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Sample records for surfactant templated mesoporous

  1. Non-surfactant synthesis of mesoporous silica with dye as template

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A novel non-surfactant method was described to synthesize mesoporous silica using dye basic fuchsin as template. Chemical reactions were introduced into the formation of mesopores rather than the weak electrostatic or hydrogen-bonding interactions in the traditional surfactant routes. The reactant composition was found to be crucial to the pore structure of objective product. The formation mechanism of mesopore was also proved.

  2. Surfactant-templating of Ordered Mesoporous Polymers and Carbons

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    1 Results Ordered mesoporous materials possess enormous potential for many high-tech applications[1] such as bioreactors, microelectrophoresis, thermal insulation and catalysts. In general, organic porous materials can be prepared by phase-separation and hard templating approach such as those employing colloidal particles[2]. However, due to the volume contraction and swelling, and the structured defects formed during template removal, most of the resulting porous polymer structures are disordered with ...

  3. Synthesis of 2D Hexagonal Mesoporous Silica Using Amino Acid-based Surfactant Templating

    Directory of Open Access Journals (Sweden)

    Xu Hailan

    2016-01-01

    Full Text Available Ordered 2D hexagonal and parallel arranged pore channel mesoporous silica materials with homogeneous size and spherical shape have been synthesized by using amino acid-based surfactant templating, their ordered mesostructures were characterized by infrared spectroscopy, X-ray diffraction patterns (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM and nitrogen sorption analysis.

  4. Dual latex/surfactant templating of hollow spherical silica particles with ordered mesoporous shells.

    Science.gov (United States)

    Tan, Bing; Rankin, Stephen E

    2005-08-30

    Hollow spherical silica particles with hexagonally ordered mesoporous shells are synthesized with the dual use of cetyltrimethylammonium bromide (CTAB) and unmodified polystyrene latex microspheres as templates in concentrated aqueous ammonia. In most of the hollow mesoporous particles, cylindrical pores run parallel to the hollow core due to interactions of CTAB/silica aggregates with the latices. Effects on the product structure of the CTAB:latex ratio, the amount of aqueous ammonia, and the latex size are studied. Hollow particles with hexagonally patterned mesoporous shells are obtained at moderate CTAB:latex ratios. Too little CTAB causes silica shell growth without surfactant templating, and too much induces nucleation of new mesoporous silica particles without latex cores. The concentration of ammonia must be large to induce co-assembly of CTAB, silica, and latex into dispersed particles. The results are consistent with the formation of particles by addition of CTAB/silica aggregates to the surface of latex microspheres. When the size and number density of the latex microspheres are changed, the size of the hollow core and the shell thickness can be controlled. However, if the microspheres are too small (50 nm in this case), agglomerated particles with many hollow voids are obtained, most likely due to colloidal instability.

  5. Simultaneous Removal of Surfactant Template from MCM-41 and Implantation of Transition Metal Complexes into Mesopores with Supercritical Fluid

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The simultaneous removal of up to 92% of the surfactant template and chemical implantation of transition metal complexes into mesopores has been successfully achieved by treating as-synthesized pure siliceous MCM-41 with supercritical CO2 modified with CH2Cl2/MeOH mixture, resulting in the formation of functionalized material with uniform pore structure.

  6. Synthesis of silica particles with lamellar and wormhole-like bi-modal mesopores using anionic surfactant as the template

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Silica particles with lamellar and wormhole-like bi-modal mesopores have been synthesized using anionic surfactant (N-lauroylsarcosine sodium) as the template. The particles with diameters of 300―500 nm possess bi-modal mesopores with pore sizes of 3 nm and 12 nm, which were ascribed to the disordered wormhole-like mesophase and lamellar mesophase, respectively. The BET surface area of the particles was 536 m2/g and the pore volume was 0.83 cm3/g. The lamellar mesophase and cylindrical mesophase were formed due to the co-assembly of the anionic surfactant and its protonized polar oil.

  7. Synthesis and characterization of pharmaceutical surfactant templated mesoporous silica: Its application to controlled delivery of duloxetine

    Energy Technology Data Exchange (ETDEWEB)

    Mani, Ganesh; Pushparaj, Hemalatha; Peng, Mei Mei; Muthiahpillai, Palanichamy [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of); Udhumansha, Ubaidulla [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of); Department of Pharmaceutics, C.L. Baid Metha College of Pharmacy, Chennai (India); Jang, Hyun Tae, E-mail: htjang@hanseo.ac.kr [Department of Chemical Engineering, Hanseo University, Seosan-si 356 706 (Korea, Republic of)

    2014-03-01

    Graphical abstract: - Highlights: • Usefulness of dual pharmaceutical surfactants in silica synthesis was evaluated. • Effects of concentration of secondary template (Tween-40) were studied. • Effects of fixed solvothermal condition on mesostructure formation were studied. • Duloxetine drug loading capability was studied. • Sustained release of duloxetine was evaluated. - Abstract: A new group of mesoporous silica nanoparticles (MSNs) were synthesized using combination pharmaceutical surfactants, Triton X-100 and Tween-40 as template and loaded with duloxetine hydrochloride (DX), for improving the sustained release of DX and patterns with high drug loading. Agglomerated spherical silica MSNs were synthesized by sol–gel and solvothermal methods. The calcined and drug loaded MSNs were characterized using X-ray diffraction (XRD), Braunner–Emmett–Teller (BET), thermogravimetric analysis (TGA), Fourier-transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), diffuse reflectance ultraviolet–visible (DRS-UV–vis) spectroscopy. MSNs with high surface area and pore volume were selected and studied for their DX loading and release. The selected MSNs can accommodate a maximum of 34% DX within it. About 90% was released at 200 h and hence, the synthesized MSNs were capable of engulfing DX and sustain its release. Further form the Ritger and Peppas, Higuchi model for mechanism drug release from all the MSN matrices follows anomalous transport or Non-Fickian diffusion with the ‘r’ and ‘n’ value 0.9 and 0.45 < n < 1, respectively. So, from this study it could be concluded that the MSNs synthesized using pharmaceutical templates were better choice of reservoir for the controlled delivery of drug which requires sustained release.

  8. Synthesis of mesoporous MCM-48 with a mixed non ionic-cationic surfactant templating pathway

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    In a hydrothermal system, we studied the influence of nonionic surfactant poly(ethylenglycol) monooctylphenyl ether (OP-10) on the self-assembling process of mesoporous molecular sieve MCM-48 and found that OP-10 can decrease the amount of cationic surfactant needed for the preparation of MCM-48 further by its stronger van der Waals force , shorten the synthetic period and produce MCM-48 with more extensive cross-linked framework. By altering the ratio of nonionic surfactant to cationic surfactant, we could obtain the mesoporous molecular sieves with different structures. When the crystallization temperature exceeded-140℃, OP-10 would separate from miceHe, lose its amphiphilic character, and then hamper the conversion of lamellar mesoporous molecular sieves into microporous materials.

  9. Synthesis and characterization of ordered hexagonal and cubic mesoporous tin oxides via mixed-surfactant templates route.

    Science.gov (United States)

    Wang, Yude; Ma, Chunlai; Sun, Xiaodan; Li, Hengde

    2005-06-15

    Ordered hexagonal and cubic mesoporous tin oxides were synthesized for the first time in the presence of mixed cationic and neutral surfactants (a mixture of cetyltrimethylammonium bromide cationic surfactant and dodecylamine neutral surfactant) with different alkali and simple inorganic precursors at room temperature. In the synthesis systems, the dodecylamine neutral surfactant may function as a polar organic cosolvent and cosurfactant. The formation of the tin oxide mesostructured material was proposed to be due to the presence of hydrogen-bonding interactions between the supramolecular template and inorganic precursors Sn4+ and OH-, which were assumed to self-assemble around the cationic surfactant molecules. The materials are characterized by X-ray powder diffraction, transmission electron microscopy, thermogravimetric analysis, and N2 adsorption/desorption isotherm. The surface areas of materials evaluated from the N2 sorption isotherms are about 248 m(2)/g for hexagonal mesoporous tin oxide (SnH) and 281 m(2)/g for cubic mesoporous tin oxide (Sn-C) for calcination at 350 degrees C.

  10. Microwave-Assisted Synthesis of Mesoporous Nano-Hydroxyapatite Using Surfactant Templates

    Science.gov (United States)

    Mesoporous nano-hydroxyapatite (n-HAP) was expeditiously synthesized using the pseudo sol-gel microwave-assisted protocol (30 min) in the presence of two novel templates, namely sodium lauryl ether sulfate (SLES) and linear alkylbenzenesulfonate (LABS). The cooperative self-assem...

  11. Triblock siloxane copolymer surfactant: template for spherical mesoporous silica with a hexagonal pore ordering.

    Science.gov (United States)

    Stébé, M J; Emo, M; Forny-Le Follotec, A; Metlas-Komunjer, L; Pezron, I; Blin, J L

    2013-02-01

    Ordered mesoporous silica materials with a spherical morphology have been prepared for the first time through the cooperative templating mechanism (CTM) by using a silicone triblock copolymer as template. The behavior of the pure siloxane copolymer amphiphile in water was first investigated. A direct micellar phase (L(1)) and a hexagonal (H(1)) liquid crystal were found. The determination of the structural parameters by SAXS measurements leads us to conclude that in the hexagonal liquid crystal phase a part of the ethylene oxide group is not hydrated as observed for the micelles. Mesoporous materials were then synthesized from the cooperative templating mechanism. The recovered materials were characterized by SAXS measurements, nitrogen adsorption-desorption analysis, and transmission and scanning electron microscopy. The results clearly evidence that one can control the morphology and the nanostructuring of the resulting material by modifying the synthesis parameters. Actually, highly ordered mesoporous materials with a spherical morphology have been obtained with a siloxane copolymer/tetramethoxysilane molar ratio of 0.10 after hydrothermal treatment at 100 °C. Our study also supports the fact that the interactions between micelles and the hydrolyzed precursor are one of the key parameters governing the formation of ordered mesostructures through the cooperative templating mechanism. Indeed, we have demonstrated that when the interactions between micelles are important, only wormhole-like structures are recovered.

  12. Preparation of Mesoporous Nano-Hydroxyapatite Using a Surfactant Template Method for Protein Delivery

    Institute of Scientific and Technical Information of China (English)

    Xiaodong Wu; Xiaofeng Song; Dongsong Li; Jianguo Liu; Peibiao Zhang; Xuesi Chen

    2012-01-01

    Mesoporous nano-hydroxyapatite (n-HA) has gained more and more attention as drug storage and release hosts.The aim of this study is to observe the effect of the ratio of surfactant to the theoretical yield of HA on the mesoporous n-HA,then to reveal the effect of the mesoporous nanostrueture on protein delivery.The mesoporous n-HA was synthesized using the wet precipitation in the presence of cetyltrimethylammonium bromide (CTAB) at ambient temperature and normal atmospheric pressure.The morphology,size,crystalline phase,chemical composition and textural characteristics of the product were well characterized by X-ray Powder Diffraction (XRD),Fourier Transform Infrared Spectroscopy (FTIR),Scanning Electron Microscopy (SEM),Transmission Electron Microscopy (TEM),Dynamic Light Scattering (DLS) and N2 adsorption/desorption,respectively.The protein adsorption/release studies were also carried out by using Bovine Serum Albumin (BSA) as a model protein.The results reveal that the mesoporous n-HA synthesized with CTAB exhibits high pure phase,low crystallinity and the typical characteristics of the mesostructure.The BSA loading increases with the specific surface area and the pore volume of n-HA,and the release rates of BSA are different due to their different pore sizes and pore structures,n-HA synthesized with 0.5% CTAB has the highest BSA loading and the slowest release rate because of its highest surface area and smaller pore size.These mesoporous n-HA materials demonstrate a potential application in the field of protein delivery due to their bioaetive,biocompatible and mesoporous properties.

  13. Synthesis of cubic Ia-3d mesoporous silica in anionic surfactant templating system with the aid of acetate.

    Science.gov (United States)

    Deng, Shao-Xin; Xu, Xue-Yan; He, Wen-Chao; Wang, Jin-Gui; Chen, Tie-Hong

    2014-08-01

    Mesoporous silica with three-dimensional (3D) bicontinuous cubic Ia-3d structure and fascinating caterpillar-like morphology was synthesized by using anionic surfactant N-lauroylsarcosine sodium (Sar-Na) as the template and 3-amionpropyltrimethoxysilane (APS) as the co-structure-directing agent (CSDA) with the aid of acetate. A phase transformation from high interfacial curvature 2D hexagonal to low interfacial curvature 3D cubic Ia-3d occurred in the presence of a proper amount of acetate. Other species of salts (excluding acetate) had the ability to induce the caterpillar-like morphology, but failed to induce the cubic Ia-3d mesostructure. Furthermore, [3-(2-aminoethyl)-aminopropyl]trimethoxysilane (DAPS) was also used as the CSDA to synthesize Ia-3d mesostructured silica under the aid of sodium acetate. After extraction of the anionic surfactants, amino and di-amine functionalized 3D bicontinuous cubic Ia-3d mesoporous silicas were obtained and used as supports to immobilize Pd nanoparticles for supported catalysts. The catalytic activity of the catalysts was tested by catalytic hydrogenation of allyl alcohol.

  14. Templating mesoporous zeolites

    DEFF Research Database (Denmark)

    Egeblad, Kresten; Christensen, Christina Hviid; Kustova, Marina

    2008-01-01

    The application of templating methods to produce zeolite materials with hierarchical bi- or trimodal pore size distributions is reviewed with emphasis on mesoporous materials. Hierarchical zeolite materials are categorized into three distinctly different types of materials: hierarchical zeolite...... crystals, nanosized zeolite crystals, and supported zeolite crystals. For the pure zeolite materials in the first two categories, the additional meso- or macroporosity can be classified as being either intracrystalline or intercrystalline, whereas for supported zeolite materials, the additional porosity...... originates almost exclusively from the support material. The methods for introducing mesopores into zeolite materials are discussed and categorized. In general, mesopores can be templated in zeolite materials by use of solid templating, supramolecular templating, or indirect templating...

  15. Three-dimensional low symmetry mesoporous silica structures templated from tetra-headgroup rigid bolaform quaternary ammonium surfactant.

    Science.gov (United States)

    Shen, Shaodian; Garcia-Bennett, Alfonso E; Liu, Zheng; Lu, Qingyi; Shi, Yifeng; Yan, Yan; Yu, Chengzhong; Liu, Weichang; Cai, Ya; Terasaki, Osamu; Zhao, Dongyuan

    2005-05-11

    Two kinds of highly ordered mesoporous silica materials (FDU-11, FDU-13) with novel three-dimensional (3-D) tetragonal and orthorhombic structures were synthesized by using tetra-headgroup rigid bolaform quaternary ammonium surfactant [(CH(3))(3)NCH(2)CH(2)CH(2)N(CH(3))(2)CH(2)(CH(2))(11)OC(6)H(4)C(6)H(4)O(CH(2))(11)CH(2)N(CH(3))(2)CH(2)CH(2)CH(2)N(CH(3))(3).4Br] (C(3-12-12)(-)(3)) as a template under alkaline conditions. High-resolution transmission electron microscopy (HRTEM), small-angle X-ray scattering (SAXS), and X-ray diffraction (XRD) show that mesoporous silica FDU-11 has primitive tetragonal P4/mmm structure with cell parameters a = b = 8.46 nm, c = 5.22 nm, and c/a ratio = 0.617. N(2) sorption isotherms show that calcined FDU-11 has a high BET surface area of approximately 1490 m(2)/g, a uniform pore size of approximately 2.72 nm, and a pore volume of approximately 1.88 cm(3)/g. Mesoporous silica FDU-13 has primitive orthorhombic Pmmm structure. The cell parameters are a = 9.81, b = 5.67, and c = 3.66 nm. N(2) sorption isotherms show that calcined FDU-13 has a high BET surface area of 1210 m(2)/g, a uniform mesopore size of approximately 1.76 nm, and a large pore volume of approximately 1.83 cm(3)/g. Such low symmetries for 3-D mesostructures (tetragonal and orthorhombic system) have not been observed before even in amphiphilic liquid crystals, which maybe resulted from an oblate aggregation of the bolaform surfactant and its strong electrostatic interaction with inorganic precursor. A probable mechanism has been proposed for the formation of such a 3-D low symmetrical mesostructure. These results will further extend the synthesis of mesoporous materials and may open up new opportunities for their new applications in catalysis, separation, and nanoscience.

  16. From Bola-Surfactant Templated Bimetal Phosphites to the Design of Crystalline Inorganic Mesoporous Frameworks.

    Science.gov (United States)

    Huang, Hui-Lin; Huang, Wen-Yen; Wang, Sue-Lein

    2017-04-11

    Reproducing inorganic modules in situ for pore augmentation of pure inorganic frameworks is challenging but can be a key to rational synthesis. After the first success of using monoamines of varied lengths as a template in producing a set of building blocks that led to a series of growing channels up to a 72-membered ring (72R), research continued into those building blocks to seek any new topologies from them. In this study, another type of template is reported that can control the same building blocks to repeatedly form in situ. By using long linear-chain bola-type surfactants, two new bimetal phosphites, a monoclinic phase exhibiting remarkable quasi-channels of 1.15 nm and an orthorhombic phase with 28R channels of 1.06 nm have been created. By taking them as the first members, two series of novel topologies can be devised, each having a general formula to predict the size and channel wall compositions. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Synthesis of mesoporous nano-hydroxyapatite by using zwitterions surfactant

    Science.gov (United States)

    Mesoporous nano-hydroxyapatite (mn-HAP) was successfully synthesized via a novel micelle-templating method using lauryl dimethylaminoacetic acid as zwitterionic surfactant. The systematic use of such a surfactant in combination with microwave energy inputenables the precise contr...

  18. Elucidation of interactive effects of synthesis conditions on the characteristics of mesoporous silicas templated using polyoxide surfactant

    Directory of Open Access Journals (Sweden)

    A.Z. Abdullah, A.H. Kamaruddin, N. Razali, H. Abdullah and S. Bhatia

    2007-01-01

    Full Text Available A series of mesoporous silicas (MS-1–MS-9 were synthesized at different gel compositions using a triblock copolymer (TCP, poly(ethylene oxide–poly(propylene oxide–poly(ethylene oxide, as the surfactant. The interactive effects of acidity, the contents of tetraethyl orthosilicate (TEOS and the surfactant, and the gelling temperature on the characteristics of the final material were simultaneously characterized. Increasing acidity favored mesopore formation. A material with a surface area of 760 m2/g, mostly in the mesoporous range, was obtained at 1.0(TEOS:0.017(TCP:7.3HCl:115.7H2O. Mesopore formation was predominantly determined by the TEOS:TCP ratio and was promoted with its increase from 1.56:1 to 2.09:1. A further increase to 2.61:1 was detrimental. Whereas increasing the TCP content to 3.5% w/w improved micellization, a further increase to 4.6% should be avoided. Mesoporous silicas showed low crystallinity but a high degree of hexagonal mesoscopic organization. The weak surface acidity was attributed to surface silanols, the number of which was proportional to mesoporosity.

  19. A simple route utilizing surfactant-assisted templating sol-gel process for synthesis of mesoporous Dy2O3 nanocrystal.

    Science.gov (United States)

    Sreethawong, Thammanoon; Chavadej, Sumaeth; Ngamsinlapasathian, Supachai; Yoshikawa, Susumu

    2006-08-01

    A simple route of combined sol-gel process with surfactant-assisted templating technique was successfully employed for the first time to synthesize nanocrystalline mesoporous Dy(2)O(3) with narrow monomodal pore size distribution under mild conditions. The nanocrystalline Dy(2)O(3) with monomodal mesoporous characteristic was ultimately achieved by controlling the hydrolysis and condensation steps of dysprosium n-butoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution. The synthesized material was methodically characterized by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), N(2) adsorption-desorption, Brunauer-Emmett-Teller (BET) surface area analysis, and Barrett-Joyner-Halenda (BJH) pore size distribution analysis. The particle size of the synthesized Dy(2)O(3) in nanosized range obtained from the SEM and HRTEM micrographs was in good accordance with the crystallite size estimated from the XRD result. The N(2) adsorption-desorption result exhibited hysteresis pattern with single loop, indicating the existence of monomodal mesopore. The extremely narrow pore size distribution with mean pore diameter in the mesopore region of the synthesized Dy(2)O(3) was also confirmed by the BJH result.

  20. SYNTHESIS OF HYBRID MESOPOROUS POLYSTYRENE-SILICA MATERIALS WITH NON-SURFACTANT CITRIC ACID AS TEMPLATE VIA SOL-GEL PROCESS

    Institute of Scientific and Technical Information of China (English)

    Jie Bai; Jin-yu Zheng; Kun-yuan Qiu; Yen Wei

    2002-01-01

    Hybrid mesoporous polystyrene-silica materials were successfully prepared through HCl-catalyzed sol-gelreactions of tetraethyl orthosilicate (TEOS) and triethoxysilyl-functionalized polystyrene obtained via atom transfer radicalpolymerization (ATRP) of styrene, in the presence of citric acid (CA) as non-surfactant template or pore-forming agent andfollowed by ethanol extraction to remove template molecules. The materials were characterized by infrared spectroscopy(IR), N2 adsorption-desorption measurements, powder X-ray diffraction (XRD), thermogravimetric analysis (TGA) andtransmission electron microscopy (TEM). The results indicate that the materials prepared with 50 wt%-60 wt% templatecontents have average pore size s of 2-3 nm and large surface areas (ca. 886 m2/g) as well as high pore volumes (ca.0.53 cm3/g). The mesoporosity arises from interconnected channels and pores with disordered arrangements. The porediameters and pore volumes increase as the template content is increased. The pore diameters show a little change uponheating at 200℃ overnight. However, the materials do not have good hydrothermal stability.

  1. Template preparation of twisted nanoparticles of mesoporous silica

    Institute of Scientific and Technical Information of China (English)

    Kui Niu; Zhongbin Ni; Chengwu Fu; Tatsuo Kaneko; Mingqing Chen

    2011-01-01

    Optical isomers of N-lauroyl-L-(or-D-) alanine sodium salt {C12-L-(or-D-)AlaS} surfactants were used for the preparation of mesoporous silica nanoparticles with a twisted hexagonal rod-like morphology. Thermogravimetric analysis (TGA) was used to determine the temperature for template removal. Circular dichroism (CD) spectra of the surfactant solution with various compositions illustrated the formation and supramolecular assembly of protein-like molecular architecture leading to formation of twisted nanoparticles. Scanning electron microscopy (SEM),high-resolution transmission electron microscopy (HRTEM)and X-ray powder diffraction (XRD) patterns of these as-synthesized mesoporous silica confirmed that the twisted morphology of these nanoparticles was closely related to the supramolecular-assembled complex of amino acid surfactants.

  2. Elongated silica nanoparticles with a mesh phase mesopore structure by fluorosurfactant templating.

    Science.gov (United States)

    Tan, Bing; Dozier, Alan; Lehmler, Hans-Joachim; Knutson, Barbara L; Rankin, Stephen E

    2004-08-17

    Mesoporous silica materials with pore structures such as 2D hexagonal close packed, bicontinuous cubic, lamellar, sponge, wormhole-like, and rectangular have been made by using surfactant templating sol-gel processes. However, there are still some "intermediate" phases, in particular mesh phases, that are formed by surfactants but which have not been made into analogous silica pore structures. Here, we describe the one-step synthesis of mesoporous silica with a mesh phase pore structure. The cationic fluorinated surfactant 1,1,2,2-tetrahydroperfluorodecylpyridinium chloride (HFDePC) is used as the template. Like many fluorinated surfactants, HFDePC forms intermediate phases in water (including a mesh phase) over a wider range of compositions than do hydrocarbon surfactants. The materials produced by this technique are novel elongated particles in which the layers of the mesh phase are oriented orthogonal to the main axis of the particles.

  3. Surfactant-assisted Nanocasting Route for Synthesis of Highly Ordered Mesoporous Graphitic Carbon and Its Application in CO2 Adsorption

    Science.gov (United States)

    Wang, Yangang; Bai, Xia; Wang, Fei; Qin, Hengfei; Yin, Chaochuang; Kang, Shifei; Li, Xi; Zuo, Yuanhui; Cui, Lifeng

    2016-05-01

    Highly ordered mesoporous graphitic carbon was synthesized from a simple surfactant-assisted nanocasting route, in which ordered mesoporous silica SBA-15 maintaining its triblock copolymer surfactant was used as a hard template and natural soybean oil (SBO) as a carbon precursor. The hydrophobic domain of the surfactant assisted SBO in infiltration into the template’s mesoporous channels. After the silica template was carbonized and removed, a higher yield of highly-ordered graphitic mesoporous carbon with rod-like morphology was obtained. Because of the improved structural ordering, the mesoporous carbon after amine modification could adsorb more CO2 compared with the amine-functionalized carbon prepared without the assistance of surfactant.

  4. Synthesis and Characterization of Mesoporous Silica Vesicles Using Cationic-anionic Binary Surfactant as Template%二元阴阳离子表面活性剂法合成介孔氧化硅囊泡

    Institute of Scientific and Technical Information of China (English)

    牟鸣薇; 彭策; 王颂; 金春阳; 曹献英; 蔡强

    2013-01-01

    Mesoporous silica vesicles were synthesized using cationic surfactant hexadecyl trimethyl ammonium bromide (CTAB) and anionic surfactants sodium dodecyl sulfonate (SDS) in molar ratios of 1.0-2.3 as templates,tetraethyl orthosilicate (TEOS) as silica source at 68 ℃ in ammonia solution medium.The samples were characterized by scanning electron microscopy(SEM),small angle X-ray diffraction (SXRD),transmission electron microscopy(TEM),thermo gravimetric analysis (TGA) and nitrogen adsorption-desorption isotherms measurments.The results indicate that the samples are the continue aggregates of mesoporous silica vesicles with diameters of ca.50 nm.The Brunauer-Emmett-Teller(BET) surface area and nonlocal density functional theory(NLDFT) pore diameter of the samples are 826 m2/g and 4.0 nm,respectively.The formation mechanism of the vesicles was also discussed.%以十二烷基磺酸钠(SDS)和十六烷基三甲基溴化铵(CTAB)为表面活性剂,在SDS与CTAB的摩尔比为1.0~2.3时,以正硅酸乙酯(TEOS)为硅源,在氨水-水体系中于68℃下合成介孔氧化硅囊泡.通过透射电子显微镜(TEM)、X射线衍射仪(XRD)、热重分析仪(TGA)和氮气吸附-脱附实验仪对合成的产物进行表征.结果表明,合成的产物为介孔氧化硅囊泡聚集体,孔径约为4nm,样品的Brunauer-Emmett-Teller (BET)比表面积为826 m2/g.对介孔氧化硅囊泡的形成机理做了初步探讨.

  5. Biocompatibility of Soft-Templated Mesoporous Carbons

    Energy Technology Data Exchange (ETDEWEB)

    Gencoglu, Maria F. [Michigan Technological Univ., Houghton, MI (United States). Dept. of Chemical Engineering; Spurri, Amanda [Widener Univ., Chester, PA (United States). Dept. of Chemical Engineering; Franko, Mitchell [Widener Univ., Chester, PA (United States). Dept. of Chemical Engineering; Chen, Jihua [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Science (CNMS); Hensley, Dale K. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Science (CNMS); Heldt, Caryn L. [Michigan Technological Univ., Houghton, MI (United States). Dept. of Chemical Engineering; Saha, Dipendu [Widener Univ., Chester, PA (United States). Dept. of Chemical Engineering

    2014-08-21

    We report that soft-templated mesoporous carbon is morphologically a non-nano type of carbon. It is a relatively newer variety of biomaterial, which has already demonstrated its successful role in drug delivery applications. To investigate the toxicity and biocompatibility, we introduced three types of mesoporous carbons with varying synthesis conditions and pore textural properties. We compared the Brunauer–Emmett–Teller (BET) surface area and pore width and performed cytotoxicity experiments with HeLa cells, cell viability studies with fibroblast cells and hemocomapatibility studies. Cytotoxicity tests reveal that two of the carbons are not cytotoxic, with cell survival over 90%. The mesoporous carbon with the highest surface area showed slight toxicity (~70% cell survival) at the highest carbon concentration of 500 μg/mL. Fibroblast cell viability assays suggested high and constant viability of over 98% after 3 days with no apparent relation with materials property and good visible cell-carbon compatibility. No hemolysis (<1%) was confirmed for all the carbon materials. Protein adsorption experiments with bovine serum albumin (BSA) and fibrinogen revealed a lower protein binding capacity of 0.2–0.6 mg/m2 and 2–4 mg/m2 for BSA and fibrinogen, respectively, with lower binding associated with an increase in surface area. The results of this study confirm the biocompatibility of soft-templated mesoporous carbons.

