DOPA, leading to the functionalization toward LDH. The structure, surface morphology, thermostability and elemental composition of as-prepared PDOPA-f-LDH were investigated by the transmission electron microscope, scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. Besides, the surface charge of the PDOPA-f-LDH was also investigated using zeta potential. The effects of various parameters, including contact time, initial MB concentration, solution pH and temperature, on the adsorption of MB onto PDOPA-f-LDH were systematically investigated. Results show that the adsorption capacity of functionalized LDH at 25°C could reach up to 102mg/g, which is much higher than that of pure LDH in the same experimental conditions. The adsorption kinetics and isotherm of MB adsorption were studied in batch experiments. The pseudo-second-order model is found to be the best to describe the adsorption kinetics. The isotherm result shows that the Freundlich isotherm is the better-fit-isotherm model to represent the equilibrium data. The values of thermodynamic parameters, including enthalpy change ΔH 0 , entropy change ΔS 0 and Gibbs free energy change ΔG 0 , were also determined. All the ΔG 0 values are negative; the ΔH 0 and ΔS 0 values of PDOPA-f-LDH were -7.824kJmol -1 and -0.01562kJmol -1 K -1 , respectively. And the activation energy of system (E a ) is calculated as 24.69k

  10. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples

    International Nuclear Information System (INIS)

    Rajabi, Maryam; Arghavani-Beydokhti, Somayeh; Barfi, Behruz; Asghari, Alireza

    2017-01-01

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2–70, 6–360, 7–725, 7–370, and 8–450 ng mL −1 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ and Ni 2+ ions, respectively, with the correlation of determinations (R 2 s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid and tap water samples. - Highlights: • A novel centrifugeless dispersive

  11. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples.

    Science.gov (United States)

    Rajabi, Maryam; Arghavani-Beydokhti, Somayeh; Barfi, Behruz; Asghari, Alireza

    2017-03-08

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2-70, 6-360, 7-725, 7-370, and 8-450 ng mL -1 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ and Ni 2+ ions, respectively, with the correlation of determinations (R 2 s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid and tap water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples

    Energy Technology Data Exchange (ETDEWEB)

    Rajabi, Maryam, E-mail: mrajabi@semnan.ac.ir; Arghavani-Beydokhti, Somayeh; Barfi, Behruz; Asghari, Alireza

    2017-03-08

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}, and Ni{sup 2+} prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2–70, 6–360, 7–725, 7–370, and 8–450 ng mL{sup −1} for the Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}and Ni{sup 2+} ions, respectively, with the correlation of determinations (R{sup 2}s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}, and Ni{sup 2+} ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid

  13. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides. An in situ X-ray powder diffraction study

    International Nuclear Information System (INIS)

    Johnsen, Rune E.; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO 3 →CoAl-Cl →CoAl-CO 3 , CoAl-Cl→CoAl-NO 3 and CoAl-CO 3 →CoAl-SO 4 . The XRPD data show that the CoAl-CO 3 →CoAl-Cl process is a two-phase transformation, where the amount of the CoAl-CO 3 phase decreases exponentially while that of the CoAl-Cl phase increases exponentially. Energy-dispersive X-ray spectroscopy (EDXS) studies of a partially chloride-exchanged CoAl-CO 3 LDH sample along with in situ XRPD data suggested that the individual particles in the CoAl-CO 3 sample are generally anion-exchanged with chloride one at a time. In contrast with the CoAl-CO 3 →CoAl-Cl transformation, the XRPD data show that the reverse CoAl-Cl→CoAl-CO 3 process is a one-phase transformation. Rietveld refinements indicate that the occupancy factors of the carbon and oxygen sites of the carbonate group increase, while that of the chloride site decreases. In the CoAl-Cl→CoAl-NO 3 anion-exchange reaction, the XRPD patterns reveal the existence of two intermediate phases in addition to the initial CoAl-Cl and final CoAl-NO 3 phases. The in situ data indicate that one of these intermediates is a mixed nitrate- and chloride-based LDH phase, where the disorder decreases as the nitrate content increases. The XRPD data of the partial CoAl-CO 3 →CoAl-SO 4 anion-exchange reaction show that the process is a two-phase transformation involving a sulfate-containing LDH with a 1H polytype structure. (orig.)

  14. Graphene-oxide-supported CuAl and CoAl layered double hydroxides as enhanced catalysts for carbon-carbon coupling via Ullmann reaction

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Nesreen S. [Department of Chemistry, Faculty of Science, King Abdulaziz University (Saudi Arabia); Surface Chemistry and Catalytic Studies Group, King Abdulaziz University (Saudi Arabia); Menzel, Robert [Department of Chemistry, Imperial College London, South Kensington Campus, London SW7 2AZ (United Kingdom); Bio Nano Consulting, The Gridiron Building, One Pancras Square, London N1C 4AG (United Kingdom); Wang, Yifan [Department of Chemistry, Imperial College London, South Kensington Campus, London SW7 2AZ (United Kingdom); Garcia-Gallastegui, Ainara [Bio Nano Consulting, The Gridiron Building, One Pancras Square, London N1C 4AG (United Kingdom); Bawaked, Salem M.; Obaid, Abdullah Y.; Basahel, Sulaiman N. [Department of Chemistry, Faculty of Science, King Abdulaziz University (Saudi Arabia); Surface Chemistry and Catalytic Studies Group, King Abdulaziz University (Saudi Arabia); Mokhtar, Mohamed, E-mail: mmokhtar2000@yahoo.com [Department of Chemistry, Faculty of Science, King Abdulaziz University (Saudi Arabia); Surface Chemistry and Catalytic Studies Group, King Abdulaziz University (Saudi Arabia)

    2017-02-15

    Two efficient catalyst based on CuAl and CoAl layered double hydroxides (LDHs) supported on graphene oxide (GO) for the carbon-carbon coupling (Classic Ullmann Homocoupling Reaction) are reported. The pure and hybrid materials were synthesised by direct precipitation of the LDH nanoparticles onto GO, followed by a chemical, structural and physical characterisation by electron microscopy, X-ray diffraction (XRD), thermogravimetric analysis (TGA), surface area measurements and X-ray photoelectron spectroscopy (XPS). The GO-supported and unsupported CuAl-LDH and CoAl-LDH hybrids were tested over the Classic Ullman Homocoupling Reaction of iodobenzene. In the current study CuAl- and CoAl-LDHs have shown excellent yields (91% and 98%, respectively) at very short reaction times (25 min). GO provides a light-weight, charge complementary and two-dimensional material that interacts effectively with the 2D LDHs, in turn enhancing the stability of LDH. After 5 re-use cycles, the catalytic activity of the LDH/GO hybrid is up to 2 times higher than for the unsupported LDH. - Graphical abstract: CuAl- and CoAl-LDHs have shown excellent yields (91% and 98%, respectively) at very short reaction times (25 min). GO provides a light-weight, charge complementary, two-dimensional material that interacts effectively with the 2D LDHs, in turn enhancing the stability of LDH. - Highlights: • CuAl LDH/GO and CoAl LDH/GO hybrid materials with different LDH compositions were prepared. • Hybrids were fully characterised and their catalytic efficiency over the Classic Ullman Reaction was studied. • CuAl- and CoAl-LDHs have shown excellent yields (91% and 98%, respectively) in 25 min reaction times. • GO provides a light-weight, charge complementary, two-dimensional material that interacts effectively with the 2D LDHs. • After 5 re-use cycles, the catalytic activity of the LDH/GO hybrid is up to 2 times higher than for the unsupported LDH.

  15. Adsorption of phosphate in hydrocalumite-like layered double hydroxides: a comparison between memory effect and ion exchange processes; Adsorcao de fosfato em [Ca-Al]-HDL: comparacao entre o efeito de memoria e troca ionica

    Energy Technology Data Exchange (ETDEWEB)

    Bernardo, M.P., E-mail: marcelapiassib@gmail.com [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil); Moreira, F.K.V.; Ribeiro, C. [Embrapa Instrumentacao (LNNA), Sao Carlos, SP (Brazil). Laboratorio Nacional de Nanotecnologia para o Agronegocio

    2016-07-01

    Phosphorus is an essential element for agriculture, but the excessive use of this element has caused severe damages to the environment. Layered double hydroxide (LDHs) are excellent candidates to remove PO{sub 4}{sup 3-} anions through adsorption process. In this work, the phosphate adsorption on hydrocalumite-like (Ca-Al) LDHs was evaluated over the ion exchange and memory effect processes. X-ray diffraction measurements revealed formation of analogous crystalline phases from both process as the phosphate concentration was increased. However, the phosphate quantity adsorbed varied according to the process used. The ion exchange route is the most efficient process to remove phosphate from aqueous medium. (author)

  16. Trace analysis of mefenamic acid in human serum and pharmaceutical wastewater samples after pre-concentration with Ni–Al layered double hydroxide nano-particles

    Directory of Open Access Journals (Sweden)

    Hossein Abdolmohammad-Zadeh

    2014-10-01

    Full Text Available In this work, the nickel–aluminum layered double hydroxide (Ni–Al LDH with nitrate interlayer anion was synthesized and used as a solid phase extraction sorbent for the selective separation and pre-concentration of mefenamic acid prior to quantification by UV detection at λmax=286 nm. Extraction procedure is based on the adsorption of mefenamate anions on the Ni–Al(NO3− LDH and/or their exchange with LDH interlayer NO3− anions. The effects of several parameters such as cations and interlayer anions type in LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent and co-existing ions on the extraction were investigated and optimized. Under the optimum conditions, the calibration graph was linear within the range of 2–1000 µg/L with a correlation coefficient of 0.9995. The limit of detection and relative standard deviation were 0.6 µg/L and 0.84% (30 µg/L, n=6, respectively. The presented method was successfully applied to determine of mefenamic acid in human serum and pharmaceutical wastewater samples. Keywords: Mefenamic acid, Solid phase extraction, Nano-sorbent, Nickel-aluminum layered double hydroxide, Ultraviolet spectroscopy

  17. Removal of phosphorus by the core-shell bio-ceramic/Zn-layered double hydroxides (LDHs) composites for municipal wastewater treatment in constructed rapid infiltration system.

    Science.gov (United States)

    Zhang, Xiangling; Guo, Lu; Huang, Hualing; Jiang, Yinghe; Li, Meng; Leng, Yujie

    2016-06-01

    Constructed rapid infiltration systems (CRIS) are a reasonable option for treating wastewater, owing to their simplicity, low cost and low energy consumption. Layered double hydroxides (LDHs), novel materials with high surface area and anion exchange capacity, faced the problem of the application in CRIS due to the powdered form. To overcome this shortcoming, Zn-LDHs (FeZn-LDHs, CoZn-LDHs, AlZn-LDHs) were prepared by co-precipitation method and in-situ coated on the surface of the natural bio-ceramic to synthesize the core-shell bio-ceramic/Zn-LDHs composites. Characterization by Scanning Electron Microscope (SEM) and X-ray Fluorescence Spectrometer (XRFS) indicated that the Zn-LDHs were successful loaded on the natural bio-ceramic. Column tests experiments indicated that the bio-ceramic/Zn-LDHs efficiently enhanced the removal performance of phosphorus. The efficiently removal rates of bio-ceramic/FeZn-LDHs were 71.58% for total phosphorous (TP), 74.91% for total dissolved phosphorous (TDP), 82.31% for soluble reactive phosphorous (SRP) and 67.58% for particulate phosphorus (PP). Compared with the natural bio-ceramic, the average removal rates were enhanced by 32.20% (TP), 41.33% (TDP), 49.06% (SRP) and 10.50% (PP), respectively. Adsorption data of phosphate were better described by the Freundlich model for the bio-ceramic/Zn-LDHs and natural bio-ceramic, except for the bio-ceramic/CoZn-LDHs. The maximum adsorption capacity of bio-ceramic/AlZn-LDHs (769.23 mg/kg) was 1.77 times of the natural bio-ceramic (434.78 mg/kg). The effective desorption of phosphate could achieve by using a mixed solution of 5 M NaCl + 0.1 M NaOH, it outperformed the natural bio-ceramic of 18.95% for FeZn-LDHs, 7.59% for CoZn-LDHs and 12.66% for AlZn-LDHs. The kinetic data of the bio-ceramic/Zn-LDHs were better described by the pseudo-second-order equation. Compared the removal amount of phosphate by the natural bio-ceramic, the physical effects were improved little, but the chemical

  18. Enhanced Removal of Arsenic and Antimony in the Mining Site by Calcined γ-Fe2O3/Layered Double Hydroxide Nanocomposite

    Science.gov (United States)

    Lee, Sang-Ho; Choi, Heechul; Kim, Kyoung-Woong

    2016-04-01

    Arsenic (As) and Antimony (Sb) have been recognized as harmful contaminants in aquatic environment due to its high toxicity and carcinogenicity. Especially, the contamination of arsenic in the mining areas is considered as a serious emerging environmental issue in Korea. Due to the hazardous effect of arsenic, the United States Environmental Protection Agency (US EPA) regulated maximum contamination level of arsenic to 10 μg/L in drinking water. The harmful effect on human health by excessive intake of antimony was also reported by previous studies, and severe contamination level (100 - 7,000 μg/L) of antimony reported in surface and groundwater of abandoned mining area in China and Slovakia. Therefore, US EPA regulated maximum contaminants level of antimony in drinking water to 6 μg/L. In order to remove anionic contaminants in drinking water, various type of nanomaterials have been developed. Layered double hydroxide (LDH) is the artificial anionic clay that is based on the layered structure of positively charged brucite-like layers with interlayers of anions. The LDH is one of the promising nanomaterials for the removal of anionic contaminants because it has high selectivity for arsenic, phosphate, chromium and antimony. However, the biggest problem of LDH for wastewater treatment is that the particles cannot be easily separated after the removal of contaminants. In this study, magnetic nanoparticles (γ-Fe2O3) supported LDH nanocomposite (γ-Fe2O3/LDH) was investigated to enhance magnetic particle recovery and removal efficiency for arsenic and antimony. The calcined γ-Fe2O3/LDH nanocomposites synthesized by co-precipitation method, and the crystallographic properties of maghemite (γ-Fe2O3) and layered structure of LDH were confirmed by X-ray diffraction. The nano-sized γ-Fe2O3 (30 to 50 nm) was stably attached on the surface of LDH (100 to 150 nm) and O1s spectrum by X-ray photoelectron spectroscopy (XPS) explained that there are both physical and

  19. Raman microprobe observation of intercalate contraction in graphite intercalation compounds

    Science.gov (United States)

    McNeil, L. E.; Steinbeck, J.; Salamanca-Riba, L.; Dresselhaus, G.

    1985-02-01

    Raman microprobe spectra of SbCl5, Br2, and FeCl3 graphite intercalation compounds have been obtained with a spatial resolution of 2 μm. Depletion of the intercalate was observed within 10 μm of the sample edge in the SbCl5-graphite samples, and this observation is found to be consistent with a model in which the intercalate contracts thermally as the sample is cooled after the intercalation reaction is completed. No depletion was observed in the Br2 and FeCl3 graphite intercalation compounds, consistent with the low intercalation temperature of the former and the small thermal expansion coefficient of the latter.

  20. Preparation of Mg/Al-LDHs intercalated with dodecanoic acid and investigation of its antiwear ability

    International Nuclear Information System (INIS)

    Zhao, Dong; Bai, Zhimin; Zhao, Fuyan

    2012-01-01

    Graphical abstract: Comparable studies of nano Mg/Al-LDHs powder on the anti-wear properties of lubricating oil were carried out on four-ball and gear testing machine. Mg/Al-NO 3 − -LDHs and Mg/Al-DA-LDHs powder in base oil possess an excellent friction-reducing property, with a friction coefficient at 23.9% and 22.2% which are lower than that of the base oil Highlights: ► We synthesized nano Mg/Al-NO 3 − (DA)-LDHs via coprecipitation and anion exchange. ► The optimal exchanging condition is as follows: water dispersion and pH value of 5. ► The tribological properties of LDHs were studied on four-ball and gear machine. ► We reported nano LHDs as anti-wear materials in lubricates for the first time. ► The greatest decline in friction coefficient of lubricates with LDHs is up to 23.9%. -- Abstract: Layered double hydroxides (LDHs) intercalated with dodecanoic acid have been prepared by anion exchange with Mg/Al-NO 3 − -LDHs as the precursor under acid condition with water and ethanol as the dispersion medium. The obtained materials were characterized by X-ray diffraction (XRD), thermogravimetric and differential thermal analyser (TG–DTA), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and BET. Patterns of XRD and FTIR show that interlayer nitrate ions have substituted with dodecanoic acid and the gallery height has increased from 0.88 nm to 1.99 nm. The interlayer distance of the intercalated materials increases with the increase of pH value due to the different arrangement of interlayer anions. The tribological performance of LDHs precursor and intercalated LDHs in base oil were studied for the first time by using four-ball wear machine and gear testing machine. Experimental results show that the LDHs precursor and intercalated LDHs powder are excellent in friction-reducing, with decreases in friction coefficient by 23.9% and 22.2% respectively comparing with base oil.

  1. Thermal behaviour of hydroxides, hydroxysalts and hydrotalcites

    Indian Academy of Sciences (India)

    Unknown

    In hydrotalcite-like layered double hydroxides, a fra- ction, x, of the M2+ ions of the brucite layers are iso- morphously substituted by M′3+ ions to give the layer composition [M1. I I. –xM′x. III(OH)2]x+. Anions and water mole- cules are incorporated in the interlayer region (Cavani et al 1991). These hydroxide materials are ...

  2. Single sheet metal oxides and hydroxides

    DEFF Research Database (Denmark)

    Huang, Lizhi

    The synthesis of layered double hydroxides (LDHs) provides a relatively easy and traditional way to build versatile chemical compounds with a rough control of the bulk structure. The delamination of LDHs to form their single host layers (2D nanosheets) and the capability to reassemble them offer ......) Delamination of the LDHs structure (oxGRC12) with the formation of single sheet iron (hydr)oxide (SSI). (3) Assembly of the new 2D nanosheets layer by layer to achieve desired functionalities....