  6. Mesoporous Silica Materials Synthesized via Sol-Gel Methods Modified with Ionic Liquid and Surfactant Molecules

    Institute of Scientific and Technical Information of China (English)

    Cun-ying Xu; Ru-lan Tang; Yi-xin Hu; Peng-xiang Zhang

    2008-01-01

    Mesoporous silica materials were synthesized via a sol-gel method employing a room temperature ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, [bmim][BF4]) as a new solvent medium and further modified with surfactant (hexadecyl-trimethyl-ammonium bromide, CTAB) as a pore templating material. The synthesized samples were characterized by the transmission electron microscopy, X-ray diffraction, and N2 adsorption-desorption techniques. The results indicated that the mesoporous silica synthesized by using [bmim][BF4] and CTAB as mixed templates showed better mesostructural order and smaller pore size, compared with mesoporous silica materials synthesized by using single [bmim][BF4]as template under the same conditions. This indicates that the presence of surfactant can affect the microstructures of silica prepared by the present synthesis method.

  7. Metathesis depolymerization for removable surfactant templates.

    Energy Technology Data Exchange (ETDEWEB)

    Zifer, Thomas (Sandia National Laboratories, Livermore, CA); Wheeler, David Roger; Rahimian, Kamayar; McElhanon, James Ross (Sandia National Laboratories, Livermore, CA); Long, Timothy Michael; Jamison, Gregory Marks; Loy, Douglas Anson (Los Alamos National Laboratories, Los Alamos, NM); Kline, Steven R. (National Institute of Standards and Technology, Gaithersburg, MD); Simmons, Blake Alexander (Sandia National Laboratories, Livermore, CA)

    2005-03-01

    Current methodologies for the production of meso- and nanoporous materials include the use of a surfactant to produce a self-assembled template around which the material is formed. However, post-production surfactant removal often requires centrifugation, calcination, and/or solvent washing which can damage the initially formed material architecture(s). Surfactants that can be disassembled into easily removable fragments following material preparation would minimize processing damage to the material structure, facilitating formation of templated hybrid architectures. Herein, we describe the design and synthesis of novel cationic and anionic surfactants with regularly spaced unsaturation in their hydrophobic hydrocarbon tails and the first application of ring closing metathesis depolymerization to surfactant degradation resulting in the mild, facile decomposition of these new compounds to produce relatively volatile nonsurface active remnants.

  8. Supramolecular-templated synthesis of mesoporous silica-zirconia nanocomposite

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Mesoporous SiO2-ZrO2 nanocomposite was successfully prepared by using supramolecular triblock copolymer as the template through evaporation-induced self-assembly approach. The textural and structural properties were characterized by X-ray diffraction, nitrogen adsorption analysis, and transmission electron microscope.Comparison between pure mesoporous silica and mesoporous silica-zirconia nanocomposite was also presented in this work. The surface area, pore size, and pore volume decreased as the Zr doping in the mesoporous silica framework. But the obtained nanocomposite maintained the cubic Im3m-type mesoporous structure.

  9. Preparation of mesoporous aluminophosphate usingpoly(amido amine) as template

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xiaofeng; LIN Shen; CHEN Xinqing; CHEN Jiebo; YANG Liuyi; LUO Minghong

    2007-01-01

    Mesoporous aluminophosphate was prepared by using G4.0 poly(amido amine)dendrimer as a template and characterized by Fourier transform infrared spectrometer(FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and N2 adsorption/desorption methods.Results show that the title compound exhibits a typical mesoporous structure with the average pore size from 5 to 8 nm. The formation mechanism of the nanoporous structure using dendrimer as a template was also discussed.

  10. Fabrication of the tricontinuous mesoporous IBN-9 structure with surfactant CTAB

    KAUST Repository

    Zhao, Yunfeng

    2011-12-13

    IBN-9 is the first tricontinuous mesoporous material, consisting of three identical interpenetrating channels that are separated by a single continuous silica wall. It was originally synthesized using a specially designed surfactant as template. The need of special surfactant in the synthesis inhibits extensive investigation of this novel structure and its applications. We demonstrate in this study that such a complicated tricontinuous mesostructure can also be fabricated from the most common and commercially available surfactant cetyltrimethylammonium bromide (CTAB) with the help of polar organic additives, e.g., n-butanol. The role of n-butanol is to finely tune the surface curvature of the organic/inorganic interface during the cooperative self-assembly process. Electron microscopic techniques are employed to identify different mesostructures from the mixture. This study reveals the possibility of discovering unprecedented mesostructures from conventional surfactant-water- silicates systems. © 2011 American Chemical Society.

  11. Mesoporous silica magnetite nanocomposite synthesized by using a neutral surfactant

    Science.gov (United States)

    Souza, K. C.; Salazar-Alvarez, G.; Ardisson, J. D.; Macedo, W. A. A.; Sousa, E. M. B.

    2008-05-01

    Magnetite nanoparticles coated by mesoporous silica were synthesized by an alternative chemical route using a neutral surfactant and without the application of any functionalization method. The magnetite (Fe3O4) nanoparticles were prepared by precipitation from aqueous media, and then coated with mesoporous silica by using nonionic block copolymer surfactants as the structure-directing agents. The mesoporous SiO2-coated Fe3O4 samples were characterized by x-ray diffraction, Fourier-transform infrared spectroscopy, N2 adsorption-desorption isotherms, transmission electron microscopy, 57Fe Mössbauer spectroscopy, and vibrating sample magnetometry. Our results revealed that the magnetite nanoparticles are completely coated by well-ordered mesoporous silica with free pores and stable (~8 nm thick) pore walls, and that the structural and magnetic properties of the Fe3O4 nanoparticles are preserved in the applied synthesis route.

  12. Mesoporous silica and organosilica films templated by nanocrystalline chitin.

    Science.gov (United States)

    Nguyen, Thanh-Dinh; Shopsowitz, Kevin E; MacLachlan, Mark J

    2013-11-04

    Liquid crystalline phases can be used to impart order into inorganic solids, creating materials that mimic natural architectures. Herein, mesoporous silica and organosilica films with layered structures and high surface areas have been templated by nanocrystalline chitin. Aqueous suspensions of spindle-shaped chitin nanocrystals were prepared by sequential deacetylation and hydrolysis of chitin fibrils isolated from king crab shells. The nanocrystalline chitin self-assembles into a nematic liquid-crystalline phase that has been used to template silica and organosilica composites. Removal of the chitin template by either calcination or sulfuric-acid-catalyzed hydrolysis gave mesoporous silica and ethylene-bridged organosilica films. The large, crack-free mesoporous films have layered structures with features that originate from the nematic organization of the nanocrystalline chitin.

  13. Highly mesoporous single-crystalline zeolite beta synthesized using a nonsurfactant cationic polymer as a dual-function template

    KAUST Repository

    Zhu, Jie

    2014-02-12

    Mesoporous zeolites are useful solid catalysts for conversion of bulky molecules because they offer fast mass transfer along with size and shape selectivity. We report here the successful synthesis of mesoporous aluminosilicate zeolite Beta from a commercial cationic polymer that acts as a dual-function template to generate zeolitic micropores and mesopores simultaneously. This is the first demonstration of a single nonsurfactant polymer acting as such a template. Using high-resolution electron microscopy and tomography, we discovered that the resulting material (Beta-MS) has abundant and highly interconnected mesopores. More importantly, we demonstrated using a three-dimensional electron diffraction technique that each Beta-MS particle is a single crystal, whereas most previously reported mesoporous zeolites are comprised of nanosized zeolitic grains with random orientations. The use of nonsurfactant templates is essential to gaining single-crystalline mesoporous zeolites. The single-crystalline nature endows Beta-MS with better hydrothermal stability compared with surfactant-derived mesoporous zeolite Beta. Beta-MS also exhibited remarkably higher catalytic activity than did conventional zeolite Beta in acid-catalyzed reactions involving large molecules. © 2014 American Chemical Society.

  14. Effects of template and precursor chemistry on structure and properties of mesoporous TiO2 thin films.

    Science.gov (United States)

    Li, X Shari; Fryxell, Glen E; Birnbaum, Jerome C; Wang, Chongmin

    2004-10-12

    Mesoporous TiO2 thin films were synthesized by sol-gel processing using an aqueous-based, inexpensive, and environmentally friendly precursor and cationic surfactants as templates under mild reaction conditions. The films were prepared by spin-coating on glass substrates followed by calcination to remove the surfactant. N2 sorption, X-ray diffraction, and transmission electron microscopy were used to characterize the porosity, pore size, and pore structure before and after calcination. Films were found to have wormlike pore structures after calcination and surface areas on the order of 200 m2/g. These results show that the mesostructure and porosity of the thin films can be controlled by the surfactant template chemistry such as surfactant/Ti ratio, pH, and rate of solvent evaporation.

  15. Soft templating strategies for the synthesis of mesoporous materials: inorganic, organic-inorganic hybrid and purely organic solids.

    Science.gov (United States)

    Pal, Nabanita; Bhaumik, Asim

    2013-03-01

    With the discovery of MCM-41 by Mobil researchers in 1992 the journey of the research on mesoporous materials started and in the 21st century this area of scientific investigation have extended into numerous branches, many of which contribute significantly in emerging areas like catalysis, energy, environment and biomedical research. As a consequence thousands of publications came out in large varieties of national and international journals. In this review, we have tried to summarize the published works on various synthetic pathways and formation mechanisms of different mesoporous materials viz. inorganic, organic-inorganic hybrid and purely organic solids via soft templating pathways. Generation of nanoscale porosity in a solid material usually requires participation of organic template (more specifically surfactants and their supramolecular assemblies) called structure-directing agent (SDA) in the bottom-up chemical reaction process. Different techniques employed for the syntheses of inorganic mesoporous solids, like silicas, metal doped silicas, transition and non-transition metal oxides, mixed oxides, metallophosphates, organic-inorganic hybrids as well as purely organic mesoporous materials like carbons, polymers etc. using surfactants are depicted schematically and elaborately in this paper. Moreover, some of the frontline applications of these mesoporous solids, which are directly related to their functionality, composition and surface properties are discussed at the appropriate places.

  16. Structurally stabilized organosilane-templated thermostable mesoporous titania.

    Science.gov (United States)

    Amoli, Vipin; Tiwari, Rashmi; Dutta, Arghya; Bhaumik, Asim; Sinha, Anil Kumar

    2014-01-13

    Structurally thermostable mesoporous anatase TiO2 (m-TiO2) nanoparticles, uniquely decorated with atomically dispersed SiO2, is reported for the first time. The inorganic Si portion of the novel organosilane template, used as a mesopores-directing agent, is found to be incorporated in the pore walls of the titania aggregates, mainly as isolated sites. This is evident by transmission electron microscopy and high-angle annular dark field scanning transmission electron microscopy, combined with electron dispersive X-ray spectroscopy. This type of unique structure provides exceptional stability to this new material against thermal collapse of the mesoporous structure, which is reflected in its high surface area (the highest known for anatase titania), even after high-temperature (550 °C) calcination. Control of crystallite size, pore diameter, and surface area is achieved by varying the molar ratios of the titanium precursor and the template during synthesis. These mesoporous materials retain their porosity and high surface area after template removal and further NaOH/HCl treatment to remove silica. We investigate their performance for dye-sensitized solar cells (DSSCs) with bilayer TiO2 electrodes, which are prepared by applying a coating of m-TiO2 onto a commercial titania (P25) film. The high surface area of the upper mesoporous layer in the P25-m-TiO2 DSSC significantly increases the dye loading ability of the photoanode. The photocurrent and fill factor for the DSSC with the bilayer TiO2 electrode are greatly improved. The large increase in photocurrent current (ca. 56%) in the P25-m-TiO2 DSSC is believed to play a significant role in achieving a remarkable increase in the photovoltaic efficiency (60%) of the device, compared to DSSCs with a monolayer of P25 as the electrode. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Synthesis of mesoporous silica microsphere from dual surfactant

    Directory of Open Access Journals (Sweden)

    Venkatathri Narayanan

    2008-12-01

    Full Text Available A new procedure is reported to synthesis mesoporous silica micro sphere for the first time. In these method two surfactants namely Span 80 and Tween 80 were used. Small angle X ray diffraction and N2 adsorption analysis shows the synthesized material has mesoporous property. The material has spherical morphology with 1-10 µm particle size. Beside the material found to have microcapsule property as observed from the Transmission electron microscopy. The Fourier transform Infrared spectroscopic analysis reveals that the materials are similar to other mesoporous materials. We also encapsulated an UV-absorber Ibuprofen inside the microcapsule, by mixing it before the synthesis. This shows a possibility of the materials in cosmetic applications.

  18. CNTs/mesostructured silica core-shell nanowires via interfacial surfactant templating

    Institute of Scientific and Technical Information of China (English)

    ZHANG Lei; QIAO ShiZhang; YAN ZiFeng; ZHENG HuaJun; LI Li; DING RongGang; LU GaoQing(Max)

    2009-01-01

    Carbon nanotubes (CNTs)/mesostructured silica core-shell nanowires with a carbon nanotube core and controllable highly ordered periodic mesoporous silica shell are syntheiszed via the interfacial surfac-tant template. The core-shell nanowires are characterized by transmission electron microscope (TEM), X-ray diffraction pattern (XRD) and nitrogen sorption/desorption. The results indicate that the core-shell nanowires have highly ordered periodic mesoporous silica shell (space group p6mm), high BET sur-face area and narrow pore size distribution. Moreover, the morphology of core-shell nanowires can be controlled by the pH value. The core-shell nanowires have promising applications in biosensors, nanoprobes and energy storage due to their good dispersibility in polar solvents.

  19. Organic-inorganic hybrid mesoporous polymers fabricated by using (CTA)2S2O8 as self-decomposed soft templates.

    Science.gov (United States)

    Chen, Tianyou; Du, Binyang; Fan, Zhiqiang

    2012-10-23

    Organic-inorganic hybrid mesoporous polymers were successfully synthesized by using a template-directed free radical polymerization technique in aqueous solution at 0-5 °C with oxidative complexes as self-decomposed soft templates. The oxidative complexes ((CTA)(2)S(2)O(8)), which were formed between anionic oxidant (S(2)O(8)(2-)) and cationic surfactant (cetyltrimethylammonium bromide, CTAB) at 0-5 °C, can be automatically decomposed due to the reduction of S(2)O(8)(2-). No additional treatment was needed to remove the templates. The reactive functional monomer, 3-(trimethoxysilyl)propyl methacrylate (TMSPMA), was used as main monomer. Styrene was used as the comonomer. With simultaneous free radical copolymerization of TMSPMA and styrene, condensation of methoxysilyl groups, and the self-decomposition of (CTA)(2)S(2)O(8), organic-inorganic hybrid mesoporous polymers were successfully obtained. The mesoporous structures and morphologies of the resultant hybrid mesoporous polymers were found to be strongly dependent on the feed amounts of TMSPMA and styrene. In the absence of styrene, the hybrid polymer PTMSPMA exhibited mesh-like bicontinuous structures with mesopores and high surface area (335 m(2)/g). With the incorporation of styrene, mesoporous nanoparticles were obtained. The surface areas of the mesoporous nanoparticles decreased with the increase of styrene contents. The adsorption capabilities of such mesoporous polymers for organic dye (Congo red) and protein (bovine serum albumin) were also studied.

  20. Synthesis of Mesoporous Titania with Surfactant and its Characterization

    Directory of Open Access Journals (Sweden)

    T. Benkacem

    2008-01-01

    Full Text Available A mesoporous titania was obtained by gelation from Ti-alkoxide in acidic solutions with addition of surfactant cetyltrimetylammonium bromide (CH3(CH215N(CH33Br using a sol-gel process. The effects of surfactant concentration on synthesis of mesoporous titania were studied. The structural characterisation was studied by differential thermal analysis, infrared spectroscopy, X-ray diffraction. Studies by X-ray diffraction showed that crystallisation of TiO2 powder occurs at 200°C, above 200°C we obtained a mixture of two forms-Anatase and rutile. The textural characterisation by nitrogen adsorption-desorption allowed us to observe the variation of the surface area, porous volume and pore diameters according to temperature and [CTAB]/[Ti-alkoxide] molar ratio. The analysis of the results shows that addition of surfactant residue increases considerably its pore diameters. The deposit thin layers has been realized with a sol prepared with the destabilization of colloidal solutions process. Scanning electron-spectroscopy observation for thermally treated (at 400 and 600°C samples, showed homogeneous layers without cracking.

  1. Improved Performance of Lipase Immobilized on Tannic Acid-Templated Mesoporous Silica Nanoparticles.

    Science.gov (United States)

    Jiang, Yanjun; Sun, Wenya; Zhou, Liya; Ma, Li; He, Ying; Gao, Jing

    2016-08-01

    Mesoporous silica nanoparticles were synthesized by using tannic acid as a pore-forming agent, which is an environmentally friendly, cheap, and non-surfactant template. SEM and TEM images indicated that the tannic acid-templated mesoporous silica nanoparticles (TA-MSNs) are monodisperse spherical-like particles with an average diameter of 195 ± 16 nm. The Brunauer-Emmett-Teller (BET) results showed that the TA-MSNs had a relatively high surface area (447 m(2)/g) and large pore volume (0.91 cm(3)/g), and the mean pore size was ca. 10.1 nm. Burkholderia cepacia lipase was immobilized on the TA-MSNs by physical adsorption for the first time, and the properties of immobilized lipase (BCL@TA-MSNs) were investigated. The BCL@TA-MSNs exhibited satisfactory thermal stability; strong tolerance to organic solvents such as methanol, ethanol, isooctane, n-hexane, and tetrahydrofuran; and high operational reusability when BCL@TA-MSNs were applied in esterification and transesterification reactions. After recycling 15 times in the transesterification reaction for biodiesel production, over 85 % of biodiesel yield can be maintained. With these desired characteristics, the TA-MSNs may provide excellent candidates for enzyme immobilization.

  2. Assistant template and co-template agents in modeling mesoporous silicas and post-synthesizing organofunctionalizations

    Science.gov (United States)

    Oliveira, Vaeudo V.; Airoldi, Claudio

    2012-12-01

    Mesoporous SBA-16 silicas were synthesized through a direct methodology using the template (F127) combined with co-templates (ethanol and n-butanol), with tetraethylorthosilicate as the silica source. These ordered mesoporous silica were characterized by elemental analyses, infrared spectroscopy, solid-state nuclear magnetic resonance for 13C (CP/MAS) and 29Si (HP/DEC) nuclei, nitrogen sorption/desorption processes, small angle X-ray analyses (SAXS) and transmission electron microscopy (TEM). SAXS and TEM results confirmed the space group Im3m and cubic 3D symmetry, typical for highly ordered SBA-16. The sorption/desorption data for SBA-16 and when functionalized gave type IV isotherms, with hysteresis loop H2. Surface areas of 836; 657 and 618 m2 g-1 and average pore diameters of 7.99; 8.10 and 9.85 nm, for SBA-16A, SBA-16B and SBA-16C were obtained, respectively. When functionalized the silicas presented a reduction in surface area, pore volume and pore diameter due to the pendant chains that interfere with nitrogen sorption in these measurements. The co-template ethanol favors the ordered mesopores with highest wall thicknesses.

  3. Soft-Template-Synthesized Mesoporous Carbon for Oral Drug Delivery

    Energy Technology Data Exchange (ETDEWEB)

    Saha, Dipendu [ORNL; Warren, Kaitlyn E [ORNL; Naskar, Amit K [ORNL

    2014-01-01

    Template-synthesized mesoporous carbons were successfully used in in vitro investigations of controlled delivery of three model drugs, captopril, furosemide, and ranitidine hydrochloride. Captopril and furosemide exhibited desorption kinetics over 30 40 h, and ranitidine HCl had a complete release time of 5 10 h. As evident from the slow release kinetics, we contend that our mesoporous carbon is an improved drug-delivery medium compared to state-of-the-art porous silica-based substrates. The mesoporous carbons, synthesized from phloroglucinol and lignin, a synthetic and a sustainable precursor, respectively, exhibit BET surface area of 200 400 m2 g-1 and pore volume of 0.2 0.6 cm3 g-1. The phloroglucinol-based carbon has narrower pore widths and higher pore volume than the lignin-derived counterpart and maintains a longer release time. Numerical modeling of the release kinetics data reveals that the diffusivities of all the drugs from lignin-based carbon media are of equivalent magnitude (10-22 to 10-24 m2 s-1). However, a tailored reduction of pore width in the sorbent reduces the diffusivity of smaller drug molecules (captopril) by an order of magnitude. Thus, engineered pore morphology in our synthesized carbon sorbent, along with its potential to tailor the chemistry of its interaction with sorbet, can be exploited for optimal delivery system of a preferred drug within its therapeutic level and below the level of toxicity.

  4. Organic materials as templates for the formation of mesoporous inorganic materials and ordered inorganic nanocomposites

    Science.gov (United States)

    Ziegler, Christopher R.

    Hierarchically structured inorganic materials are everywhere in nature. From unicellular aquatic algae such as diatoms to the bones and/or cartilage that comprise the skeletal systems of vertebrates. Complex mechanisms involving site-specific chemistries and precision kinetics are responsible for the formation of such structures. In the synthetic realm, reproduction of even the most basic hierarchical structure effortlessly produced in nature is difficult. However, through the utilization of self-assembling structures or "templates", such as polymers or amphiphilic surfactants, combined with some favorable interaction between a chosen inorganic, the potential exists to imprint an inorganic material with a morphology dictated via synthetic molecular self-assembly. In doing so, a very basic hierarchical structure is formed on the angstrom and nanometer scales. The work presented herein utilizes the self-assembly of either surfactants or block copolymers with the desired inorganic or inorganic precursor to form templated inorganic structures. Specifically, mesoporous silica spheres and copolymer directed calcium phosphate-polymer composites were formed through the co-assembly of an organic template and a precursor to form the desired mesostructured inorganic. For the case of the mesoporous silica spheres, a silica precursor was mixed with cetyltrimethylammonium bromide and cysteamine, a highly effective biomimetic catalyst for the conversion of alkoxysilanes to silica. Through charge-based interactions between anionic silica species and the micelle-forming cationic surfactant, ordered silica structures resulted. The incorporation of a novel, effective catalyst was found to form highly condensed silica spheres for potential application as catalyst supports or an encapsulation media. Ordered calcium phosphate-polymer composites were formed using two routes. Both routes take advantage of hydrogen bonding and ionic interactions between the calcium and phosphate precursors

  5. PEG-templated mesoporous silica nanoparticles exclusively target cancer cells

    Science.gov (United States)

    Morelli, Catia; Maris, Pamela; Sisci, Diego; Perrotta, Enrico; Brunelli, Elvira; Perrotta, Ida; Panno, Maria Luisa; Tagarelli, Antonio; Versace, Carlo; Casula, Maria Francesca; Testa, Flaviano; Andò, Sebastiano; Nagy, Janos B.; Pasqua, Luigi

    2011-08-01

    Mesoporous silica nanoparticles (MSNs) have been proposed as DNA and drug delivery carriers, as well as efficient tools for fluorescent cell tracking. The major limitation is that MSNs enter cells regardless of a target-specific functionalization. Here we show that non functionalized MSNs, synthesized using a PEG surfactant-based interfacial synthesis procedure, do not enter cells, while a highly specific, receptor mediated, cellular internalization of folic acid (FOL) grafted MSNs (MSN-FOL), occurs exclusively in folate receptor (FR) expressing cells. Neither the classical clathrin pathway nor macropinocytosis is involved in the MSN endocytic process, while fluorescent MSNs (MSN-FITC) enter cells through aspecific, caveolae-mediated, endocytosis. Moreover, internalized particles seem to be mostly exocytosed from cells within 96 h. Finally, cisplatin (Cp) loaded MSN-FOL were tested on cancerous FR-positive (HeLa) or normal FR-negative (HEK293) cells. A strong growth arrest was observed only in HeLa cells treated with MSN-FOL-Cp. The results presented here show that our mesoporous nanoparticles do not enter cells unless opportunely functionalized, suggesting that they could represent a promising vehicle for drug targeting applications.Mesoporous silica nanoparticles (MSNs) have been proposed as DNA and drug delivery carriers, as well as efficient tools for fluorescent cell tracking. The major limitation is that MSNs enter cells regardless of a target-specific functionalization. Here we show that non functionalized MSNs, synthesized using a PEG surfactant-based interfacial synthesis procedure, do not enter cells, while a highly specific, receptor mediated, cellular internalization of folic acid (FOL) grafted MSNs (MSN-FOL), occurs exclusively in folate receptor (FR) expressing cells. Neither the classical clathrin pathway nor macropinocytosis is involved in the MSN endocytic process, while fluorescent MSNs (MSN-FITC) enter cells through aspecific, caveolae

  6. One-pot template-free preparation of mesoporous TiO{sub 2} hollow spheres and their photocatalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Kang, Shizhao; Yin, Dieer; Li, Xiangqing; Li, Liang [School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418 (China); Mu, Jin, E-mail: mujin@sit.edu.cn [School of Chemical and Environmental Engineering, Shanghai Institute of Technology, 100 Haiquan Road, Shanghai 201418 (China)

    2012-11-15

    Highlights: ► Mesoporous TiO{sub 2} hollow spheres were prepared in a one-pot process. ► The process does not involve any templates and surfactants. ► The TiO{sub 2} hollow spheres display high photocatalytic activity. -- Abstract: Mesoporous TiO{sub 2} hollow spheres were prepared in a solvothermal process, which did not involve any templates and surfactants. Meanwhile, the photocatalytic activity of TiO{sub 2} hollow spheres was studied using methyl orange as a probe. The results indicate that the anatase TiO{sub 2} hollow spheres with mesoporous walls and high specific surface area (141 m{sup 2} g{sup −1}) can be obtained using this simple method. The mean diameter and wall thickness of spheres are about 700 nm and 90 nm, respectively. Moreover, the as-prepared TiO{sub 2} hollow spheres display high photocatalytic activity with 98% of degradation ratio of methyl orange after 30 min irradiation.

  7. Synthesis of mesoporous carbon as electrode material for supercapacitor by modified template method

    Institute of Scientific and Technical Information of China (English)

    ZHAO Jia-chang; LAI Chun-yan; DAI Yang; XIE Jing-ying

    2005-01-01

    The pore structures and electrochemical performances of mesoporous carbons prepared by silica sol template method as electrode material for supercapacitor were investigated. The mean pore size and mass specific capacitance of the mesoporous carbons increase with the increase of mass ratio of silica sol to carbon source (glucose). A modified template method, combining silica sol template method and ZnCl2 chemical activation method, was proposed to improve the mass specific capacitance of the mesoporous carbon with an improved BET surface area. The correlation of rate capability and pore structure was studied by constant current discharge and electrochemical impedance spectroscopy. A commercially available microporous carbon was used for comparison. The result shows that mesoporous carbon with a larger pore size displays a higher rate capability. Mesoporous carbon synthesized by modified template method has both high mass specific capacitance and good rate capability.

  8. Mesoporous sol-gel WO{sub 3} thin films via poly(styrene-co-allyl-alcohol) copolymer templates

    Energy Technology Data Exchange (ETDEWEB)

    Ozkan Zayim, Esra [Department of Physics, Faculty of Science and Letters, Istanbul Technical University, Maslak, Istanbul 80626 (Turkey); Liu, Ping; Lee, Se-Hee; Tracy, C. Edwin; Pitts, J. Roland; Deb, Satyen K. [National Renewable Energy Laboratory, Golden, CO 80401 (United States); Turner, John A.