  3. Preparation and estimation of thermodynamic properties of Fe(II)-, Co(II)-, Ni(II)- and Zr(IV)-containing layered double hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    Rozov, Konstantin; Curtius, Hilde; Bosbach, Dirk [Forschungszentrum Juelich GmbH (Germany). Inst. for Nuclear Waste Management and Reactor Safety (IEK-6)

    2015-07-01

    The investigation of layered double hydroxides (LDHs) was performed because they and similar 'green rust' phases were identified as specific secondary phases forming during the evolution of the disposed research reactor fuel elements under nuclear repository relevant conditions. LDHs or 'hydrotalcite-like' solids are of interest in environmental geochemistry because they can substitute various cations and especially due to the anion-exchange properties and, therefore, can be considered as buffer materials for retention of mobile and hazardous radionuclides (like, {sup 14}C, {sup 129}I, {sup 36}Cl, {sup 79}Se etc.). In our study Fe{sup 2+}-, Co{sup 2+}-, Ni{sup 2+}- and Zr{sup 4+}-containing LDHs have been synthesized by co-precipitation method and characterized (PXRD, FT-IR, SEM-EDX, TGA-DSC) in order to investigate the effect of substitution of 2- and 4-valent cations on the stability of LDHs. PXRD measurements demonstrated that: (1) pure Mg-Al-Fe(II) LDHs are existing in the range of the mole fraction of iron x{sub Fe} = Fe/(Mg+Fe) between 0 and 0.13. Unit-cell parameters (a{sub o}=b{sub o}) as a function of x{sub Fe} follow Vegard's law corroborating the existence of a solid solution when x{sub Fe} = 0 - 0.13. Products of syntheses with x{sub Fe} ≥ 0.13 contain detectable amounts (≥1-2 wt%) of additional phases (like, magnetite, maghemite, lepidocrocite); (2) pure Ni{sup 2+}- and Co{sup 2+}-containing LDHs (mole fractions of Ni and Co were equal to 0.1) have been synthesized successfully; (3) Mg-Al-Zr(IV) precipitates with mole fraction of zirconium x{sub Zr} = Zr/(Zr+Al) = 0.0 - 0.5 show PXRD patterns attributed to pure LDHs and the variation of lattice parameters a{sub o}=b{sub o} as a function of x{sub Zr} is in agreement with Vegard's law demonstrating the presence of solid solution. In contrast, PXRD analyses of precipitates with x{sub Zr} ≥ 0.5 have shown the presence of additional X-ray reflexes typical for brucite. The

  4. CO2 capture at low temperatures (30-80 °C) and in the presence of water vapor over a thermally activated Mg-Al layered double hydroxide.

    Science.gov (United States)

    Torres-Rodríguez, Daniela A; Lima, Enrique; Valente, Jaime S; Pfeiffer, Heriberto

    2011-11-10

    The carbonation process of a calcined Mg-Al layered double hydroxide (LDH) was systematically analyzed at low temperatures, varying the relative humidity. Qualitative and quantitative experiments were performed. In a first set of experiments, the relative humidity was varied while maintaining a constant temperature. Characterization of the rehydrated products by thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR) and solid-state NMR revealed that the samples did not recover the LDH structure; instead hydrated MgCO(3) was produced. The results were compared with similar experiments performed on magnesium oxide for comparison purposes. Then, in the second set of experiments, a kinetic analysis was performed. The results showed that the highest CO(2) capture was obtained at 50 °C and 70% of relative humidity, with a CO(2) absorption capacity of 2.13 mmol/g.

  5. Sodium hydroxide poisoning

    Science.gov (United States)

    Sodium hydroxide is a very strong chemical. It is also known as lye and caustic soda. This ... poisoning from touching, breathing in (inhaling), or swallowing sodium hydroxide. This article is for information only. Do ...

  6. Construction of hierarchically porous graphitized carbon-supported NiFe layered double hydroxides with a core-shell structure as an enhanced electrocatalyst for the oxygen evolution reaction.

    Science.gov (United States)

    Ni, Yuanman; Yao, Lihua; Wang, Yin; Liu, Bing; Cao, Minhua; Hu, Changwen

    2017-08-17

    The oxygen evolution reaction (OER) is a vital half-reaction in water splitting and metal-air batteries. Developing earth-abundant, highly efficient and durable OER catalysts has faced huge challenges until now, because OER is a strict kinetic sluggish process. Herein, we report the construction of hierarchically porous graphitized carbon (HPGC) supported NiFe layered double hydroxides (LDHs) with a core-shell structure (denoted as HPGC@NiFe) by a facile strategy. The HPGC was first obtained by pyrolysing phenolic resin nanospheres with FeCl 3 and ZnCl 2 as the catalyst and the activator, respectively. Then the NiFe LDH arrays were directly grown on the HPGC by a one-step hydrothermal method. The as-synthesized HPGC@NiFe reveals excellent OER properties with a low onset potential, a lower overpotential of 265 mV (corresponding to the current density at 10 mA cm -2 ) and a small Tafel slope (56 mV per decade). And its catalytic activity is even superior to that of the start-of-the-art noble-metal catalyst IrO 2 /C. Notably, the HPGC@NiFe electrode shows admirable stability measured by performing 2000 cycle CVs and long-term electrolysis for 50 h. The prominent performance can be attributed to the synergistic effect between the NiFe-LDHs and the hierarchically porous graphitized carbon, in which the former can increase the exposure of the active sites, while the latter can increase the charge transfer efficiency. Our research implies the possibility for the development of low-cost layered double hydroxides as a promising candidate in electrochemical energy storage and conversion equipment.

  7. Magnetism in intercalated graphene

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Sajid [Department of Electrical Engineering, Indian Institute of Technology Madras, Chennai – 600036 (India); Nanda, B. R. K. [Department of Physics, Indian Institute of Technology Madras, Chennai – 600036 (India)

    2016-05-23

    Using density functional calculations we explore the possibilities of inducing spin moments in otherwise non-magnetic electronic structure of graphene. Through intercalation of H, N, O and F atoms between two hexagonal stacked graphene layers, we show that unpaired electrons can be generated when the planar coordinates of the functional atoms coincide with the center of the graphene hexagon. The spin-half states are realized at the functional sites for certain values of interlayer separations. For oxygen and fluorine these interlayer separations represent the natural stable phases and for hydrogen and nitrogen they induce instability which can be overcome by applying external pressure. We attribute the formation of spin-half states to the one dimensional confinement potential exerted by the graphene layers on the valence electrons of the functional elements.

  8. Line broadening in the PXRD patterns of layered hydroxides: The ...

    Indian Academy of Sciences (India)

    Unknown

    valent hydroxides are replete with structural disorder, and that the excessive and non-uniform broadening of lines in the PXRD patterns is on account of struc- tural disorder rather than due to crystallite size effects. We now extend these studies to another class of layered compounds, the layered double hydroxides. (LDHs).6 ...

  9. Electrostatic-Induced Assembly of Graphene-Encapsulated Carbon@Nickel-Aluminum Layered Double Hydroxide Core-Shell Spheres Hybrid Structure for High-Energy and High-Power-Density Asymmetric Supercapacitor.

    Science.gov (United States)

    Wu, Shuxing; Hui, Kwan San; Hui, Kwun Nam; Kim, Kwang Ho

    2017-01-18

    Achieving high energy density while retaining high power density is difficult in electrical double-layer capacitors and in pseudocapacitors considering the origin of different charge storage mechanisms. Rational structural design became an appealing strategy in circumventing these trade-offs between energy and power densities. A hybrid structure consists of chemically converted graphene-encapsulated carbon@nickel-aluminum layered double hydroxide core-shell spheres as spacers among graphene layers (G-CLS) used as an advanced electrode to achieve high energy density while retaining high power density for high-performance supercapacitors. The merits of the proposed architecture are as follows: (1) CLS act as spacers to avoid the close restacking of graphene; (2) highly conductive carbon sphere and graphene preserve the mechanical integrity and improve the electrical conductivity of LDHs hybrid. Thus, the proposed hybrid structure can simultaneously achieve high electrical double-layer capacitance and pseudocapacitance resulting in the overall highly active electrode. The G-CLS electrode exhibited high specific capacitance (1710.5 F g -1 at 1 A g -1 ) under three-electrode tests. An ASC fabricated using the G-CLS as positive electrode and reduced graphite oxide as negative electrode demonstrated remarkable electrochemical performance. The ASC device operated at 1.4 V and delivered a high energy density of 35.5 Wh kg -1 at a 670.7 W kg -1 power density at 1 A g -1 with an excellent rate capability as well as a robust long-term cycling stability of up to 10 000 cycles.

  10. Effective inhibition of colon cancer cell growth with MgAl-layered double hydroxide (LDH loaded 5-FU and PI3K/mTOR dual inhibitor BEZ-235 through apoptotic pathways

    Directory of Open Access Journals (Sweden)

    Chen J

    2014-07-01

    Full Text Available Jiezhong Chen,1,2 Renfu Shao,3 Li Li,4 Zhi Ping Xu,4 Wenyi Gu4 1School of Biomedical Sciences, University of Queensland, St Lucia, Queensland, 2Faculty of Science, Medicine and Health, University of Wollongong, Wollongong, New South Wales, 3GeneCology Research Centre, Faculty of Science, Health, Education and Engineering, University of the Sunshine Coast, Maroochydore, Queensland, 4Australian Institute of Bioengineering and Nanotechnology, University of Queensland, St Lucia, Queensland, Australia Abstract: Colon cancer is the third most common cancer and the third largest cause of cancer-related death. Fluorouracil (5-FU is the front-line chemotherapeutic agent for colon cancer. However, its response rate is less than 60%, even in combination with other chemotherapeutic agents. The side effects of 5-FU also limit its application. Nanoparticles have been used to deliver 5-FU, to increase its effectiveness and reduce side effects. Another common approach for colon cancer treatment is targeted therapy against the phosphoinositide 3-kinase (PI3K/protein kinase B (Akt pathway. A recently-invented inhibitor of this pathway, BEZ-235, has been tested in several clinical trials and has shown effectiveness and low side effects. Thus, it is a very promising drug for colon cancer treatment. The combination of these two drugs, especially nanoparticle-packed 5-FU and BEZ-235, has not been studied. In the present study, we demonstrated that nanoparticles of layered double hydroxide (LDH loaded with 5-FU were more effective than a free drug at inhibiting colon cancer cell growth, and that a combination treatment with BEZ-235 further increased the sensitivity of colon cancer cells to the treatment of LDH-packed 5-FU (LDH-5-FU. BEZ-235 alone can decrease colon cancer HCT-116 cell viability to 46% of the control, and the addition of LDH-5-FU produced a greater effect, reducing cell survival to 8% of the control. Our data indicate that the combination therapy of

  11. Aging of trivalent metal hydroxide/oxide gels in divalent metal salt ...

    Indian Academy of Sciences (India)

    Unknown

    Aging of trivalent metal hydroxide/oxide gels in divalent metal salt solutions: Mechanism of formation of layered double hydroxides (LDHs). A V RADHA and P ..... This situation promotes coprecipitation of the two metal hydroxides, by virtue of which the titrations yield the. Zn–Al LDH. The LDHs isolated before and after ...

  12. Phase Transformation Mechanism of Li-Ion Storage in Iron(III) Hydroxide Phosphates

    DEFF Research Database (Denmark)

    Henriksen, Christian; Wegeberg, Christina; Ravnsbæk, Dorthe B.

    2018-01-01

    and discharge kinetics. Iron(III) hydroxide phosphate, Fe2-y(PO4)(OH)3-3y(H2O)3y-2 is a promising new cathode material with high Li-ion storage capacity, low production costs and low toxicity. Previous reports on this material indicate that the Li-ion intercalation and extraction in this material is accompanied...

  13. A comparative study of supercapacitive performances of nickel cobalt layered double hydroxides coated on ZnO nanostructured arrays on textile fibre as electrodes for wearable energy storage devices.

    Science.gov (United States)

    Trang, Nguyen Thi Hong; Ngoc, Huynh Van; Lingappan, Niranjanmurthi; Kang, Dae Joon

    2014-02-21

    We demonstrated an efficient method for the fabrication of novel, flexible electrodes based on ZnO nanoflakes and nickel-cobalt layered double hydroxides (denoted as ZnONF/NiCoLDH) as a core-shell nanostructure on textile substrates for wearable energy storage devices. NiCoLDH coated ZnO nanowire (denoted as ZnONW/NiCoLDH) flexible electrodes are also prepared for comparison. As an electrode for supercapacitors, ZnONF/NiCoLDH exhibits a high specific capacitance of 1624 F g(-1), which is nearly 1.6 times greater than ZnONW/NiCoLDH counterparts. It also shows a maximum energy density of 48.32 W h kg(-1) at a power density of 27.53 kW kg(-1), and an excellent cycling stability with capacitance retention of 94% and a Coulombic efficiency of 93% over 2000 cycles. We believe that the superior performance of the ZnONF/NiCoLDH hybrids is due primarily to the large surface area of the nanoflake structure and the open spaces between nanoflakes, both of which provide a large space for the deposition of NiCoLDH, resulting in reduced internal resistance and improved capacitance performance. Our results are significant for the development of electrode materials for high-performance wearable energy storage devices.

  14. Interactions and Supramolecular Organization of Sulfonated Indigo and Thioindigo Dyes in Layered Hydroxide Hosts.

    Science.gov (United States)

    Costa, Ana L; Gomes, Ana C; Pereira, Ricardo C; Pillinger, Martyn; Gonçalves, Isabel S; Pineiro, Marta; Seixas de Melo, J Sérgio

    2018-01-09

    Supramolecularly organized host-guest systems have been synthesized by intercalating water-soluble forms of indigo (indigo carmine, IC) and thioindigo (thioindigo-5,5'-disulfonate, TIS) in zinc-aluminum-layered double hydroxides (LDHs) and zinc-layered hydroxide salts (LHSs) by coprecipitation routes. The colors of the isolated powders were dark blue for hybrids containing only IC, purplish blue or dark lilac for cointercalated samples containing both dyes, and ruby/wine for hybrids containing only TIS. The as-synthesized and thermally treated materials were characterized by Fourier transform infrared, Fourier transform Raman, and nuclear magnetic resonance spectroscopies, powder X-ray diffraction, scanning electron microscopy, and elemental and thermogravimetric analyses. The basal spacings found for IC-LDH, TIS-LDH, IC-LHS, and TIS-LHS materials were 21.9, 21.05, 18.95, and 21.00 Å, respectively, with intermediate spacings being observed for the cointercalated samples that either decreased (LDHs) or increased (LHSs) with increasing TIS content. UV-visible and fluorescence spectroscopies (steady-state and time-resolved) were used to probe the molecular distribution of the immobilized dyes. The presence of aggregates together with the monomer units is suggested for IC-LDH, whereas for TIS-LDH, IC-LHS, and TIS-LHS, the dyes are closer to the isolated situation. Accordingly, while emission from the powder H 2 TIS is strongly quenched, an increment in the emission of about 1 order of magnitude was observed for the TIS-LDH/LHS hybrids. Double-exponential fluorescence decays were obtained and associated with two monomer species interacting differently with cointercalated water molecules. The incorporation of both TIS and IC in the LDH and LHS hosts leads to an almost complete quenching of the fluorescence, pointing to a very efficient energy transfer process from (fluorescent) TIS to (nonfluorescent) IC.

  15. Adsorption and intercalation of anionic surfactants onto layered ...

    Indian Academy of Sciences (India)

    Layered double hydroxides (LDH) with brucite like structure was modified with various anionic surfactants containing sulfonate, carboxyl, phosphonate and sulfate end group through ion-exchange method. XRD reports indicated that the sulfonate group containing surfactants led to an adsorption process whereas the sulfate ...

  16. Adsorption and intercalation of anionic surfactants onto layered ...

    Indian Academy of Sciences (India)

    Unknown

    Abstract. Layered double hydroxides (LDH) with brucite like structure was modified with various anionic surfactants containing sulfonate, carboxyl, phosphonate and sulfate end group through ion-exchange method. XRD reports indicated that the sulfonate group containing surfactants led to an adsorption process whereas.

  17. Application of magnesium hydroxide and barium hydroxide for the ...

    African Journals Online (AJOL)

    Application of magnesium hydroxide and barium hydroxide for the removal of metals and sulphate from mine water. ... equivalent to the Ba(OH)2 dosage. During CO2-dosing, CaCO3 is precipitated to the saturation level of CaCO3. Keywords: Magnesium hydroxide; barium hydroxide; sulphate removal; water treatment ...

  18. Superconductivity in graphite intercalation compounds

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Robert P. [Cavendish Laboratory, University of Cambridge, Madingley Road, Cambridge CB3 0HE (United Kingdom); Weller, Thomas E.; Howard, Christopher A. [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom); Dean, Mark P.M. [Department of Condensed Matter Physics and Materials Science, Brookhaven National Laboratory, Upton, NY 11973 (United States); Rahnejat, Kaveh C. [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom); Saxena, Siddharth S. [Cavendish Laboratory, University of Cambridge, Madingley Road, Cambridge CB3 0HE (United Kingdom); Ellerby, Mark, E-mail: mark.ellerby@ucl.ac.uk [Department of Physics & Astronomy, University College of London, Gower Street, London WCIE 6BT (United Kingdom)

    2015-07-15

    Highlights: • Historical background of graphite intercalates. • Superconductivity in graphite intercalates and its place in the field of superconductivity. • Recent developments. • Relevant modeling of superconductivity in graphite intercalates. • Interpretations that pertain and questions that remain. - Abstract: The field of superconductivity in the class of materials known as graphite intercalation compounds has a history dating back to the 1960s (Dresselhaus and Dresselhaus, 1981; Enoki et al., 2003). This paper recontextualizes the field in light of the discovery of superconductivity in CaC{sub 6} and YbC{sub 6} in 2005. In what follows, we outline the crystal structure and electronic structure of these and related compounds. We go on to experiments addressing the superconducting energy gap, lattice dynamics, pressure dependence, and how these relate to theoretical studies. The bulk of the evidence strongly supports a BCS superconducting state. However, important questions remain regarding which electronic states and phonon modes are most important for superconductivity, and whether current theoretical techniques can fully describe the dependence of the superconducting transition temperature on pressure and chemical composition.

  19. REPORT ON QUALITATIVE VALIDATION EXPERIMENTS USING LITHIUM-ALUMINUM LAYERED DOUBLE-HYDROXIDES FOR THE REDUCTION OF ALUMINUM FROM THE WASTE TREATMENT PLANT FEEDSTOCK

    International Nuclear Information System (INIS)

    Huber, H.J.; Duncan, J.B.; Cooke, G.A.

    2010-01-01

    A process for removing aluminum from tank waste simulants by adding lithium and precipitating Li-Al-dihydroxide (Lithiumhydrotalcite, (LiAl 2 (OH) 6 ) + X - ) has been verified. The tests involved a double-shell tank (DST) simulant and a single-shell tank (SST) simulant. In the case of the DST simulant, the product was the anticipated Li-hydrotalcite. For the SST simulant, the product formed was primarily Li-phosphate. However, adding excess Li to the solution did result in the formation of traces of Li-hydrotalcite. The Li-hydrotalcite from the DST supernate was an easily filterable solid. After four water washes the filter cake was a fluffy white material made of < 100 (micro)m particles made of smaller spheres. These spheres are agglomerates of ∼ 5 (micro)m diameter platelets with < 1 (micro)m thickness. Chemical and mineralogical analyses of the filtrate, filter cake, and wash waters indicate a removal of 90+ wt% of the dissolved Al for the DST simulant. For the SST simulant, the main competing reaction to the formation of lithium hydrotalcite appears to be the formation of lithium phosphate. In case of the DST simulant, phosphorus co-precipitated with the hydrotalcite. This would imply the added benefit of the removal of phosphorus along with aluminum in the pre-treatment part of the waste treatment and immobilization plant (WTP). For this endeavor to be successful, a serious effort toward process parameter optimization is necessary. Among the major issues to be addressed are the dependency of the reaction yield on the solution chemistry, as well as residence times, temperatures, and an understanding of particle growth.

  20. A comparative study of supercapacitive performances of nickel cobalt layered double hydroxides coated on ZnO nanostructured arrays on textile fibre as electrodes for wearable energy storage devices

    Science.gov (United States)

    Trang, Nguyen Thi Hong; Ngoc, Huynh Van; Lingappan, Niranjanmurthi; Kang, Dae Joon

    2014-01-01

    We demonstrated an efficient method for the fabrication of novel, flexible electrodes based on ZnO nanoflakes and nickel-cobalt layered double hydroxides (denoted as ZnONF/NiCoLDH) as a core-shell nanostructure on textile substrates for wearable energy storage devices. NiCoLDH coated ZnO nanowire (denoted as ZnONW/NiCoLDH) flexible electrodes are also prepared for comparison. As an electrode for supercapacitors, ZnONF/NiCoLDH exhibits a high specific capacitance of 1624 F g-1, which is nearly 1.6 times greater than ZnONW/NiCoLDH counterparts. It also shows a maximum energy density of 48.32 W h kg-1 at a power density of 27.53 kW kg-1, and an excellent cycling stability with capacitance retention of 94% and a Coulombic efficiency of 93% over 2000 cycles. We believe that the superior performance of the ZnONF/NiCoLDH hybrids is due primarily to the large surface area of the nanoflake structure and the open spaces between nanoflakes, both of which provide a large space for the deposition of NiCoLDH, resulting in reduced internal resistance and improved capacitance performance. Our results are significant for the development of electrode materials for high-performance wearable energy storage devices.We demonstrated an efficient method for the fabrication of novel, flexible electrodes based on ZnO nanoflakes and nickel-cobalt layered double hydroxides (denoted as ZnONF/NiCoLDH) as a core-shell nanostructure on textile substrates for wearable energy storage devices. NiCoLDH coated ZnO nanowire (denoted as ZnONW/NiCoLDH) flexible electrodes are also prepared for comparison. As an electrode for supercapacitors, ZnONF/NiCoLDH exhibits a high specific capacitance of 1624 F g-1, which is nearly 1.6 times greater than ZnONW/NiCoLDH counterparts. It also shows a maximum energy density of 48.32 W h kg-1 at a power density of 27.53 kW kg-1, and an excellent cycling stability with capacitance retention of 94% and a Coulombic efficiency of 93% over 2000 cycles. We believe that the

  1. Kaolinite Nanocomposite Platelets Synthesized by Intercalation and Imidization of Poly(styrene-co-maleic anhydride)

    Science.gov (United States)

    Samyn, Pieter; Schoukens, Gustaaf; Stanssens, Dirk

    2015-01-01

    A synthesis route is presented for the subsequent intercalation, exfoliation and surface modification of kaolinite (Kln) by an imidization reaction of high-molecular weight poly(styrene-co-maleic anhydride) or SMA in the presence of ammonium hydroxide. In a first step, the intercalation of ammonolyzed SMA by guest displacement of intercalated dimethylsulfoxide has been proven. In a second step, the imidization of ammonolyzed SMA at 160 °C results in exfoliation of the kaolinite layers and deposition of poly(styrene-co-maleimide) or SMI nanoparticles onto the kaolinite surfaces. Compared with a physical mixture of Kln/SMI, the chemically reacted Kln/SMI provides more efficient exfoliation and hydrogen bonding between the nanoparticles and the kaolinite. The kaolinite nanocomposite particles are synthesized in aqueous dispersion with solid content of 65 wt %. The intercalation and exfoliation are optimized for a concentration ratio of Kln/SMI = 70:30, resulting in maximum intercalation and interlayer distance in combination with highest imide content. After thermal curing at 135 °C, the imidization proceeds towards a maximum conversion of the intermediate amic acid moieties. The changes in O–H stretching and kaolinite lattice vibrations have been illustrated by infrared and FT-Raman spectroscopy, which allow for a good quantification of concentration and imidization effects. PMID:28793445

  2. Kaolinite Nanocomposite Platelets Synthesized by Intercalation and Imidization of Poly(styrene-co-maleic anhydride

    Directory of Open Access Journals (Sweden)

    Pieter Samyn

    2015-07-01

    Full Text Available A synthesis route is presented for the subsequent intercalation, exfoliation and surface modification of kaolinite (Kln by an imidization reaction of high-molecular weight poly(styrene-co-maleic anhydride or SMA in the presence of ammonium hydroxide. In a first step, the intercalation of ammonolyzed SMA by guest displacement of intercalated dimethylsulfoxide has been proven. In a second step, the imidization of ammonolyzed SMA at 160 °C results in exfoliation of the kaolinite layers and deposition of poly(styrene-co-maleimide or SMI nanoparticles onto the kaolinite surfaces. Compared with a physical mixture of Kln/SMI, the chemically reacted Kln/SMI provides more efficient exfoliation and hydrogen bonding between the nanoparticles and the kaolinite. The kaolinite nanocomposite particles are synthesized in aqueous dispersion with solid content of 65 wt %. The intercalation and exfoliation are optimized for a concentration ratio of Kln/SMI = 70:30, resulting in maximum intercalation and interlayer distance in combination with highest imide content. After thermal curing at 135 °C, the imidization proceeds towards a maximum conversion of the intermediate amic acid moieties. The changes in O–H stretching and kaolinite lattice vibrations have been illustrated by infrared and FT-Raman spectroscopy, which allow for a good quantification of concentration and imidization effects.

  3. Synthesis of three-dimensional mesoporous Cu-Al layered double hydroxide/g-C3N4nanocomposites on Ni-foam for enhanced supercapacitors with excellent long-term cycling stability.

    Science.gov (United States)

    Adhikari, Surya Prasad; Awasthi, Ganesh Prasad; Kim, Kyung-Suk; Park, Chan Hee; Kim, Cheol Sang

    2018-03-26

    In this study, a novel composite of Cu-Al layered double hydroxide (LDH) nanosheets and g-C3N4-covered Ni-foam was fabricated via a simple and facile two-step process. First, g-C3N4 sheets were deposited on Ni-foam by via electrodeposition method on a three-electrode system (Ni-foam@g-C3N4) and then, Cu-Al LDH nanosheets were grown on the Ni-foam via in situ redox reaction using a hydrothermal process (Ni-foam@Cu-Al LDH/g-C3N4). The FE-SEM image confirmed that the Cu-Al LDH nanosheets arose vertically and were anchored on the surface of electrodeposited g-C3N4 sheets, thus generating unique 3D porous interconnected networks. The electrochemical capacitive performances of the as-prepared samples were evaluated by cyclic volatammetry (CV), galvanostatic charge/discharge tests, and electrochemical impedance spectra (EIS) Nyquist plots. The specific capacitances of the Ni-foam@Cu-Al LDH/g-C3N4 nanocomposite measured from the CV curve (770.98 F g-1 at 50 mV s-1) and the galvanostatic charge/discharge curve (831.871 at 0.4 A g-1) were significantly higher than the others. Moreover, the Ni-foam@Cu-Al LDH/g-C3N4 nanocomposite revealed a remarkable high-current capacitive behavior and the capacitance retention could be maintained at 92.71% even after 5000 cycles of CV. Thus, the obtained results demonstrated that the as-prepared nanocomposite has great potential to be used as a novel supercapacitor electrode.

  4. Sodium Hydroxide and Calcium Hydroxide Hybrid Oxygen Bleaching with System

    Science.gov (United States)

    Doelle, K.; Bajrami, B.

    2018-01-01

    This study investigates the replacement of sodium hydroxide in the oxygen bleaching stage using a hybrid system consisting of sodium hydroxide calcium hydroxide. Commercial Kraft pulping was studied using yellow pine Kraft pulp obtained from a company in the US. The impact of sodium hydroxide, calcium hydroxide hybrid system in regard to concentration, reaction time and temperature for Kraft pulp was evaluated. The sodium hydroxide and calcium hydroxide dosage was varied between 0% and 15% based on oven dry fiber content. The bleaching reaction time was varied between 0 and 180 minutes whereas the bleaching temperature ranged between 70 °C and 110 °C. The ability to bleach pulp was measured by determining the Kappa number. Optimum bleaching results for the hybrid system were achieved with 4% sodium hydroxide and 2% calcium hydroxide content. Beyond this, the ability to bleach pulp decreased.

  5. Intercalation chemistry and chemical bonding

    Science.gov (United States)

    Hagenmuller, Paul

    In contrast to amphoteric graphite, the layer-type oxides or chalcogenides generally play the role of acceptors in chemical or electrochemical intercalation reactions. Due to the more ionic character of the MO bonds, the structural evolution of the oxides may usually be explained on hand of electrostatic considerations, or in terms of cation oxido-reduction. For the more covalent chalcogenides, the occupancy of higher energy levels in the band structure by the transferred electrons constitute mostly a prevailing factor, giving rise to structural changes but also to modifications of the physical properties. The ionic character of the MO bonds accounts for the strong tendency of the oxides to undergo 2D→3D transformations as a result of intercalation processes. Such features are determining for the choice of the electrode materials for lithium-ion batteries as far as users require high electrode capacity, stability, and cyclability.

  6. Water-mediated potassium acetate intercalation in kaolinite as revealed by molecular simulation.

    Science.gov (United States)

    Ható, Zoltán; Makó, Éva; Kristóf, Tamás

    2014-03-01

    Molecular simulations are suitable tools to study the adsorption and intercalation of molecules in clays. In this work, a recently proposed thermodynamically consistent force field for inorganic compounds (INTERFACE, Heinz H, Lin TJ, Mishra RK, Emami FS (2013) Langmuir 29:1754-1765), which enables accurate simulations of inorganic-organic interfaces, was tested for a two-sheet type clay mineral. All-atom NpT molecular dynamics simulations were used to describe the characteristics (basal spacing, loading, molecular orientation) of some intercalate complexes of kaolinite with potassium acetate and the results were compared with the available experimental data. The most probable structural configurations of the kaolinite/potassium acetate intercalate complexes were determined from the simulations. Our examinations confirmed some supposed (single- or double-layered) arrangements of guest molecules. The need of interlayer water in the intercalate complex, which can be produced by the basic synthesis procedure in air atmosphere, was verified.

  7. Intercalation behavior of barium phenylphosphonate

    Czech Academy of Sciences Publication Activity Database

    Beneš, L.; Melánová, Klára; Svoboda, Jan; Zima, Vítězslav

    2010-01-01

    Roč. 71, č. 4 (2010), s. 530-533 ISSN 0022-3697. [15th International Symposium on Intercalation Compounds. Beijing, 11.05.2009-15.05.2009] R&D Projects: GA ČR GA203/08/0208 Institutional research plan: CEZ:AV0Z40500505 Keywords : inorganic compounds * organic compounds * X-ray diffraction Subject RIV: CA - Inorganic Chemistry Impact factor: 1.384, year: 2010

  8. Surface and interlayer base-characters in lepidocrocite titanate: The adsorption and intercalation of fatty acid

    Energy Technology Data Exchange (ETDEWEB)

    Maluangnont, Tosapol, E-mail: tosapol.ma@kmitl.ac.th [College of Nanotechnology, King Mongkut' s Institute of Technology Ladkrabang, Bangkok 10520 (Thailand); Catalytic Chemistry Research Unit, Faculty of Science, King Mongkut' s Institute of Technology Ladkrabang, Bangkok 10520 (Thailand); Arsa, Pornanan [Catalytic Chemistry Research Unit, Faculty of Science, King Mongkut' s Institute of Technology Ladkrabang, Bangkok 10520 (Thailand); Department of Chemistry, Faculty of Science, King Mongkut' s Institute of Technology Ladkrabang, Bangkok 10520 (Thailand); Limsakul, Kanokporn; Juntarachairot, Songsit; Sangsan, Saithong [Department of Chemistry, Faculty of Science, King Mongkut' s Institute of Technology Ladkrabang, Bangkok 10520 (Thailand); Gotoh, Kazuma [Graduate School of Natural Science & Technology, Okayama University, 3-1-1 Tsushima-naka, Okayama 700-8530 (Japan); Sooknoi, Tawan, E-mail: kstawan@gmail.com [Catalytic Chemistry Research Unit, Faculty of Science, King Mongkut' s Institute of Technology Ladkrabang, Bangkok 10520 (Thailand); Department of Chemistry, Faculty of Science, King Mongkut' s Institute of Technology Ladkrabang, Bangkok 10520 (Thailand)

    2016-06-15

    While layered double hydroxides (LDHs) with positively-charged sheets are well known as basic materials, layered metal oxides having negatively-charged sheets are not generally recognized so. In this article, the surface and interlayer base-characters of O{sup 2−} sites in layered metal oxides have been demonstrated, taking lepidocrocite titanate K{sub 0.8}Zn{sub 0.4}Ti{sub 1.6}O{sub 4} as an example. The low basicity (0.04 mmol CO{sub 2}/g) and low desorption temperature (50–300 °C) shown by CO{sub 2}− TPD suggests that O{sup 2−} sites at the external surfaces is weakly basic, while those at the interlayer space are mostly inaccessible to CO{sub 2}. The liquid-phase adsorption study, however, revealed the uptake as much as 37% by mass of the bulky palmitic acid (C{sub 16} acid). The accompanying expansion of the interlayer space by ~0.1 nm was detected by PXRD and TEM. In an opposite manner to the external surfaces, the interlayer O{sup 2−} sites can deprotonate palmitic acid, forming the salt (i.e., potassium palmitate) occluded between the sheets. Two types of basic sites are proposed based on ultrafast {sup 1}H MAS NMR and FTIR results. The interlayer basic sites in lepidocrocite titanate leads to an application of this material as a selective and stable two-dimensional (2D) basic catalyst, as demonstrated by the ketonization of palmitic acid into palmitone (C{sub 31} ketone). Tuning of the catalytic activity by varying the type of metal (Zn, Mg, and Li) substituting at Ti{sup IV} sites was also illustrated. - Graphical abstract: Interlayer basic sites in lepidocrocite titanate, K{sub 0.8}Zn{sub 0.4}Ti{sub 1.6}O{sub 4}, lead to an intercalation of palmitic acid with a layer expansion. Display Omitted - Highlights: • K{sub 0.8}Zn{sub 0.4}Ti{sub 1.6}O{sub 4} intercalates palmitic acid, forming the occluded potassium salt. • The interlayer expansion is evidenced by PXRD patterns and TEM image. • Two types of basic sites are deduced from ultrafast

  9. Ageing behaviour of unary hydroxides in trivalent metal salt solutions

    Indian Academy of Sciences (India)

    Unknown

    Figure 2. Powder X-ray diffractogram of CuO (a) compared with those of CuO aged in aluminium nitrate for 2 days (b) and 4 days (c). Feature marked by asterisk is due to impurities. Table 2. Powder X-ray diffraction data of layered double hydroxides obtained by the ageing of unary hydroxides in Al (or Cr) salt solutions. d/Å.

  10. molecules in a functionalized layered double hydroxide

    Indian Academy of Sciences (India)

    Unknown

    be integrated, a new family of host structure can be envisaged. Indeed, such organic–inorganic .... figure 2b along with the assignments for the reso- nances. The positions of the .... Raman spectral positions and assignments of naphthalene (solid), LDH-CMCD, LDH-CMCD (naphtha- lene)0⋅45 at room temperature and at ...

  11. Development of Drug Delivery Systems Based on Layered Hydroxides for Nanomedicine

    Directory of Open Access Journals (Sweden)

    Farahnaz Barahuie

    2014-05-01

    Full Text Available Layered hydroxides (LHs have recently fascinated researchers due to their wide application in various fields. These inorganic nanoparticles, with excellent features as nanocarriers in drug delivery systems, have the potential to play an important role in healthcare. Owing to their outstanding ion-exchange capacity, many organic pharmaceutical drugs have been intercalated into the interlayer galleries of LHs and, consequently, novel nanodrugs or smart drugs may revolutionize in the treatment of diseases. Layered hydroxides, as green nanoreservoirs with sustained drug release and cell targeting properties hold great promise of improving health and prolonging life.

  12. Magnetism in intercalated compounds of layered manganese ...

    Indian Academy of Sciences (India)

    Administrator

    Magnetism in intercalated compounds of layered manganese thiophosphate. N V VENKATRAMAN and S VASUDEVAN. Department of Inorganic and Physical Chemistry, Indian Institute of Science,. Bangalore 560 012, India. Layered manganese thiophosphate MnPS3 undergoes an unusual ion-exchange intercalation ...