    2003-12-01

    In this study a copolymer poly(styrene-co-allyl-alcohol), [-CH{sub 2}CH(C{sub 6}H{sub 5})-]{sub x}[-CH{sub 2}CH-(CH{sub 2}OH)-]{sub y} has been employed as a novel template in a sol-gel synthesis process to direct the formation of mesoporous tungsten oxide. The copolymer, due to its rigid hydrophobic block of polystyrene, is a more effective surfactant in an alcohol solution than polypropylene oxide-polyethylene oxide based compounds. The films have been prepared by a spin-coating technique from an ethanol solution of tungsten hexachloride. At room temperature, ultraviolet illumination method has been found to be very suitable for removing the polymer template, leading to the formation of a high-quality mesoporous structure. The electrochromic and optical properties of the mesoporous films are described and compared to standard sol-gel tungsten oxide films. Mesoporous materials exhibit superior high-rate ion-insertion performance when used as electrochromic layers.

  9. SiO2@MgO nanoparticles templated mesoporous carbon with rich electro-active oxygenic functionalities and enhanced supercapacitive performances

    Science.gov (United States)

    Tian, Zhengfang; Duan, Shuyi; Shen, Yu; Xie, Mingjiang; Guo, Xuefeng

    2017-06-01

    As a member of carbon-based materials, ordered mesoporous carbon (OMC) still suffers from poor capacity for supercapacitive applications. Functionalization the skeleton with pseudocapacitive functionalities is an efficient way to enhance the capacity of OMCs. Herein, a designed SiO2@MgO nanoparticle with uniform diameters was employed as template towards the synthesis of pseudocapacitive oxygen functionalized OMC. The obtained carbons possess ordered mesoporous structure, large surface area, and rich pseudocapacitive oxygen species. As electrode for supercapacitor in 1.0 M H2SO4, the SiO2@MgO templated OMC achieves higher capacitance (257 F/g) than pure SiO2 templated OMC (180 F/g), surfactant templated OMC (152 F/g) and commercial activated carbon (110 F/g) owing to the high pseudocapacitive oxygen functionalities, providing more capacity by reversible Faradaic reaction.

  10. Preparation of Mesoporous Silica Templated Metal Nanowire Films on Foamed Nickel Substrates

    Energy Technology Data Exchange (ETDEWEB)

    Campbell, Roger [University of Alabama, Tuscaloosa; Kenik, Edward A [ORNL; Bakker, Martin [University of Alabama, Tuscaloosa; Havrilla, George [Los Alamos National Laboratory (LANL); Montoya, Velma [Los Alamos National Laboratory (LANL); Shamsuzzoha, Mohammed [University of Alabama, Tuscaloosa

    2006-01-01

    A method has been developed for the formation of high surface area nanowire films on planar and three-dimensional metal electrodes. These nanowire films are formed via electrodeposition into a mesoporous silica film. The mesoporous silica films are formed by a sol-gel process using Pluronic tri-block copolymers to template mesopore formation on both planar and three-dimensional metal electrodes. Surface area increases of up to 120-fold have been observed in electrodes containing a templated film when compared to the same types of electrodes without the templated film.

  11. Templated assembly of BiFeO₃ nanocrystals into 3D mesoporous networks for catalytic applications.

    Science.gov (United States)

    Papadas, I T; Subrahmanyam, K S; Kanatzidis, M G; Armatas, G S

    2015-03-19

    The self-assembly of uniform nanocrystals into large porous architectures is currently of immense interest for nanochemistry and nanotechnology. These materials combine the respective advantages of discrete nanoparticles and mesoporous structures. In this article, we demonstrate a facile nanoparticle templating process to synthesize a three-dimensional mesoporous BiFeO₃ material. This approach involves the polymer-assisted aggregating assembly of 3-aminopropanoic acid-stabilized bismuth ferrite (BiFeO₃) nanocrystals followed by thermal decomposition of the surfactant. The resulting material consists of a network of tightly connected BiFeO₃ nanoparticles (∼6-7 nm in diameter) and has a moderately high surface area (62 m(2) g(-1)) and uniform pores (ca. 6.3 nm). As a result of the unique mesostructure, the porous assemblies of BiFeO₃ nanoparticles show an excellent catalytic activity and chemical stability for the reduction of p-nitrophenol to p-aminophenol with NaBH4.

  12. Biosynthesis of amorphous mesoporous aluminophosphates using yeast cells as templates

    Energy Technology Data Exchange (ETDEWEB)

    Sifontes, Ángela B., E-mail: asifonte@ivic.gob.ve [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); González, Gema [Centro de Ingeniería de Materiales y Nanotecnología, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Tovar, Leidy M.; Méndez, Franklin J. [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Gomes, Maria E. [Centro de Ingeniería de Materiales y Nanotecnología, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Cañizales, Edgar [Área de Análisis Químico Inorgánico, PDVSA, INTEVEP, Los Teques 1070-A (Venezuela, Bolivarian Republic of); Niño-Vega, Gustavo; Villalobos, Hector [Centro de Microbiología y Biología Celular, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Brito, Joaquin L. [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of)

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Amorphous aluminophosphates can take place using yeast as template. ► A mesoporous material was obtained. ► The specific surface area after calcinations ranged between 176 and 214 m{sup 2} g{sup −1}. -- Abstract: In this study aluminophosphates have been synthesized from aluminum isopropoxide and phosphoric acid solutions using yeast cells as template. The physicochemical characterization was carried out by thermogravimetric analysis; X-ray diffraction; Fourier transform infrared; N{sub 2} adsorption–desorption isotherms; scanning electron microscopy; transmission electron microscopy and potentiometric titration with N-butylamine for determination of: thermal stability; crystalline structure; textural properties; morphology and surface acidity, respectively. The calcined powders consisted of an intimate mixture of amorphous and crystallized AlPO particles with sizes between 23 and 30 nm. The average pore size observed is 13–16 nm and the specific surface area after calcinations (at 650 °C) ranged between 176 and 214 m{sup 2} g{sup −1}.

  13. Chelating-Template-Assisted in Situ Encapsulation of Zinc Ferrite Inside Silica Mesopores for Enhanced Gas-Sensing Characteristics.

    Science.gov (United States)

    Niu, Kui; Liang, Liman; Peng, Fei; Zhang, Fan; Gu, Yao; Tian, Hongyan

    2016-09-21

    A facile in situ approach has been designed to synthesize zinc ferrite/mesoporous silica guest-host composites. Chelating surfactant, N-hexadecyl ethylenediamine triacetic acid, was employed as structure-directing agent to fabricate mesoporous silica skeleton and simultaneously as complexing agent to incorporate stoichiometric amounts of zinc and iron ions into silica cavities. On this basis, spinel zinc ferrite nanoparticles with grain sizes less than 3 nm were encapsulated in mesoporous channels after calcination. The silica mesostructure, meanwhile, displayed a successive transformation from hexagonal p6mm through bicontinuous cubic Ia3̅d to lamellar phase with increasing the dopant concentration in the initial template solution. In comparison with zinc ferrite nanopowder prepared without silica host, the composite with bicontinuous architecture exhibited higher sensitivity, lower detection limit, lower optimum working temperature, quicker response, and shorter recovery time in sensing performance toward hydrogen sulfide. The significant improvements are from the high surface-to-volume ratio of the guest oxides and the three-dimensional porous structure of the composite. We believe the encapsulation route presented here may pave the way for directly introducing complex metal oxide into mesoporous silica matrix with tailorable mesophases for applications in sensing or other fields.

  14. Bimodal mesoporous titanium dioxide anatase films templated by a block polymer and an ionic liquid: influence of the porosity on the permeability.

    Science.gov (United States)

    Sallard, Sébastien; Schröder, Michael; Boissière, Cédric; Dunkel, Christian; Etienne, Mathieu; Walcarius, Alain; Oekermann, Torsten; Wark, Michael; Smarsly, Bernd M

    2013-12-21

    In the present paper, we report the synthesis of bimodal mesoporous anatase TiO2 films by the EISA (Evaporation-Induced Self-Assembly) method using sol-gel chemistry combining two porogen agents, a low molecular weight ionic template and a neutral block copolymer. The surfactant template (C16mimCl) generates non-oriented worm-like pores (8 to 10 nm) which connect the regularly packed ellipsoidal mesopores (15 to 20 nm diameter) formed by an amphiphilic block copolymer of the type poly(isobutylene)-b-poly(ethylene oxide) (PIB-PEO). The surfactant template can also significantly influence the size and packing of the ellipsoidal mesopores. The mesostructural organization and mesoporosity of the films are studied by Environmental Ellipsometry-Porosimetry (EEP), Grazing-Incidence Small-Angle X-ray Scattering (GISAXS) and electron microscopy techniques. Electrochemical characterization is performed to study the permeability of the films to liquid solutions, using two types of probe moieties (K3Fe(III)(CN)6 and Ru(bpy)3(2+)) by the wall-jet technique. An optimum ratio of C16mimCl/PIB-PEO provides anatase films with a continuous bimodal mesopore structure, possessing a permeability up to two times higher than that of the mesoporous films templated by PIB-PEO only (with partially isolated mesopores). When C16mimCl is used in large quantities, up to 20% weight vs. PIB-PEO, large overall porous volume and surface area are obtained, but the mesostructure is increasingly disrupted, leading to a severe loss of permeability of the bimodal films. A dye-sensitized solar cell set-up is used with anatase films as the photoelectrode. The photosensitizer loading and the total energy conversion efficiency of the solar cells using the mesoporous films templated by an optimal ratio of the two porogen agents C16mimCl and PIB-PEO can be substantially increased in comparison with the solar cells using mesoporous films templated by PIB-PEO only.

  15. Iron oxide nanoparticle layer templated by polydopamine spheres: a novel scaffold toward hollow-mesoporous magnetic nanoreactors.

    Science.gov (United States)

    Huang, Liang; Ao, Lijiao; Xie, Xiaobin; Gao, Guanhui; Foda, Mohamed F; Su, Wu

    2015-01-14

    Superparamagnetic iron oxide nanoparticle layers with high packing density and controlled thickness were in situ deposited on metal-affinity organic templates (polydopamine spheres), via one-pot thermal decomposition. The as synthesized hybrid structure served as a facile nano-scaffold toward hollow-mesoporous magnetic carriers, through surfactant-assisted silica encapsulation and its subsequent calcination. Confined but accessible gold nanoparticles were successfully incorporated into these carriers to form a recyclable catalyst, showing quick magnetic response and a large surface area (642.5 m(2) g(-1)). Current nano-reactors exhibit excellent catalytic performance and high stability in reduction of 4-nitrophenol, together with convenient magnetic separability and good reusability. The integration of compact iron oxide nanoparticle layers with programmable polydopamine templates paves the way to fabricate magnetic-response hollow structures, with high permeability and multi-functionality.

  16. Biomimetic Templating of Porous Lamellar Silicas by Vesicular Surfactant Assemblies

    Science.gov (United States)

    Tanev, Peter T.; Pinnavaia, Thomas J.

    1996-03-01

    A biomimetic templating approach to the synthesis of lamellar silicas is demonstrated. The procedure is based on the hydrolysis and cross-linking of a neutral silicon alkoxide precursor in the interlayered regions of multilamellar vesicles formed from a neutral diamine bola-amphiphile. Unlike earlier surfactant-templating approaches, this method produces porous lamellar silicas (designated MSU-V) with vesicular particle morphology, exceptional thermal stability, a high degree of framework cross-linking, unusually high specific surface area and pore volume, and sorption properties that are typical of pillared lamellar materials. This approach circumvents the need for a separate pillaring step in building porosity into a lamellar host structure and offers new opportunities for the direct fabrication of adsorbents, catalysts, and nanoscale devices.

  17. Iron oxide nanoparticle layer templated by polydopamine spheres: a novel scaffold toward hollow-mesoporous magnetic nanoreactors

    Science.gov (United States)

    Huang, Liang; Ao, Lijiao; Xie, Xiaobin; Gao, Guanhui; Foda, Mohamed F.; Su, Wu

    2014-12-01

    Superparamagnetic iron oxide nanoparticle layers with high packing density and controlled thickness were in situ deposited on metal-affinity organic templates (polydopamine spheres), via one-pot thermal decomposition. The as synthesized hybrid structure served as a facile nano-scaffold toward hollow-mesoporous magnetic carriers, through surfactant-assisted silica encapsulation and its subsequent calcination. Confined but accessible gold nanoparticles were successfully incorporated into these carriers to form a recyclable catalyst, showing quick magnetic response and a large surface area (642.5 m2 g-1). Current nano-reactors exhibit excellent catalytic performance and high stability in reduction of 4-nitrophenol, together with convenient magnetic separability and good reusability. The integration of compact iron oxide nanoparticle layers with programmable polydopamine templates paves the way to fabricate magnetic-response hollow structures, with high permeability and multi-functionality.Superparamagnetic iron oxide nanoparticle layers with high packing density and controlled thickness were in situ deposited on metal-affinity organic templates (polydopamine spheres), via one-pot thermal decomposition. The as synthesized hybrid structure served as a facile nano-scaffold toward hollow-mesoporous magnetic carriers, through surfactant-assisted silica encapsulation and its subsequent calcination. Confined but accessible gold nanoparticles were successfully incorporated into these carriers to form a recyclable catalyst, showing quick magnetic response and a large surface area (642.5 m2 g-1). Current nano-reactors exhibit excellent catalytic performance and high stability in reduction of 4-nitrophenol, together with convenient magnetic separability and good reusability. The integration of compact iron oxide nanoparticle layers with programmable polydopamine templates paves the way to fabricate magnetic-response hollow structures, with high permeability and multi

  18. Preparation of Hierarchical Mesoporous Silica Nanoparticles through a Single-Templating Approach

    Institute of Scientific and Technical Information of China (English)

    陈媛丽; 肖敏; 庄伟; 李艺; 李宝宗; 杨永刚

    2012-01-01

    Silicas with hierarchical porous architectures attracted much attention, due to their potential applications in catalysis and separation. Generally, they were prepared through dualor triple-templating approaches. Herein, mesoporous silica nanoparticles with rod-like pore channels inside and lamellar mesopores on the surfaces were prepared using the self-assemblies of a chiral low-molecular-weight amphiphile as templates through a single-templating approach. The formation of the lamellar mesopores was studied by taking field-emission scanning electron microscopy and transmission electron microscopy images after different reaction times. The lamellar pores were proposed to be formed by merging rod-like micelles during the sol-gel process. Moreover, helical nanofibers with rod-like pore channels inside and lamellar mesopores on the surfaces were prepared with the addition of n-octanol as a co-structure-directing agent.

  19. Preparation of Mesoporous Molecular Sieves Al-MSU-S Using Ionic Liquids as Template

    Institute of Scientific and Technical Information of China (English)

    YU Xin-Yu; LIU Cai-Hua; YANG Jian-Guo; WU Hai-Hong; WU Peng; HE Ming-Yuan

    2006-01-01

    Mesoporous molecular sieves Al-MSU-S has been prepared from the precursor of zeolite Y using ionic liquids l-hexadecane-3-methylimidazolium bromide (CMIMB) as a template in basic medium, which exhibited larger pore diameter, pore volume and surface area than that synthesized using cetyl trimethyl ammonium bromide (CTAB)template.

  20. A self-template strategy for the synthesis of mesoporous carbon nanofibers as advanced supercapacitor electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Li, Wei; Zhang, Fan; Dou, Yuqian; Wu, Zhangxiong; Liu, Haijing; Qian, Xufang; Gu, Dong; Xia, Yongyao; Tu, Bo; Zhao, Dongyuan [Department of Chemistry, Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials and Laboratory of Advanced Materials, Fudan University, Shanghai 200433 (China)

    2011-05-15

    Self-construction: A facile self-templating strategy is presented for the synthesis of mesoporous carbon nanofibers by using zinc glycolate fibers as the built-in template. The spectacular architectures show excellent performances as recommended electrode material for electrochemical capacitors. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  1. Enhancing the Porosity of Mesoporous Carbon-Templated ZSM-5 by Desilication

    DEFF Research Database (Denmark)

    Holm, Martin Spangsberg; Egeblad, Kresten; Vennestrøm, Peter Nicolai Ravnborg

    2008-01-01

    A tunable desilication protocol applied on a mesoporous ZSM-5 zeolite synthesized by carbon-templating is reported. The strategy enables a systematic manufacture of zeolite catalysts with moderate to very high mesoporosities. Coupling carbon-templating and desilication thus allow for more than...

  2. Template-mediated, Hierarchical Engineering of Ordered Mesoporous Films and Powders

    Science.gov (United States)

    Tian, Zheng

    Hierarchical control over pore size, pore topology, and meso/mictrostructure as well as material morphology (e.g., powders, monoliths, thin films) is crucial for meeting diverse materials needs among applications spanning next generation catalysts, sensors, batteries, sorbents, etc. The overarching goal of this thesis is to establish fundamental mechanistic insight enabling new strategies for realizing such hierarchical textural control for carbon materials that is not currently achievable with sacrificial pore formation by 'one-pot' surfactant-based 'soft'-templating or multi-step inorganic 'hard-templating. While 'hard'-templating is often tacitly discounted based upon its perceived complexity, it offers potential for overcoming key 'soft'-templating challenges, including bolstering pore stability, accommodating a more versatile palette of replica precursors, realizing ordered/spanning porosity in the case of porous thin films, simplifying formation of bi-continuous pore topologies, and inducing microstructure control within porous replica materials. In this thesis, we establish strategies for hard-templating of hierarchically porous and structured carbon powders and tunable thin films by both multi-step hard-templating and a new 'one-pot' template-replica precursor co-assembly process. We first develop a nominal hard-templating technique to successfully prepare three-dimensionally ordered mesoporous (3DOm) and 3DOm-supported microporous carbon thin films by exploiting our ability to synthesize and assemble size-tunable silica nanoparticles into scalable, colloidal crystalline thin film templates of tunable mono- to multi-layer thickness. This robust thin film template accommodates liquid and/or vapor-phase infiltration, polymerization, and pyrolysis of various carbon sources without pore contraction and/or collapse upon template sacrifice. The result is robust, flexible 3DOm or 3DOm-supported ultra-thin microporous films that can be transferred by stamp

  3. Enhancing pseudocapacitive charge storage in polymer templated mesoporous materials.

    Science.gov (United States)

    Rauda, Iris E; Augustyn, Veronica; Dunn, Bruce; Tolbert, Sarah H

    2013-05-21

    Growing global energy demands coupled with environmental concerns have increased the need for renewable energy sources. For intermittent renewable sources like solar and wind to become available on demand will require the use of energy storage devices. Batteries and supercapacitors, also known as electrochemical capacitors (ECs), represent the most widely used energy storage devices. Supercapacitors are frequently overlooked as an energy storage technology, however, despite the fact that these devices provide greater power, much faster response times, and longer cycle life than batteries. Their limitation is that the energy density of ECs is significantly lower than that of batteries, and this has limited their potential applications. This Account reviews our recent work on improving pseudocapacitive energy storage performance by tailoring the electrode architecture. We report our studies of mesoporous transition metal oxide architectures that store charge through surface or near-surface redox reactions, a phenomenon termed pseudocapacitance. The faradaic nature of pseudocapacitance leads to significant increases in energy density and thus represents an exciting future direction for ECs. We show that both the choice of material and electrode architecture is important for producing the ideal pseudocapacitor device. Here we first briefly review the current state of electrode architectures for pseudocapacitors, from slurry electrodes to carbon/metal oxide composites. We then describe the synthesis of mesoporous films made with amphiphilic diblock copolymer templating agents, specifically those optimized for pseudocapacitive charge storage. These include films synthesized from nanoparticle building blocks and films made from traditional battery materials. In the case of more traditional battery materials, we focus on using flexible architectures to minimize the strain associated with lithium intercalation, that is, the accumulation of lithium ions or atoms between the

  4. Mesoporous silica-magnetite nanocomposite synthesized by using a neutral surfactant.

    Science.gov (United States)

    Souza, K C; Salazar-Alvarez, G; Ardisson, J D; Macedo, W A A; Sousa, E M B

    2008-05-07

    Magnetite nanoparticles coated by mesoporous silica were synthesized by an alternative chemical route using a neutral surfactant and without the application of any functionalization method. The magnetite (Fe(3)O(4)) nanoparticles were prepared by precipitation from aqueous media, and then coated with mesoporous silica by using nonionic block copolymer surfactants as the structure-directing agents. The mesoporous SiO(2)-coated Fe(3)O(4) samples were characterized by x-ray diffraction, Fourier-transform infrared spectroscopy, N(2) adsorption-desorption isotherms, transmission electron microscopy, (57)Fe Mössbauer spectroscopy, and vibrating sample magnetometry. Our results revealed that the magnetite nanoparticles are completely coated by well-ordered mesoporous silica with free pores and stable (∼8 nm thick) pore walls, and that the structural and magnetic properties of the Fe(3)O(4) nanoparticles are preserved in the applied synthesis route.

  5. Mesoporous silica-magnetite nanocomposite synthesized by using a neutral surfactant

    Energy Technology Data Exchange (ETDEWEB)

    Souza, K C; Sousa, E M B [Laboratorio de Biomateriais, Centro de Desenvolvimento da Tecnologia Nuclear, 30123-970 Belo Horizonte, MG (Brazil); Salazar-Alvarez, G [Institut Catala de Nanotecnologia (ICN), Edifici CM7, Campus Universitat Autonoma de Barcelona, E-08193 Bellaterra (Barcelona) (Spain); Ardisson, J D; Macedo, W A A [Laboratorio de Fisica Aplicada, Centro de Desenvolvimento da Tecnologia Nuclear, 30123-970 Belo Horizonte, MG (Brazil)], E-mail: sousaem@cdtn.br

    2008-05-07

    Magnetite nanoparticles coated by mesoporous silica were synthesized by an alternative chemical route using a neutral surfactant and without the application of any functionalization method. The magnetite (Fe{sub 3}O{sub 4}) nanoparticles were prepared by precipitation from aqueous media, and then coated with mesoporous silica by using nonionic block copolymer surfactants as the structure-directing agents. The mesoporous SiO{sub 2}-coated Fe{sub 3}O{sub 4} samples were characterized by x-ray diffraction, Fourier-transform infrared spectroscopy, N{sub 2} adsorption-desorption isotherms, transmission electron microscopy, {sup 57}Fe Moessbauer spectroscopy, and vibrating sample magnetometry. Our results revealed that the magnetite nanoparticles are completely coated by well-ordered mesoporous silica with free pores and stable ({approx}8 nm thick) pore walls, and that the structural and magnetic properties of the Fe{sub 3}O{sub 4} nanoparticles are preserved in the applied synthesis route.

  6. Pore Structure Control of Ordered Mesoporous Silica Film Using Mixed Surfactants

    Directory of Open Access Journals (Sweden)

    Tae-Jung Ha

    2011-01-01

    Full Text Available Materials with nanosized and well-arranged pores have been researched actively in order to be applied to new technology fields. Especially, mesoporous material containing various pore structures is expected to have different pore structure. To form a mixed pore structure, ordered mesoporous silica films were prepared with a mixture of surfactant; Brij-76 and P-123 block copolymer. In mixed surfactant system, mixed pore structure was observed in the region of P-123/(Brij-76 + P-123 with about 50.0 wt.% while a single pore structure was observed in regions which have large difference in ratio between Brij-76 and P-123 through the X-ray diffraction analysis. Regardless of surfactant ratio, porosity was retained almost the same. It is expected that ordered mesoporous silica film with mixed pore structure can be one of the new materials which has distinctive properties.

  7. Vertically oriented hexagonal mesoporous zirconia thin films by block copolymer templating

    OpenAIRE

    Miko, Annamaria ; Demirel, A. Levent ; Somer, Mehmet

    2012-01-01

    We report the synthesis of vertically oriented, long-range ordered hexagonal mesoporous zirconia thin ?lms. The orientation of hexagonally ordered cylindrical mesopores in thin ?lms was effectively controlled by taking advantage of the temperature dependent hydrophobicity of the templating block copolymer PEO–PPO–PEO. Vertical orientation was obtained when temperature was 30 C or above throughout the process. Dehydration and enhanced chemical incompatibility between the PEO and PPO b...

  8. Synthesis, characterizations and photocatalytic studies of mesoporous titania prepared by using four plant skins as templates

    Energy Technology Data Exchange (ETDEWEB)

    Miao Yingchun [Department of Applied Chemistry, Key Laboratory of Medicinal Chemistry for Natural Resource, Ministry of Education, Yunnan University, Kunming 650091 (China); Faculty of Chemical and Life Sciences, Qujing Normal University, Qujing 655000 (China); Zhai Zhongbiao [Department of Applied Chemistry, Key Laboratory of Medicinal Chemistry for Natural Resource, Ministry of Education, Yunnan University, Kunming 650091 (China); Kunming Metallurgy Research Institute, Kunming 650031 (China); He Jiao; Li Bin; Li Junjie [Department of Applied Chemistry, Key Laboratory of Medicinal Chemistry for Natural Resource, Ministry of Education, Yunnan University, Kunming 650091 (China); Wang Jiaqiang, E-mail: jqwang@ynu.edu.cn [Department of Applied Chemistry, Key Laboratory of Medicinal Chemistry for Natural Resource, Ministry of Education, Yunnan University, Kunming 650091 (China)

    2010-07-20

    Anatase mesoporous titania with novel morphologies were synthesized by using the skins of tomatoes, bulb onions, grapes, and garlic bulbs, respectively, as templates and used for the photodegradation of Gentian violet, methyl violet, xylenol orange, and Rhodamine B under UV light. The samples were characterized by a combination of various physicochemical techniques, such as X-ray diffraction, SEM, HRTEM, N{sub 2} adsorption/desorption, diffuse reflectance UV-Vis, and FT-IR. It was found that all of the synthesized mesoporous titania samples exhibited similar morphologies to those of the original templates. The photoactivity of P25 TiO{sub 2} for the four dyes is nearly the same while the mesoporous titania samples synthesized by using the four skins as templates exhibited varied photoactivities for the four dyes.

  9. Effect of fat chain length of sorbitan surfactant on the porosity of mesoporous silica

    Directory of Open Access Journals (Sweden)

    Marco Antonio Utrera Martines

    2009-08-01

    Full Text Available The influence of the fat chain length of sorbitan surfactant was systematically explored, especially its influence on the material pore size. Then, mesoporous silica was synthesized according to a two-step process that provides intermediary stable hybrid micelles using ethoxylated derivative of fatty esters of sorbitan surfactants as the directing-structure agent and tetraethyl orthosilicate Si(OEt4 as the silica source. Finally, the materials’ porosity could be controlled by adjusting the preparation parameters during the two steps synthesis of mesoporous silica.

  10. Self-Templated Synthesis of Mesoporous Carbon from Carbon Tetrachloride Precursor for Supercapacitor Electrodes.

    Science.gov (United States)

    Tang, Duihai; Hu, Shi; Dai, Fang; Yi, Ran; Gordin, Mikhail L; Chen, Shuru; Song, Jiangxuan; Wang, Donghai

    2016-03-23

    A high-surface-area mesoporous carbon material has been synthesized using a self-templating approach via reduction of carbon tetrachloride by sodium potassium alloy. The advantage is the reduction-generated salt templates can be easily removed with just water. The produced mesoporous carbon has a high surface area and a narrow pore size distribution. When used as a supercapacitor electrode, this material exhibits a high specific capacitance (259 F g(-1)) and excellent cycling performance (>92% capacitance retention for 6000 cycles).