  13. Intercalation chemistry of zirconium 4-sulfophenylphosphonate

    International Nuclear Information System (INIS)

    Svoboda, Jan; Zima, Vítězslav; Melánová, Klára; Beneš, Ludvík; Trchová, Miroslava

    2013-01-01

    Zirconium 4-sulfophenylphosphonate is a layered material which can be employed as a host for the intercalation reactions with basic molecules. A wide range of organic compounds were chosen to represent intercalation ability of zirconium 4-sulfophenylphosphonate. These were a series of alkylamines from methylamine to dodecylamine, 1,4-phenylenediamine, p-toluidine, 1,8-diaminonaphthalene, 1-aminopyrene, imidazole, pyridine, 4,4′-bipyridine, poly(ethylene imine), and a series of amino acids from glycine to 6-aminocaproic acid. The prepared compounds were characterized by powder X-ray diffraction, thermogravimetry analysis and IR spectroscopy and probable arrangement of the guest molecules in the interlayer space of the host is proposed based on the interlayer distance of the prepared intercalates and amount of the intercalated guest molecules. - Graphical abstract: Nitrogen-containing organic compounds can be intercalated into the interlayer space of zirconium 4-sulfophenylphosphonate. - Highlights: • Zirconium 4-sulfophenylphosphonate was examined as a host material in intercalation chemistry. • A wide range of nitrogen-containing organic compounds were intercalated. • Possible arrangement of the intercalated species is described

  14. Concerted intercalation and minor groove recognition of DNA by a homodimeric thiazole orange dye

    DEFF Research Database (Denmark)

    Bunkenborg, Jakob; Gadjev, N I; Deligeorgiev, T

    2000-01-01

    The thiazole orange dye TOTO binds to double-stranded DNA (dsDNA) by a sequence selective bis-intercalation. Each chromophore is sandwiched between two base pairs in a (5'-CpT-3'):(5'-ApG-3') site, and the linker spans two base pairs in the minor groove. We have used one- and two-dimensional NMR ...

  15. Copper-mediated reductive dechlorination by green rust intercalated with dodecanoate

    DEFF Research Database (Denmark)

    Huang, Li-Zhi; Yin, Zhou; Cooper, Nicola G A

    2018-01-01

    A layered FeII-FeIII hydroxide (green rust, GR) was intercalated with dodecanoate (known as GRC12) and then amended with CuII (GRC12(Cu)) before reaction with chloroform (CF), carbon tetrachloride (CT), trichloroethylene (TCE) or tetrachloroethylene (PCE). Reduction of CT by GRC12(Cu) was 37 times...... faster than with GRC12 alone before the active Cu species was consumed. The Cu mediated reaction followed the dichloroelimination pathway as observed for GRC12 alone, with carbon monoxide (82.5%) and formate (26.6%) as main degradation products. Also, CF was reduced by GRC12(Cu), which is not seen...

  16. Fabrication of Li-intercalated bilayer graphene

    Directory of Open Access Journals (Sweden)

    K. Sugawara

    2011-06-01

    Full Text Available We have succeeded in fabricating Li-intercalated bilayer graphene on silicon carbide. The low-energy electron diffraction from Li-deposited bilayer graphene shows a sharp 3×3R30° pattern in contrast to Li-deposited monolayer graphene. This indicates that Li atoms are intercalated between two adjacent graphene layers and take the same well-ordered superstructure as in bulk C6Li. The angle-resolved photoemission spectroscopy has revealed that Li atoms are fully ionized and the π bands of graphene are systematically folded by the superstructure of intercalated Li atoms, producing a snowflake-like Fermi surface centered at the Γ point. The present result suggests a high potential of Li-intercalated bilayer graphene for application to a nano-scale Li-ion battery.

  17. 21 CFR 184.1631 - Potassium hydroxide.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Potassium hydroxide. 184.1631 Section 184.1631 Food... Specific Substances Affirmed as GRAS § 184.1631 Potassium hydroxide. (a) Potassium hydroxide (KOH, CAS Reg... pellets, flakes, sticks, lumps, and powders. Potassium hydroxide is obtained commercially from the...

  18. Efficacy and safety of topical application of 15% and 10% potassium hydroxide for the treatment of Molluscum contagiosum.

    Science.gov (United States)

    Teixidó, Concepció; Díez, Olga; Marsal, Josep R; Giner-Soriano, Maria; Pera, Helena; Martinez, Mireia; Galindo-Ortego, Gisela; Schoenenberger, Joan A; Real, Jordi; Cruz, Ines; Morros, Rosa

    2018-02-26

    Molluscum contagiosum is the most common skin infection in children. One topical treatment used for Molluscum contagiosum is potassium hydroxide. The objective of this study was to compare the efficacy of potassium hydroxide topical treatment at different concentrations with that of placebo in terms of complete clearing of Molluscum contagiosum lesions and to assess the safety and tolerance of potassium hydroxide topical treatment. This was a double-blind randomized clinical trial of three treatments (potassium hydroxide 10%, potassium hydroxide 15%, placebo) applied once daily up to complete clearing of lesions (maximum duration 60 days) in 53 children aged 2-6 years in primary health care pediatric offices in Catalonia, Spain. In the intention-to-treat analysis, potassium hydroxide 10% (58.8%, P = .03) and potassium hydroxide 15% (64.3%, P = .02) had efficacy superior to that of placebo (18.8%). The number of Molluscum contagiosum lesions was significantly reduced with potassium hydroxide 10% and 15%. The main efficacy outcome was achieved in 58.8% of children in the potassium hydroxide 10% group (P = .03 vs placebo) and in 64.3% of children in the potassium hydroxide 15% group (P = .02 vs placebo). Potassium hydroxide 10% and 15% were not significantly different in efficacy from each other. Potassium hydroxide 10% and placebo were better tolerated than potassium hydroxide 15%. No adverse events were reported during the study period. Potassium hydroxide 10% and 15% demonstrated high rates of efficacy in clearing Molluscum contagiosum lesions, with potassium hydroxide 10% being better tolerated. © 2018 Wiley Periodicals, Inc.

  19. Nickel hydroxides and related materials: a review of their structures, synthesis and properties

    Science.gov (United States)

    Hall, David S.; Lockwood, David J.; Bock, Christina; MacDougall, Barry R.

    2015-01-01

    This review article summarizes the last few decades of research on nickel hydroxide, an important material in physics and chemistry, that has many applications in engineering including, significantly, batteries. First, the structures of the two known polymorphs, denoted as α-Ni(OH)2 and β-Ni(OH)2, are described. The various types of disorder, which are frequently present in nickel hydroxide materials, are discussed including hydration, stacking fault disorder, mechanical stresses and the incorporation of ionic impurities. Several related materials are discussed, including intercalated α-derivatives and basic nickel salts. Next, a number of methods to prepare, or synthesize, nickel hydroxides are summarized, including chemical precipitation, electrochemical precipitation, sol–gel synthesis, chemical ageing, hydrothermal and solvothermal synthesis, electrochemical oxidation, microwave-assisted synthesis, and sonochemical methods. Finally, the known physical properties of the nickel hydroxides are reviewed, including their magnetic, vibrational, optical, electrical and mechanical properties. The last section in this paper is intended to serve as a summary of both the potentially useful properties of these materials and the methods for the identification and characterization of ‘unknown’ nickel hydroxide-based samples. PMID:25663812

  20. Effect of Intercalation Agents on Morphology of Exfoliated Kaolinite

    OpenAIRE

    Xiaochao Zuo; Ding Wang; Shilong Zhang; Qinfu Liu; Huaming Yang

    2017-01-01

    Kaolinite intercalation compounds were prepared by intercalating fatty acids and quaternary ammonium salts into kaolinite layers, using methanol-grafted kaolinite as the precursor. Meanwhile, massive lamellas were exfoliated during the intercalation process. The interlayer structure, chemical bonding and morphology of kaolinite before and after intercalation were characterized in detail. As the alkyl chain length increases, the basal spacing of kaolinite increases gradually. The morphology an...

  1. Homogeneous Precipitation of Nickel Hydroxide Powders

    Energy Technology Data Exchange (ETDEWEB)

    Mavis, Bora [Iowa State Univ., Ames, IA (United States)

    2003-01-01

    Precipitation and characterization of nickel hydroxide powders were investigated. A comprehensive precipitation model incorporating the metal ion hydrolysis, complexation and precipitation reactions was developed for the production of the powders with urea precipitation method. Model predictions on Ni2+ precipitation rate were confirmed with precipitation experiments carried out at 90 C. Experimental data and model predictions were in remarkable agreement. Uncertainty in the solubility product data of nickel hydroxides was found to be the large contributor to the error. There were demonstrable compositional variations across the particle cross-sections and the growth mechanism was determined to be the aggregation of primary crystallites. This implied that there is a change in the intercalate chemistry of the primary crystallites with digestion time. Predicted changes in the concentrations of simple and complex ions in the solution support the proposed mechanism. The comprehensive set of hydrolysis reactions used in the model described above allows the investigation of other systems provided that accurate reaction constants are available. the fact that transition metal ions like Ni2+ form strong complexes with ammonia presents a challenge in the full recovery of the Ni2+. On the other hand, presence of Al3+ facilitates the complete precipitation of Ni2+ in about 3 hours of digestion. A challenge in their predictive modeling studies had been the fact that simultaneous incorporation of more than one metal ion necessitates a different approach than just using the equilibrium constants of hydrolysis, complexation and precipitation reactions. Another limitation of using equilibrium constants is that the nucleation stage of digestion, which is controlled mainly by kinetics, is not fully justified. A new program released by IBM Almaden Research Center (Chemical Kinetics Simulator™, Version 1.01) lets the user change

  2. Insight into the structure of layered zinc hydroxide salts intercalated with dodecyl sulfate anions

    Czech Academy of Sciences Publication Activity Database

    Demel, Jan; Hynek, Jan; Kovář, P.; Day, Y.; Taviot-Guého, Ch.; Demel, Ondřej; Pospíšil, M.; Lang, Kamil

    Roč. 118, č. 46 ( 2014 ), s. 27131-27141 ISSN 1932-7447 R&D Projects: GA ČR GA13-05114S Institutional support: RVO:61388980 ; RVO:61388955 Keywords : Distribution functions * Molecular dynamics * Salts * X ray diffraction * Zinc Subject RIV: CA - Inorganic Chemistry ; CF - Physical ; Theoretical Chemistry (UFCH-W) Impact factor: 4.772, year: 2014

  3. clay nanocomposite by solution intercalation technique

    Indian Academy of Sciences (India)

    Polymer–clay nanocomposites of commercial polystyrene (PS) and clay laponite were prepared via solution intercalation technique. Laponite was modified suitably with the well known cationic surfactant cetyltrimethyl ammonium bromide by ion-exchange reaction to render laponite miscible with hydrophobic PS.

  4. Bromine intercalated graphite for lightweight composite conductors

    KAUST Repository

    Amassian, Aram

    2017-07-20

    A method of fabricating a bromine-graphite/metal composite includes intercalating bromine within layers of graphite via liquid-phase bromination to create brominated-graphite and consolidating the brominated-graphite with a metal nanopowder via a mechanical pressing operation to generate a bromine-graphite/metal composite material.

  5. Synthesis and Characterization of Salicylate-zinc Layered Hydroxide Nano hybrid for Antiinflammatory Active Delivery

    International Nuclear Information System (INIS)

    Mohd Zobir Hussein; Mohd Zobir Hussein; Munirah Ramli; Khatijah Yusoff

    2011-01-01

    The emergence of nano technology has prompted much advancement in various areas of research that includes cellular delivery systems, particularly those dealing with delivery of compounds with therapeutic effects. This study aimed at investigating the use of a layered nano material for formation of a new organic-inorganic nano hybrid material. In this work, a compound of zinc layered hydroxide (ZLH) used as a host for a guest, anti-inflammatory agent salicylate (SA) was synthesized. Through simple, direct reaction of SA solution at various concentrations with commercial zinc oxide, SA was found to be intercalated between the ZLH inorganic layers. Powder x-ray diffraction (PXRD) patterns revealed that the basal spacing of the nano hybrid is around 16.14 Angstrom. Further characterizations also confirmed that SA was successfully intercalated into the interlayers of the nano hybrid. Results generated from this work provide information beneficial for development of a new delivery system for therapeutic compounds consisting of antiinflammatory agents. (author)

  6. Enhancement of the fluorescence intensity of DNA intercalators using nano-imprinted 2-dimensional photonic crystal

    International Nuclear Information System (INIS)

    Endo, Tatsuro; Ueda, China; Hisamoto, Hideaki; Kajita, Hiroshi; Okuda, Norimichi; Tanaka, Satoru

    2013-01-01

    We have fabricated polymer-based 2-dimensional photonic crystals that play a key role in enhancing the fluorescence of DNA intercalators. Highly ordered 2-dimensional photonic crystals possessing triangle-shaped and nm-sized hole arrays were fabricated on a 100 μm thick polymer film using nano-imprint lithography. Samples of double-stranded DNAs (sizes: 4361 and 48502 bp; concentration: 1 pM to 10 nM) were adsorbed on the surface of the 2-dimensional photonic crystal by electrostatic interactions and then treated with intercalators. It is found that the fluorescence intensity of the intercalator is enhanced by a factor of up to 10 compared to the enhancement in the absence of the 2-dimensional photonic crystal. Fluorescence intensity increases with increasing length and concentration of the DNAs. If the 2-dimensional photonic crystal is used as a Bragg reflection mirror, the enhancement of fluorescence intensity can be easily observed using a conventional spectrofluorometer. These results suggest that the printed photonic crystal offers a great potential for highly sensitive intercalator-based fluorescent detection of DNAs. (author)

  7. Intercalation events visualized in single microcrystals of graphite.

    Science.gov (United States)

    White, Edward R; Lodico, Jared J; Regan, B C

    2017-12-06

    The electrochemical intercalation of layered materials, particularly graphite, is fundamental to the operation of rechargeable energy-storage devices such as the lithium-ion battery and the carbon-enhanced lead-acid battery. Intercalation is thought to proceed in discrete stages, where each stage represents a specific structure and stoichiometry of the intercalant relative to the host. However, the three-dimensional structures of the stages between unintercalated and fully intercalated are not known, and the dynamics of the transitions between stages are not understood. Using optical and scanning transmission electron microscopy, we video the intercalation of single microcrystals of graphite in concentrated sulfuric acid. Here we find that intercalation charge transfer proceeds through highly variable current pulses that, although directly associated with structural changes, do not match the expectations of the classical theories. Evidently random nanoscopic defects dominate the dynamics of intercalation.

  8. Aluminum hydroxide issue closure package

    International Nuclear Information System (INIS)

    Bergman, T.B.

    1998-01-01

    Aluminum hydroxide coatings on fuel elements stored in aluminum canisters in K West Basin were measured in July and August 1998. Good quality data was produced that enabled statistical analysis to determine a bounding value for aluminum hydroxide at a 99% confidence level. The updated bounding value is 10.6 kg per Multi-Canister Overpack (MCO), compared to the previously estimated bounding value of 8 kg/MCO. Thermal analysis using the updated bounding value, shows that the MCO generates oxygen concentrate that are below the lower flammability limits during the 40-year interim storage period and are, therefore, acceptable

  9. Phosphate-stabilized Lithium intercalation compounds

    Energy Technology Data Exchange (ETDEWEB)

    Richardson, Thomas J.

    2002-07-22

    Four manganese and iron phosphates with alluaudite or fillowite structures have been prepared by solid state reactions: Na2FeMn2(PO4)3, LiNaFeMn2(PO4)3, NaFe3(PO4)3, and Na2Mn3(PO4)3. LixNa2-xFeMn2(PO4)3 with x close to 2 was prepared from Na2FeMn2(PO4)3 by molten salt ion exchange. These materials are similar in stoichiometry to the phospho-olivines LiFe(Mn)PO4, but have a more complex structure that can accommodate mixed transition metal oxidation states. They are of interest as candidates for lithium battery cathodes because of their somewhat higher electronic conductivity, high intercalant ion mobility, and ease of preparation. Their performance as intercalation electrodes in non-aqueous lithium cells was, however, poor.

  10. Fast photoinduced electron transfer through DNA intercalation.

    Science.gov (United States)

    Murphy, C J; Arkin, M R; Ghatlia, N D; Bossmann, S; Turro, N J; Barton, J K

    1994-01-01

    We report evidence for fast photoinduced electron transfer mediated by the DNA helix that requires metal complexes that are avid intercalators of DNA. Here the donor bis(phenanthroline)(dipyridophenazine)ruthenium(II) [Ru(phen)2dppz2+] and acceptor bis(9,10-phenanthrenequinone diimine)(phenanthroline)rhodium(III) [Rh(phi)2phen3+] intercalate into DNA with Kb > 10(6) M-1. Luminescence quenching experiments in the presence of two different lengths of DNA yield upward-curving Stern-Volmer plots and the loss of luminescence intensity far exceeds the change in emission lifetimes. In the presence of a nonintercalative electron acceptor, Ru(NH3)3+(6), Ru(phen)2dppz2+ luminescence is quenched much less efficiently compared to that found for the intercalative Rh(phi)2phen3+ quencher and follows linear Stern-Volmer kinetics; steady-state and time-resolved Stern-Volmer plots are comparable in scale. These experiments are consistent with a model involving fast long-range electron transfer between intercalators through the DNA helix. Images PMID:8202486

  11. Flexibility of short ds-DNA intercalated by a dipyridophenazine ligand

    Directory of Open Access Journals (Sweden)

    Fuchao eJia

    2015-04-01

    Full Text Available We use Förster Resonant Energy Transfer (FRET in order to measure the increase of flexibility of short ds-DNA induced by the intercalation of dipyridophenazine (dppz ligand in between DNA base pairs. By using a DNA double strand fluorescently labeled at its extremeties, it is shown that the end-to-end length increase of DNA due to the intercalation of one dppz ligand is smaller than the DNA base pair interdistance. This may be explained either by a local bending of the DNA or by an increase of its flexibility. The persistence length of the formed DNA/ligand is evaluated. The described structure may have implications in the photophysical damages induced by the complexation of DNA by organometallic molecules.