  11. Surfactant-directed synthesis of mesoporous films made single-step by a tandem photosol-gel/photocalcination route

    Directory of Open Access Journals (Sweden)

    Héloïse De Paz-Simon

    2014-11-01

    Full Text Available In view of their technological impact in materials chemistry, a simplified and more efficient synthetic route to mesoporous films is highly sought. We report, herein, a smart UV-mediated approach coupling in a one-stage process sol-gel photopolymerization and photoinduced template decomposition/ablation to making mesoporous silica films. Performed at room temperature with a solvent-free solution of silicate precursor and amphiphilic poly(ethylene oxide-poly(propylene oxide-poly(ethylene oxide block copolymer, the synthesis relies on photoacid generation to induce the fast formation (≈10 min of mesostructured silica/surfactant domains. Continuation of UV exposure for three additional hours enables subsequent and complete photodegradation of the polyether copolymer, resulting in ordered or disordered mesoporous silica film. One of the most attractive features is that the one-step procedure relies on a continuous illumination provided by the same conventional medium-pressure Hg-Xe arc lamp equipped with a 254 nm reflector to enhance the emission of energetic photons <300 nm. In addition to X-ray diffraction and transmission electron microscopy, time-resolved Fourier transform infrared spectroscopy has proved to be a powerful in situ technique to probe the different chemical transformations accompanying irradiation. Photocalcination strengthens the inorganic network, while allowing to preserve a higher fraction of residual silanol groups compared with thermal calcination. A polyether chain degradation mechanism based on oxygen reactive species-mediated photo-oxidation is proposed.

  12. Templated assembly of BiFeO3 nanocrystals into 3D mesoporous networks for catalytic applications

    Science.gov (United States)

    Papadas, I. T.; Subrahmanyam, K. S.; Kanatzidis, M. G.; Armatas, G. S.

    2015-03-01

    The self-assembly of uniform nanocrystals into large porous architectures is currently of immense interest for nanochemistry and nanotechnology. These materials combine the respective advantages of discrete nanoparticles and mesoporous structures. In this article, we demonstrate a facile nanoparticle templating process to synthesize a three-dimensional mesoporous BiFeO3 material. This approach involves the polymer-assisted aggregating assembly of 3-aminopropanoic acid-stabilized bismuth ferrite (BiFeO3) nanocrystals followed by thermal decomposition of the surfactant. The resulting material consists of a network of tightly connected BiFeO3 nanoparticles (~6-7 nm in diameter) and has a moderately high surface area (62 m2 g-1) and uniform pores (ca. 6.3 nm). As a result of the unique mesostructure, the porous assemblies of BiFeO3 nanoparticles show an excellent catalytic activity and chemical stability for the reduction of p-nitrophenol to p-aminophenol with NaBH4.The self-assembly of uniform nanocrystals into large porous architectures is currently of immense interest for nanochemistry and nanotechnology. These materials combine the respective advantages of discrete nanoparticles and mesoporous structures. In this article, we demonstrate a facile nanoparticle templating process to synthesize a three-dimensional mesoporous BiFeO3 material. This approach involves the polymer-assisted aggregating assembly of 3-aminopropanoic acid-stabilized bismuth ferrite (BiFeO3) nanocrystals followed by thermal decomposition of the surfactant. The resulting material consists of a network of tightly connected BiFeO3 nanoparticles (~6-7 nm in diameter) and has a moderately high surface area (62 m2 g-1) and uniform pores (ca. 6.3 nm). As a result of the unique mesostructure, the porous assemblies of BiFeO3 nanoparticles show an excellent catalytic activity and chemical stability for the reduction of p-nitrophenol to p-aminophenol with NaBH4. Electronic supplementary information (ESI

  13. Selective adsorption of nonionic surfactant on hexagonal mesoporous silicates (HMSs) in the presence of ionic dyes.

    Science.gov (United States)

    Punyapalakul, Patiparn; Takizawa, Satoshi

    2006-10-01

    Selective adsorption of alkylphenol polyethoxylates (APnEOs) from synthetic textile wastewater was investigated using hexagonal mesoporous silicates (HMSs). HMSs are synthetic silicate that have uniform mesopores, large surface areas and uniform surface functional groups. Five different types of HMSs were synthesized by surfactant-templating methods, and three of them were grafted with organic surface functional groups, i.e., n-octyldimethyl-, 3-aminopropyltriethoxy-, and 3-mercaptopropyl-groups. Titanium-substituted HMS was also made in the same way as HMS. Adsorption capacities and selectivities of these HMSs for APnEOs were investigated in batch adsorption experiments either in single-solute APnEO solutions or in mixed solutions with ionic dyes. Triton X-100 was used as a model APnEO and either Basic Yellow 1 or Acid Blue 45 was used as cationic or anionic dyes, respectively. All the HMSs except 3-aminopropyltriethoxy-grafted HMS had higher adsorption capacities of Triton X-100 than powdered activated carbon. HMS and Ti-HMS had the highest BET surface areas and mesopore volumes measured by the nitrogen adsorption method, and thereby the highest adsorption capacities for Triton X-100. Surface charge was the most important attractive force between HMSs and dyes. FT-IR spectra proved that hydrophilic HMSs adsorbed both Basic Yellow 1 and Acid Blue 45 by hydrogen bonding. Acid-base titration experiments revealed that all the HMSs except 3-aminopropyltriethoxy-grafted HMS were negatively charged at neutral pH, whereas PAC and 3-aminopropyltriethoxy-grafted HMS were positively charged. Due to negative surface charge, the anionic dye (Acid Blue 45) was not adsorbed on the four HMSs, which proves high selectivities of these HMSs for Triton X-100 over Acid Blue 45. On the contrary, a small amount of cationic dye (Basic Yellow 1) was adsorbed on all HMSs, but 3-aminopropyltriethoxy-grafted HMS showed the lowest adsorption capacity for Basic Yellow 1 due to positive

  14. A novel, efficient and facile method for the template removal from mesoporous materials

    KAUST Repository

    Chen, Lu

    2014-11-12

    © 2014, Jilin University, The Editorial Department of Chemical Research in Chinese Universities and Springer-Verlag GmbH. A new catalytic-oxidation method was adopted to remove the templates from SBA-15 and MCM-41 mesoporous materials via Fenton-like techniques under microwave irradiation. The mesoporous silica materials were treated with different Fenton agents based on the template’s property and textural property. The samples were characterized by powder X-ray diffraction(XRD) measurement, N2 adsorption-desorption isotherms, infrared spectroscopy, 29Si MAS NMR and thermo gravimetric analysis(TGA). The results reveal that this is an efficient and facile approach to the thorough template-removal from mesoporous silica materials, as well as to offering products with more stable structures, higher BET surface areas, larger pore volumes and larger quantity of silanol groups.

  15. Bio-templated synthesis of highly ordered macro-mesoporous silica material for sustained drug delivery

    Science.gov (United States)

    Qu, Fengyu; Lin, Huiming; Wu, Xiang; Li, Xiaofeng; Qiu, Shilun; Zhu, Guangshan

    2010-05-01

    The bimodal porous structured silica materials consisting of macropores with the diameter of 5-20 μm and framework-like mesopores with the diameter of 4.7-6.0 nm were prepared using natural Manchurian ash and mango linin as macropored hard templates and P123 as mesopore soft templates, respectively. The macroporous structures of Manchurian ash and mango linin were replicated with the walls containing highly ordered mesoporous silica as well. As-synthesized dual porous silica was characterized by scanning electron microscope (SEM), powder X-ray diffraction (XRD), transmission electron microscope (TEM) and nitrogen adsorption/desorption, fourier transform IR (FTIR) spectroscopy, and thermo-gravimetric analyzer (TGA). Ibuprofen (Ibu) was employed as a model drug and the release profiles showed that the dual porous material had a sustained drug delivery capability. And such highly ordered dual pore silica materials may have potential applications for bimolecular adsorption/separation and tissue repairing.

  16. Mesoporous carbon prepared from carbohydrate as hard template for hierarchical zeolites

    DEFF Research Database (Denmark)

    Egeblad, Kresten; Christensen, Claus H.

    2007-01-01

    treatment of a mixture of sucrose and ammonia followed by carbonization of the mixture in N-2 at high temperatures. The porous carbon produced by this method was subsequently applied as a hard template in the synthesis of mesoporous silicalite-1 and removed by combustion after synthesis. X-ray diffraction...

  17. Soft-templated synthesis of mesoporous carbon nanospheres and hollow carbon nanofibers

    Science.gov (United States)

    Cheng, Youliang; Li, Tiehu; Fang, Changqing; Zhang, Maorong; Liu, Xiaolong; Yu, Ruien; Hu, Jingbo

    2013-10-01

    Using coal tar pitch based amphiphilic carbonaceous materials (ACMs) as the precursor and amphiphilic triblock copolymer Plutonic P123 as the only soft template, carbon nanospheres with partially ordered mesopores and hollow carbon nanofibers were synthesized. The concentration of P123, cp, and the mass ratio of P123 to ACM, r, are the key parameters of controlling the shape of the as-prepared products. Mesoporous carbon nanospheres with diameter of 30-150 nm were prepared under the condition of cp = 13.3 g/L and r = 1.2. When cp = 26.7 g/L and r = 2, hollow carbon nanofibers with diameters of 50-200 nm and mesopores/macropores were obtained. Carbon nanospheres and hollow carbon fibers were amorphous materials. The mesoporous carbon nanospheres show good stability in the cyclic voltammograms and their specific capacitance at 10 mV s-1 is 172.1 F/g.

  18. Large-scale template-free synthesis of ordered mesoporous platinum nanocubes and their electrocatalytic properties

    Science.gov (United States)

    Cao, Yanqin; Yang, Yong; Shan, Yufeng; Fu, Chaoli; Viet Long, Nguyen; Huang, Zhengren; Guo, Xiangxin; Nogami, Masayuki

    2015-11-01

    Here we report a facile, one-pot and template-free approach to synthesize mesoporous monocrystalline Pt nanocubes with uniform shapes and sizes, in which small Pt particles with a size of ~5 nm are three-dimensionally and periodically built up into cubes with a size of ~50 nm. The forming process is illustrated through a novel meso-crystal self-assembly mechanism. Very interestingly, the mesoporous structures are ordered, which are thought to be beneficial to increase their catalytic activity. Compared with nonporous Pt nanoparticles and porous Pt nanoparticles without order, the ordered mesoporous Pt nanocubes exhibit a highly improved electrocatalytic ability for methanol and formic acid oxidation, and are potentially applicable as electrocatalysts for direct methanol and formic acid fuel cells. Furthermore, this approach can be used to synthesize other Pt-series metallic mesoporous nanoparticles, such as Pd.Here we report a facile, one-pot and template-free approach to synthesize mesoporous monocrystalline Pt nanocubes with uniform shapes and sizes, in which small Pt particles with a size of ~5 nm are three-dimensionally and periodically built up into cubes with a size of ~50 nm. The forming process is illustrated through a novel meso-crystal self-assembly mechanism. Very interestingly, the mesoporous structures are ordered, which are thought to be beneficial to increase their catalytic activity. Compared with nonporous Pt nanoparticles and porous Pt nanoparticles without order, the ordered mesoporous Pt nanocubes exhibit a highly improved electrocatalytic ability for methanol and formic acid oxidation, and are potentially applicable as electrocatalysts for direct methanol and formic acid fuel cells. Furthermore, this approach can be used to synthesize other Pt-series metallic mesoporous nanoparticles, such as Pd. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr05772h

  19. Tunable hierarchical macro/mesoporous gold microwires fabricated by dual-templating and dealloying processes.

    Science.gov (United States)

    Sattayasamitsathit, Sirilak; Gu, Yonge; Kaufmann, Kevin; Minteer, Shelley; Polsky, Ronen; Wang, Joseph

    2013-09-07

    Tailor-made highly ordered macro/mesoporous hierarchical metal architectures have been created by combining sphere lithography, membrane template electrodeposition and alloy-etching processes. The new double-template preparation route involves the electrodeposition of Au/Ag alloy within the interstitial (void) spaces of polystyrene (PS) microspheres which are closely packed within the micropores of a polycarbonate membrane (PC), followed by dealloying of the Ag component and dissolution of the microsphere and membrane templates. The net results of combining such sphere lithography and silver etching is the creation of highly regular three-dimensional macro/mesoporous gold architecture with well-controlled sizes and shapes. The morphology and porosity of the new hierarchical porous structures can be tailored by controlling the preparation conditions, such as the composition of the metal mixture plating solution, the size of the microspheres template, or the dealloying time. Such tunable macro/mesoporous hierarchical structures offer control of the electrochemical reactivity and of the fuel mass transport, as illustrated for the enhanced oxygen reduction reaction (ORR) and hydrogen-peroxide detection. The new double templated electrodeposition method provides an attractive route for preparing highly controllable multiscale porous materials and diverse morphologies based on different materials and hence holds considerable promise for designing electrocatalytic or bioelectrocatalytic surfaces for a variety sensing and energy applications.

  20. Synthesis of ZSM-5 with intracrystal or intercrystal mesopores by polyvinyl butyral templating method.

    Science.gov (United States)

    Zhu, Haibo; Liu, Zhicheng; Kong, Dejin; Wang, Yangdong; Yuan, Xiaohong; Xie, Zaiku

    2009-03-15

    Three facile routes were utilized to synthesize ZSM-5 materials with intracrystal or intercrystal mesopores, where the polyvinyl butyral gel served as mesopore directing template. The three routes were divided into two synthesis strategies: the hydrothermal treatment of silica/PVB composite and re-crystallization of preformed zeolite precursor with the assistance of PVB gel. The fabrication of silica/PVB composite was accomplished by two routes including sol-gel process and impregnation method. The resulting composite was undergone hydrothermal treatment. During the crystallization PVB was occluded in the ZSM-5 crystal, creating intracrystal mesopores in the zeolite. The last route for the synthesis of mesoporous ZSM-5 was realized by re-crystallization of preformed ZSM-5 zeolite in the presence of PVB. This route involved the pre-crystallization of the amorphous aluminosilicate to produce the pre-formed ZSM-5 precursor. Upon further crystallization of the mixture of PVB gel and pre-formed ZSM-5, the ZSM-5 precursor was transformed into ZSM-5 aggregate of nanocrystals, while the PVB gel was occluded in the ZSM-5 particles. Removal of the template generated the typical microporosity associated with ZSM-5 structure along with intercrystal mesoporosity produced from the PVB. The mesoporous ZSM-5 exhibited enhanced catalytic activity in the toluene disproportionation and transalkylation with C(9) and C(10) aromatics.

  1. Surfactant-free nickel-silver core@shell nanoparticles in mesoporous SBA-15 for chemoselective hydrogenation of dimethyl oxalate.

    Science.gov (United States)

    Li, Molly Meng-Jung; Ye, Linmin; Zheng, Jianwei; Fang, Huihuang; Kroner, Anna; Yuan, Youzhu; Tsang, Shik Chi Edman

    2016-02-11

    Surfactant-free bimetallic Ni@Ag nanoparticles in mesoporous silica, SBA-15 prepared by simple wet co-impregnation catalyse hydrogenation of dimethyl oxalate to methyl glycolate or ethylene glycol in high yield.

  2. Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia

    Directory of Open Access Journals (Sweden)

    Ward Antony

    2011-01-01

    Full Text Available Abstract A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

  3. Nucleation Pathways of CO2 Condensation under Mesoporous Templated Glass

    Science.gov (United States)

    Wang, Bo; Byran, Matthew S.; Warren, Garfield T.; Sokol, Paul E.; Indiana University Team; NIST Collaboration

    2015-03-01

    Carbon capture and storage (CCS) are important elements in reducing greenhouse gas emission and combating global warming. The adsorption behavior of CO2 under mesoporous confinement at room temperature is particularly relevant. , Small Angle Scattering of X-ray (SAXS) and Neutron (SANS) were used to probe the adsorption process of CO2 under such mesoporous confinement MCM-41 and details of nucleation pathways were mapped out by fitting the scattering intensities with adsorption models. From both experiments, the nucleation of CO2 on the inner pore surface of MCM-41 is found to be a two-step process; high density liquid phase CO2 first forms uniform layers following the long range translational symmetry of the porous matrix, above one CO2 filling, determined by the pore size and temperature, capillary condensation initiates. The nucleation sites formed during capillary condensation start to separate the long range symmetry from the one at uniform layers. Finally, SAXS and SANS techniques are compared and they both showed their unique properties of probing the filling-dependent structures of adsorbed CO2 under such mesoporous system.

  4. Synthesis of siliceous hollow spheres with large mesopore wall structure by supercritical CO2-in-water interface templating.

    Science.gov (United States)

    Wang, Jiawei; Xia, Yongde; Wang, Wenxin; Mokaya, Robert; Poliakoff, Martyn

    2005-01-14

    Hollow silica spheres with large mesopore wall structures have been synthesized via CO(2)-in-water emulsion templating in the presence of PEO-PPO-PEO block copolymers under supercritical fluid conditions.

  5. Three-dimensionally ordered mesoporous Pd networks templated by a silica super crystal and their application in formic acid electrooxidation.

    Science.gov (United States)

    Ye, Lin; Wang, Yu; Chen, Xueying; Yue, Bin; Tsang, Shik Chi; He, Heyong

    2011-07-14

    Three-dimensionally ordered mesoporous Pd networks fabricated by a simple reduction method in solution using a face centered cubic silica super crystal as template exhibit high electroactivity in formic acid oxidation.

  6. Discoid Bicelles as Efficient Templates for Pillared Lamellar Periodic Mesoporous Silicas at pH 7 and Ultrafast Reaction Times

    Directory of Open Access Journals (Sweden)

    Mohanty Paritosh

    2011-01-01

    Full Text Available Abstract We report the first synthesis of periodic mesoporous silicas templated by bicelles. The obtained materials form novel pillared lamellar structures with a high degree of periodic order, narrow pore size distributions, and exceptionally high surface areas.

  7. Formation at low surfactant concentrations and characterization of mesoporous MCM-41

    Institute of Scientific and Technical Information of China (English)

    陈晓银; 丁国忠; 陈海鹰; 李全芝

    1997-01-01

    At low concentrations of cetyltrimethylammonium bromide,all silica-based mesoporous materials with hexagonal phase have been synthesized via interactions between self-assembled surfactant molecule aggregates and aniomc silicate polymers.The resulting materials are characterized by XRD,FT-IR,solid state 29Si MAS NMR,thermal analysis and N2 adsorption-desorption measurements.After soluble ions are removed,the interactors between surfactant micelles and silicate polymers are reorganized and then form mesostructures 1 he hexagonal framework is sonsistent with amorphous silica gel.The structures of materials depend on the synthesis conditions Hydrothermal process improves the interactions between molecules and increases the degree of framework silicon atom polymerization The.surface area and the mesopore volume of the material prepared at 100℃ increase by 87% and 71 %,respectively,compared with those obtained at room temperature.

  8. Microwave Absorption Behavior of Mesoporous Transition Metal Oxide Templated from SBA-15 and KIT-6

    Science.gov (United States)

    Wu, Hongjing; Wang, Liuding; Wang, Yiming

    2014-12-01

    In this paper, we have synthesized meso-oxides (i.e., Co3O4 and NiO) by using mesoporous silica as hard template. The microstructures and chemical compositions of the corresponding meso-oxides were characterized by the Transmission electron microscope-selected area electron diffusion (TEM-SAED), X-ray diffraction (XRD), scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDS), respectively. And, their electromagnetic and microwave absorption properties were investigated in the frequency range of 2-18 GHz. The results indicate that meso-oxide templated from KIT-6 (i.e., meso-K-Co/Ni) exhibit a dual absorption characteristic compared with those using SBA-15 as hard template. This phenomenon suggests that meso-oxides templated from SBA-15 and KIT-6 can exhibit different microwave absorption behaviors due to their respective microstructures.

  9. Template-Free Mesoporous Electrochromic Films on Flexible Substrates from Tungsten Oxide Nanorods.

    Science.gov (United States)

    Heo, Sungyeon; Kim, Jongwook; Ong, Gary K; Milliron, Delia J

    2017-09-13

    Low-temperature processed mesoporous nanocrystal thin films are platforms for fabricating functional composite thin films on flexible substrates. Using a random arrangement of anisotropic nanocrystals can be a facile solution to generate pores without templates. However, the tendency for anisotropic particles to spontaneously assemble into a compact structure must be overcome. Here, we present a method to achieve random networking of nanorods during solution phase deposition by switching their ligand-stabilized colloidal nature into a charge-stabilized nature by a ligand-stripping chemistry. Ligand-stripped tungsten suboxide (WO2.72) nanorods result in uniform mesoporous thin films owing to repulsive electrostatic forces preventing nanorods from densely packing. Porosity and pore size distribution of thin films are controlled by changing the aspect ratio of the nanorods. This template-free mesoporous structure, achieved without annealing, provides a framework for introducing guest components, therefore enabling our fabrication of inorganic nanocomposite electrochromic films on flexible substrates. Following infilling of niobium polyoxometalate clusters into pores and successive chemical condensation, a WOx-NbOx composite film is produced that selectively controls visible and near-infrared light transmittance without any annealing required. The composite shows rapid switching kinetics and can be stably cycled between optical states over 2000 times. This simple strategy of using anisotropic nanocrystals gives insight into mesoporous thin film fabrication with broader applications for flexible devices.

  10. Nano-hard template synthesis of pure mesoporous NiO and its application for streptavidin protein immobilization.

    Science.gov (United States)

    Wahab, Mohammad A; Darain, Farzana

    2014-04-25

    A simple and efficient immobilization of streptavidin protein (with hexa-histidine tag) onto the surface of mesoporous NiO is described. Before immobilization of streptavidin protein (with hexa-histidine tag) onto the surface of mesoporous NiO, we first synthesized well-organized mesoporous NiO by a nanocasting method using mesoporous silica SBA-15 as the hard template. Then, the well-organized mesoporous NiO particles were characterized by small angle x-ray diffraction (XRD), wide angle XRD, nitrogen adsorption/desorption, and transmission electron microscopy (TEM). TEM and small angle XRD suggested the formation of mesoporous NiO materials, whereas the wide angle XRD pattern of mesoporous NiO indicated that the nickel precursor had been transformed into crystalline NiO. The N2 sorption experiments demonstrated that the mesoporous NiO particles had a high surface area of 281 m2 g(-1), a pore volume of 0.51 cm3 g(-1) and a pore size of 4.8 nm. Next, the immobilization of streptavidin protein (with hexa-histidine tag) onto the surface of mesoporous NiO was studied. Detailed analysis using gel electrophoresis confirmed that this approach can efficiently bind his-tagged streptavidin onto the surface of mesoporous NiO material since the mesoporous NiO provides sufficient surface sites for the binding of streptavidin via non-covalent ligand binding with the histidine tag.

  11. Effects of Template Contents on the Physicochemical Sorption Properties of Zr—Incorporated Mesoporous Titania Materials

    Institute of Scientific and Technical Information of China (English)

    郑金玉; 丘坤元; 危岩

    2002-01-01

    Zr-Incorporated mesoporous titania materials were prepared via nonsurfactant templated sol-gel process of zirconium(IV) butoxide(ZBT) and titanium(IV) butoxide(TBT) in the presence of urea molecules as template or pore forming agent.The effcets of template contents on the pore parameters of the materials synthesized with fixed Zr incorporation contents were investigated by mitrogen adsorption-desrption measurements,powder X-ray diffraction(XRD) study and transmission electron microscopy(TEM).The changes of template contents play significant roles on the pore parameters at low incorporsation content of Zr.The pore diameters display a clear increase tendency with the increase of template contents.When high Zr incorporation content is used,the template contents have less effect on the pore diameters that almost keep unchanged with the increase of template contents.All the materials possess type IV isotherms with H2 hysteresis loops suggesting the formation of mesophase.The materials with low Zr incorporation content have anatase structures;however,it can not be found in the materials with high Zr incorporation content.TEM images show that some accumulated inter-particulate pores and welldistributed worm-like pores are present in the Zr-incorporated materials.

  12. Mesoporous MEL, BEA, and FAU zeolite crystals obtained by in situ formation of carbon template over metal nanoparticles

    DEFF Research Database (Denmark)

    Abildstrøm, Jacob Oskar; Ali, Zahra Nasrudin; Mentzel, Uffe Vie

    2016-01-01

    nanoparticles supported on silica, a carbon–silica composite is obtained and exploited as a combined carbon template/silica source for the zeolite synthesis. The mesoporous zeolite materials were all prepared by hydrothermal crystallization in alkaline media followed by removal of the carbon template...

  13. Supercritical Fluid Extraction of a Novel Template from Mesoporous Zirconia and the Effect on Porous Structure

    Institute of Scientific and Technical Information of China (English)

    MA Fu; ZHAO Hongjian

    2013-01-01

    Mesoporous zirconia was synthesized by a new and simple method.Zirconium n-propoxide was used as the zirconium source.A small,inexpensive nonsurfactant,triethanolamine,was used as the template.The template was removed by thermal treatment in air and supercritical fluid extraction using CO2.The structure of the resulting materials was characterized by X-ray diffraction,transmission electron microscopy,and N2 adsorption-desorption analyses.The materials are found to have narrowly distributed average pore diameters and wormhole-like pore channels.However,higher surface area and larger pore volume are exhibited after supercdtical fluid extraction with CO2.The removal of the template by thermal treatment also leads to condensation and mild shrinkage of the zirconia framework.

  14. Effects of Template Contents on the Physicochemical Sorption Properties of Zr-Incorporated Mesoporous Titania Materials

    Institute of Scientific and Technical Information of China (English)

    ZHENG,Jin-Yu(郑金玉); QIU,Kun-Yuan(丘坤元); WEI,Yan(危岩)

    2002-01-01

    Zr-Incorporated mesoporous titania materials were prepared via nonsurfactant templated sol-gel process of zirconium (Ⅳ)butoxide (ZBT) and titanium (Ⅳ) butoxide (TBT) in the presence of urea molecules as template or pore forming agent.The effects of template contents on the pore parameters of the materials synthesized with fixed Zr incorporation contents were investigated by nitrogen adsorption-desorption measurements,powder X-ray diffraction ( XRD) study and transmission electron microscopy (TEM). The changes of template contents play significant roles on the pore parameters at low incorporation content of Zr. The pore diameters display a clear increase tendency with the increase of template contents. When high Zr incorporation content is used, the template contents have less effect on the pore diameters that almost keep unchanged with the increase of temptate contents. All the materials possess type Ⅳ isotherms with H2 hysteresis loops suggesting the formation of mesophase. The materials with low Zr incorporation content have anatase structures; however, it can not be found in the materials with high Zr incorporation content. TEM images show that some accumulated inter-particulate pores and welldistributed worm-like pores are present in the Zr-incorporated materials.

  15. Capillary Condensation Pathways of CO2 under Templated Mesoporous Silica Confinement

    Science.gov (United States)

    Wang, Bo; Sokol, Paul

    2014-03-01

    Adsorption of CO2 in porous medium has been of great current interest due to its potential for mitigating the global warming caused by greenhouse gases. In particular, the behavior of confined CO2 in mesoporous media near room temperature is particularly relevant to sequestration efforts. Realistic mesoporous systems, such as shales and coals, represent a complex fractal pore structure that complicates the interpretation of adsorption studies. We present the results of a study focused on the adsorption of CO2 in model mesoporous media with well-defined pore structures. Templated porous glasses, such as MCM-41 which has a regular network of 1D pores, provide an ideal system for fundamental studies of the adsorption process. In this study, we focus on the structure of adsorbed CO2 films which evolves in a mixture of phases and the development of nucleation occurs during the formation of high density liquid CO2 inside the confining matrix. We have used Small Angle Neutron Scattering to study the spatial distribution of material radially and transversely within the pores. The 30m SANS NG7 at NIST was used to map out the details of CO2 condensation pathway under mesoporous silica confinement.

  16. Synthesis of ternary metal nitride nanoparticles using mesoporous carbon nitride as reactive template.

    Science.gov (United States)

    Fischer, Anna; Müller, Jens Oliver; Antonietti, Markus; Thomas, Arne

    2008-12-23

    Mesoporous graphitic carbon nitride was used as both a nanoreactor and a reactant for the synthesis of ternary metal nitride nanoparticles. By infiltration of a mixture of two metal precursors into mesoporous carbon nitride, the pores act first as a nanoconfinement, generating amorphous mixed oxide nanoparticles. During heating and decomposition, the carbon nitride second acts as reactant or, more precisely, as a nitrogen source, which converts the preformed mixed oxide nanoparticles into the corresponding nitride (reactive templating). Using this approach, ternary metal nitride particles with diameters smaller 10 nm composed of aluminum gallium nitride (Al-Ga-N) and titanium vanadium nitride (Ti-V-N) were synthesized. Due to the confinement effect of the carbon nitride matrix, the composition of the resulting metal nitride can be easily adjusted by changing the concentration of the preceding precursor solution. Thus, ternary metal nitride nanoparticles with continuously adjustable metal composition can be produced.

  17. Visualizing the enhanced chemical reactivity of mesoporous ceria; simulating templated crystallization in silica scaffolds at the atomic level.

    Science.gov (United States)

    Sayle, Thi X T; Sayle, Dean C

    2014-03-12

    Unique physical, chemical, and mechanical properties can be engineered into functional nanomaterials via structural control. However, as the hierarchical structural complexity of a nanomaterial increases, so do the challenges associated with generating atomistic models, which are sufficiently realistic that they can be interrogated to reliably predict properties and processes. The structural complexity of a functional nanomaterial necessarily emanates during synthesis. Accordingly, to capture such complexity, we have simulated each step in the synthetic protocol. Specifically, atomistic models of mesoporous ceria were generated by simulating the infusion and confined crystallization of ceria in a mesoporous silica scaffold. After removing the scaffold, the chemical reactivity of the templated mesoporous ceria was calculated and predicted to be more reactive compared to mesoporous ceria generated without template; visual "reactivity fingerprints" are presented. The strategy affords a general method for generating atomistic models, with hierarchical structural complexity, which can be used to predict a variety of properties and processes enabling the nanoscale design of functional materials.

  18. Exoelectrogenic biofilm as a template for sustainable formation of a catalytic mesoporous structure

    KAUST Repository

    Yates, Matthew D.

    2014-06-04

    © 2014 Wiley Periodicals, Inc. Actively respiring biofilms of Geobacter sulfurreducens were used as a biotemplate to form a palladium mesoporous layer directly on an electrode surface. Cells and proteins within the biofilm acted as the reductant and stabilizer to facilitate the reduction, dispersion, and attachment of palladium nanoparticles to the electrode surface without using synthetic chemicals. © 2014 Wiley Periodicals, Inc. Mesoporous structures can increase catalytic activity by maximizing the ratio of surface area to volume, but current synthesis techniques utilize expensive polymers and toxic chemicals. A Geobacter sulfurreducens biofilm was used as a sustainable template to form mesoporous Pd structures while eliminating the need for synthetic chemicals. The bulk of the biofilm material was removed by thermal treatments after nanoparticle formation, producing a catalytic Pd mesoporous (pore size 9.7±0.1nm) structure attached to the graphite electrode with a 1.5-2μm thick backbone composed of nanoparticles (~200nm). A control electrode electrochemically plated with Pd in the absence of a biofilm exhibited a variable planar Pd base (~0.5-3μm thick) with sporadic Pd extrusions (~2μm across, 1-5μm tall) from the surface. The biotemplated mesoporous structure produced 15-20% higher stable current densities during H2 oxidation tests than the electrochemically plated control electrode, even though 30% less Pd was present in the biotemplated catalyst. These results indicate that electroactive biofilms can be used as a sustainable base material to produce nanoporous structures without the need for synthetic polymers. Biotechnol. Bioeng. 2014;111: 2349-2354.

  19. Soft-Templating Synthesis of Mesoporous Silica-Based Materials for Environmental Applications

    Science.gov (United States)

    Gunathilake, Chamila Asanka

    Dissertation research is mainly focus on: 1) the development of mesoporous silica materials with organic pendant and bridging groups (isocyanurate, amidoxime, benzene) and incorporated metal (aluminum, zirconium, calcium, and magnesium) species for high temperature carbon dioxide (CO2) sorption, 2) phosphorous-hydroxy functionalized mesoporous silica materials for water treatment, and 3) amidoxime-modified ordered mesoporous silica materials for uranium sorption under seawater conditions. The goal is to design composite materials for environmental applications with desired porosity, surface area, and functionality by selecting proper metal oxide precursors, organosilanes, tetraethylorthosilicate, (TEOS), and block copolymer templates and by adjusting synthesis conditions. The first part of dissertation presents experimental studies on the merge of aluminum, zirconium, calcium, and magnesium oxides with mesoporous silica materials containing organic pendant (amidoxime) and bridging groups (isocyanurate, benzene) to obtain composite sorbents for CO2 sorption at ambient (0-25 °C) and elevated (60-120 °C) temperatures. These studies indicate that the aforementioned composite sorbents are fairly good for CO2 capture at 25 °C via physisorption mechanism and show a remarkably high affinity toward CO2 chemisorption at 60-120 °C. The second part of dissertation is devoted to silica-based materials with organic functionalities for removal of heavy metal ions such as lead from contaminated water and for recovery of metal ions such as uranium from seawater. First, ordered mesoporous organosilica (OMO) materials with diethylphosphatoethyl and hydroxyphosphatoethyl surface groups were examined for Pb2+ adsorption and showed unprecedented adsorption capacities up to 272 mg/g and 202 mg/g, respectively However, the amidoxime-modified OMO materials were explored for uranium extraction under seawater conditions and showed remarkable capacities reaching 57 mg of uranium per gram

  20. Preparation and Characterization of Mesoporous Zirconia Made by Using a Poly (methyl methacrylate Template

    Directory of Open Access Journals (Sweden)

    Zhang Chunxiang

    2008-01-01

    Full Text Available AbstractSuperfine powders of poly (methyl methacrylate (PMMA have been prepared by means of an emulsion polymerization method. These have been used as templates in the synthesis of tetragonal phase mesoporous zirconia by the sol–gel method, using zirconium oxychloride and oxalic acid as raw materials. The products have been characterized by infrared spectroscopy, X-ray diffraction analysis, transmission electron microscopy, N2adsorption-desorption isotherms, and pore size distribution. The results indicate that the average pore size was found to be 3.7 nm.

  1. Synthesis of Polydopamine-Like Nanocapsules via Removal of a Sacrificial Mesoporous Silica Template with Water.

    Science.gov (United States)

    Nador, Fabiana; Guisasola, Eduardo; Baeza, Alejandro; Villaecija, Miguel Angel Moreno; Vallet-Regí, Maria; Ruiz-Molina, Daniel

    2017-02-24

    Hollow polymeric polydopamine (PDA) micro-/nanocapsules have been obtained through a very simple, mild, and straightforward method that involves coating of silica mesoporous nanoparticles through an ammonia-triggered polymerization of PDA and the posterior removal of the sacrificial template simply by dispersion in water, without the need of any harsh chemical reagent, either in the presence or absence of active principles, from doxorubicin to iron oxide nanoparticles. To demonstrate the potential of the nanocapsules obtained with this new approach, they have been successfully used as nanocarriers for drug delivery. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Synthesis of mesoporous cerium-zirconium mixed oxides by hydrothermal templating method

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Mesoporous cerium-zirconium mixed oxides were prepared by hydrothermal method using cetyl trimethyl ammonium bromide (CTAB) as template.The effects of amount of template,pH value of solution and hydrothermal temperature on mesostructure of samples were systematically investigated.The final products were characterized by XRD,TEM,FT-IR,and BET.The results indicate that all the cerium-zirconium mixed oxides present a meso-structure.At molar ratio of n(CTAB)/n((Ce)+(Zr))=0.15,pH value of 9,and hydrothermal temperature of 120 ℃,the samples obtained possess a specific surface area of 207.9 m2/g with pore diameter of 3.70 nm and pore volume of 0.19 cm3/g.

  3. Electronic state of polyaniline deposited on carbon nanotube or ordered mesoporous carbon templates

    Energy Technology Data Exchange (ETDEWEB)

    Bulusheva, L.G.; Fedorovskaya, E.O.; Okotrub, A.V.; Maximovskiy, E.A. [Nikolaev Institute of Inorganic Chemistry, SB RAS, 3 Acad. Lavrentiev ave., 630090 Novosibirsk (Russian Federation); Vyalikh, D.V. [Institute of Solid State Physics, Dresden University of Technology, 01062 Dresden (Germany); Chen, Xiaohong; Song, Huaihe [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029 (China)

    2011-11-15

    Polyaniline (PANI) has been deposited on a carbon template by chemical oxidation of aniline chloride in acidic aqueous medium using sodium persulfate as oxidant. Two kinds of templates were used: array of aligned multiwall carbon nanotubes (CNTs) grown on silicon substrate and ordered mesoporous carbon (OMC) material. Electronic structure of composites was examined using near-edge X-ray absorption spectroscopy and X-ray photoelectron spectroscopy. Analysis of the spectra showed that PANI developed on the CNT surface is mainly protonated while it contains a marked amount of imine (=N-) nitrogen when deposited into the porous of OMC. Testing of electrochemical cell indicated enhancement of performance of composite electrodes as compared with unsupported PANI. XPS N 1s spectra of composites of PANI with OMC material (PANI/OMC) and aligned multiwall CNTs (PANI/CNT). (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  4. Synthesis of mesoporous alumina using polyvinyl alcohol template as porosity control additive

    Directory of Open Access Journals (Sweden)

    Zoltán Ecsedi

    2007-12-01

    Full Text Available The effects of polyvinyl alcohol (PVA template and calcinations temperatures on the characteristics of the alumina films were investigated. The samples were prepared by sol-gel method using aluminium triisopropylate precursor. The variation of microstructure, pore size and pore volume, were determined by nitrogen adsorption/desorption analysis and the macropore size distribution was determined using mercury porosimetry. TEM and SEM were used to observe the texture of these samples and the particle morphology. Experimental observation after drying and annealing shows that it is possible to produce crack free nanoporous alumina films using polyvinyl alcohol template. The obtained alumina samples have macroporous microstructure (with the average pore diameter dav = 34.9 μm, for sample prepared with 42.5 wt% of PVA addition and annealed at 1000°C with high portion of mesopores (with the average pore diameter Dav = 14.0 nm for the same sample.

  5. Template-directed assembly of metal-chalcogenide nanocrystals into ordered mesoporous networks.

    Energy Technology Data Exchange (ETDEWEB)

    Vamvasakis, Ioannis; Subrahmanyam, Kota S.; Kanatzidis, Mercouri G.; Armatas, Gerasimos S.

    2015-04-01

    Although great progress in the synthesis of porous networks of metal and metal oxide nanoparticles with highly accessible pore surface and ordered mesoscale pores has been achieved, synthesis of assembled 3D mesostructures of metal-chalcogenide nanocrystals is still challenging. In this work we demonstrate that ordered mesoporous networks, which comprise well-defined interconnected metal sulfide nanocrystals, can be prepared through a polymer-templated oxidative polymerization process. The resulting self-assembled mesostructures that were obtained after solvent extraction of the polymer template impart the unique combination of light-emitting metal chalcogenide nanocrystals, three-dimensional open-pore structure, high surface area, and uniform pores. We show that the pore surface of these materials is active and accessible to incoming molecules, exhibiting high photocatalytic activity and stability, for instance, in oxidation of 1-phenylethanol into acetophenone. We demonstrate through appropriate selection of the synthetic components that this method is general to prepare ordered mesoporous materials from metal chalcogenide nanocrystals with various sizes and compositions.

  6. Ordered mesoporous carbons obtained by a simple soft template method as sulfur immobilizers for lithium-sulfur cells.

    Science.gov (United States)

    Moreno, Noelia; Caballero, Alvaro; Hernán, Lourdes; Morales, Julián; Canales-Vázquez, Jesús

    2014-08-28

    Carbon materials with ordered mesoporous structures were synthesized using soft template methods and then activated by CO2 treatment. Sulfur was incorporated in these carbons via a simple chemical deposition method in aqueous solutions and the resulting composites were tested as electrodes in Li-S cells. The electrochemical results showed that well-ordered mesoporous carbons perform better than those with a random mesopore arrangement (wormhole-like mesoporous structure). The mesopore ordering yields a framework of well-connected empty sites that results in an enhancement of both the charge carrier mobility and the reversibility of the electrochemical reaction. Although the activation with CO2 partially destroys the mesopore arrangement, which adversely affects the electrode performance, it notably increases the surface area and the micropore content which improves the connectivity between the mesopores. The final observation was an irrelevant effect of the activation process at low current densities. However, at higher rates the activated carbon composite delivered higher capacities. The hierarchical pore structure formed by micro- and mesopores should guarantee the required fast mobility of the Li(+).

  7. Porous gold nanobelts templated by metal-surfactant complex nanobelts.

    Science.gov (United States)

    Li, Lianshan; Wang, Zhijian; Huang, Teng; Xie, Jinglin; Qi, Limin

    2010-07-20

    Unique, porous gold nanobelts consisting of self-organized nanoparticles were synthesized in a high yield by morphology-preserved transformation from metal-surfactant complex precursor nanobelts formed by a bolaform surfactant dodecane-1,12-bis(trimethylammonium bromide) (N-C(12)-NBr(2)) and HAuCl(4). It was revealed that the precursor nanobelts of the stoichiometric N-C(12)-N(AuCl(4))(2) complex formed through electrostatic combination of the positively charged quaternary ammonium headgroups of N-C(n)-NBr(2) and the negatively charged AuCl(4)(-) ions. They were subsequently converted into porous gold nanobelts with shrunken sizes upon reduction by NaBH(4). The morphology of the produced gold nanostructures could be adjusted by changing the mixing ratio between N-C(12)-NBr(2) and HAuCl(4) in the reaction solution. It was found that the obtained porous Au nanobelts exhibited enhanced catalytic activity toward reduction of 4-nitrophenol compared with solid gold nanobelts, probably owing to their larger surface area and more active sites.

  8. Dual template synthesis of a highly mesoporous SSZ-13 zeolite with improved stability in the methanol-to-olefins reaction

    OpenAIRE

    Wu, Leilei; Degirmenci, Volkan; Magusin, Pieter; Szyja, Bartlomiej M; Hensen, Emiel J.M.

    2012-01-01

    The dual template synthesis of zeolite SSZ-13 by use of trimethyl-adamantanammonium hydroxide and a diquaternary-ammonium mesoporogen induces considerable mesoporosity without impeding zeolite microporosity. The strongly improved accessibility of Brønsted sites in mesoporous SSZ-13 increases its stability during application as an acid catalyst in the methanol-to-olefins reaction.

  9. Dual template synthesis of a highly mesoporous SSZ-13 zeolite with improved stability in the methanol-to-olefins reaction.

    Science.gov (United States)

    Wu, Leilei; Degirmenci, Volkan; Magusin, Pieter C M M; Szyja, Bartłomiej M; Hensen, Emiel J M

    2012-10-04

    The dual template synthesis of zeolite SSZ-13 by use of trimethyl-adamantanammonium hydroxide and a diquaternary-ammonium mesoporogen induces considerable mesoporosity without impeding zeolite microporosity. The strongly improved accessibility of Brønsted sites in mesoporous SSZ-13 increases its stability during application as an acid catalyst in the methanol-to-olefins reaction.

  10. Comparative study on pore structures of mesoporous ZSM-5 from resorcinol-formaldehyde aerogel and carbon aerogel templating.

    Science.gov (United States)

    Tao, Yousheng; Hattori, Yoshiyuki; Matumoto, Akihiko; Kanoh, Hirofumi; Kaneko, Katsumi

    2005-01-13

    Resorcinol-formaldehyde aerogels and carbon aerogels of different mesoporosities have been used as templates for preparing bimodal zeolites of mesopores. Samples were thoroughly characterized with X-ray diffraction, field emission scanning electron microscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy, N(2) adsorption at 77 K, as well as FT-IR spectroscopy and (29)Si nuclear magnetic resonance spectroscopy. The mesoporous ZSM-5 zeolites have additional mesopores of 9-25 nm in widths and 0.07-0.2 cm(3)/g in volumes, besides their perfect inherent micropores. Experimental results show the mesoporous systems of the finally obtained zeolites can be influenced by proper preparation of resorcinol-formaldehyde aerogels and carbon aerogels through solution chemistry. Consequently, zeolites of tunable mesoporosities can be prepared with this unique methodology.

  11. Structural and magnetic properties of Ni nanowires grown in mesoporous silicon templates

    Energy Technology Data Exchange (ETDEWEB)

    Dolgiy, A.L.; Redko, S.V.; Komissarov, I.; Bondarenko, V.P. [Belarusian State University of Informatics and Radioelectronics, P. Brovka 6, Minsk 220013 (Belarus); Yanushkevich, K.I. [Scientific and Practical Materials Research Center, Institute of Semiconductor and Solid State Physics, Belarusian Academy of Sciences, P. Brovka 19, Minsk 220072 (Belarus); Prischepa, S.L., E-mail: prischepa@bsuir.by [Belarusian State University of Informatics and Radioelectronics, P. Brovka 6, Minsk 220013 (Belarus)

    2013-09-30

    Structural and magnetic properties of Ni nanowires electrochemically deposited into pores of mesoporous silicon template under the stationary galvanostatic regime have been investigated. Samples have been exhaustively studied by using scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy and specific magnetization measurements. SEM analysis revealed the formation of porous silicon/nickel nanocomposite at the initial stages of Ni deposition with the characteristic dimension of Ni nanoparticles in the range of 40–60 nm. After 60 min of deposition Ni continuous nanowires of 10 μm length have been formed. XRD analysis confirmed the polycrystalline structure of Ni in the mesoporous silicon template with the preferential orientation along [111] axis. Also some amount of silicide Ni{sub 2}Si was formed, which diffraction peak at 2Θ ≈ 33° was especially pronounced for low deposition times. The possible mechanism of nickel silicide formation during the electrochemical process has been discussed. It was supposed that, the presence of amorphous silicon on pore walls facilitates the diffusion of Ni inside silicon matrix with subsequent nickel silicide formation without heating. The idea has been confirmed by the fact that on crystalline silicon the formation of nickel silicide was not observed. The magnetic properties have been investigated by studying the temperature dependence (77 K–700 K) of the specific magnetization σ. The measured σ values were lower with respect to that of bulk Ni. The effect has been explained by the influence of uncontrolled formation of nickel silicide, which causes, after heating, larger irreversibility of σ(T) curves for samples with less deposition time. The obtained σ(T) dependencies allowed us to determine the Curie temperature, T{sub C}, which for low deposition times of Ni was lower (575 K) with respect to the bulk Ni (630 K). This is caused by the influence of dimensional effects on T{sub C} value

  12. Multifunctional organized mesoporous tin oxide films templated by graft copolymers for dye-sensitized solar cells.

    Science.gov (United States)

    Park, Jung Tae; Ahn, Sung Hoon; Roh, Dong Kyu; Lee, Chang Soo; Kim, Jong Hak

    2014-07-01

    The synthesis of organized mesoporous SnO2 films with high porosity, larger pores, and good interconnectivity, obtained by sol-gel templating with an amphiphilic graft copolymer, poly(vinyl chloride)-graft-poly(oxyethylene methacrylate), is reported. An improved performance of dye-sensitized solar cells (DSSCs) is demonstrated by the introduction of a 400 nm thick organized mesoporous SnO2 interfacial (om-SnO2 IF) layer between nanocrystalline TiO2 (nc-TiO2 ) and a fluorine-doped tin oxide substrate. To elucidate the improved efficiency, the structural, optical, and electrochemical properties of the devices were characterized by SEM, UV/Vis spectroscopy, noncontact 3D surface profilometry, intensity-modulated photocurrent/voltage spectroscopy, incident photon-to-electron conversion efficiency, and electrochemical impedance spectroscopy measurements. The energy-conversion efficiency of the solid polymerized ionic liquid based DSSC fabricated with the om-SnO2 IF/nc-TiO2 photoanode reached 5.9% at 100 mW cm(-2) ; this is higher than those of neat nc-TiO2 (3.5%) and organized mesoporous TiO2 interfacial/nc-TiO2 layer (5.4%) photoanodes. The improved efficiency is attributed to the antireflective property, cascadal energy band gap, good interconnectivity, and high electrical conductivity of the om-SnO2 IF layer, which results in enhanced light harvesting, increased electron transport, reduced charge recombination, and decreased interfacial/internal resistance.

  13. Mesoporous phenylalanine ammonia lyase microspheres with improved stability through calcium carbonate templating.

    Science.gov (United States)

    Cui, Jiandong; Zhao, Yamin; Tan, Zhilei; Zhong, Cheng; Han, Peipei; Jia, Shiru

    2017-05-01

    Cross-linked enzyme aggregates (CLEAs) have recently emerged as a promising method for enzyme immobilization due to its simplicity and low cost. However, a lack of good size and morphological control over the as-prepared CLEAs has limited their practical applications in some cases. Here, monodisperse spherical CLEAs of phenylalanine ammonia lyase (PAL microspheres) were prepared based on CaCO3 microtemplates. The preparation procedure involves filling porous CaCO3 microtemplates with the protein by salt precipitation, glutaraldehyde crosslinking, and dissolution of the microtemplates. The formulation of CaCO3 templates with controlled size was studied in detail. Characterization of the prepared PAL microspheres was investigated. The results showed that the PAL microspheres with high immobilization efficiency (79%) exhibited excellent stability, including increased tolerance to proteolysis, low pH, and denaturants, and excellent mechanical properties. For example, free PAL almost lost all activity after they were incubated in the presence of trypsin for 2min, whereas PAL microspheres still retained 95% of their initial activity. Moreover, scanning electron microscope, transmission electron microscope, and N2 adsorption-desorption isotherms revealed that the resultant PAL microspheres possessed good monodispersity and mesoporous structure instead of the amorphous clusters of conventional CLEAs with few pores. Compared with conventional CLEAs, the monodisperse PAL microspheres with mesoporous make them more potentially useful for biomedical and biotechnological applications.

  14. Synthesis of ZSM-5@Ordered Mesoporous Silica Composites by Dodecylamine Surfactant

    Institute of Scientific and Technical Information of China (English)

    MA Kuoyan; YU Haijun; FENG Guanglin; WANG Changguo; DAI Ya

    2014-01-01

    The core-shell structures of ZSM-5 coated with mesoporous silica were synthesized by means of dodecylamine (DDA) surfactant. The results show that the mesoporous silica shells are coated on ZSM-5 cores and result in the formation of hierarchical porous structures. The thickness of the coating shell can be controlled by changing the adding amount of TEOS. The core-shell composites with the thickness of 35 nm possess high surface areas (about 528 m2·g-1), large pores (about 3.5 nm in diameter) on the silica shells. The composite molecular sieves display higher adsorption capacity for benzene (140.2 mg·g-1) and butyraldehyde (213.7 mg·g-1) than that of pristine ZSM-5 for benzene (99.2 mg·g-1) and butyraldehyde (134.7 mg·g-1). The composite molecular sieves show a wide application foreground for harmful gas adsorbent for environmental protection.

  15. Adsorption of quinolone antibiotics in spherical mesoporous silica: Effects of the retained template and its alkyl chain length.

    Science.gov (United States)

    Liang, Zhijie; Zhaob, Zhiwei; Sun, Tianyi; Shi, Wenxin; Cui, Fuyi

    2016-03-15

    In this study, mesoporous silica (meso-silica) MCM-41 and those with the templates retained were synthesized and characterized. Adsorption capacities of the synthesized materials towards typical quinolone antibiotic pollutants, enrofloxacin and norfloxacin as representative, were investigated, and effects of the alkyl chain length of the templates on the adsorption capacity were evaluated. The results of this study indicated that the retained templates enhanced the adsorption capacities (Qmax) of the meso-silica MCM-41 toward hydrophobic enrofloxacin, but had an inhibitory effect on that towards hydrophilic norfloxacin, which were attributed to the hydrophobic inter-environment created by the long alkyl chains of the retained templates. Importantly, the adsorption capacity increased with the increase of the alkyl chain length of the retained templates. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Mesopore generation by organosilane surfactant during LTA zeolite crystallization, investigated by high-resolution SEM and Monte Carlo simulation

    Science.gov (United States)

    Cho, Kanghee; Ryoo, Ryong; Asahina, Shunsuke; Xiao, Changhong; Klingstedt, Miia; Umemura, Ayako; Anderson, Michael W.; Terasaki, Osamu

    2011-04-01

    The crystallization of LTA zeolite under a hydrothermal synthesis condition that contained a quaternary ammonium-type organosilane surfactant was studied with X-ray powder diffraction (XRD), high-resolution scanning electron microscopy (HRSEM) and Monte Carlo simulation of the crystal growth. The hydrothermal reaction products were collected at various crystallization times, and investigated with XRD and HRSEM. The HRSEM images of the final zeolite products were taken as synthesized and also after cross-sectioning with an argon ion beam. The HRSEM investigation revealed presence of a disordered network of mesoporous channels that penetrated the microporous zeolite crystal. Unless the loading of the surfactant was exceedingly high, the microporous zeolite particles exhibited truncated cubic morphologies that were almost like single crystals, despite penetration by the mesopores. The outline of the zeolite particle became progressively rounded as the mesoporosity was increased according to the surfactant loading. The mesoporosity in the zeolite crystals was well maintained against crystal-ripening processes for 6 d. This result supports the fact that the organosilane surfactant micelles became incorporated inside the zeolite crystal as a mesopore generator during the crystallization process. Data from Monte Carlo simulation agreed with these experimental results.

  17. Morphological control of porous SiC templated by As-synthesized form of mesoporous silica.

    Science.gov (United States)

    Selvan, Sakthivel Tamil; Aldeyab, Salem S; Zaidi, S M Javaid; Arivuoli, Dakshinamoorthy; Ariga, Katsuhiko; Mori, Toshiyuki; Vinu, Ajayan

    2011-08-01

    Porous silicon carbide with fiber like morphology was successfully prepared via a hard templating approach using as-synthesized form of mesoporous silica SBA-15 as template and sucrose as carbon precursor. The obtained materials have been characterized by various sophisticated techniques such as XRD, nitrogen adsorption, HRTEM, HRSEM, FT-IR and TGA. The XRD and the nitrogen adsorption results revealed that the materials are highly crystalline and exhibit porous structure with excellent textural characteristics. It has been demonstrated that the morphology of the materials can be finely controlled from rod shaped morphology to fiber like nanostructures by the simple adjustment of the reaction time from 5 to 12 h at the reaction temperature of 1300 degrees C. The reaction time of 12 h at 1300 degrees C was found to be the best condition to obtain highly crystalline nanofiber like morphology. The obtained materials display beautiful nanofiber morphology which has the diameter of 20 to 60 nm and a length of 7 to 10 microm which is much longer than the previously reported SiC nanofibers.

  18. Fabrication of Mesoporous Silica Shells on Solid Silica Spheres Using Anionic Surfactants and Their Potential Application in Controlling Drug Release

    Directory of Open Access Journals (Sweden)

    Mansour Al-Hoshan

    2012-11-01

    Full Text Available In this work, mesoporous shells were constructed on solid silica cores by employing anionic surfactante. A co-structure directing agent (CSDA has assisted the electrostatic interaction between negatively charged silica particles and the negatively charged surfactant molecules. Synthetic parameters such as reaction time and temperature had a significant impact on the formation of mesoporous silica shelld and their textural properties such as surface area and pore volume. Core-mesoporous shell silica spheres were characterized by small angle X-ray scattering, transmission electron microscopy, and N2 adsorption–desorption analysis. The synthesized particles have a uniformly mesoporous shell of 34–65 nm and possess a surface area of ca. 7–324 m2/g, and pore volume of ca. 0.008–0.261 cc/g. The core-mesoporous shell silica spheres were loaded with ketoprofen drug molecules. The in vitro drug release study suggested that core-mesoporous shell silica spheres are a suitable nanocarrier for drug molecules offering the possibility of having control over their release rate.

  19. Fabrication of mesoporous silica shells on solid silica spheres using anionic surfactants and their potential application in controlling drug release.