  12. 21 CFR 582.1631 - Potassium hydroxide.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Potassium hydroxide. 582.1631 Section 582.1631 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) ANIMAL... Additives § 582.1631 Potassium hydroxide. (a) Product. Potassium hydroxide. (b) Conditions of use. This...

  13. Charge carrier density in Li-intercalated graphene

    KAUST Repository

    Kaloni, Thaneshwor P.

    2012-05-01

    The electronic structures of bulk C 6Li, Li-intercalated free-standing bilayer graphene, and Li-intercalated bilayer and trilayer graphene on SiC(0 0 0 1) are studied using density functional theory. Our estimate of Young\\'s modulus suggests that Li-intercalation increases the intrinsic stiffness. For decreasing Li-C interaction, the Dirac point shifts to the Fermi level and the associated band splitting vanishes. For Li-intercalated bilayer graphene on SiC(0 0 0 1) the splitting at the Dirac point is tiny. It is also very small at the two Dirac points of Li-intercalated trilayer graphene on SiC(0 0 0 1). For all the systems under study, a large enhancement of the charge carrier density is achieved by Li intercalation. © 2012 Elsevier B.V. All rights reserved.

  14. Synthesis and stability of Br2, ICl and IBr intercalated pitch-based graphite fibers

    Science.gov (United States)

    Wessbecher, Dorothy E.; Forsman, William C.; Gaier, James R.

    1988-01-01

    The intercalation of halogens in pitch-based fiber is studied as well as the stability of the resultant intercalation compounds. It is found that IBr intercalates P-100 to yield a high-sigma GIC with attractive stability properties. During ICl intercalation, the presence of O2 interferes with the reaction and necessitates a higher threshold pressure for intercalation.

  15. Analysis of barium hydroxide and calcium hydroxide slurry carbonation reactors

    International Nuclear Information System (INIS)

    Patch, K.D.; Hart, R.P.; Schumacher, W.A.

    1980-05-01

    The removal of CO 2 from air was investigated by using a continuous-agitated-slurry carbonation reactor containing either barium hydroxide [Ba(OH) 2 ] or calcium hydroxide [Ca(OH) 2 ]. Such a process would be applied to scrub 14 CO 2 from stack gases at nuclear-fuel reprocessing plants. Decontamination factors were characterized for reactor conditions which could alter hydrodynamic behavior. An attempt was made to characterize reactor performance with models assuming both plug flow and various degrees of backmixing in the gas phase. The Ba(OH) 2 slurry enabled increased conversion, but apparently the process was controlled under some conditions by phenomena differing from those observed for carbonation by Ca(OH) 2 . Overall reaction mechanisms are postulated

  16. Morphological Evaluation of Variously Intercalated Pre-baked Clay

    Directory of Open Access Journals (Sweden)

    Ullah Hameed

    2014-06-01

    Full Text Available The use of porous materials is enjoying tremendous popularity and attention of the advance scientific communities due to their excellent adsorptive and catalytic activities. Clays are one of the most important candidates in the porous community which shows the above mentioned activities after modifing with a different intercalating agent. The paper is focused on the infiuence of some inorganic intercalating agents (NaOH on the morphology of the variously intercalated clay samples. The alkali metal was used as the inorganic intercalating agent. The effect of intercalation temperature, intercalation agent concentration and intercalation time on the pre-baked clay morphology were also part of the study. Scanning electron microscopy (SEM study was performed to evaluate the morphological changes of the resultant intercalates. Different morphological properties were improved significantly in the case of the inorganically modified clay samples. Thus, such intercalations are suggested to be effective if the clays under study are to be used for different industrial process at elevated conditions.

  17. Síntese de hidróxidos duplos lamelares do sistema Cu, Zn, Al-CO3: propriedades morfológicas, estruturais e comportamento térmico Synthesis of layered double hydroxides of the Cu, Zn, Al-CO3 system: morphological and structural properties and thermal behavior

    Directory of Open Access Journals (Sweden)

    S. S. dos Santos

    2011-09-01

    Full Text Available Hidrotalcitas são argilas aniônicas, também conhecidas como Hidróxidos Duplos Lamelares (HDLs e possuem estrutura semelhante ao mineral brucita. Os HDLs do sistema Cu, Zn, Al-CO3 foram sintetizados em condições que favorecem a formação de cristais pequenos e de elevada área superficial. A caracterização foi feita por difração de raios X, análise termogravimétrica, espectroscopia na região do infravermelho e microscopia eletrônica de varredura. A síntese foi feita pelo método de coprecipitação em pH variável, utilizando sulfatos de cobre e zinco, soluções de alumínio e solução de hidróxido sódio. Os difratogramas de raios X mostram que os compostos sintetizados possuem alta cristalinidade; a intensidade e a largura dos picos comprovam que os materiais se apresentam bem organizados e com empilhamento das lamelas. Os espectros de infravermelho apresentaram bandas associadas ao ânion carbonato presente na região interlamelar dos HDLs.Hydrotalcite-like compounds are anionic clays, also known as layered double hydroxides (LDH, which have structure similar to brucite mineral. The LDHs of the system Cu, Zn, Al-CO3 were synthesized under conditions to promote the formation of small crystals with high surface area. The characterization was done by X-ray diffraction, thermogravimetric analysis, FTIR spectroscopy, and scanning electron microscopy. The synthesis were based on the co-precipitation method, under different conditions (hydrothermal bath, titration time using copper and zinc sulfate, aluminum and sodium hydroxide solutions. The X-ray diffraction patterns show that synthesized compounds have high crystallinity, the peak intensities show that they are well organized and stacked with the lamellae. The infrared spectrum shows bands associated with carbonate anion in the interlayer region.

  18. Synthesis and controlled release properties of 2,4-dichlorophenoxy acetate–zinc layered hydroxide nanohybrid

    Energy Technology Data Exchange (ETDEWEB)

    Bashi, Abbas M., E-mail: abbasmatrood@yahoo.com [Department of Medical Analysis, Faculty of Medical Science, Karbala University (Iraq); Hussein, Mohd Zobir; Zainal, Zulkarnain [Chemistry Department Faculty of Science-UPM (Malaysia); Tichit, Didier [Institut Charles Gerhardt UMR 5253 CNRS/UM2/ENSCM/UM1, Matériaux Avancés pour la Catalyse et la Santé, 8 rue Ecole Normale, 34296 Montpellier Cedex 5 (France)

    2013-07-15

    Direct reaction of ZnO with 2,4-dichlorophenoxyacetic acid (24D) solutions of different concentrations allows obtaining new organic–inorganic nanohybrid materials formed by intercalation of 24D into interlayers of zinc layered hydroxide (ZLH). XRD patterns show a progressive evolution of the structure as 24D concentration increases. The nanohybrid obtained at higher 24D concentration (24D–ZLH(0.4)) reveals a well ordered layered structure with two different basal spacings at 25.2 Å and 24 Å. The FTIR spectrum showing the vibrations bands of the functional groups of 24D and of the ZLH confirms the intercalation. SEM images are in agreement with the structural evolution observed by XRD and reveal the ribbon morphology of the nanohybrids. The release studies of 24D showed a rapid release of 94% for the first 100 min governed by the pseudo-second order kinetic model. - Graphical abstract: The phenomenon indicates that the optical energy gap is enlarged with the increase of molar concentrations in 2,4-dichlorophenoxy acetate anion content into ZnO to create a ZLH–24D nanohybrid. - Highlights: • Nanohybrid was synthesized from 2,4-dichlorophenoxy acetate with-Zinc LHD, using wet chemistry. • Characterized using SEM, TEM, EDX, FTIR, XRD and TGA. • Ribbon-shaped 24D–Zn-layered hydroxide nanoparticles with (003) diffractions of 2.5 nm phase were synthesized.

  19. The dynamics of copper intercalated molybdenum ditelluride.

    Science.gov (United States)

    Onofrio, Nicolas; Guzman, David; Strachan, Alejandro

    2016-11-21

    Layered transition metal dichalcogenides are emerging as key materials in nanoelectronics and energy applications. Predictive models to understand their growth, thermomechanical properties, and interaction with metals are needed in order to accelerate their incorporation into commercial products. Interatomic potentials enable large-scale atomistic simulations connecting first principle methods and devices. We present a ReaxFF reactive force field to describe molybdenum ditelluride and its interactions with copper. We optimized the force field parameters to describe the energetics, atomic charges, and mechanical properties of (i) layered MoTe 2 , Mo, and Cu in various phases, (ii) the intercalation of Cu atoms and small clusters within the van der Waals gap of MoTe 2 , and (iii) bond dissociation curves. The training set consists of an extensive set of first principles calculations computed using density functional theory (DFT). We validate the force field via the prediction of the adhesion of a single layer MoTe 2 on a Cu(111) surface and find good agreement with DFT results not used in the training set. We characterized the mobility of the Cu ions intercalated into MoTe 2 under the presence of an external electric field via finite temperature molecular dynamics simulations. The results show a significant increase in drift velocity for electric fields of approximately 0.4 V/Å  and that mobility increases with Cu ion concentration.

  20. Comparison of lithium and sodium intercalation materials

    Directory of Open Access Journals (Sweden)

    Vujković Milica

    2015-01-01

    Full Text Available Low abundance of lithium in Earth’s crust and its high participation in overall cost of lithium-ion batteries incited intensive investigation of sodium-ion batteries, in hope that they may become similar in basic characteristics: specific energy and specific power. Furthermore, over the last years the research has been focused on the replacement of organic electrolytes of Li- and Na-ion batteries, by aqueous electrolytes, in order to simplify the production and improve safety of use. In this lecture, some recent results on the selected intercalation materials are presented: layered structure vanadium oxides, olivine and nasicon phosphates, potentially usable in both Li and Na aqueous rechargeable batteries. After their characterization by X-ray diffraction and electron microscopy, the electrochemical behavior was studied by both cyclic voltammetry and hronopotenciometry. By comparing intercalation kinetics and coulombic capacity of these materials in LiNO3 and NaNO3 solutions, it was shown that the following ones: Na1.2V3O8, Na2V6O16/C , NaFePO4/C and NaTi2(PO43/C may be used as electrode materials in aqueous alkali-ion batteries.

  1. Intercalation processes of copper complexes in DNA

    Science.gov (United States)

    Galindo-Murillo, Rodrigo; García-Ramos, Juan Carlos; Ruiz-Azuara, Lena; Cheatham, Thomas E.; Cortés-Guzmán, Fernando

    2015-01-01

    The family of anticancer complexes that include the transition metal copper known as Casiopeínas® shows promising results. Two of these complexes are currently in clinical trials. The interaction of these compounds with DNA has been observed experimentally and several hypotheses regarding the mechanism of action have been developed, and these include the generation of reactive oxygen species, phosphate hydrolysis and/or base-pair intercalation. To advance in the understanding on how these ligands interact with DNA, we present a molecular dynamics study of 21 Casiopeínas with a DNA dodecamer using 10 μs of simulation time for each compound. All the complexes were manually inserted into the minor groove as the starting point of the simulations. The binding energy of each complex and the observed representative type of interaction between the ligand and the DNA is reported. With this extended sampling time, we found that four of the compounds spontaneously flipped open a base pair and moved inside the resulting cavity and four compounds formed stacking interactions with the terminal base pairs. The complexes that formed the intercalation pocket led to more stable interactions. PMID:25958394

  2. Structural, energetic and electronic properties of intercalated boron

    Indian Academy of Sciences (India)

    The effects of chirality and the intercalation of transitional metal atoms inside single walled BN nanotubes on structural, energetic and electronic properties have been considered in this paper. The thermodynamic stability of BN nanotubes can be improved by the intercalation of cobalt or nickel. BN nanotubes can behave ...

  3. Structural, energetic and electronic properties of intercalated boron ...

    Indian Academy of Sciences (India)

    The effects of chirality and the intercalation of transitional metal atoms inside single walled BN nanotubes on structural, energetic and electronic properties have been considered in this paper. The thermodynamic stability of BN nanotubes can be improved by the intercalation of cobalt or nickel. BN nanotubes can behave ...

  4. Hybrid n-Alkylamine Intercalated Layered Titanates for Solid Lubrication

    NARCIS (Netherlands)

    Gonzalez Rodriguez, P.; Yuan, H.; van den Nieuwenhuijzen, Karin Jacqueline Huberta; Lette, W.; Schipper, Dirk J.; ten Elshof, Johan E.

    2016-01-01

    The intercalation of different primary n-alkylamines in the structure of a layered titanate of the lepidocrocite type (H1.07Ti1.73O4) for application in high-temperature solid lubrication is reported. The intercalation process of the amines was explored by means of in situ small-angle X-ray

  5. Structural, energetic and electronic properties of intercalated boron ...

    Indian Academy of Sciences (India)

    Abstract. The effects of chirality and the intercalation of transitional metal atoms inside single walled BN nano- tubes on structural, energetic and electronic properties have been considered in this paper. The thermodynamic stability of BN nanotubes can be improved by the intercalation of cobalt or nickel. BN nanotubes can ...

  6. Syntheses, structure and intercalation properties of low-dimensional ...

    Indian Academy of Sciences (India)

    Unknown

    X-ray diffraction study of their intercalated products. These efforts have led to the successful synthesis ... phenylarsonates, 1–4 and the intercalation products were recorded on an XD-D1 X-ray diffractometer, ..... and π–π stacking, in slanted fashion to the chains and thus accounts for the lower d020 value (figure 1).

  7. K-intercalated carbon systems: Effects of dimensionality and substrate

    KAUST Repository

    Kaloni, Thaneshwor P.

    2012-06-01

    Density functional theory is employed to investigate the electronic properties of K-intercalated carbon systems. Young\\'s modulus indicates that the intercalation increases the intrinsic stiffness. For K-intercalated bilayer graphene on SiC(0001) the Dirac cone is maintained, whereas a trilayer configuration exhibits a small splitting at the Dirac point. Interestingly, in contrast to many other intercalated carbon systems, the presence of the SiC(0001) substrate does not suppress but rather enhances the charge carrier density. Reasonably high values are found for all systems, the highest carrier density for the bilayer. The band structure and electron-phonon coupling of free-standing K-intercalated bilayer graphene points to a high probability for superconductivity in this system. © 2012 Europhysics Letters Association.

  8. Quasi-freestanding graphene on Ni(111) by Cs intercalation

    KAUST Repository

    Alattas, Maha Hassan Mohssen

    2017-01-08

    It is of technological interest to achieve quasi-freestanding graphene on a substrate. A possible approach is the intercalation of alkali metal atoms. Cs intercalation between graphene and Ni(111) is investigated using density functional theory, incorporating van der Waals corrections. It is known that direct contact between graphene and Ni(111) perturbs the Dirac states. Cs intercalation restores the linear dispersion characteristic of Dirac fermions, which is in agreement with experiments1, but the Dirac cone is shifted to lower energy, i.e., the graphene sheet is n-doped. Cs intercalation therefore effectively decouples the graphene sheet from the substrate except for a charge transfer. On the other hand, the spin polarization of Ni(111) does not extend through the intercalated atoms to the graphene sheet, for which we find virtually spin-degeneracy.

  9. Quasi-freestanding graphene on Ni(111) by Cs intercalation

    KAUST Repository

    Alattas, Maha Hassan Mohssen

    2016-05-26

    A possible approach to achieve quasi-freestanding graphene on a substrate for technological purpose is the intercalation of alkali metal atoms. Cs intercalation between graphene and Ni(111) therefore is investigated using density functional theory, incorporating van der Waals corrections. It is known that direct contact between graphene and Ni(111) perturbs the Dirac states. We find that Cs intercalation restores the linear dispersion characteristic of Dirac fermions, which agrees with experiments, but the Dirac cone is shifted to lower energy, i.e., the graphene sheet is n-doped. Cs intercalation therefore decouples the graphene sheet from the substrate except for a charge transfer. On the other hand, the spin polarization of Ni(111) does not extend through the intercalated atoms to the graphene sheet, for which we find virtually spin-degeneracy.