    Science.gov (United States)

    El-Toni, Ahmed Mohamed; Khan, Aslam; Ibrahim, Mohamed Abbas; Al-Hoshan, Mansour; Labis, Joselito Puzon

    2012-11-06

    In this work, mesoporous shells were constructed on solid silica cores by employing anionic surfactante. A co-structure directing agent (CSDA) has assisted the electrostatic interaction between negatively charged silica particles and the negatively charged surfactant molecules. Synthetic parameters such as reaction time and temperature had a significant impact on the formation of mesoporous silica shelld and their textural properties such as surface area and pore volume. Core-mesoporous shell silica spheres were characterized by small angle X-ray scattering, transmission electron microscopy, and N(2) adsorption–desorption analysis. The synthesized particles have a uniformly mesoporous shell of 34–65 nm and possess a surface area of ca. 7–324 m2/g, and pore volume of ca. 0.008–0.261 cc/g. The core-mesoporous shell silica spheres were loaded with ketoprofen drug molecules. The in vitro drug release study suggested that core-mesoporous shell silica spheres are a suitable nanocarrier for drug molecules offering the possibility of having control over their release rate.

  20. Synthesis of tantalum carbide and nitride nanoparticles using a reactive mesoporous template for electrochemical hydrogen evolution

    KAUST Repository

    Alhajri, Nawal Saad

    2013-01-01

    Tantalum carbide and nitride nanocrystals were prepared through the reaction of a tantalum precursor with mesoporous graphitic (mpg)-C 3N4. The effects of the reaction temperature, the ratio of the Ta precursor to the reactive template (mpg-C3N4), and the selection of the carrier gas (Ar, N2 and NH3) on the resultant crystal phases and structures were investigated. The produced samples were characterized using powder X-ray diffraction (XRD), CHN elemental analyses, thermogravimetric analyses (TGA), nitrogen sorption, a temperature-programmed reaction with mass spectroscopy (MS), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). The results indicate that the different tantalum phases with cubic structure, TaN, Ta2CN, and TaC, can be formed under a flow of nitrogen when formed at different temperatures. The Ta3N5 phase with a Ta5+ oxidation state was solely obtained at 1023 K under a flow of ammonia, which gasified the C 3N4 template and was confirmed by detecting the decomposed gaseous products via MS. Significantly, the formation of TaC, Ta2CN, and TaN can be controlled by altering the weight ratio of the C 3N4 template relative to the Ta precursor at 1573 K under a flow of nitrogen. The high C3N4/Ta precursor ratio generally resulted in high carbide content rather than a nitride one, consistent with the role of mpg-C3N4 as a carbon source. Electrochemical measurements revealed that the synthesized nanomaterials were consistently able to produce hydrogen under acidic conditions (pH 1). The obtained Tafel slope indicates that the rate-determining step is the Volmer discharge step, which is consistent with adsorbed hydrogen being weakly bound to the surface during electrocatalysis. © 2013 The Royal Society of Chemistry.

  1. Templated synthesis of monodisperse mesoporous maghemite/silica microspheres for magnetic separation of genomic DNA

    Science.gov (United States)

    Chen, Feng; Shi, Ruobing; Xue, Yun; Chen, Lei; Wan, Qian-Hong

    2010-08-01

    A novel method is described for the preparation of superparamagnetic mesoporous maghemite (γ-Fe 2O 3)/silica (SiO 2) composite microspheres to allow rapid magnetic separation of DNA from biological samples. With magnetite (Fe 3O 4) and silica nanoparticles as starting materials, such microspheres were synthesized by the following two consecutive steps: (1) formation of monodispersed organic/inorganic hybrid microspheres through urea-formaldedyde (UF) polymerization and (2) removal of the organic template and phase transformation of Fe 3O 4 to γ-Fe 2O 3 by calcination at elevated temperatures. The as-synthesized particles obtained by heating at temperature 300 °C feature spherical shape and uniform particle size ( dparticle=1.72 μm), high saturation magnetization ( Ms=17.22 emu/g), superparamagnetism ( Mr/ Ms=0.023), high surface area ( SBET=240 m 2/g), and mesoporosity ( dpore=6.62 nm). The composite microsphere consists of interlocked amorphous SiO 2 nanoparticles, in which cubic γ-Fe 2O 3 nanocrystals are homogeneously dispersed and thermally stable against γ- to α-phase transformation at temperatures up to 600 °C. With the exposed iron oxide nanoparticles coated with a thin layer of silica shell, the magnetic microspheres were used as a solid-phase adsorbent for rapid extraction of genomic DNA from plant samples. The results show that the DNA templates isolated from pea and green pepper displayed single bands with molecular weights greater than 8 kb and A260/ A280 values of 1.60-1.72. The PCR amplification of a fragment encoding the endogenous chloroplast ndhB gene confirmed that the DNA templates obtained were inhibitor-free and amenable to sensitive amplification-based DNA technologies.

  2. Tungsten Oxide and Polyaniline Composite Fabricated by Surfactant-Templated Electrodeposition and Its Use in Supercapacitors

    Directory of Open Access Journals (Sweden)

    Benxue Zou

    2014-01-01

    Full Text Available Composite nanostructures of tungsten oxide and polyaniline (PANI were fabricated on carbon electrode by electrocodeposition using sodium dodecylbenzene sulfonate (SDBS as the template. The morphology of the composite can be controlled by changing SDBS surfactant and aniline monomer concentrations in solution. With increasing concentration of aniline in surfactant solution, the morphological change from nanoparticles to nanofibers was observed. The nanostructured WO3/PANI composite exhibited enhanced capacitive charge storage with the specific capacitance of 201 F g−1 at 1.28 mA cm−2 in large potential window of -0.5~ 0.65 V versus SCE compared to the bulk composite film. The capacitance retained about 78% when the sweeping potential rate increased from 10 to 150 mV/s.

  3. Surfactant-Free Solvothermal Method for Synthesis of Mesoporous Nanocrystalline TiO2 Microspheres with Tailored Pore Size

    Directory of Open Access Journals (Sweden)

    Yajing Zhang

    2013-01-01

    Full Text Available TiO2 mesoporous microspheres self-assembled from nanoparticles were synthesized by a surfactant-free solvothermal route. The TiO2 precursors were fabricated by tetrabutyl titanate, glacial acetic acid, and urea in the ethanol solution at 140°C for 20 h, and TiO2 mesoporous microspheres were obtained by a postcalcination at temperatures of 450°C for promoting TiO2 crystallization and the removal of residual organics. The phase structure, morphology, and pore nature were characterized by XRD, SEM, and nitrogen adsorption-desorption measurements. The as-prepared TiO2 microspheres are in anatase phase, with 2-3 μm in diameter, and narrow pore distribution range is 3-4 nm. The adjustments of the synthetic parameters lead to the formation of the mesoporous TiO2 microspheres with tuned pore size distributions and morphology.

  4. Mesoporous polymer networks-ultraporous DVB resins by hard-templating of close-packed silica spheres.

    Science.gov (United States)

    Wilke, Antje; Weber, Jens

    2012-05-14

    The preparation of ultraporous polymer resins using a straightforward hard-templating synthesis is presented. Self-assembly of silica nanospheres into densely packed glasses allows an easy preparation of templates. Polydivinylbenzene resins with surface areas of up to 1000 m(2) g(-1) are synthesized as a model system and porosity analysis reveals bimodal porosity (spherical mesopores and micropores within the pore walls). The prepared systems can be further functionalized without loss of porosity as demonstrated by sulfonation. Because of their large pore sizes (13-28 nm), they are efficient adsorbents also for large molecules. Finally, the systems can also be used as model systems for the study of the pore drying and collapse process, which is of crucial importance for any application of mesoporous polymers.

  5. Effect of surfactant concentration on characteristics of mesoporous bioactive glass prepared by evaporation induced self-assembly process

    Science.gov (United States)

    Shih, Chi-Chung; Chien, Chi-Sheng; Kung, Jung-Chang; Chen, Jian-Chih; Chang, Shy-Shin; Lu, Pei-Shan; Shih, Chi-Jen

    2013-01-01

    Mesoporous bioactive glasses were prepared by the evaporation-induced self-assembly method. The main objective of the present study is to determine the effect of surfactant concentration on the synthesis of SiO2-CaO-P2O5 mesoporous bioactive glasses; the characterization techniques used include X-ray diffraction, scanning electron microscopy and nitrogen adsorption and desorption isotherms. The results show that the specific surface area initially increased with increasing surfactant concentrations in the range of 2.1-9.1 wt% and significantly decreased from 328.7 to 204.0 m2/g in the concentration range of 9.1-12.5 wt%. For texture evaluation, the selected area electron diffraction patterns of the mesoporous bioactive glass precursor gels (9.1 wt% F127) calcined at different temperatures were analyzed; these patterns support the notion that some glassy structures in bioactive glasses become crystalline following heat treatment. The scanning electron microscopy images and X-ray diffraction patterns obtained agree with the inductively coupled plasma with atomic emission spectroscopy results as the mesoporous bioactive glasses can induce the formation of an apatite-like layer on their surface in SBF, even after short soaking periods.

  6. Magnetic studies of mesoporous nanostructured iron oxide materials synthesized by one-step soft-templating.

    Science.gov (United States)

    Jin, Jing; Hines, William A; Kuo, Chung-Hao; Perry, David M; Poyraz, Altug S; Xia, Yan; Zaidi, Taha; Nieh, Mu-Ping; Suib, Steven L

    2015-07-14

    A combined magnetization and (57)Fe spin-echo nuclear magnetic resonance (NMR) study has been carried out on mesoporous nanostructured materials consisting of the magnetite (Fe3O4) and maghemite (γ-Fe2O3) phases. Two series of samples were synthesized using a recently developed one-step soft-templating approach with systematic variations in calcination temperature and reaction atmosphere. Nuclear magnetic resonance has been shown to be a valuable tool for distinguishing between the two magnetic iron oxide spinel phases, Fe3O4 and γ-Fe2O3, on the nanoscale as well as monitoring phase transformation resulting from oxidation. For the Fe3O4 and γ-Fe2O3 phases, peaks in the NMR spectra are attributed to Fe in the tetrahedral (A) sites and octahedral (B) sites. The magnetic field dependence of the peaks was observed and confirmed the site assignments. Fe3O4 on a nanoscale readily oxidizes to form γ-Fe2O3 and this was clearly evident in the NMR spectra. As evidenced by transmission electron microscope (TEM) images, the porous mesostructure for the iron oxide materials is formed by a random close-packed aggregation of nanoparticles; correspondingly, superparamagnetic behavior was observed in the magnetic measurements. Although X-ray diffraction (XRD) shows the spinel structure for the Fe3O4 and γ-Fe2O3 phases, unlike NMR, it is difficult to distinguish between the two phases with XRD. Nitrogen sorption isotherms characterize the mesoporous structures of the materials, and yield BET surface area values and limited BJH pore size distribution curves.

  7. Electrochemical Synthesis of CdSe Quantum Dot Array on Graphene Basal Plane using Mesoporous Silica Thin Film Templates

    OpenAIRE

    Kim, Yong-Tae; Han, Jung Hee; Hong, Byung Hee; Kwon, Young-Uk

    2010-01-01

    We report on the synthesis of CdSe quantum dots on a graphene surface by an electrochemical deposition method. By using a mesoporous silica film formed on the graphene surface as a template and a potential equalizer between the edge/defect sites and the basal plane of the graphene, CdSe quantum dots can be grown on the basal plane into a regular hexagonal array.

  8. Preparation of mesoporous Ag/AgBr/TiO2 nanocomposites with comb-type polymer as template

    Directory of Open Access Journals (Sweden)

    Li XU

    Full Text Available The mesoporous TiO2 nanocomposites were fabricated in a water bath at lower temperatures using the sol-gel method with a comb-type polymer as template and tetrabutyl titanate as Ti source. The Ag/AgBr/TiO2 nanocomposites with higher specific surface areas were obtained by the introduction of Ag/AgBr on the surface of the mesoporous TiO2 using a deposition-precipitation method. The as-prepared nanocomposites were characterized by X-ray diffraction (XRD, N2 sorption analysis, transmission electron microscope (TEM and UV-vis diffuse reflectance spectroscopy (UV-vis DRS. The results showed that both the as-prepared TiO2 and Ag/AgBr/TiO2 exhibited mesoporous structure. The introduction of Ag/AgBr not only decreased the specific surface area of the mesoporous TiO2 from 346 m2/g to 253 m2/g, but also significantly increased its visible light photocatalytic activity. The degradation rate of methyl orange under visible light irradiation over Ag/AgBr/TiO2 was 145 and 60 times of those over the commercial TiO2 P25 and the mesoporous TiO2, respectively.

  9. Template-Engaged In Situ Synthesis of Carbon-Doped Monoclinic Mesoporous BiVO4: Photocatalytic Treatment of Rhodamine B

    Science.gov (United States)

    Yao, Mingming; Gan, Lihua; Liu, Mingxian; Tripathi, Pranav K.; Liu, Yafei; Hu, Zhonghua

    2015-06-01

    In this paper, carbon-doped monoclinic scheelite mesoporous bismuth vanadate was synthesized through template-engaged in situ method. The bismuth nitrate pentahydrate and ammonia metavanadate were used as bismuth and vanadium precursors, respectively, glucose as carbon source, and mesoporous SiO2 aerogel as a hard template. Carbon-doped monoclinic mesoporous BiVO4 were obtained by heat treatment of BiVO4/glucose/template to carbonize glucose and form monoclinic crystal, followed by etching with NaOH solution to remove the SiO2 template. The samples were characterized by x-ray diffraction, N2 adsorption and desorption, UV-visible spectroscopy, Energy dispersive spectrometry, Raman spectroscopy, and Transmission electron microscopy. It was found that the sample with a carbon content of 0.5 wt.% possesses a specific surface area of 10.2 m2/g and has mesoporous structure with the most probable pore size of 13.9 nm. The band gap of carbon-doped monoclinic mesoporous BiVO4 was estimated to be 2.33 eV, indicating the superior photocatalytic activity under visible light. The photocatalytic efficiency of carbon-doped monoclinic mesoporous BiVO4 for the degradation of Rhodamine B under visible light (λ > 400 nm) in 120 min reaches 98.7%, Besides, the carbon-doped monoclinic mesoporous BiVO4 photocatalyst still showed high stability: 85% for Rhodamine B degradation after ten recycles.

  10. Synthesis of polymer nanostructures via the use of surfactant surface aggregates as templates

    Science.gov (United States)

    Marquez, Maricel

    The subject of this work is the synthesis of polymer nanostructures via the use of surfactant surface aggregates as templates, also termed Template Assisted Admicellar Polymerization (TAAP). The first chapter reviews some of the most current nanopatterning techniques (including both top-down and bottom-up approaches), with particular emphasis on the fabrication of organic and inorganic patterned nanostructures via particle lithography. In chapter 2, highly ordered hexagonal arrays of latex spheres were prepared on highly ordered pyrolytic graphite (HOPG) from a variation of the Langmuir Blodgett technique, using an anionic surfactant (SDS), and a low molecular weight (ca. 10000) polyacrylamide as spreading agents. When a nonionic polyethoxylated (EO = 9) surfactant was used as the spreading agent, no ordered arrays were observed. Based on the correlation found between the surface tension in the presence of the latex particles and the critical concentration at which hexagonal arrangements of latex spheres occurs; a model was proposed to explain the role of the spreading agent in forming stable monolayers at the air/liquid interface, which in turn are necessary for the formation of well-ordered monolayers on a solid substrate from the LB technique. According to this model, solid-like regions of small numbers of latex spheres form at the liquid-air interface, which are then transferred to the substrate. These ordered regions then act as nuclei for the formation of 2D arrays of latex spheres on the surface upon water evaporation. The role of other factors such as relative humidity, substrate and solvent choice, and pulling vs. compression speed were also found to affect the quality of the monolayers formed. Finally, a simple, easy to automate, yet effective surface tension method was proposed to predict the optimal conditions for the formation of ordered monolayers using a variation of the LB deposition method from any monodisperse set of spheres. In chapter 3, a novel

  11. Templated synthesis of monodisperse mesoporous maghemite/silica microspheres for magnetic separation of genomic DNA

    Energy Technology Data Exchange (ETDEWEB)

    Chen Feng; Shi Ruobing; Xue Yun; Chen Lei [School of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072 (China); Wan Qianhong, E-mail: qhwan@tju.edu.c [School of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072 (China)

    2010-08-15

    A novel method is described for the preparation of superparamagnetic mesoporous maghemite (gamma-Fe{sub 2}O{sub 3})/silica (SiO{sub 2}) composite microspheres to allow rapid magnetic separation of DNA from biological samples. With magnetite (Fe{sub 3}O{sub 4}) and silica nanoparticles as starting materials, such microspheres were synthesized by the following two consecutive steps: (1) formation of monodispersed organic/inorganic hybrid microspheres through urea-formaldedyde (UF) polymerization and (2) removal of the organic template and phase transformation of Fe{sub 3}O{sub 4} to gamma-Fe{sub 2}O{sub 3} by calcination at elevated temperatures. The as-synthesized particles obtained by heating at temperature 300 deg. C feature spherical shape and uniform particle size (d{sub particle}=1.72 mum), high saturation magnetization (M{sub s}=17.22 emu/g), superparamagnetism (M{sub r}/M{sub s}=0.023), high surface area (S{sub BET}=240 m{sup 2}/g), and mesoporosity (d{sub pore}=6.62 nm). The composite microsphere consists of interlocked amorphous SiO{sub 2} nanoparticles, in which cubic gamma-Fe{sub 2}O{sub 3} nanocrystals are homogeneously dispersed and thermally stable against gamma- to alpha-phase transformation at temperatures up to 600 deg. C. With the exposed iron oxide nanoparticles coated with a thin layer of silica shell, the magnetic microspheres were used as a solid-phase adsorbent for rapid extraction of genomic DNA from plant samples. The results show that the DNA templates isolated from pea and green pepper displayed single bands with molecular weights greater than 8 kb and A{sub 260}/A{sub 280} values of 1.60-1.72. The PCR amplification of a fragment encoding the endogenous chloroplast ndhB gene confirmed that the DNA templates obtained were inhibitor-free and amenable to sensitive amplification-based DNA technologies.

  12. Preparation of High Surface Area, Large Pore Volume Alumina by Using β-Cyclodextrin as a Non-surfactant Template

    Institute of Scientific and Technical Information of China (English)

    Lai Jun WANG; Ming Fen WEN; Yu Shan LI; Dong YANG; Jing CHEN; Chong Li SONG

    2006-01-01

    A series of alumina samples were prepared using β-cyclodextrin as the non-surfactant template. These samples were characterized by XRD, BET and TEM. The results showed that the alumina samples prepared using β-cyclodextrin template had the higher surface areas (124-484 m2/g), larger pore volumes (0.7-1.27 mL/g) and more thermal stability than samples prepared without using β-cyclodextrin.

  13. Visible-Light Degradation of Dyes and Phenols over Mesoporous Titania Prepared by Using Anthocyanin from Red Radish as Template

    Directory of Open Access Journals (Sweden)

    Zhiying Yan

    2014-01-01

    Full Text Available Heterogeneous photocatalysis is able to operate effectively to eliminate organic compounds from wastewater in the presence of semiconductor photocatalyst and a light source. Although photosensitization of titania by organic dyes is one of the conventional ways for visible-light utilization of titania, previous studies have not yet addressed the use of natural food coloring agents as templates in the synthesis of mesostructured materials, let alone the simultaneous achievement of highly crystalline mesoscopic framework and visible-light photocatalytic activity. In this work, anthocyanin, a natural pigment from red radish was directly used as template in synthesis of highly crystalline mesoporous titania. The synthesized mesoporous titania samples were characterized by a combination of various physicochemical techniques, such as XRD, SEM, HRTEM, nitrogen adsorption/desorption, and diffuse reflectance UV-Vis. The prepared mesoporous titania photocatalyst exhibited significant activity under visible-light irradiation for the degradation of dyes and phenols due to its red shift of band-gap-absorption onset and visible-light response as a result of the incorporation of surface carbon species.

  14. Aligned mesoporous architectures and devices.

    Energy Technology Data Exchange (ETDEWEB)

    Brinker, C. Jeffrey; Lu, Yunfeng (University of California Los Angeles, Los Angeles, CA)

    2011-03-01

    This is the final report for the Presidential Early Career Award for Science and Engineering - PECASE (LDRD projects 93369 and 118841) awarded to Professor Yunfeng Lu (Tulane University and University of California-Los Angeles). During the last decade, mesoporous materials with tunable periodic pores have been synthesized using surfactant liquid crystalline as templates, opening a new avenue for a wide spectrum of applications. However, the applications are somewhat limited by the unfavorabe pore orientation of these materials. Although substantial effort has been devoted to align the pore channels, fabrication of mesoporous materials with perpendicular pore channels remains challenging. This project focused on fabrication of mesoporous materials with perpendicularly aligned pore channels. We demonstrated structures for use in water purification, separation, sensors, templated synthesis, microelectronics, optics, controlled release, and highly selective catalysts.

  15. Effect of calcination temperature on physical parameters and photocatalytic activity of mesoporous titania spheres using chitosan/poly(vinyl alcohol) hydrogel beads as a template

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, R. [Department of Environmental Engineering, Taizhou University, Taizhou 318000 (China); Zhejiang Provincial Key Laboratory of Plant Evolutionary Ecology and Conservation, College of Life Science, Taizhou University, Taizhou 318000 (China); State Laboratory of Silica Materials and Department of Chemistry, Zhejiang University, Hangzhou 310027 (China); Zhu, H.-Y., E-mail: zhuhuayue@126.com [Department of Environmental Engineering, Taizhou University, Taizhou 318000 (China); Zhejiang Provincial Key Laboratory of Plant Evolutionary Ecology and Conservation, College of Life Science, Taizhou University, Taizhou 318000 (China); Chen, H.-H. [State Laboratory of Silica Materials and Department of Chemistry, Zhejiang University, Hangzhou 310027 (China); Yao, J. [Department of Environmental Engineering, Taizhou University, Taizhou 318000 (China); Zhejiang Provincial Key Laboratory of Plant Evolutionary Ecology and Conservation, College of Life Science, Taizhou University, Taizhou 318000 (China); Fu, Y.-Q. [Zhejiang Provincial Key Laboratory of Plant Evolutionary Ecology and Conservation, College of Life Science, Taizhou University, Taizhou 318000 (China); Zhang, Z.-Y. [Department of Environmental Engineering, Taizhou University, Taizhou 318000 (China); Xu, Y.-M., E-mail: xuym@css.zju.edu.cn [State Laboratory of Silica Materials and Department of Chemistry, Zhejiang University, Hangzhou 310027 (China)

    2014-11-15

    Highlights: • Mesoporous titania spheres were prepared using CS/PVA hydrogel beads as a template. • The titania spheres prepared was mesoporous structure. • The photocatalytic activity of the mesoporous titania spheres calcined at 500 °C was highest. - Abstract: Mesoporous titania spheres were prepared by modified sol–gel method using chitosan/poly(vinyl alcohol) hydrogel beads as a template. Effects of calcination temperature on physical parameters were investigated by X-ray diffraction (XRD), N{sub 2} adsorption–desorption, Fourier transform infrared (FT-IR) spectra, thermogravimetry and differential thermal analyses (TG-DTA), high-resolution transmission electron microscope (HRTEM) and scanning electron microscopy (SEM). The photocatalytic activity of mesoporous titania spheres prepared was also evaluated by photocatalytic degradation of phenol as a model molecule under UV irradiation. With increasing calcination temperature, average crystallite size and pore size increased. In contrast, Brunauer–Emmett–Teller (BET) specific surface areas, porosity and pore volumes steadily decreased. Results of characterization proved that prepared titania spheres with highly organized pores were mesoporous structure. The photocatalytic activity of mesoporous titania spheres calcined at 500 °C was more effective than those calcined at other temperatures, which were attributed to the porous structure, large BET surface area, crystalline, and smaller crystallite size. This work may provide new insights into the preparation of novel mesoporous titania spheres and further practical applications in the treatment of wastewater.

  16. Sm doped mesoporous CeO2 nanocrystals: aqueous solution-based surfactant assisted low temperature synthesis, characterization and their improved autocatalytic activity.

    Science.gov (United States)

    Mandal, Bappaditya; Mondal, Aparna; Ray, Sirsendu Sekhar; Kundu, Amar

    2016-01-28

    Mesoporous Sm(3+) doped CeO2 (Ce-Sm) with a nanocrystalline framework, a high content of Ce(3+) and surface area (184 m(2) g(-1)), have been synthesized through a facile aqueous solution-based surfactant assisted route by using inorganic precursors and sodium dodecyl sulphate as a template. The XRD results indicate that the calcined Ce-Sm and even the as-prepared material have a cubic fluorite structure of CeO2 with no crystalline impurity phase. XRD studies along with HRTEM results confirmed the formation of mesoporous nanocrystalline CeO2 at a lower temperature as low as 100 °C. A detailed analysis revealed that Sm(3+) doping in CeO2 has increased the lattice volume, surface area, mesopore volume and engineered the surface defects. Higher concentrations of Ce(3+) and oxygen vacancies of Ce-Sm resulted in lowering of the band gap. It is evident from the H2-TPR results that Sm(3+) doping in CeO2 strongly modified the reduction behavior of CeO2 by shifting the bulk reduction at a much lower temperature, indicating increased oxygen mobility in the sample which enables enhanced oxygen diffusion at lower temperatures, thus promoting reducibility, i.e., the process of Ce(4+)→ Ce(3+). UV-visible transmission studies revealed improved autocatalytic performance due to easier Ce(4+)/Ce(3+) recycling in the Sm(3+) doped CeO2 nanoparticles. From the in vitro cytotoxicity of both pure CeO2 and Sm(3+) doped CeO2 calcined at 500 °C in a concentration as high as 100 μg mL(-1) (even after 120 h) on MG-63 cells, no obvious decrease in cell viability is observed, confirming their excellent biocompatibility. The presence of an increased amount of surface hydroxyl groups, mesoporosity, and surface defects have contributed towards an improved autocatalytic activity of mesoporous Ce-Sm, which appear to be a potential candidate for biomedical (antioxidant) applications.

  17. Template Directed Synthesis and Characterization of Organic Mesoporous Polymers and their Adsorption Performance for Lysozyme

    Science.gov (United States)

    Sridhar, Manasa

    Three homologous series of MCFs with diverse pore topologies have been synthesized by symbiotic interplay of TMB/P123 (R1) and TEOS/P123 (R2) weight ratios in the initial microemulsion. It was found that the MCFs synthesized at R2 greater than the conventional value suffered significant lag in the mesopore volumes and areas at low concentrations of TMB. However, when R1 is increased beyond 1.0, the difference in the pore volumes and areas became negligible. Many key findings were reported through this study. TEM images revealed that the MCFs synthesized at higher values of R2 prematurely attained larger average pore sizes accompanied with portions displaying constricted worm-like mesostructures. Such bimodal mesophases are accounted by the swelling action of excess amounts of ethanol discharged due to the hydrolysis of increased amounts of TEOS present in the microemulsion along with partial TEOS dissolution in the hydrophobic PPO cores of the TMB/P123 micelles. MCFs synthesized at highest R2 value of 4.4 exhibits unique interconnected rod-like morphologies which are usually not observed for conventional MCFs. MCF produced using R1 = 2.5 and R2 = 3.0 exhibit bimodal mesophases consisting of polyhedral nanofoam-like textures along with regular spherical pores. USAXS results indicate wall thickness as large as 11 nm for MCFs produced at R2 =4.4. These MCFs of interesting mesostructures were employed as nanoscopic templates to produce Mesocellular Phenol Formaldehyde Foams (MPFFs) using vacuum-assisted incipient wetness impregnation technique. The nanocasted MPFFs show large pore volumes up to 1.4 cm3/g, BET surface areas more than 900 m2/g and large pore diameters in the range 27--99 nm depending on the MCF scaffold used. All the MPFFs showed faithful replication of the cavity sizes of their corresponding MCF parent templates. Stunningly, trimodal MPFFs resulted from the nanocasting of MCFs with R1 > 2.2. The resulting pore sizes were attributed to the original

  18. Minute-made and low carbon fingerprint microwave synthesis of high quality templated mesoporous silica

    KAUST Repository

    Chaignon, J.