  10. Voreloxin is an anticancer quinolone derivative that intercalates DNA and poisons topoisomerase II.

    Directory of Open Access Journals (Sweden)

    Rachael E Hawtin

    2010-04-01

    Full Text Available Topoisomerase II is critical for DNA replication, transcription and chromosome segregation and is a well validated target of anti-neoplastic drugs including the anthracyclines and epipodophyllotoxins. However, these drugs are limited by common tumor resistance mechanisms and side-effect profiles. Novel topoisomerase II-targeting agents may benefit patients who prove resistant to currently available topoisomerase II-targeting drugs or encounter unacceptable toxicities. Voreloxin is an anticancer quinolone derivative, a chemical scaffold not used previously for cancer treatment. Voreloxin is completing Phase 2 clinical trials in acute myeloid leukemia and platinum-resistant ovarian cancer. This study defined voreloxin's anticancer mechanism of action as a critical component of rational clinical development informed by translational research.Biochemical and cell-based studies established that voreloxin intercalates DNA and poisons topoisomerase II, causing DNA double-strand breaks, G2 arrest, and apoptosis. Voreloxin is differentiated both structurally and mechanistically from other topoisomerase II poisons currently in use as chemotherapeutics. In cell-based studies, voreloxin poisoned topoisomerase II and caused dose-dependent, site-selective DNA fragmentation analogous to that of quinolone antibacterials in prokaryotes; in contrast etoposide, the nonintercalating epipodophyllotoxin topoisomerase II poison, caused extensive DNA fragmentation. Etoposide's activity was highly dependent on topoisomerase II while voreloxin and the intercalating anthracycline topoisomerase II poison, doxorubicin, had comparable dependence on this enzyme for inducing G2 arrest. Mechanistic interrogation with voreloxin analogs revealed that intercalation is required for voreloxin's activity; a nonintercalating analog did not inhibit proliferation or induce G2 arrest, while an analog with enhanced intercalation was 9.5-fold more potent.As a first-in-class anticancer

  11. Nanoparticle intercalation-induced interlayer-gap-opened graphene–polyaniline nanocomposite for enhanced supercapacitive performances

    Energy Technology Data Exchange (ETDEWEB)

    Im, Sungjin; Park, Young Ran [Graphene Research Institute & Department of Chemistry, Sejong University, Seoul 05006 (Korea, Republic of); Park, Sanghyuk [Graphene Research Institute & Department of Chemistry, Sejong University, Seoul 05006 (Korea, Republic of); Department of Energy and Mineral Resources Engineering, Sejong University, Seoul 05006 (Korea, Republic of); Kim, Hyeong Jin [Department of Nanotechnology and Advanced Materials Engineering, Sejong University, Seoul 05006 (Korea, Republic of); Doh, Ji Hoon [Graphene Research Institute & Department of Chemistry, Sejong University, Seoul 05006 (Korea, Republic of); Division of Electron Microscopy Research, Korea Basic Science Institute (KBSI), Daejeon 34133 (Korea, Republic of); Kwon, Kyungjung [Department of Energy and Mineral Resources Engineering, Sejong University, Seoul 05006 (Korea, Republic of); Hong, Won G. [Division of Electron Microscopy Research, Korea Basic Science Institute (KBSI), Daejeon 34133 (Korea, Republic of); Kim, Byungnam [Radiation Equipment Research Division, Korea Atomic Energy Research Institute, Daejeon 34057 (Korea, Republic of); Yang, Woo Seok [Electronic Material and Device Research Center, Korea Electronics Technology Institute, Seongnam, Gyeonggi-do 13509 (Korea, Republic of); Kim, TaeYoung [Department of Bionanotechnology, Gachon University, Seongnam, Gyeonggi-do 13120 (Korea, Republic of); Hong, Young Joon, E-mail: yjhong@sejong.ac.kr [Department of Nanotechnology and Advanced Materials Engineering, Sejong University, Seoul 05006 (Korea, Republic of)

    2017-08-01

    Highlights: • High energy–power supercapacitor electrode is demonstrated using EDLC–PC hybridized rGO–PANi nanocomposite. • A method for perpetuated intercalation of nanoparticles into interlayer gap of rGO is developed. • The intercalaction (i) exfoliates rGO layers, (ii) prevents self-agglomeration, and (iii) enlarges specific surface area of rGO for high power performance. • Electric resistance is substantially reduced by forming more rGO–PANi links via grafting of PANi to well-opened rGO edges. - Abstract: This study demonstrates a method for improving supercapacitive performance of two-dimensional nanosheet-based composite electrode. As a hybridized electrostatic double layer capacitor–electrochemical pseudocapacitor (EDLC–PC) electrode, we synthesized reduced graphene oxide–polyaniline nanofibers (rGO–PANi NFs) composite electrode. For the enhanced supercapacitive performances, insulator silver chloride nanoparticles (AgCl NPs) were intercalated into the interlayer gap of rGO. The AgCl NP intercalation (i) exfoliated rGO layers and (ii) prevented rGO-self-agglomeration that makes it difficult to utilize the high surface-to-volume ratio of ideal mono- (or few-) atomic-thick rGO layers. As a result, (iii) the specific capacitance was improved in accordance with the enlarged specific surface area of rGO. Furthermore, (iv) the well-developed rGO edges, which were opened by the AgCl intercalation, enabled formation of more bonds between PANi and rGO by selective grafting of PANi to the rGO edges. Hence, the bonds of PANi–rGO, as conducting paths, substantially reduced the total electrical resistance. Enhanced specific capacitance, ion diffusion efficiency, and reduced electrical resistance indicated the bi-functional roles of AgCl NP insertion for high performance hybridized EDLC–PC electrodes.

  12. Preparation and characterization of an anti-inflammatory agent based on a zinc-layered hydroxide-salicylate nanohybrid and its effect on viability of Vero-3 cells

    Directory of Open Access Journals (Sweden)

    Ramli M

    2013-01-01

    Full Text Available Munirah Ramli,1,2 Mohd Zobir Hussein,1,3 Khatijah Yusoff41Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology, Universiti Putra Malaysia, Serdang, Selangor, 2Department of Industrial Biotechnology, Faculty of Biosciences and Bioengineering, Universiti Teknologi Malaysia, Skudai, Johor, 3Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, Serdang, Selangor, 4Department of Microbiology, Faculty of Biotechnology and Biomolecular Sciences, Universiti Putra Malaysia, Serdang, Selangor, MalaysiaAbstract: A new organic-inorganic nanohybrid based on zinc-layered hydroxide intercalated with an anti-inflammatory agent was synthesized through direct reaction of salicylic acid at various concentrations with commercially available zinc oxide. The basal spacing of the pure phase nanohybrid was 15.73 Å, with the salicylate anions arranged in a monolayer form and an angle of 57 degrees between the zinc-layered hydroxide interlayers. Fourier transform infrared study further confirmed intercalation of salicylate into the interlayers of zinc-layered hydroxide. The loading of salicylate in the nanohybrid was estimated to be around 29.66%, and the nanohybrid exhibited the properties of a mesoporous-type material, with greatly enhanced thermal stability of the salicylate compared with its free counterpart. In vitro cytotoxicity assay revealed that free salicylic acid, pure zinc oxide, and the nanohybrid have a mild effect on viability of African green monkey kidney (Vero-3 cells.Keywords: anti-inflammatory, salicylic acid, zinc-layered hydroxide, zinc oxide, nanohybrid, cytotoxicity

  13. Possible Mg intercalation mechanism at the Mo6 S8 cathode surface proposed by first-principles methods

    Science.gov (United States)

    Wan, Liwen; Prendergast, David

    2015-03-01

    In recent years, great attention has been paid to the development of divalent Mg-ion batteries, which can potentially double the energy density and volumetric capacity compared to monovalent Li-ion batteries. The prototype Mg-ion battery, comprising Mg(anode)/Mg(AlCl2BuEt)2.THF(electrolyte)/Mo6S8(cathode), was established in 2000 by Aurbach et al. Despite the remarkable success of this prototype system, we still lack a clear understanding of the fundamental Mg intercalation/deposition mechanism at the electrolyte/electrode interfaces that perhaps results in the observed sluggish Mg transport process. Our previous work has shown that Mg-ions are strongly coordinated in the bulk electrolyte by a combination of counterion, Cl-, and organic aprotic solvent, THF. In this work, we use first-principles methods to study Mg intercalation behavior at the Mo6S8 cathode surface with the presence of solvent molecules. It is found that the image charge, formed on this metallic cathode surface, can effectively weaken the solvent-surface interactions and facilitate Mg intercalation. A detailed Mg intercalation mechanism is proposed and the unique role of Mo6S8 as the cathode material is emphasized. This work is supported as part of the Joint Center for Energy Storage Research (JCESR), an Energy Innovation Hub funded by the U.S. Department of Energy, Office of Science, Basic Energy Sciences.

  14. Renal intercalated cells and blood pressure regulation

    Directory of Open Access Journals (Sweden)

    Susan M. Wall

    2017-12-01

    Full Text Available Type B and non-A, non-B intercalated cells are found within the connecting tubule and the cortical collecting duct. Of these cell types, type B intercalated cells are known to mediate Cl⁻ absorption and HCO₃⁻ secretion largely through pendrin-dependent Cl⁻/HCO₃⁻ exchange. This exchange is stimulated by angiotensin II administration and is also stimulated in models of metabolic alkalosis, for instance after aldosterone or NaHCO₃ administration. In some rodent models, pendrin-mediated HCO₃⁻ secretion modulates acid-base balance. However, the role of pendrin in blood pressure regulation is likely of more physiological or clinical significance. Pendrin regulates blood pressure not only by mediating aldosterone-sensitive Cl⁻ absorption, but also by modulating the aldosterone response for epithelial Na⁺ channel (ENaC-mediated Na⁺ absorption. Pendrin regulates ENaC through changes in open channel of probability, channel surface density, and channels subunit total protein abundance. Thus, aldosterone stimulates ENaC activity through both direct and indirect effects, the latter occurring through its stimulation of pendrin expression and function. Therefore, pendrin contributes to the aldosterone pressor response. Pendrin may also modulate blood pressure in part through its action in the adrenal medulla, where it modulates the release of catecholamines, or through an indirect effect on vascular contractile force. This review describes how aldosterone and angiotensin II-induced signaling regulate pendrin and the contributory role of pendrin in distal nephron function and blood pressure.

  15. The effect of an intercalated BSc on subsequent academic performance.

    Science.gov (United States)

    Mahesan, Nishanthan; Crichton, Siobhan; Sewell, Hannah; Howell, Simon

    2011-10-03

    The choice of whether to undertake an intercalated Bachelor of Science (BSc) degree is one of the most important decisions that students must make during their time at medical school. An effect on exam performance would improve a student's academic ranking, giving them a competitive edge when applying for foundation posts. Retrospective data analysis of anonymised student records. The effects of intercalating on final year exam results, Foundation Programme score, application form score (from white-space questions), quartile rank score, and success with securing Foundation School of choice were assessed using linear and ordered logistic regression models, adjusted for course type, year of graduation, graduate status and baseline (Year 1) performance. The study included 1158 students, with 54% choosing to do an intercalated BSc, and 9.8% opting to do so at an external institution. Doing an intercalated BSc was significantly associated with improved outcome in Year 5 exams (P = 0.004). This was irrespective of the year students chose to intercalate, with no significant difference between those that intercalated after years 2, 3 and 4 (p = 0.3096). There were also higher foundation application scores (P BSc leads to an improvement in subsequent exam results and develops the skills necessary to produce a strong foundation programme application. It also leads to greater success with securing preferred Foundation School posts in students. Differences between internally- and externally-intercalating students may be due to varying course structures or greater challenge in adjusting to a new study environment.

  16. Prediction of superconductivity in Li-intercalated bilayer phosphorene

    Energy Technology Data Exchange (ETDEWEB)

    Huang, G. Q. [Department of Physics, Nanjing Normal University, Nanjing 210023 (China); National Laboratory of Solid State Microstructures, Nanjing University, Nanjing 210093 (China); Xing, Z. W., E-mail: zwxing@nju.edu.cn [National Laboratory of Solid State Microstructures, Nanjing University, Nanjing 210093 (China); Synergetic Innovation Center of Quantum Information and Quantum Physics, University of Science and Technology of China, Hefei, Anhui 230026 (China); Xing, D. Y. [National Laboratory of Solid State Microstructures, Nanjing University, Nanjing 210093 (China); Collaborative Innovation Center of Advanced Microstructures and Department of Physics, Nanjing University, Nanjing 210093 (China)

    2015-03-16

    It is shown that bilayer phosphorene can be transformed from a direct-gap semiconductor to a BCS superconductor by intercalating Li atoms. For the Li-intercalated bilayer phosphorene, we find that the electron occupation of Li-derived band is small and superconductivity is intrinsic. With increasing the intercalation of Li atoms, both increased metallicity and strong electron-phonon coupling are favorable for the enhancement of superconductivity. The obtained electron-phonon coupling λ can be larger than 1 and the superconducting temperature T{sub c} can be increased up to 16.5 K, suggesting that phosphorene may be a good candidate for a nanoscale superconductor.

  17. Strain Lattice Imprinting in Graphene by C60 Intercalation at the Graphene/Cu Interface

    NARCIS (Netherlands)

    Monazami, Ehsan; Bignardi, Luca; Rudolf, Petra; Reinke, Petra

    2015-01-01

    Intercalation of C60 molecules at the graphene-substrate interface by annealing leads to amorphous and crystalline intercalated structures. A comparison of topography and electronic structure with wrinkles and moiré patterns confirms intercalation. The intercalated molecules imprint a local

  18. Zn-Al Layered Double Hydroxide: Synthesis and Optical Properties

    International Nuclear Information System (INIS)

    Abdullah Ahmed Ali Ahmed; Zainal Abidin Talib

    2011-01-01

    Zn-Al-NO 3 -LDH was prepared by co-precipitation method at constant pH 7 and ratio of Zn/ Al=4. Thermal treatment was performed for LDH at various temperatures. The Powder XRD patterns showed stability in structure of LDH samples below 200 degree Celsius. Infrared spectra of samples showed the characteristic peaks of LDH and the changes of these peaks after thermal treatment above 150 degree Celsius. The energy gaps of the samples were found by diffuse reflectance spectroscopy which showed more than one energy gaps at sintered temperatures less than 200 degree Celsius. These energy gaps were assigned to the presence of NO 3 - in interlayer of LDH. At sintered temperature of 200 degree Celsius and above, the LDH samples have one energy gap which was around 3.3 eV. The photo catalytic activity increased due to ZnO crystal size increases by increasing of the sintered temperature of samples.(author)

  19. Thermal decomposition of Co–Al layered double hydroxide ...

    Indian Academy of Sciences (India)

    All other reflections are extinguished on account of. turbostratic disorder which destroys all ℎ reflections and; layer aperiodicity, which destroys all two dimensional ℎ reflections. Given its topochemical relationship with the spinel structure, such an intermediate is a necessary precursor to spinel formation.

  20. Interaction of pristine hydrotalcite-like layered double hydroxides ...

    Indian Academy of Sciences (India)

    The [Mg–Al–NO3]x LDHs were prepared by coprecipita- tion using ammonia. Ammonia precipitation not only helps to avoid carbonate contamination,22 but also provides a con- stant pH ∼11 for the precipitation. In a typical coprecipita- tion, the mixed metal nitrate solution was added to a beaker containing ammonia (1 mol ...

  1. Synthesis and structure refinement of layered double hydroxides of ...

    Indian Academy of Sciences (India)

    Administrator

    space group R-3m) in the struc- ture of the ... Mg, Ca, Co, Ni, Cu, Zn; M′. III. = Al ... There have been many attempts to synthesize ordered. LDHs. Most of these have been modifications of the co- precipitation technique (Reichle 1986). Grosso et al.

  2. Oxidative leaching of chromium from layered double hydroxides ...

    Indian Academy of Sciences (India)

    Unknown

    ) (Miyata 1980), the LDH of Zn with Cr3+ has a unique composition corresponding to x = 0⋅33 (Boclair and Braterman 1998). This leads to the for- mula, Zn2Cr(OH)6(CO3)1/2⋅yH2O (y = 2⋅0). We abbreviate the formula of these LDHs as ...

  3. Layered rare-earth hydroxide nanocones with facile host composition modification and anion-exchange feature: topotactic transformation into oxide nanocones for upconversion.

    Science.gov (United States)

    Zhong, Yishun; Chen, Gen; Liu, Xiaohe; Zhang, Dan; Zhang, Ning; Li, Junhui; Liang, Shuquan; Ma, Renzhi; Qiu, Guanzhou

    2017-06-22

    Conical structures with hollow interiors, namely, nanocones (NCs), may exhibit better carrier transport properties than nanorods or nanotubes, which make them promising candidates for potential applications in optical/display devices, electronics and optoelectronics. Generally, conical structures belong to a metastable state between lamellar and tubular forms due to the extreme curvature causing the increase of internal strain energy. Therefore, it is very difficult to prepare NCs in high yield and purity under mild conditions. Here we firstly demonstrate a general strategy for the synthesis of layered rare-earth hydroxide (LRH) NCs intercalating dodecyl sulfate anions (C 12 H 25 SO 4 - , DS - ) using hexamethylenetetramine (C 6 H 12 N 4 , HMT) hydrolysis. The rare-earth cations (RE 3+ ) in the host layer can be conveniently modified and/or doped, resulting in a large family of monometallic (Y, Tb, Er), bi- (Y-Tb, Y-Er) and even tri-metallic (Y-Yb-Er) LRH NCs with adjustable ratios. Moreover, the DS - -intercalated LRH NCs can be readily modified with various inorganic or organic anions (e.g., NO 3 - , Cl - , and CH 3 COO - , etc.) through a conventional anion-exchange procedure, and the original conical morphology can be perfectly maintained. The anion-exchanged product, for example, NO 3 - -intercalated NCs, can be more easily and topotactically transformed into oxide NCs than the original DS - -intercalated form, exempt from the formation of rare-earth oxysulfates induced by the combustion of interlayer DS anions. Taking advantage of this protocol, tri-metallic (Y-Yb-Er) LRH NCs were anion-exchanged into the NO 3 - -intercalated form and subsequently calcined into Y 2 O 3 :Yb,Er oxide NCs, which showed efficient upconversion photoluminescence properties. The current strategy may become a general method for the designed synthesis of other related hydroxide and oxide NCs for a wide range of potential applications.

  4. Davis-Beirut Reaction: Alkoxide versus Hydroxide Addition to the Key o-Nitrosoimine Intermediate.

    Science.gov (United States)

    Zhu, Jie S; Duong, Matthew R; Teuthorn, Andrew P; Lu, Julia Y; Son, Jung-Ho; Haddadin, Makhluf J; Kurth, Mark J

    2018-03-02

    Reaction options, alkoxide vs hydroxide vs amine addition to the key intermediate (o-nitrosoimine) generated in the Davis-Beirut reaction of an o-nitrobenzylamine substrate, are reported to explain the nucleophilic addition selectivity of this one-pot indazole-forming process. The hydroxide addition/deprotection pathway as well as the fate of the resulting o-nitrosobenzaldehyde were both uncovered with several o-nitrobenzylamine substrates, and design elements required for an efficient double Davis-Beirut reaction, inspired by new mechanistic insights, were defined.

  5. Removal of cesium ions from clays by cationic surfactant intercalation.

    Science.gov (United States)

    Park, Chan Woo; Kim, Bo Hyun; Yang, Hee-Man; Seo, Bum-Kyoung; Moon, Jei-Kwon; Lee, Kune-Woo

    2017-02-01

    We propose a new approach to remediate cesium-contaminated clays based on intercalation of the cationic surfactant dodecyltrimethylammonium bromide (DTAB) into clay interlayers. Intercalation of DTAB was found to occur very rapidly and involved exchanging interlayer cations. The reaction yielded efficient cesium desorption (∼97%), including of a large amount of otherwise non-desorbable cesium ions by cation exchange with ammonium ions. In addition, the intercalation of DTAB afforded an expansion of the interlayers, and an enhanced desorption of Cs by cation exchange with ammonium ions even at low concentrations of DTAB. Finally, the residual intercalated surfactants were easily removed by a decomposition reaction with hydrogen peroxide in the presence of Cu 2+ /Fe 2+ catalysts. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Method for intercalating alkali metal ions into carbon electrodes

    Science.gov (United States)

    Doeff, Marca M.; Ma, Yanping; Visco, Steven J.; DeJonghe, Lutgard

    1995-01-01

    A low cost, relatively flexible, carbon electrode for use in a secondary battery is described. A method is provided for producing same, including intercalating alkali metal salts such as sodium and lithium into carbon.

  7. Intercalation of Carbon Nanotube Fibers to Improve their Conductivity

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to increase the electrical conductivity of fibers made up of carbon nanotubes by intercalation with bromine. We further expect that the resulting fibers...

  8. A label-free photoelectrochemical cocaine aptasensor based on an electropolymerized ruthenium-intercalator complex

    International Nuclear Information System (INIS)

    Haddache, Fatima; Le Goff, Alan; Spinelli, Nicolas; Gairola, Priyanka; Gorgy, Karine; Gondran, Chantal; Defrancq, Eric; Cosnier, Serge

    2016-01-01

    Highlights: • Electrodes were modified by an electrogenerated Ru(II) complex which demonstrates photosensitive properties and intercalating properties towards the stem-loop base pairing domain of cocaine aptamers. • Cocaine aptamers were immobilized as mono-and double-fragment which showed different behaviour towards photocurrent generation. • The binding of aptamer could be followed by photelectrochemistry and modelized using a Langmuir-Freundlich isotherm. • Using the double-fragment aptamer, a label-free photoelectrochemical aptasensor was designed, exhibiting a LOD of 10 nmol L −1 and linear range of 1 10 −8 –5 10 −4 mol L −1 . - Abstract: A photoelectrode was designed by electrodeposition of a pyrrole monomer modified with a polypyridyl Ru(II) complex bearing benzo[i]dipyrido-[3,2-a:2′.3′-c]phenazine (dppn) ligand. Owing to the intercalating properties of these immobilized complexes towards DNA double helix, cocaine aptamer was immobilized on the modified electrodes thanks to its stem-loop configuration in order to design a photoelectrochemical cocaine aptasensor. Especially using a double-fragment aptamer strategy, the binding of cocaine and the formation of the aptamer/cocaine complex was successfully observed and modeled by a Langmuir-Freundlich isotherm, giving access to an apparent dissociation constant K d of 3.8 mmol L −1 . The photoelectrochemical aptasensor exhibits a LOD of 10 nmol L −1 and linear range of 1 10 −8 –5 10 −4 mol L −1 .

  9. Synthesis of graphene nanoplatelets from peroxosulfate graphite intercalation compounds

    OpenAIRE

    MELEZHYK A.V.; TKACHEV A.G.

    2014-01-01

    Ultrasonic exfoliation of expanded graphite compound obtained by cold expansion of graphite intercalated with peroxodisulfuric acid was shown to allow the creation of graphene nanoplatelets with thickness of about 5-10 nm. The resulting graphene material contained surface oxide groups. The expanded graphite intercalation compound was exfoliated by ultrasound much easier than thermally expanded graphite. A mechanism for the cleavage of graphite to graphene nanoplatelets is proposed. It include...

  10. Síntese e caracterização de Nanocompósitos Esfoliados de Poliestireno: Hidróxido Duplo Lamelar via polimerização in situ Synthesis and characterization of Exfoliated Polystyrene: Layered Double Hydroxide Nanocomposites via in situ polymerization

    Directory of Open Access Journals (Sweden)

    Rodrigo Botan

    2011-01-01

    Full Text Available Nanocompósitos Esfoliados de Poliestireno (PS e Hidróxido Duplo Lamelar (HDL composto por zinco, alumínio e dodecil sulfato de sódio, como ânion interlamelar, foram sintetizados via polimerização in situ. O efeito de diferentes composições de HDL (0,5, 1, 3 e 5% em massa foi avaliado. Os nanocompósitos obtidos foram caracterizados através de ensaios de Difração de Raios X (DRX, Espectroscopia no Infravermelho por Transformada de Fourier (FTIR, Microscopia Eletrônica de Transmissão (MET e Análise Termogravimétrica (TGA. Os resultados obtidos através das análises de DRX e MET mostraram que todos os nanocompósitos produzidos apresentaram morfologia esfoliada. Os resultados das TGA, quando se utilizam 50% de perda de peso como ponto para comparação, apresentaram ganhos significativos de estabilidade térmica para todas as composições dos nanocompósitos em comparação ao poliestireno puro. Este comportamento possibilita uma vasta gama de aplicação destes novos materiais em diversos campos da indústria e pesquisa.Exfoliated nanocomposites of polystyrene (PS and layered double hydroxide (LDH compound of zinc, aluminium and sodium dodecyl sulfate, as interlayer anion, have been synthesized via in situ polymerization. The effect from the LDH compositions (0.5, 1, 3, 5% weight was studied. The nanocomposites were characterized by X-ray Diffraction (XRD, Fourier Transform Infrared Spectroscopy (FTIR, Transmission Electron Microscopy (TEM and Thermogravimetric Analysis (TGA. The XRD and TEM results showed an exfoliated morphology for the nanocomposites in all compositions. With the 50% weight loss taken as a reference, the TGA results indicated significant improvement in thermal stability for all compositions of the nanocomposites, in comparison to pure polystyrene. This is promising for the application of these new materials in many fields of industry and research.

  11. Obtaining graphene nanoplatelets from various graphite intercalation compounds

    Science.gov (United States)

    Melezhyk, A.; Galunin, E.; Memetov, N.

    2015-11-01

    The work compares the exfoliation ability of different graphite materials (expanded graphite intercalation compound, thermally expanded and oxidatively intercalated graphites) and describes the properties of graphene nanoplatelets (GNPs) obtained dependently on intercalation/deintercalation conditions and reagents. Among the studied materials, the graphite intercalated with ammonium persulfate in sulfuric acid and expanded at 40 °C possesses the maximum ability for ultrasonic exfoliation in the presence of a surfactant. The exfoliation efficiency strongly depends on the content of water in sulfuric acid during the intercalation. The highest efficiency was achieved for the expanded graphite intercalation compound (EGIC) prepared in sulfuric acid containing diluted oleum, which may be explained by increased acidity of the medium and, correspondingly, redox potential of the persulfate compound. This is also related to increased amounts of oxygen groups in the GNPs obtained from the EGIC synthesized in 100% sulfuric acid and diluted oleum. Besides, the nature of surface groups on the GNPs strongly depends on the nature of a deintercalating reagent. Thus, the treatment of the EGIC with different nucleophilic molecules (such as water, ammonia, carbamide, hexamethylenetetramine, organic amines, etc.) can yield GNPs with various surface groups. The interaction between the EGIC and nucleophilic molecules does not only include the substitution of sulfate groups, but also redox reactions with participation of graphene layers. Depending on the nature of the nucleophile, those reactions can lead to the formation of different groups attached to the graphene surface. GNPs with almost pure surface were obtained when using ammonia and carbamide.

  12. Discriminating Intercalative Effects of Threading Intercalator Nogalamycin, from Classical Intercalator Daunomycin, Using Single Molecule Atomic Force Spectroscopy.

    Science.gov (United States)

    Banerjee, T; Banerjee, S; Sett, S; Ghosh, S; Rakshit, T; Mukhopadhyay, R

    2016-01-01

    DNA threading intercalators are a unique class of intercalating agents, albeit little biophysical information is available on their intercalative actions. Herein, the intercalative effects of nogalamycin, which is a naturally-occurring DNA threading intercalator, have been investigated by high-resolution atomic force microscopy (AFM) and spectroscopy (AFS). The results have been compared with those of the well-known chemotherapeutic drug daunomycin, which is a non-threading classical intercalator bearing structural similarity to nogalamycin. A comparative AFM assessment revealed a greater increase in DNA contour length over the entire incubation period of 48 h for nogalamycin treatment, whereas the contour length increase manifested faster in case of daunomycin. The elastic response of single DNA molecules to an externally applied force was investigated by the single molecule AFS approach. Characteristic mechanical fingerprints in the overstretching behaviour clearly distinguished the nogalamycin/daunomycin-treated dsDNA from untreated dsDNA-the former appearing less elastic than the latter, and the nogalamycin-treated DNA distinguished from the daunomycin-treated DNA-the classically intercalated dsDNA appearing the least elastic. A single molecule AFS-based discrimination of threading intercalation from the classical type is being reported for the first time.

  13. Discriminating Intercalative Effects of Threading Intercalator Nogalamycin, from Classical Intercalator Daunomycin, Using Single Molecule Atomic Force Spectroscopy.

    Directory of Open Access Journals (Sweden)

    T Banerjee

    Full Text Available DNA threading intercalators are a unique class of intercalating agents, albeit little biophysical information is available on their intercalative actions. Herein, the intercalative effects of nogalamycin, which is a naturally-occurring DNA threading intercalator, have been investigated by high-resolution atomic force microscopy (AFM and spectroscopy (AFS. The results have been compared with those of the well-known chemotherapeutic drug daunomycin, which is a non-threading classical intercalator bearing structural similarity to nogalamycin. A comparative AFM assessment revealed a greater increase in DNA contour length over the entire incubation period of 48 h for nogalamycin treatment, whereas the contour length increase manifested faster in case of daunomycin. The elastic response of single DNA molecules to an externally applied force was investigated by the single molecule AFS approach. Characteristic mechanical fingerprints in the overstretching behaviour clearly distinguished the nogalamycin/daunomycin-treated dsDNA from untreated dsDNA-the former appearing less elastic than the latter, and the nogalamycin-treated DNA distinguished from the daunomycin-treated DNA-the classically intercalated dsDNA appearing the least elastic. A single molecule AFS-based discrimination of threading intercalation from the classical type is being reported for the first time.

  14. Synthesis and Physico-Chemical Properties of Zinc Layered Hydroxide-4-Chloro-2-Methylphenoxy Acetic Acid (ZMCPA) Nanocomposite

    Science.gov (United States)

    Salleh, N. M.; Mohsin, SM N.; Sarijo, S. H.; Ghazali, S. A. I. S. M.

    2017-05-01

    Hybrid nanocomposite zinc layered hydroxide-4-chloro-2-methylphenoxyacetic acid (ZMCPA) was successfully synthesized via direct reaction of 4-chloro-2-methylphenoxy acetic acid (MCPA) with zinc oxide (ZnO) under an aqueous environment. The pure phase and well-ordered ZMCPA was obtained when ZMCPA was synthesized at 0.3 M MCPA. The resulting nanocomposite, ZMCPA was characterized by powder X-ray diffraction (PXRD), fourier transform infrared(FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), thermogravimetric and differential thermogravimetric analyses (TGA/DTG) and CHNS Analyzer. Basal spacing showed that the gallery height of zinc layered hydroxide (ZLH) expanded from 11.Å to 24.1 Å, indicating that the MCPA anions were successfully intercalated into the interlayer space of ZLH. The FTIR spectrum of the ZMCPA shows it resembles the spectra of ZnO and MCPA that confirms the intercalation of MCPA between the ZLH sheets. FESEM shows the ZnO precursor has granular structure and transformed into a flake-like structure when the nanohybrid is formed. Percentage loading of MCPA interleaved in the nanohybrid is 50.2%.

  15. Intercalation of metals and silicon at the interface of epitaxial graphene and its substrates

    International Nuclear Information System (INIS)

    Huang Li; Xu Wen-Yan; Que Yan-De; Mao Jin-Hai; Meng Lei; Pan Li-Da; Li Geng; Wang Ye-Liang; Du Shi-Xuan; Gao Hong-Jun; Liu Yun-Qi

    2013-01-01

    Intercalations of metals and silicon between epitaxial graphene and its substrates are reviewed. For metal intercalation, seven different metals have been successfully intercalated at the interface of graphene/Ru(0001) and form different intercalated structures. Meanwhile, graphene maintains its original high quality after the intercalation and shows features of weakened interaction with the substrate. For silicon intercalation, two systems, graphene on Ru(0001) and on Ir(111), have been investigated. In both cases, graphene preserves its high quality and regains its original superlative properties after the silicon intercalation. More importantly, we demonstrate that thicker silicon layers can be intercalated at the interface, which allows the atomic control of the distance between graphene and the metal substrates. These results show the great potential of the intercalation method as a non-damaging approach to decouple epitaxial graphene from its substrates and even form a dielectric layer for future electronic applications. (topical review - low-dimensional nanostructures and devices)

  16. Organoelemental intercalation compounds in the system PbI2-ethan olamine

    International Nuclear Information System (INIS)

    Gurina, G.I.; Evtushenko, V.D.; Muraeva, O.A.; Ignatyuk, V.P.; Koshkin, V.M.

    1985-01-01

    Two intercalation phases with different stoichiometry in system PbI 2 -ethanolamine are identified, using the methods of IR spectroscopy, spectroscopy of diffusion reflection, X-ray phase and thermogravimetric analyses. Formation kinetics of intercalation compounds in the system, having two phases, differing in the content of intercalant in the matrix layers, is studied. In conformity with thermodynamic theory of intercalation, it is shown experimentally, that the value of a charge, transferred from intercalant molecules to the matrix layer, decreases with the increase in intercalant content in interlayer spaces

  17. Thermodynamics of Lithium Intercalation in Randomly Oriented High Graphene Carbon

    Directory of Open Access Journals (Sweden)

    Rahul S. Kadam

    2017-01-01

    Full Text Available This paper covers details of systematic investigation of the thermodynamics (entropy and enthalpy of intercalation associated with lithium ion in a structurally novel carbon, called Randomly Oriented High Graphene (ROHG carbon and graphite. Equilibrated OCV (Open Circuit Voltage versus temperature relationship is investigated to determine the thermodynamic changes with the lithium intercalation. ROHG carbon shows entropy of 9.36 J·mol−1·K−1 and shows no dependency on the inserted lithium concentration. Graphite shows initial entropy of 84.27 J·mol−1·K−1 and shows a strong dependence on lithium concentration. ROHG carbon (from −90.85 kJ mol−1 to −2.88 kJ mol−1 shows gradual change in the slope of enthalpy versus lithium ion concentration plot compared to graphite (−48.98 kJ mol−1 to 1.84 kJ mol−1. The study clearly shows that a lower amount of energy is required for the lithium ion intercalation into the ROHG structure compared to graphite structure. Randomly oriented graphene platelet cluster structure of ROHG carbon makes it easier for the intercalation or deintercalation of lithium ion. The ease of intercalation and the small cluster structure of ROHG as opposed to the long linear platelet structure of graphite lead to higher rates of the charge-discharge process for ROHG, when used as an electrode material in electrochemical applications.

  18. Adsorbed or intercalated: Na on graphene/Ir(111)

    Science.gov (United States)

    Pervan, Petar; Lazić, Predrag

    2017-09-01

    Interaction of sodium with graphene (Gr) on Ir(111) was studied with the aim to resolve the issue of Na adsorption/intercalation kinetics. The system Na/Gr/Ir(111) was studied by means of angle-resolved photoemission spectroscopy, low-energy electron diffraction, and ab initio density functional theory (DFT) calculation. It has been found that at room temperature (RT) and low concentrations Na is dominantly adsorbed on graphene. At higher concentrations, an intercalation process sets in so that it is possible to observe the coexistence of these two states. Eventually, all Na atoms are found in the intercalated state as determined by exposure to oxygen. While adsorption of Na on graphene already intercalated by Na [Na/Gr/Na/Ir(111) system] at RT was not possible, we could observe Li adsorption through the increase of Dirac point binding energy. Li coadsorption strongly affects the binding energy of the iridium surface state as well. This finding was supported by DFT calculations of adsorption energy of Na and Li on bare and fully Na intercalated graphene.

  19. Hybrid n-Alkylamine Intercalated Layered Titanates for Solid Lubrication.

    Science.gov (United States)

    Gonzalez Rodriguez, Pablo; Yuan, Huiyu; van den Nieuwenhuizen, Karin J H; Lette, Walter; Schipper, Dik J; Ten Elshof, Johan E

    2016-10-26

    The intercalation of different primary n-alkylamines in the structure of a layered titanate of the lepidocrocite type (H 1.07 Ti 1.73 O 4 ) for application in high-temperature solid lubrication is reported. The intercalation process of the amines was explored by means of in situ small-angle X-ray scattering (SAXS), with variations in alkyl chain length (3-12 carbon atoms) and the amine/titanate ratio. The intercalation process was found to be completed within 5 min after mixing of the precursors in water at 80 °C. The topotactic transformation of the layered titanate is driven by an acid-base reaction. The thermal degradation of the modified titanates was investigated by thermogravimetric analysis (TGA), and the chemical changes were investigated by temperature-dependent infrared spectroscopy (DRIFTS). The coefficient of friction of the lubricants was assessed by means of high-temperature pin-on-disc experiments up to 580 °C. The intercalation of amine rendered a deformable layered ceramic upon heating. It was found that the hydrocarbon chain length exerts an influence on the mechanical properties of the titanates, resulting in lower friction forces for lubricants with longer intercalated amine molecules. Films of solid lubricants with longer amine chain lengths showed coefficients of friction as low as 0.01, lower than that of the state-of-the-art material graphite.

  20. Intercalation and Exfoliation of Kaolinite with Sodium Dodecyl Sulfate

    Directory of Open Access Journals (Sweden)

    Xiaochao Zuo

    2018-03-01

    Full Text Available Kaolinite (Kaol was intercalated with dimethyl sulfoxide (DMSO and subsequently methanol (MeOH to prepare intercalation compounds Kaol-DMSO and Kaol-MeOH. Kaol-MeOH was used as an intermediate to synthesize Kaol-sodium dodecyl sulfate (SDS intercalation compound (Kaol-SDS via displacement reaction. The ultrasonic exfoliation of Kaol-SDS produced a resultant Kaol-SDS-U. The samples were characterized by X-ray diffraction (XRD, Fourier transformation infrared spectroscopy (FTIR, thermal analysis, scanning electronic microscopy (SEM, transmission electron microscopy (TEM and particle size analysis. The results revealed that the intercalation of sodium dodecyl sulfate into kaolinite layers caused an obvious increase of the basal spacing from 0.72–4.21 nm. The dehydroxylation temperature of Kaol-SDS was obviously lower than that of original kaolinite. During the intercalation process of sodium dodecyl sulfate, a few kaolinite layers were exfoliated and curled up from the edges of the kaolinite sheets. After sonication treatment, the kaolinite layers were further transformed into nanoscrolls, and the exfoliated resultant Kaol-SDS-U possessed a smaller particle size close to nanoscale.