    2015-01-01

    © The Royal Society of Chemistry 2015. Hexagonal mesostructured templated silicas were produced in less than 10 minutes using an ultra-fast microwave assisted hydrothermal synthesis. Typically, 10 g can be prepared at once in a commercial microwave device usually devoted to analytical digestion. Undesired alcohol side-products were avoided using inexpensive water colloidal silica instead of silicon alkoxides as the silicon source. In comparison with classical heating activation, the absence of pore expansion and pore wall thickening even for synthesis temperatures as high as 190 °C evidenced that heat transfer and diffusion of matter had no time to take place. Comparison between the chemically extracted and calcined samples shows that the structure was better stabilized for autoclaving above 150 °C. However, a fast temperature ramping and final temperatures above 180 °C were required to sear structures of the highest quality comparable to that of the best conventional methods. This is rationalized by assuming a sequential flake-by-flake assembly of the pore-wall at the micelle palisade. Notably, tosylate counterions yielded better structural characteristics than bromide counterions and allowed better opportunities for surfactant recycling.

  19. Dual-template ordered mesoporous carbon/Fe2O3 nanowires as lithium-ion battery anodes

    Science.gov (United States)

    Hu, Junkai; Sun, Chuan-Fu; Gillette, Eleanor; Gui, Zhe; Wang, Yuhuang; Lee, Sang Bok

    2016-06-01

    Ordered mesoporous carbons (OMCs) are ideal host materials that can provide the desirable electrical conductivity and ion accessibility for high-capacity oxide electrode materials in lithium-ion batteries (LIBs). To this end, however, it is imperative to establish the correlations among material morphology, pore structure and electrochemical performance. Here, we fabricate an ordered mesoporous carbon nanowire (OMCNW)/Fe2O3 composite utilizing a novel soft-hard dual-template approach. The structure and electrochemical performance of OMCNW/Fe2O3 were systematically compared with single-templated OMC/Fe2O3 and carbon nanowire/Fe2O3 composites. This dual-template strategy presents synergetic effects combining the advantages of both soft and hard single-template methods. The resulting OMCNW/Fe2O3 composite enables a high pore volume, high structural stability, enhanced electrical conductivity and Li+ accessibility. These features collectively enable excellent electrochemical cyclability (1200 cycles) and a reversible Li+ storage capacity as high as 819 mA h g-1 at a current density of 0.5 A g-1. Our findings highlight the synergistic benefits of the dual-template approach to heterogeneous composites for high performance electrochemical energy storage materials.Ordered mesoporous carbons (OMCs) are ideal host materials that can provide the desirable electrical conductivity and ion accessibility for high-capacity oxide electrode materials in lithium-ion batteries (LIBs). To this end, however, it is imperative to establish the correlations among material morphology, pore structure and electrochemical performance. Here, we fabricate an ordered mesoporous carbon nanowire (OMCNW)/Fe2O3 composite utilizing a novel soft-hard dual-template approach. The structure and electrochemical performance of OMCNW/Fe2O3 were systematically compared with single-templated OMC/Fe2O3 and carbon nanowire/Fe2O3 composites. This dual-template strategy presents synergetic effects combining the

  20. Template synthesis of 3-D bimodal ordered porous silica

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    A dual template synthesis combined with a modified bulk sol-gel process was used to prepare the three dimensional bimodal ordered porous silica, in which the macropore wall is mesoporous and both the pores are interconnected. The macropores were replicated from the template of the dried polystyrene colloidal crystal after being removed by calcination at high temperature, whislt the mesopores were achieved by burning off the surfactant in the gel. The ordered morphologies and interconnection of both the macropores and the mesopores were evidenced by the characterizations with SEM and TEM attached with electron diffraction. Nitrogen adsorption results also confirmed the interconnectivity, sizes and their distribution of the two sorts of pores. The effect of surfactant concentration and calcination conditions on mesopore size and its distribution was also investigated.

  1. PEO-surfactant Assisted Alcothermal or Hydrothermal Synthesis of Hierarchically Mesoporous Titania Materials%PEO-表面活性剂辅助醇热或水热合成分级介孔氧化钛材料

    Institute of Scientific and Technical Information of China (English)

    任铁真; 袁忠勇; 苏宝连

    2007-01-01

    在烷基聚乙烯氧化物(PEO)表面活性剂存在下采用水热或醇热方法合成出了介孔氧化钛,并与无模板体系室温溶胶-凝胶制备的介孔氧化钛进行了比较.这些不同方法制备的氧化钛的结构和特性及形成机理都有明显的不同.在酸性水溶液介质中可合成出双结晶(锐钛矿和板钛矿)结构的、热稳定的、介孔氧化钛,而在醇介质中合成出具有内部大孔结构的介孔氧化钛,其中的介孔是无序分布的呈蠕虫状、由锐钛矿相的氧化钛纳米颗粒聚集形成.无模板溶胶-凝胶制备的介孔氧化钛在焙烧后可得到孔分布11.2 nm的不规则介孔洞.对表面活性剂在介孔结构氧化钛合成中的作用进行了讨论.%Mesoporous titanias have been synthesized by either hydrothermal or alcothermal method in the presence of alkyl poly(ethylene oxide) (PEO) surfactants, and compared with those prepared by template-free room-temperature sol-gel route. The structures and properties of these titania materials are quite different, as well as their formation mechanisms. Thermostable mesoporous titanias with bicrystlline (anatase and brookite)structure were synthesized in acidic aqueous media. Mesoporous titanias with an interior macroporous structure were prepared in ethanol media, in which the mesopores were disordered, wormhole-like, formed by the agglomeration of titania nanoparticles with anatase phase. Narrow pore size distribution at 11.2 nm of irregular mesovoids was obtained in the template-free sol-gel prepared titania after calcination. The role of surfactant templates in the synthesis of mesostructured titanias is discussed.

  2. Effect of drying on the mesoporous structure of sol-gel derived silica with PPO-PEO-PPO template block copolymer.

    Science.gov (United States)

    Pei, Lihua; Kurumada, Ken-Ichi; Tanigaki, Masataka; Hiro, Masahiko; Susa, Kenzo

    2005-04-01

    The effects of drying method on the pore structure of mesoporous silica were studied from the viewpoint of enhancing closed porosity in mesoporous silica. The mesoporous silica was prepared via a sol-gel process using polyethyleneoxide-polypropyleneoxide-polyethyleneoxide (PEO-PPO-PEO) triblock copolymer (Pluronic P123) as the structure-directing template. The closed porosity was evaluated from the apparent mass density of the sample measured by a helium pycnometer. These mesoporous silicas were also characterized by transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and nitrogen adsorption. The drying method was shown to be responsible for the finally templated mesoporous structure of the silica. More rapid drying is more preferable for enhancing the closed porosity of the mesoporous silica. The closed pores were formed by immediate immobilization of copolymer molecular assemblies in the silica matrix due to the instant removal of the solvent and solidification at higher temperatures. The drying method, mainly affecting the drying rate, is highly influential on the finally replicated mesoporous structure in silica.

  3. Controllable synthesis of nitrogen-doped hollow mesoporous carbon spheres using ionic liquids as template for supercapacitors

    Science.gov (United States)

    Chen, Aibing; Li, Yunqian; Liu, Lei; Yu, Yifeng; Xia, Kechan; Wang, Yuying; Li, Shuhui

    2017-01-01

    We have demonstrated a facile and controllable synthesis of monodispersed nitrogen-doped hollow mesoporous carbon spheres (N-HMCSs) using resorcinol/formaldehyde resin as a carbon precursor, tetraethyl orthosilicate as a structure-assistant agent, ionic liquids (ILs) as soft template, partial carbon sources, and nitrogen sources. The sizes and the architectures including hollow and yolk-shell of resultant carbon spheres can be efficiently controlled through the adjustment of the content of ILs. Alkyl chain length of the ILs also has an important effect on the formation of N-HMCSs. With proper alkyl chain length and content of ILs, the resultant N-HMCSs show monodispersed hollow spheres with high surface areas (up to 1158 m2 g-1), large pore volumes (up to 1.70 cm3 g-1), and uniform mesopore size (5.0 nm). Combining the hollow mesoporous structure, high porosity, large surface area, and nitrogen functionality, the as-synthesized N-HMCSs have good supercapacitor performance with good capacitance (up to 159 F g-1) and favorable capacitance retention (88% capacitive retention after 5000 cycles).

  4. Fabrication of Meso-Porous Sintered Metal Thin Films by Selective Etching of Silica Based Sacrificial Template

    Directory of Open Access Journals (Sweden)

    Ludovic F. Dumee

    2014-08-01

    Full Text Available Meso-porous metal materials have enhanced surface energies offering unique surface properties with potential applications in chemical catalysis, molecular sensing and selective separation. In this paper, commercial 20 nm diameter metal nano-particles, including silver and copper were blended with 7 nm silica nano-particles by shear mixing. The resulted powders were cold-sintered to form dense, hybrid thin films. The sacrificial silica template was then removed by selective etching in 12 wt% hydrofluoric acid solutions for 15 min to reveal a purely metallic meso-porous thin film material. The impact of the initial silica nano-particle diameter (7–20 nm as well as the sintering pressure (5–20 ton·m−2 and etching conditions on the morphology and properties of the final nano-porous thin films were investigated by porometry, pyknometery, gas and liquid permeation and electron microscopy. Furthermore, the morphology of the pores and particle aggregation during shear mixing were assessed through cross-sectioning by focus ion beam milling. It is demonstrated that meso-pores ranging between 50 and 320 nm in average diameter and porosities up to 47% can be successfully formed for the range of materials tested.

  5. Activated mesoporous carbon nanofibers fabricated using water etching-assisted templating for high-performance electrochemical capacitors.

    Science.gov (United States)

    An, Geon-Hyoung; Koo, Bon-Ryul; Ahn, Hyo-Jin

    2016-03-01

    Activated mesoporous carbon nanofibers (AMCNFs) are synthesized by a sequential process of electrospinning, water etching-assisted templating, and acid treatment. Their morphologies, crystal structures, melting behavior, chemical bonding states, surface properties, and electrochemical performance are investigated for three different polyacrylonitrile (PAN) to polyvinylpyrrolidone (PVP) weight ratios - PAN : PVP = 8 : 2, 7 : 3, and 6 : 4. Compared to other samples, the AMCNFs with an optimum weight ratio of 6 : 4 show the highest specific surface area of 692 m(2) g(-1), a high volume percentage of mesopores of 43.9%, and an increased amount of carboxyl groups (10.5%). This results in a high specific capacitance of 207 F g(-1), a high-rate capability with a capacitance retention of 93%, a high energy density of 24.8-23.1 W h kg(-1), and an excellent cycling durability of up to 3000 cycles. The electrochemical performance improvement can be explained by the combined effect of the high surface area relative to the increased electrical double-layers, the high volume fraction of mesopores relative to shorter diffusion routes and low resistance pathways for ions, and the increased amount of carboxyl groups on the CNF surface relative to enhanced wettability.

  6. Nanocasting of carbon films with interdigitated bimodal three-dimensionally ordered mesopores by template-replica coassembly.

    Science.gov (United States)

    Tian, Zheng; Snyder, Mark A

    2014-10-21

    Carbon films with interdigitated bimodal three-dimensionally ordered mesoporosity (ib3DOm) are realized by a scalable nanoreplication process that removes the common need plaguing hard-templating strategies for multistep prefabrication of porous sacrificial templates. Specifically, evaporation-induced convective codeposition of size-tunable (ca. 20-50 nm) silica nanoparticles with a surrogate molecular carbon precursor (glucose), followed by carbonization and template etching, leads to remarkably ordered, crack-free mesoporous carbon films of tunable thickness (ca. 100-1000 nm) and pore size. Association of the molecular carbon precursor with the assembling pore forming particles is found to transition the system among three distinct film morphologies (collapsed, ib3DOm C, disordered), thereby establishing a pseudophase behavior controlled by silica solids content and incipient glucose concentration. Namely, a parametric window wherein ib3DOm C films can be realized is identified, with a diffuse lower phase boundary associated with collapsing carbon films, and a more distinct order-to-disorder transition encountered at higher glucose concentrations. Mechanistic insight suggests that glucose association with the lysine-silica nanoparticle surface modulates the lattice spacing, d, of the periodically ordered mesopores in the coassembled films, with the onset of the order-to-disorder transition occurring at a critical normalized lattice spacing, dc/D ∼ 1.16. This appears to apply across the phase space associated with D = 50 nm silica particles and to translate among other phase spaces associated with smaller particles (e.g., 30 nm). We briefly demonstrate the robustness of the codeposition process for realizing ib3DOm C films on rough FTO glass substrates and show that, in this form, these materials hold potential as low-cost alternatives to costly platinum electrodes for dye-sensitized solar cells.

  7. Alcohols solubilization in a nonionic fluorinated surfactant based system: effects on the characteristics of mesoporous silica.

    Science.gov (United States)

    Blin, J L; Du, N; Stébé, M J

    2012-05-01

    In this study, we have used hydrogenated alcohols with different chain lengths and one fluorinated alcohol as additives to determine their effect on the characteristics of mesoporous materials prepared from fluorinated micelles.

  8. Effect of Surfactant/Silica and Hydrothermal Time on the Specific Surface Area of Mesoporous Materials from Coal-Measure Kaolin

    Institute of Scientific and Technical Information of China (English)

    WU Qisheng; LI Shuiping

    2011-01-01

    Mesoporous materials with the highest surface area were synthesized by hydrothermal treatment from coal-measure kaolin using cetyltrimethylammonium bromide (CTAB) as template. The effect of several factors on surface area of products also had been discussed. The products were characterized by FTIR, HRTEM and N2 adsorption and desorption isotherm plot methods. There was typical structure as Si-O, Si-OH and Si-O-Si of mesoporous materials in the framework of synthesized materials; the pore size distributions of the products showed a sharp peak at 3.82 nm. The effect of hydrothermal treatment time and the amount of template on the specific surface area of mesoporous materials was important, when the Surf/Si = 0.135, and hydrothermal time = 12 h, and the surface area of the product reached up to 1 070 m2/g, which was higher than other products.

  9. Modeling micelle-templated mesoporous material SBA-15: atomistic model and gas adsorption studies.

    Science.gov (United States)

    Bhattacharya, Supriyo; Coasne, Benoit; Hung, Francisco R; Gubbins, Keith E

    2009-05-19

    We report the development of a realistic molecular model for mesoporous silica SBA-15, which includes both the large cylindrical mesopores and the smaller micropores in the pore walls. The methodology for modeling the SBA-15 structure involves molecular and mesoscale simulations combined with geometrical interpolation techniques. First, a mesoscale model is prepared by mimicking the synthesis process using lattice Monte Carlo simulations. The main physical features of this mesoscale pore model are then carved out of an atomistic silica block; both the mesopores and the micropores are incorporated from the mimetic simulations. The calculated pore size distribution, surface area, and simulated TEM images of the model structure are in good agreement with those obtained from experimental samples of SBA-15. We then investigate the adsorption of argon in this structure using Grand Canonical Monte Carlo (GCMC) simulations. The adsorption results for our SBA-15 model are compared with those for a similar model that does not include the micropores; we also compare with results obtained in a regular cylindrical pore. The simulated adsorption isotherm for the SBA-15 model shows semiquantitative agreement with the experimental isotherm for a SBA-15 sample having a similar pore size. We observe that the presence of the micropores leads to increased adsorption at low pressure compared to the case of a model without micropores in the pore walls. At higher pressures, for all models, the filling proceeds via the monolayer-multilayer adsorption on the mesopore surface followed by capillary condensation, which is mainly controlled by the mesopore diameter and is not influenced by the presence of the micropores.

  10. Sol-gel synthesis of mesoporous assembly of Nd 2O 3 nanocrystals with the aid of structure-directing surfactant

    Science.gov (United States)

    Sreethawong, Thammanoon; Chavadej, Sumaeth; Ngamsinlapasathian, Supachai; Yoshikawa, Susumu

    2008-01-01

    The aim of this work was to demonstrate a simple route to synthesize mesoporous assembly of nanocrystalline neodymium oxide (Nd 2O 3) with predominant pore size distribution in the mesopore region, which was successfully done for the first time under mild conditions by a modified sol-gel process with the aid of structure-directing surfactant. Properly manipulated hydrolysis and condensation steps of neodymium n-butoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution were performed to obtain the assembled Nd 2O 3 nanocrystal. Various techniques, including thermogravimetric and differential thermal analyses (TG-DTA), X-ray diffraction (XRD), N 2 adsorption-desorption, Brunauer-Emmett-Teller (BET) surface area analysis, Barrett-Joyner-Halenda (BJH) pore size distribution analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected-area electron diffraction (SAED), were used to characterize the synthesized Nd 2O 3 nanocrystal. The N 2 adsorption-desorption isotherm of the synthesized Nd 2O 3 nanocrystal calcined at 500 °C exhibited single hysteresis loop with IUPAC type IV-like pattern, indicating the existence of foremost mesopore. BJH pore size distribution result revealed that the synthesized Nd 2O 3 nanocrystals possessed mostly mesopore due to their assembly with a small extent of macropore, resulting in very small mean pore diameter in the mesopore region. The particle size determined from both SEM and TEM micrographs was also extremely small of approximately 10 nm.

  11. Studies of mesoporous inorganic materials

    Science.gov (United States)

    Khushalani, Deepa

    Studies in synthesis and characterization of mesoporous silica have been performed. In particular, four aspects have been studied. Primarily, a new synthetic route to enlarge the porosity of mesoporous silica materials has been developed. The synthetic strategy involves aging the syntheses mixture in the mother liquor and depending on the aging time, a gradual increase in pore sizes is observed from 40 to 65 A. The growth process involves restructuring of the mesopores under mild aqueous conditions without changing the length of the alkyl chain of the surfactant or addition of auxiliary hydrocarbon molecules. The pore-enlarged products retain the crystal morphology of the starting materials and appreciable solubilization of the structure is not observed during the aging process. Templating behavior of cetylpyridinium chloride in the synthesis of mesoporous silica has also been evaluated. Noticeable improvement in the quality of the resulting product is observed through PXRD, TEM, and adsorption analyses. Synthesis of mesoporous silica is also demonstrated using templating behavior of a mixture of two surfactants: cetylpyridinium chloride (CPCl) and cetyltrimethylammonium chloride (CTACl). As the CPCl :CTACl molar ratio is decreased, a gradual increase in the d100-spacing is observed starting at ca. 41 A and in sub-angstrom increments reaching to that of ca. 43 A. A model is presented that simultaneously accounts for the higher degree of structural order of the mesoporous silica templated with CPCl and the ability to fine tune d-spacings on a sub-angstrom length scale using CPCl/CTACl mixtures. In addition, a novel non-aqueous route to formation of lamellar and hexagonal phase of mesoporous silica has been developed. Ethylene glycol is employed as a solvent and as a chelating agent. The chelate effect results in stable glycosilicate(IV) complexes which are necessary for the syntheses and the framework thermal stability of the products has been found to increase via

  12. Polymer-templated mesoporous carbons synthesized in the presence of nickel nanoparticles, nickel oxide nanoparticles, and nickel nitrate

    Science.gov (United States)

    Choma, Jerzy; Jedynak, Katarzyna; Marszewski, Michal; Jaroniec, Mietek

    2012-02-01

    Mesoporous carbon composites, containing nickel and nickel oxide nanoparticles, were obtained by soft-templating method. Samples were synthesized under acidic conditions using resorcinol and formaldehyde as carbon precursors, poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock co-polymer Lutrol F127 as a soft template and nickel and nickel oxide nanoparticles, and nickel nitrate as metal precursors. In addition, a one set of samples was obtained by impregnation of mesoporous carbons with a nickel nitrate solution followed by further annealing at 400 °C. Wide angle X-ray powder diffraction along with thermogravimetric analysis proved the presence of nickel nanoparticles in the final composites obtained using nickel and nickel oxide nanoparticles, and Ni(NO3)2 solution. Whereas, the impregnation of carbons with a nickel nitrate solution followed by annealing at 400 °C resulted in needle-like nickel oxide nanoparticles present inside the composites’ pores. Low-temperature (-196 °C) nitrogen physisorption, X-ray powder diffraction, and thermogravimetric analysis confirmed good adsorption and structural properties of the synthesized nickel-carbon composites, in particular, the samples possessed high surface areas (>600 m2/g), large total pore volumes (>0.50 cm3/g), and maxima of pore size distribution functions at circa 7 nm. It was found that the composites were partially graphitized during carbonization process at 850 °C. The samples are stable in an air environment below temperature of 500 °C. All these features make the synthesized nickel-carbon composites attractive materials for adsorption, catalysis, energy storage, and environmental applications.

  13. Pore Orientation Effects on the Kinetics of Mesostructure Loss in Surfactant Templated Titania Thin Films

    Energy Technology Data Exchange (ETDEWEB)

    Das, Saikat; Nagpure, Suraj R.; Garlapalli, Ravinder Kumar; Wu, Qingliu; Islam, Syed Z.; Strzalka, Joseph; Rankin, Stephen E.

    2016-01-28

    The mesostructure loss kinetics are measured as a function of the orientation of micelles in 2D hexagonal close packed (HCP) columnar mesostructured titania thin films using in situ grazing incidence small angle x-ray scattering (GISAXS). Complementary supporting information is provided by ex situ scanning electron microscopy. Pluronic surfactant P123 acts as the template to synthesize HCP structured titania thin films. When the glass substrates are modified with crosslinked P123, the micelles of the HCP mesophase align orthogonal to the films, whereas a mix of parallel and orthogonal alignment is found on unmodified glass. The rate of mesostructure loss of orthogonally oriented (o-HCP) thin films (~60 nm thickness) prepared on modified substrate is consistently found to be less by a factor of 2.5±0.35 than that measured for mixed orientation HCP films on unmodified substrates. The activation energy for mesostructure loss is only slightly greater for films on modified glass (155±25 kJ/mol) than on unmodified (128 kJ/mol), which implies that the rate difference stems a greater activation entropy for mesostructure loss in o-HCP titania films. Nearly perfect orthogonal orientation of micelles on modified surfaces contributes to the lower rate of mesostructure loss by supporting the anisotropic stresses that develop within the films during annealing due to continuous curing, sintering and crystallization into the anatase phase during high temperature calcination (>450 °C). Because the film thickness dictates the propagation of orientation throughout the films and the degree of confinement, thicker (~250 nm) films cast onto P123-modified substrates have a much lower activation energy for mesostructure loss (89±27 kJ/mol) due to the mix of orientations found in the films. Thus, this kinetic study shows that thin P123- templated o-HCP titania films are not only better able to achieve good orthogonal alignment of 3 the mesophase relative to thicker films or films on

  14. Pore orientation effects on the kinetics of mesostructure loss in surfactant templated titania thin films.

    Science.gov (United States)

    Das, Saikat; Nagpure, Suraj; Garlapalli, Ravinder K; Wu, Qingliu; Islam, Syed Z; Strzalka, Joseph; Rankin, Stephen E

    2016-01-28

    The mesostructure loss kinetics are measured as a function of the orientation of micelles in 2D hexagonal close packed (HCP) columnar mesostructured titania thin films using in situ grazing incidence small angle X-ray scattering (GISAXS). Complementary supporting information is provided by ex situ scanning electron microscopy. Pluronic surfactant P123 acts as the template to synthesize HCP structured titania thin films. When the glass substrates are modified with crosslinked P123, the micelles of the HCP mesophase align orthogonal to the films, whereas a mix of parallel and orthogonal alignment is found on unmodified glass. The rate of mesostructure loss of orthogonally oriented (o-HCP) thin films (∼60 nm thickness) prepared on modified substrate is consistently found to be less by a factor of 2.5 ± 0.35 than that measured for mixed orientation HCP films on unmodified substrates. The activation energy for mesostructure loss is only slightly greater for films on modified glass (155 ± 25 kJ mol(-1)) than on unmodified (128 kJ mol(-1)), which implies that the rate difference stems from a greater activation entropy for mesostructure loss in o-HCP titania films. Nearly perfect orthogonal orientation of micelles on modified surfaces contributes to the lower rate of mesostructure loss by supporting the anisotropic stresses that develop within the films during annealing due to continuous curing, sintering and crystallization into the anatase phase during high temperature calcination (>450 °C). Because the film thickness dictates the propagation of orientation throughout the films and the degree of confinement, thicker (∼250 nm) films cast onto P123-modified substrates have a much lower activation energy for mesostructure loss (89 ± 27 kJ mol(-1)) due to the mix of orientations found in the films. Thus, this kinetic study shows that thin P123-templated o-HCP titania films are not only better able to achieve good orthogonal alignment of the mesophase relative to

  15. Breakthrough and future: nanoscale controls of compositions, morphologies, and mesochannel orientations toward advanced mesoporous materials.

    Science.gov (United States)

    Yamauchi, Yusuke; Suzuki, Norihiro; Radhakrishnan, Logudurai; Wang, Liang

    2009-01-01

    Currently, ordered mesoporous materials prepared through the self-assembly of surfactants have attracted growing interests owing to their special properties, including uniform mesopores and a high specific surface area. Here we focus on fine controls of compositions, morphologies, mesochannel orientations which are important factors for design of mesoporous materials with new functionalities. This Review describes our recent progress toward advanced mesoporous materials. Mesoporous materials now include a variety of inorganic-based materials, for example, transition-metal oxides, carbons, inorganic-organic hybrid materials, polymers, and even metals. Mesoporous metals with metallic frameworks can be produced by using surfactant-based synthesis with electrochemical methods. Owing to their metallic frameworks, mesoporous metals with high electroconductivity and high surface areas hold promise for a wide range of potential applications, such as electronic devices, magnetic recording media, and metal catalysts. Fabrication of mesoporous materials with controllable morphologies is also one of the main subjects in this rapidly developing research field. Mesoporous materials in the form of films, spheres, fibers, and tubes have been obtained by various synthetic processes such as evaporation-mediated direct templating (EDIT), spray-dried techniques, and collaboration with hard-templates such as porous anodic alumina and polymer membranes. Furthermore, we have developed several approaches for orientation controls of 1D mesochannels. The macroscopic-scale controls of mesochannels are important for innovative applications such as molecular-scale devices and electrodes with enhanced diffusions of guest species.

  16. Synthesis of MgO templated mesoporous carbons and its use for capacitor electrode

    Directory of Open Access Journals (Sweden)

    Yasushi Soneda

    2013-01-01

    Full Text Available Mesoporous carbons (MPCs with large specificsurface area are synthesized by the heat-treatmentand subsequent acid treatment of magnesium citrate.The MPCs obtained are examined as electrodematerials for electric double layer capacitor and showthe huge gravimetric capacitance with superior rateperformance in sulphuric acid electrolyte. The MPCsalso realize the larger capacitance than conventionalactivated carbon in organic electrolyte andextraordinary high retention of capacitance at verylow temperature, such as 80% of room temperaturevalue at -60 °C.

  17. New triblock copolymer templates, PEO-PB-PEO, for the synthesis of titania films with controlled mesopore size, wall thickness, and bimodal porosity.

    Science.gov (United States)

    Ortel, Erik; Fischer, Anna; Chuenchom, Laemthong; Polte, Jörg; Emmerling, Franziska; Smarsly, Bernd; Kraehnert, Ralph

    2012-01-23

    The synthesis and properties of a series of new structure-directing triblock copolymers with PEO-PB-PEO structure (PEO = poly(ethylene oxide) and PB = polybutadiene) and their application as superior pore-templates for the preparation of mesoporous titania coatings are reported. Starting from either TiCl4 or from preformed TiO2 nanocrystalline building blocks, mesoporous crystalline titanium oxide films with a significant degree of mesoscopic ordered pores are derived, and the pore size can be controlled by the molecular mass of the template polymer. Moreover, the triblock copolymers form stable micelles already at very low concentration, i.e., prior to solvent evaporation during the evaporation-induced self-assembly process (EISA). Consequently, the thickness of pore walls can be controlled independently of pore size by changing the polymer-to-precursor ratio. Thus, unprecedented control of wall thickness in the structure of mesoporous oxide coatings is achieved. In addition, the micelle formation of the new template polymers is sufficiently distinct from that of typical commercial PPO-PEO-PPO polymers (Pluronics; PPO = poly(propylene oxide)), so that a combination of both polymers facilitates bimodal porosity via dual micelle templating.