  1. Highly n -doped graphene generated through intercalated terbium atoms

    Science.gov (United States)

    Daukiya, L.; Nair, M. N.; Hajjar-Garreau, S.; Vonau, F.; Aubel, D.; Bubendorff, J. L.; Cranney, M.; Denys, E.; Florentin, A.; Reiter, G.; Simon, L.

    2018-01-01

    We obtained highly n -type doped graphene by intercalating terbium atoms between graphene and SiC(0001) through appropriate annealing in ultrahigh vacuum. After terbium intercalation angle-resolved-photoelectron spectroscopy (ARPES) showed a drastic change in the band structure around the K points of the Brillouin zone: the well-known conical dispersion band of a graphene monolayer was superposed by a second conical dispersion band of a graphene monolayer with an electron density reaching 1015cm-2 . In addition, we demonstrate that atom intercalation proceeds either below the buffer layer or between the buffer layer and the monolayer graphene. The intercalation of terbium below a pure buffer layer led to the formation of a highly n -doped graphene monolayer decoupled from the SiC substrate, as evidenced by ARPES and x-ray photoelectron spectroscopy measurements. The band structure of this highly n -doped monolayer graphene showed a kink (a deviation from the linear dispersion of the Dirac cone), which has been associated with an electron-phonon coupling constant one order of magnitude larger than those usually obtained for graphene with intercalated alkali metals.

  2. Investigating the Intercalation Chemistry of Alkali Ions in Fluoride Perovskites

    Energy Technology Data Exchange (ETDEWEB)

    Yi, Tanghong; Chen, Wei; Cheng, Lei; Bayliss, Ryan D.; Lin, Feng; Plews, Michael R.; Nordlund, Dennis; Doeff, Marca M.; Persson, Kristin A.; Cabana, Jordi (LBNL); (SLAC); (UIC); (UCB)

    2017-02-07

    Reversible intercalation reactions provide the basis for modern battery electrodes. Despite decades of exploration of electrode materials, the potential for materials in the nonoxide chemical space with regards to intercalation chemistry is vast and rather untested. Transition metal fluorides stand out as an obvious target. To this end, we report herein a new family of iron fluoride-based perovskite cathode materials AxK1–xFeF3 (A = Li, Na). By starting with KFeF3, approximately 75% of K+ ions were subsequently replaced by Li+ and Na+ through electrochemical means. X-ray diffraction and Fe X-ray absorption spectroscopy confirmed the existence of intercalation of alkali metal ions in the perovskite structure, which is associated with the Fe2+/3+ redox couple. A computational study by density functional theory showed agreement with the structural and electrochemical data obtained experimentally, which suggested the possibility of fluoride-based materials as potential intercalation electrodes. This study increases our understanding of the intercalation chemistry of ternary fluorides, which could inform efforts toward the exploration of new electrode materials.

  3. A DNA biosensor based on the electrocatalytic oxidation of amine by a threading intercalator

    International Nuclear Information System (INIS)

    Gao Zhiqiang; Tansil, Natalia

    2009-01-01

    An electrochemical biosensor for the detection of DNA based a peptide nucleic acid (PNA) capture probe (CP) modified indium tin oxide electrode (ITO) is described in this report. After hybridization, a threading intercalator, N,N'-bis[(3-propyl)-imidazole]-1,4,5,8-naphthalene diimide (PIND) imidazole complexed with Ru(bpy) 2 Cl (PIND-Ru, bpy = 2,2'-bipyridine), was introduced to the biosensor. PIND-Ru selectively intercalated to double-stranded DNA (ds-DNA) and became immobilized on the biosensor surface. Voltammetric tests showed highly stable and reversible electrochemical oxidation/reduction processes and the peak currents can directly be utilized for DNA quantification. When the tests were conducted in an amine-containing medium, Tris-HCl buffer for example, a remarkable improvement in the voltammetric response and noticeable enhancements of voltammetric and amperometric sensitivities were observed due to the electrocatalytic activity of the [Ru(bpy) 2 Cl] redox moieties. Electrocatalytic current was observed when as little as 3.0 attomoles of DNA was present in the sample solution

  4. Role of intercalation and redox potential in DNA photosensitization by ruthenium(II) polypyridyl complexes: assessment using DNA repair protein tests.

    Science.gov (United States)

    Gicquel, Etienne; Souchard, Jean-Pierre; Magnusson, Fay; Chemaly, Jad; Calsou, Patrick; Vicendo, Patricia

    2013-08-01

    Here we report that the photoreactivity of ruthenium(II) complexes with nucleobases may not only be modulated by their photoredox properties but also by their DNA binding mode. The damage resulting from photolysis of synthetic oligonucleotides and plasmid DNA by [Ru(bpz)3](2+), [Ru(bipy)3](2+) and the two DNA intercalating agents [Ru(bpz)2dppz](2+) and [Ru(bipy)2dppz](2+) has been monitored by polyacrylamide gel electrophoresis and by tests using proteins involved in DNA repair processes (DNA-PKCs, Ku80, Ku70, and PARP-1). The data show that intercalation controls the nature of the DNA damage photo-induced by ruthenium(II) complexes reacting with DNA via an electron transfer process. The intercalating agent [Ru(bpz)2dppz](2+) is a powerful DNA breaker inducing the formation of both single and double (DSBs) strand breaks which are recognized by the PARP-1 and DNA-PKCs proteins respectively. [Ru(bpz)2dppz](2+) is the first ruthenium(II) complex described in the literature that is able to induce DSBs by an electron transfer process. In contrast, its non-intercalating parent compound, [Ru(bpz)3](2+), is mostly an efficient DNA alkylating agent. Photoadducts are recognized by the proteins Ku70 and Ku80 as with cisplatin adducts. This result suggests that photoaddition of [Ru(bpz)2dppz](2+) is strongly affected by its DNA intercalation whereas its photonuclease activity is exalted. The data clearly show that DNA intercalation decreases drastically the photonuclease activity of ruthenium(II) complexes oxidizing guanine via the production of singlet oxygen. Interestingly, the DNA sequencing data revealed that the ligand dipyridophenazine exhibits on single-stranded oligonucleotides a preference for the 5'-TGCGT-3' sequence. Moreover the use of proteins involved in DNA repair processes to detect DNA damage was a powerful tool to examine the photoreactivity of ruthenium(II) complexes with nucleic acids.

  5. First-principles estimates of free energy barriers for Mg desolvation and intercalation at electrolyte/electrode interfaces

    Science.gov (United States)

    Wan, Liwen; Prendergast, David

    2014-03-01

    There is a growing interest in developing multivalent ion batteries that could, in principle, double or triple the energy density compared to the monovalent Li-ion batteries. However, the strong electrostatic interaction caused by the extra charge also makes it very challenging to find appropriate intercalation compounds that allow for relatively fast and reversible ion transport. An established working multivalent battery is comprised of Mg(AlCl2BuEt)2 salts in THF solution as the electrolyte, and Mg metal and Mo6S8 Chevrel phase as the anode and cathode, respectively. Currently, we lack a clear understanding of the mechanism for Mg desolvation and intercalation at the interface between the electrolyte and Chevrel phase surfaces, which is critical in designing new advanced battery systems with improved ion diffusion rate. Here, we present a theoretical investigation of the dynamics and kinetics of the Mg desolvation/intercalation process. The surface properties of Mo6S8 are studied for the first time using density functional theory (DFT) and its interaction with the electrolyte is simulated via an ab initio molecular dynamics (AIMD) approach. The free energy barrier for Mg diffusing through the interface is then calculated by performing a set of biased AIMD simulations. This work is supported as part of the Joint Center for Energy Storage Research (JCESR), an Energy Innovation Hub funded by the U.S. Department of Energy, Office of Science, Basic Energy Sciences.

  6. Lithium intercalation in heat-treated petroleum cokes

    Science.gov (United States)

    Tran, T. D.; Spellman, L. M.; Goldberger, W. M.; Song, X.; Kinoshita, K.

    Petroleum needle cokes were processed by air-milling and heat treatment at three temperatures 1800, 2100 and 2350 °C, to produce a final average particle size of 10 p.m. The effects of air-milling (before and after heat treatment) on the physical and microstructural properties of the petroleum coke particles were examined. The results obtained for electrochemical lithium intercalation/de-intercalation in 0.5 M LiN(CF 3SO 2) 2/EC:DMC electrolyte using these petroleum cokes after the different processing conditions are reported.

  7. Structural Investigation of Zn(II) Insertion in Bayerite an Aluminum Hydroxide

    DEFF Research Database (Denmark)

    Puschparaj, Suraj S. C.; Jensen, Nicholai Daugaard; Forano, Claude

    2016-01-01

    Bayerite was treated under hydrothermal conditions (120, 130, 140, and 150 °C) in order to prepare a series of layered double hydroxides (LDHs) with an ideal composition of ZnAl4(OH)12(SO4)0.5nH2O (ZnAl4-LDHs). These products were investigated by both bulk techniques (PXRD, TEM, and elemental an...

  8. Textural and chemical characterizations of adsorbent prepared from palm shell by potassium hydroxide impregnation at different stages.

    Science.gov (United States)

    Guo, Jia; Lua, Aik Chong

    2002-10-15

    Preparation and characterization of activated carbon from palm shell, a carbonaceous agricultural solid waste, by potassium hydroxide treatment at different stages were studied. The effects of activation temperature and chemical to sample ratio on the characteristics of the activated carbon were investigated. Fixed-bed adsorption of sulfur dioxide (SO(2)) gas was carried out to evaluate the adsorptive capacity of the samples. Desorption tests were conducted to verify the occurrence of chemisorption due to some surface functional groups or of chemical reaction between SO(2) and KOH. It was found that pre-impregnation of raw palm shell was involved in replacement of some hydrogen ions with potassium ions to form cross-linked complexes, which retarded the tar formation during carbonization, resulting in a relatively high yield. Moreover, these potassium ions accelerated the reaction as catalysts during gasification of chars by carbon dioxide. For chars with mid-impregnation, potassium hydroxide acted in two ways: (i) formation of metallic potassium by dehydration and (ii) conversion into potassium carbonate. Metallic potassium intercalated to the carbon matrix accounted for pore development and potassium carbonate layer prevented the sample from over burn-off. Post-impregnation of final products modified the textural characteristics of the sample as some pore entrances were blocked by chemicals. However, potassium hydroxide enhanced the amount of SO(2) uptaken via formation of potassium sulfite.

  9. Iodine Sequestration Using Delafossites and Layered Hydroxides

    Energy Technology Data Exchange (ETDEWEB)

    J.D. Pless; J.B. Chwirka; J.L. Krumhansl

    2006-03-28

    The objective of this document is to report on early success for sequestering {sup 129}I. Sorption coefficients (K{sub d}) for I{sup -} and IO{sub 3}{sup -} onto delafossites, spinels and layered metal hydroxides were measured in order to compare their applicability for sequestering {sup 129}I. The studies were performed using a dilute fluid composition representative of groundwater indigenous to the Yucca mountain area. Delafossites generally exhibited relatively poor sorption coefficients (< 10{sup 1.7} mL/g). In contrast, the composition of the layered hydroxides significantly affects their ability to sorb I. Cu/Al and Cu/Cr layered hydroxide samples exhibit K{sub d}'s greater than 10{sup 3} mL/g for both I{sup -} and IO{sub 3}{sup -}.

  10. Intercalation of Si between MoS2 layers

    NARCIS (Netherlands)

    van Bremen, Rik; Yao, Qirong; Banerjee, Soumya; Cakir, Deniz; Oncel, Nuri; Zandvliet, Harold J.W.

    2017-01-01

    We report a combined experimental and theoretical study of the growth of sub-monolayer amounts of silicon (Si) on molybdenum disulfide (MoS2). At room temperature and low deposition rates we have found compelling evidence that the deposited Si atoms intercalate between the MoS2 layers. Our evidence

  11. Enantiospecific kinking of DNA by a partially intercalating metal complex

    KAUST Repository

    Reymer, Anna

    2012-01-01

    Opposite enantiomers of [Ru(phenanthroline) 3] 2+ affect the persistence length of DNA differently, a long speculated effect of helix kinking. Our molecular dynamics simulations confirm a substantial change of duplex secondary structure produced by wedge-intercalation of one but not the other enantiomer. This effect is exploited by several classes of DNA operative proteins. © The Royal Society of Chemistry 2012.

  12. Measurement of thermal stress in graphite intercalated with bromine

    Energy Technology Data Exchange (ETDEWEB)

    Chung, D.D.L.; Wong, L.W.

    1988-03-01

    The thermal stress of graphite intercalated with bromine was found to increase from zero at about 100/degree/C to about 1.3 MPa at 200/degree/C. The effect was reversible with hysteresis. The thermal stress increase had a sharp temperature dependence due to its association with the exfoliation phase transition.

  13. Exfoliation of Hexagonal Boron Nitride via Ferric Chloride Intercalation

    Science.gov (United States)

    Hung, Ching-cheh; Hurst, Janet; Santiago, Diana; Rogers, Richard B.

    2014-01-01

    Sodium fluoride (NaF) was used as an activation agent to successfully intercalate ferric chloride (FeCl3) into hexagonal boron nitride (hBN). This reaction caused the hBN mass to increase by approx.100 percent, the lattice parameter c to decrease from 6.6585 to between 6.6565 and 6.6569 ?, the x-ray diffraction (XRD) (002) peak to widen from 0.01deg to 0.05deg of the full width half maximum value, the Fourier transform infrared (FTIR) spectrum's broad band (1277/cm peak) to change shape, and new FTIR bands to emerge at 3700 to 2700 and 1600/cm. This indicates hBN's structural and chemical properties are significantly changed. The intercalated product was hygroscopic and interacted with moisture in the air to cause further structural and chemical changes (from XRD and FTIR). During a 24-h hold at room temperature in air with 100 percent relative humidity, the mass increased another 141 percent. The intercalated product, hydrated or not, can be heated to 750 C in air to cause exfoliation. Exfoliation becomes significant after two intercalation-air heating cycles, when 20-nm nanosheets are commonly found. Structural and chemical changes indicated by XRD and FTIR data were nearly reversed after the product was placed in hydrochloric acid (HCl), resulting in purified, exfoliated, thin hBN products.

  14. Preparation of intercalated polyaniline/clay nanocomposite and its

    Indian Academy of Sciences (India)

    Intercalated composite of polyaniline and clay has been reported. The composite was prepared by in situ polymerization of aniline within the layers of `illite' clay. The composite was characterized for its structural, spectral, and microscopic properties. At higher level of loading the layered structure of composite breaks ...

  15. H-D exchange on graphite-potassium intercalation compounds

    International Nuclear Information System (INIS)

    Rummel, S.; Herrmann, M.; Wahren, M.; Junusov, S.M.; Ilatovskaja, M.A.; Isaev, Ju.B.; Lapkina, N.D.; Novikov, Ju.N.; Shur, V.B.

    1991-01-01

    Potassium Graphite Intercalation Compounds are able to activate C-H bonds of hydrocarbons at room temperature. In this paper the hydrogen-deuterium exchange of CHD 3 in the presence of C 8 K, C 24 K and C 36 K are described. (orig.)

  16. Adsorption and intercalation of anionic surfactants onto layered ...

    Indian Academy of Sciences (India)

    Unknown

    MS received 12 October 2004; revised 10 January 2005. Abstract. Layered ... son 2004). Bifunctional short chain anionic surfactant such as tartrate and succinate intercalated Zn/Cr LDH was prepared by Prevot and co-workers (1998). Terephthalate ..... He L, Yin S and Sato T 2003 Solid State Chem. 77 51. Isupov V P and ...

  17. Structural, energetic and electronic properties of intercalated boron ...

    Indian Academy of Sciences (India)

    an ideal non-interacting hosts for these one-dimensional chains of metal atoms. Their electronic properties are insignificantly modified. Keywords. Intercalated boron–nitride nanotubes; quantum chemical calculations. 1. Introduction. According to theoretical studies, carbon nanotubes are pre- dicted to be either metallic or ...

  18. Ionic liquid intercalated V2O5 nanorods: synthesis and ...

    Indian Academy of Sciences (India)

    Administrator

    Abstract. In this work, ionic liquid (IL) intercalated V2O5 (IL-V2O5) nanorods have been synthesized through the IL-assisted hydrothermal method using imidazolium-based functionalized IL at 130°C for 3 days. The structure and morphology of the obtained product was characterized using various techniques. X-ray.

  19. Electrochemical lithium intercalation into vanadium pentoxide xerogel film electrode

    Energy Technology Data Exchange (ETDEWEB)

    Pyun, Su Il; Bae, Joon Sung [Korea Advanced Inst. of Science and Technology, Daejon (Korea, Republic of). Dept. of Materials Science and Engineering

    1997-10-01

    The lithium-ion transport in vanadium pentoxide xerogel film electrodes has been investigated by using cyclic voltammetry and electrochemical impedance spectroscopy. The oxide xerogel film electrodes were prepared by spin-coating a viscous gel on an indium tin oxide (ITO) substrate. The spin-coated xerogel films were dried under vacuum at 130 and 270 C, respectively. The lithium intercalation into the xerogel film electrode dried at 270 C is limited by the interfacial reaction at the electrolyte/electrode interface rather than the lithium-ion transport in the oxide electrode. On the other hand, lithium intercalation into the film electrode dried at 130 C is largely limited by the lithium transport in the oxide film, and the chemical diffusivity of the lithium ion in the oxide film was determined to decrease from 10{sup -10} to 10{sup -12} cm{sup 2} s{sup -1} as the electrode potential of the oxide film fell from 3.0 to 2.2 V{sub Li/Li{sup +}}. The tranition of the diffusion-controlled intercalation to the interfacial reaction-controlled intercalation into the oxide xerogel film with decreasing drying temperature was explained in terms of the modification of the oxide lattice to a more open-structured lattice by structural modification of the oxide film by water molecules incorporated into the film. (orig.)

  20. Preparation of intercalated polyaniline/clay nanocomposite and its ...

    Indian Academy of Sciences (India)

    Intercalated composite of polyaniline and clay has been reported. The composite was prepared by in situ polymerization of aniline within the layers of `illite' clay. The composite was characterized for its structural, spectral, and microscopic properties. At higher level of loading the layered structure of composite breaks ...