  18. A General Silica-Templating Synthesis of Alkaline Mesoporous Carbon Catalysts for Highly Efficient H2S Oxidation at Room Temperature.

    Science.gov (United States)

    Zhang, Zixiao; Jiang, Wuyou; Long, Donghui; Wang, Jitong; Qiao, Wenming; Ling, Licheng

    2017-01-25

    A general synthesis of alkaline mesoporous carbons (AMCs) is developed based on a simplified silica-templating method for room-temperature catalytic oxidation of H2S. The key to the success relies on dissolving the silica templates to create the interconnected mesoporous structure as well as leaving parts of the alkaline products in the pores; both of them are prerequisites for H2S oxidation. By adjusting the alkaline etching degree and organic/inorganic ratio, the porosity and basicity of the AMC could be simultaneously tuned, allowing the AMCs direct use for H2S catalytic oxidation with an unprecedented removal capacities of 4.49 ± 0.12 g/g. Such excellent catalytic performance should be attributed to the developed pore structure that stores the product sulfur and the strong basicity that promotes the dissociation of H2S into HS(-) ions. Moreover, this simplified silica-templating method could be easily extended to the preparation of various silica templated mesoporous carbon catalysts. All these AMCs demonstrate a successful combination of low cost with high performance, which may well be the answer for the technical development of industrial H2S removal.

  19. Synthesis of Mesoporous Carbon Using Halloyiste As Template%埃洛石为模板合成中孔炭

    Institute of Scientific and Technical Information of China (English)

    周述慧; 传秀云

    2014-01-01

    以天然矿物埃洛石为模板,蔗糖为碳源合成了具有“壳-核”结构的中孔炭。通过 SEM、TEM、N2吸附、XRD、Raman、TG 对样品进行了形貌和结构表征。结果表明:模板炭具有一维管状结构,与埃洛石具有相似的形貌。经过700℃和900℃炭化后的模板炭比表面积达到了945 m2/g和1147 m2/g,孔容和中孔率也较埃洛石有了很大的提高。去除模板后得到的模板炭具有很高的纯度,为无定形炭。升高炭化温度,模板炭的拉曼特征参数R值降低,热分解温度由563℃提高到623℃。同时,对模板炭的形成过程及孔道形成机理进行了分析和讨论。%Mesoporous carbons with“core-shell”structure were synthesized using halloysite as template and sucrose as carbon precursor by a template method. Field-emission scanning electron microscope (FE-SEM), transmission elec-tron microscope (TEM), nitrogen adsorption, X-ray diffraction, Raman spectra and Thermogravimetry (TG) were em-ployed to cheracterize the as-synthesized materials. Results indicate that the morphology and structure of the templated carbons are similar to that of halloysite. The carbons exhibit higher specific surface area (945 m2/g and 1147 m2/g), higher pore volumes and mesopore volume fraction than that of halloysite. The carbons present high purity and amor-phous structure. Raising the carbonization temperature, the Raman characteristic parameter (R) of the carbons de-creases and their decomposition temperature increases from 563℃ to 623℃. At the same time, the formation mecha-nism of the carbons and their pores is also discussed.

  20. Electrochromic and chemochromic performance of mesoporous thin-film vanadium oxide

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ping; Lee, Se-Hee; Tracy, C. Edwin; Turner, John A.; Pitts, J. Roland; Deb, Satyen K. [National Renewable Energy Laboratory, 1617 Cole Blvd., Golden, CO 80401 (United States)

    2003-12-01

    Mesoporous vanadium oxide thin films have been deposited electrochemically from a water/ethanol solution of vanadyl sulfate and a nonionic polymer surfactant. Aggregates of the polymer surfactant serve as templates that result in the formation of a mesoporous structure. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicate the presence of both macroporosity and mesoporosity in the electrodeposited film. Chemochromic behavior of mesoporous vanadium oxide is demonstrated in a palladium/vanadium oxide thin-film device, which colors when exposed to hydrogen gas. A comparison of results with evaporated vanadium oxide reveals that the mesoporous film displays an improved kinetic performance, which is most likely attributable to its highly porous structure. Also, the electrochemical properties have been explored in a lithium-battery configuration. Mesoporous vanadium oxide exhibits a very high lithium storage capacity and greatly enhanced charge-discharge rate. In situ optical measurements show that the film exhibits a multicolor electrochromic effect.

  1. Template-less surfactant-free hydrothermal synthesis NiO nanoflowers and their photoelectrochemical hydrogen production

    KAUST Repository

    Qurashi, Ahsanulhaq

    2015-12-01

    A facile direct surfactant-free template-less hydrothermal method is employed for the growth of high surface-area NiO nanoflowers made up of complex and assembled nanosheets network.Field emission scanning electron microscopy revealed that each nanosheet is about 50-60nm thick. Detailed structural analysis reveals single-crystalline nature of NiO nanoflowers with cubic crystal structure. The optical absorption bands in the wavelength range of 350-800nm illustrated in terms of ligand field theory. The photoelectrochemical (PEC), water splitting performance on the NiO nanoflowers were also investigated. © 2015 Hydrogen Energy Publications, LLC.

  2. Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning 13C and 29Si NMR Enhanced by Dynamic Nuclear Polarization

    Energy Technology Data Exchange (ETDEWEB)

    Lafon, Olivier [Universite de Lille Nord de France; Thankamony, Aany S. Lilly [Universite de Lille Nord de France; Kokayashi, Takeshi [Ames Laboratory; Carnevale, Diego [Ecole Polytechnique Federale de Lausanne; Vitzthum, Veronika [Ecole Polytechnique Federale de Lausanne; Slowing, Igor I. [Ames Laboratory; Kandel, Kapil [Ames Laboratory; Vezin, Herve [Universite de Lille Nord de France; Amoureux, Jean-Paul [Universite de Lille Nord de France; Bodenhausen, Geoffrey [Ecole Polytechnique Federale de Lausanne; Pruski, Marek [Ames Laboratory

    2012-12-21

    We show that dynamic nuclear polarization (DNP) can be used to enhance NMR signals of 13C and 29Si nuclei located in mesoporous organic/inorganic hybrid materials, at several hundreds of nanometers from stable radicals (TOTAPOL) trapped in the surrounding frozen disordered water. The approach is demonstrated using mesoporous silica nanoparticles (MSN), functionalized with 3-(N-phenylureido)propyl (PUP) groups, filled with the surfactant cetyltrimethylammonium bromide (CTAB). The DNP-enhanced proton magnetization is transported into the mesopores via 1H–1H spin diffusion and transferred to rare spins by cross-polarization, yielding signal enhancements εon/off of around 8. When the CTAB molecules are extracted, so that the radicals can enter the mesopores, the enhancements increase to εon/off ≈ 30 for both nuclei. A quantitative analysis of the signal enhancements in MSN with and without surfactant is based on a one-dimensional proton spin diffusion model. The effect of solvent deuteration is also investigated.

  3. Evaluating the Critical Thickness of TiO 2 Layer on Insulating Mesoporous Templates for Efficient Current Collection in Dye-Sensitized Solar Cells

    KAUST Repository

    Chandiran, Aravind Kumar

    2013-01-15

    In this paper, a way of utilizing thin and conformal overlayer of titanium dioxide on an insulating mesoporous template as a photoanode for dye-sensitized solar cells is presented. Different thicknesses of TiO2 ranging from 1 to 15 nm are deposited on the surface of the template by atomic layer deposition. This systematic study helps unraveling the minimum critical thickness of the TiO2 overlayer required to transport the photogenerated electrons efficiently. A merely 6-nm-thick TiO2 film on a 3-μm mesoporous insulating substrate is shown to transport 8 mA/cm 2 of photocurrent density along with ≈900 mV of open-circuit potential when using our standard donor-π-acceptor sensitizer and Co(bipyridine) redox mediator. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Mesoporous Silicon Hollow Nanocubes Derived from Metal-Organic Framework Template for Advanced Lithium-Ion Battery Anode.

    Science.gov (United States)

    Yoon, Taeseung; Bok, Taesoo; Kim, Chulhyun; Na, Younghoon; Park, Soojin; Kim, Kwang S

    2017-05-23

    Controlling the morphology of nanostructured silicon is critical to improving the structural stability and electrochemical performance in lithium-ion batteries. The use of removable or sacrificial templates is an effective and easy route to synthesize hollow materials. Herein, we demonstrate the synthesis of mesoporous silicon hollow nanocubes (m-Si HCs) derived from a metal-organic framework (MOF) as an anode material with outstanding electrochemical properties. The m-Si HC architecture with the mesoporous external shell (∼15 nm) and internal void (∼60 nm) can effectively accommodate volume variations and relieve diffusion-induced stress/strain during repeated cycling. In addition, this cube architecture provides a high electrolyte contact area because of the exposed active site, which can promote the transportation of Li ions. The well-designed m-Si HC with carbon coating delivers a high reversible capacity of 1728 mAhg(-1) with an initial Coulombic efficiency of 80.1% after the first cycle and an excellent rate capability of >1050 mAhg(-1) even at a 15 C-rate. In particular, the m-Si HC anode effectively suppresses electrode swelling to ∼47% after 100 cycles and exhibits outstanding cycle stability of 850 mAhg(-1) after 800 cycles at a 1 C-rate. Moreover, a full cell (2.9 mAhcm(-2)) comprising a m-Si HC-graphite anode and LiCoO2 cathode exhibits remarkable cycle retention of 72% after 100 cycles at a 0.2 C-rate.

  5. Polystyrene-block-poly(ethylene oxide) copolymers as templates for stacked, spherical large-mesopore silica coatings: dependence of silica pore size on the PS/PEO ratio

    OpenAIRE

    2016-01-01

    Large-mesopore silica films with a narrow pore size distribution and high porosity have been obtained by a sol–gel reaction of a silicon oxide precursor (TEOS) and using polystyrene-block-poly(ethylene oxide) (PS-b-PEO) copolymers as templates in an acidic environment. PS-b-PEO copolymers with different molecular weight and composition have been studied in order to assess the effects of the block length on the pore size of the templated silica films. The changes in the morphology of the porou...

  6. Carbon as amorphous shell and interstitial dopant in mesoporous rutile TiO2: Bio-template assisted sol-gel synthesis and photocatalytic activity

    Science.gov (United States)

    Mohamed, Mohamad Azuwa; Wan Salleh, Wan Norharyati; Jaafar, Juhana; Rosmi, Mohamad Saufi; Mohd. Hir, Zul Adlan; Abd Mutalib, Muhazri; Ismail, Ahmad Fauzi; Tanemura, Masaki

    2017-01-01

    Regenerated cellulose membrane was used as bio-template nanoreactor for the formation of rutile TiO2 mesoporous, as well as in-situ carbon dopant in acidified sol-gel system. The effects of calcination temperature on the physicochemical characteristic of core-shell nanostructured of bio-templated C-doped mesoporous TiO2 are highlighted in this study. By varying the calcination temperature, the thickness of the carbon shell coating on TiO2, crystallinity, surface area, and optical properties could be tuned as confirmed by HRTEM, nitrogen adsorption/desorption measurement, XRD and UV-vis-NIR spectroscopy. The results suggested that increment in the calcination temperature would lead to the band gap narrowing from 2.95 to 2.80 eV and the thickness of carbon shell increased from 0.40 to 1.20 nm. The x-ray photoelectron spectroscopy showed that the visible light absorption capability was mainly due to the incorporation of carbon dopant at interstitial position in the TiO2 to form Osbnd Tisbnd C or Tisbnd Osbnd C bond. In addition, the formation of the carbon core-shell nanostructured was due to carbonaceous layer grafted onto the surface of TiO2 via Tisbnd Osbnd C and Tisbnd OCO bonds. The result indicated that bio-templated C-doped core-shell mesoporous TiO2 prepared at 300 °C exhibited the highest photocatalytic activity. It is worthy to note that, the calcination temperature provided a huge impact towards improving the physicochemical and photocatalytic properties of the prepared bio-templated C-doped core-shell mesoporous TiO2.

  7. Effect of calcination temperature on physical parameters and photocatalytic activity of mesoporous titania spheres using chitosan/poly(vinyl alcohol) hydrogel beads as a template

    Science.gov (United States)

    Jiang, R.; Zhu, H.-Y.; Chen, H.-H.; Yao, J.; Fu, Y.-Q.; Zhang, Z.-Y.; Xu, Y.-M.

    2014-11-01

    Mesoporous titania spheres were prepared by modified sol-gel method using chitosan/poly(vinyl alcohol) hydrogel beads as a template. Effects of calcination temperature on physical parameters were investigated by X-ray diffraction (XRD), N2 adsorption-desorption, Fourier transform infrared (FT-IR) spectra, thermogravimetry and differential thermal analyses (TG-DTA), high-resolution transmission electron microscope (HRTEM) and scanning electron microscopy (SEM). The photocatalytic activity of mesoporous titania spheres prepared was also evaluated by photocatalytic degradation of phenol as a model molecule under UV irradiation. With increasing calcination temperature, average crystallite size and pore size increased. In contrast, Brunauer-Emmett-Teller (BET) specific surface areas, porosity and pore volumes steadily decreased. Results of characterization proved that prepared titania spheres with highly organized pores were mesoporous structure. The photocatalytic activity of mesoporous titania spheres calcined at 500 °C was more effective than those calcined at other temperatures, which were attributed to the porous structure, large BET surface area, crystalline, and smaller crystallite size. This work may provide new insights into the preparation of novel mesoporous titania spheres and further practical applications in the treatment of wastewater.

  8. Selective adsorption and release of cationic organic dye molecules on mesoporous borosilicates

    Energy Technology Data Exchange (ETDEWEB)

    Paul, Manidipa; Pal, Nabanita; Bhaumik, Asim, E-mail: msab@iacs.res.in

    2012-08-01

    Mesoporous materials can play a pivotal role as a host material for delivery application to a specific part of a system. In this work we explore the selective adsorption and release of cationic organic dye molecules such as safranine T (ST) and malachite green (MG) on mesoporous borosilicate materials. The mesoporous silica SBA-15 and borosilicate materials (MBS) were prepared using non-ionic surfactant Pluronic P123 as template via evaporation induced self-assembly (EISA) method. After template removal the materials show high surface areas and in some cases ordered mesopores of dimensions ca. 6-7 nm. High surface area, mesoporosity and the presence of heteroatom (boron) help this mesoporous borosilicate material to adsorb high amount of cationic dye molecules at its surface from the respective aqueous solutions. Furthermore, the mesoporous borosilicate samples containing higher percentage adsorbed dyes show excellent release of ST or MG dye in simulated body fluid (SBF) solution at physiological pH = 7.4 and temperature 310 K. The adsorption and release efficiency of mesoporous borosilicate samples are compared with reference boron-free mesoporous pure silica material to understand the nature of adsorbate-adsorbent interaction at the surfaces. - Graphical abstract: Highly ordered 2D-hexagonal mesoporous borosilicate materials have been synthesized by using Pluronic P123 as template. The materials show very good adsorption and release of organic cationic dye molecules under physiological conditions. Highlights: Black-Right-Pointing-Pointer Highly ordered 2D-hexagonal mesoporous borosilicate. Black-Right-Pointing-Pointer Nonionic Pluoronic P123 templated mesoporous material. Black-Right-Pointing-Pointer Adsorption of organic dyes at the mesopore surface. Black-Right-Pointing-Pointer Controlled release of dyes under physiological pH and temperature. Black-Right-Pointing-Pointer Release of safranine T (ST) and malachite green (MG) dyes in simulated body fluids.

  9. Synthesis of mesoporous silica materials with ascorbic acid as template via sol-gel process

    Institute of Scientific and Technical Information of China (English)

    PANG, Jie-Bina; QIU, Kun- Yuan; WEI, Yen

    2000-01-01

    Mesoporous silica materials with pore diameters of 2-5 nm have been prepared using ascorbic acid as a nonsurfactant tem plate or pore-forming agent in HCl-catalyzed sol-gel reactions of tetraethylorthosilicate, followed by removing the ascorbic acid compound by extrraction with ethanol. Characteriztion results from nitrogen sorption isotherm, powder X-ray diffraction and transmission electron microscopy indicate that the materials have large specific surface areas ( e. g. 1000 m2/g) and pore vohmes ( e. g. 0.8 cm3/g). The mesoporosity is arisen from interconnecting disordered wormlike channels and pores with relatively broad size distributions. As the ascorbic acid concen tration is increased, the pore diameters and pore volumes of the materials increase.

  10. Reprint of “Influence of chitosan–PEG binary template on the crystallite characteristics of sol–gel synthesised mesoporous nanotitania photocatalyst”

    Energy Technology Data Exchange (ETDEWEB)

    Preethi, T.; Abarna, B.; Rajarajeswari, G.R., E-mail: rajiaravind@gmail.com

    2014-11-15

    Highlights: • Binary templated (PEG and chitosan) mesoporous nano titania was prepared by sol–gel method. • PEG:chitosan in the ratio of 1:3 (P1-C3 titania) offered the best template effect. • P1-C3 titania had superior activity in degrading 4-chlorophenol under UV irradiation. • While, PEG acted as a physical template for mesopore formation. • Chitosan played a major role in defining the crystallite dimensions. - Abstract: Nano-titania is by far, the most studied material for its photocatalytic application in air and water pollution abatement. In this study, we have demonstrated the advantage offered by using a binary template of PEG and chitosan for the sol–gel synthesis of titania. Nano-titania samples were prepared using PEG, chitosan and the binary combination of these two as templates. XRD showed that all synthesized samples preserved the anatase structure. Titania sample prepared on 1% PEG and 3% chitosan as template (P1-C3 titania) possessed spherical shaped particles with an average particle size of 12.3 nm, a surface area of 82.9 m{sup 2}/g and uniform dispersion. DRS UV–Vis spectra indicated that, P1-C3 titania showed blue shift in its absorption profile due to decrease in particle size. Consistent with the characteristics, the P1-C3 titania exhibited the highest photocatalytic activity for the degradation of 4-chlorophenol under UV irradiation, in comparison with all the synthesized photocatalytic systems and Degussa-P25. The chitosan bio template is believed to offer controlled growth of titania through Lewis base type interaction with Ti metallic centers in TiO{sub 2}. Such controlled growth route will be significant in synthesizing custom-made titania for its advanced applications in catalytic processes.

  11. Influence of chitosan–PEG binary template on the crystallite characteristics of sol–gel synthesized mesoporous nano-titania photocatalyst

    Energy Technology Data Exchange (ETDEWEB)

    Preethi, T.; Abarna, B.; Rajarajeswari, G.R., E-mail: rajiaravind@gmail.com

    2014-10-30

    Highlights: • Binary templated (PEG and chitosan) mesoporous nano titania was prepared by sol–gel method. • PEG:chitosan in the ratio of 1:3 (P1-C3 titania) offered the best template effect. • P1-C3 titania had superior activity in degrading 4-chlorophenol under UV irradiation. • PEG acted as a physical template for mesopore formation. • Chitosan played a major role in defining the crystallite dimensions. - Abstract: Nano-titania is by far, the most studied material for its photocatalytic application in air and water pollution abatement. In this study, we have demonstrated the advantage offered by using a binary template of PEG and chitosan for the sol–gel synthesis of titania. Nano-titania samples were prepared using PEG, chitosan and the binary combination of these two as templates. XRD showed that all synthesized samples preserved the anatase structure. Titania sample prepared on 1% PEG and 3% chitosan as template (P1-C3 titania) possessed spherical shaped particles with an average particle size of 12.3 nm, a surface area of 82.9 m{sup 2}/g and uniform dispersion. DRS UV–Vis spectra indicated that, P1-C3 titania showed blue shift in its absorption profile due to decrease in particle size. Consistent with the characteristics, the P1-C3 titania exhibited the highest photocatalytic activity for the degradation of 4-chlorophenol under UV irradiation, in comparison with all the synthesized photocatalytic systems and Degussa-P25. The chitosan bio template is believed to offer controlled growth of titania through Lewis base type interaction with Ti metallic centers in TiO{sub 2}. Such controlled growth route will be significant in synthesizing custom-made titania for its advanced applications in catalytic processes.

  12. Surfactant-assisted sol gel preparation of high-surface area mesoporous TiO{sub 2} nanocrystalline Li-ion battery anodes

    Energy Technology Data Exchange (ETDEWEB)

    Casino, S. [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Di Lupo, F., E-mail: francesca.dilupo@polito.it [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Francia, C. [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Tuel, A. [IRCELYON, Institut de Recherches sur la Catalyse et l’environnement de Lyon, UMR 5256, CNRS-Université de Lyon 1, 2 Avenue Albert Einstein, 69626 Villeurbanne Cedex (France); Bodoardo, S. [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy); Gerbaldi, C., E-mail: claudio.gerbaldi@polito.it [GAME Lab, Department of Applied Science and Technology – DISAT, Institute of Chemistry, Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino (Italy)

    2014-05-01

    Highlights: • Mesoporous TiO{sub 2} nanocrystalline lithium battery anodes with tunable morphology. • Simple sol–gel technique using different cationic surfactants is adopted. • Textural/morphological characteristics define the electrochemical behaviour. • TiO{sub 2} anatase using C16TAB exhibits stable performance after 200 cycles. • It shows promising prospects as high-voltage safe Li-ion battery anode. - Abstract: We here investigate the physico-chemical/morphological characteristics and cycling behaviour of several kinds of nanocrystalline TiO{sub 2} Li-ion battery anodes selectively prepared through a simple sol–gel strategy based on a low-cost titanium oxysulfate precursor, by mediation of different cationic surfactants having different features (e.g., chain lengths, counter ion, etc.): i.e., cetyl-trimethylammonium bromide (CTAB), cetyl-trimethylammonium chloride (CTAC), benzalkonium chloride (BC) or octadecyl-trimethyl ammonium bromide (C{sub 18}TAB). X-ray diffraction profiles reveal single phase anatase having good correspondence with the reference pattern when using short chain CTAB, while in the other cases the presence of chloride and/or an increased chain length affect the purity of the samples. FESEM analysis reveal nanosized particles forming cauliflower-like aggregates. TiO{sub 2} materials demonstrate mesoporous characteristics and large specific surface area ranging from 250 to 30 m{sup 2} g{sup −1}. Remarkably stable electrode performance are achieved by appropriately selecting the cationic surfactant and the surfactant/precursor ratio. Detailed analysis is provided on the effect of the reaction conditions upon the formation of mesoporous crystalline titania enlightening new directions for the development of high performing lithium storage electrodes by a simple and low cost sol–gel strategy.

  13. Polystyrene-block-poly(ethylene oxide) copolymers as templates for stacked, spherical large-mesopore silica coatings: dependence of silica pore size on the PS/PEO ratio.

    Science.gov (United States)

    Nisticò, Roberto; Magnacca, Giuliana; Jadhav, Sushilkumar A; Scalarone, Dominique

    2016-01-01

    Large-mesopore silica films with a narrow pore size distribution and high porosity have been obtained by a sol-gel reaction of a silicon oxide precursor (TEOS) and using polystyrene-block-poly(ethylene oxide) (PS-b-PEO) copolymers as templates in an acidic environment. PS-b-PEO copolymers with different molecular weight and composition have been studied in order to assess the effects of the block length on the pore size of the templated silica films. The changes in the morphology of the porous systems have been investigated by transmission electron microscopy and a systematic analysis has been carried out, evidencing the dependence between the hydrophilic/hydrophobic ratio of the two polymer blocks and the size of the final silica pores. The obtained results prove that by tuning the PS/PEO ratio, the pore size of the templated silica films can be easily and finely predicted.

  14. High-temperature synthesis of highly hydrothermal stable mesoporous silica and Fe-SiO 2 using ionic liquid as a template

    Science.gov (United States)

    Liu, Hong; Wang, Mengyang; Hu, Hongjiu; Liang, Yuguang; Wang, Yong; Cao, Weiran; Wang, Xiaohong

    2011-03-01

    Mesoporous silicas and Fe-SiO 2 with worm-like structures have been synthesized using a room temperature ionic liquid, 1-hexadecane-3-methylimidazolium bromide, as a template at a high aging temperature (150-190 °C) with the assistance of NaF. The hydrothermal stability of mesoporous silica was effectively improved by increasing the aging temperature and adding NaF to the synthesis gel. High hydrothermally stable mesoporous silica was obtained after being aged at 190 °C in the presence of NaF, which endured the hydrothermal treatment in boiling water at least for 10 d or steam treatment at 600 °C for 6 h. The ultra hydrothermal stability could be attributed to its high degree of polymerization of silicate. Furthermore, highly hydrothermal stable mesoporous Fe-SiO 2 has been synthesized, which still remained its mesostructure after being hydrothermally treated at 100 °C for 12 d or steam-treated at 600 °C for 6 h.

  15. Effect of Solvent Variations in the Alcothermal Synthesis of Template-Free Mesoporous Titania for Dye-Sensitized Solar Cells Applications

    Science.gov (United States)

    Wawrzyńczak, Agata; Półrolniczak, Paulina; Sobuś, Jan; Schroeder, Grzegorz; Jurga, Stefan; Selli, Elena

    2016-01-01

    A series of 14 mesoporous titania materials has been synthesized using the simple alcothermal template-free method and various alcohols, such as methanol, propanols and butanols, as solvents. All materials were characterized by both wide and small angle XRD, which exhibited the anatase phase with short-range ordered mesoporous structure that is still forming during post synthetic temperature treatment in most of the investigated materials. Nitrogen adsorption–desorption isotherms confirmed the mesoporous structure with surface area ranging from 241 to 383 m2g- 1 and pore volumes from 0.162 to 0.473 m3g-1, UV-Vis diffuse reflectance showed the redshift of the absorption edge and the bandgap decrease after post synthetic calcination of the materials presented. The TEM, FT-IR, DTA and TG measurements have been made to well characterize the materials synthesized. The mesoporous samples obtained were applied as anode materials for dye-sensitized solar cells and showed good activity in photon-to-current conversion process with efficiency values ranging from 0.54% to 4.6% and fill factors in the 52% to 67% range. The photovoltaic performances were not as high as those obtained for the materials synthesized by us earlier employing ethanol as a solvent. The differences in the electron lifetime, calculated from electrochemical impedance spectroscopy results and varying between 4.3 to 17.5 ms, were found as a main factor determining the efficiency of the investigated photovoltaic cells. PMID:27741313

  16. Hydrogenated/fluorinated catanionic surfactants as potential templates for nanostructure design.

    Science.gov (United States)

    Hassan, Natalia; Ruso, Juan M; Piñeiro, Ángel

    2011-08-16

    The structure and physicochemical properties of the nanoparticles spontaneously formed within aqueous mixtures of the hydrogenated/fluorinated catanionic surfactant cetyltrimetylammonium perfluorooctanoate in the absence of counterions as a function of its concentration are investigated by a combined experimental/computational study at room temperature. Apparent molar volumes, isentropic apparent molar compressibilities, and dynamic light scattering measurements together with transmission and cryo-scanning electron as well as confocal laser microscopy images, and computational molecular dynamics simulations indicate that a variety of structures of different sizes coexist in solution with vesicles of ∼160 nm diameter. Interestingly, the obtained nanostructures were observed to self-assemble from a random distribution of monomers in a time scale easily accessible by atomistic classical molecular dynamics simulations, allowing to provide a comprehensive structural and dynamic characterization of the surfactant molecules at atomic level within the different aggregates. Overall, it is demonstrated that the use of mixed fluorinated hydrogenated surfactant systems represents an easy strategy for the design of specific nanoscale structures. The detailed structural analysis provided in the present work is expected to be useful as a reference to guide the design of new nanoparticles based on different hydrogenated/fluorinated catanionic surfactants.

  17. The oxidation of water by cerium(IV) catalysed by nanoparticulate RuO2 on mesoporous silica.

    Science.gov (United States)

    King, Nicola C; Dickinson, Calum; Zhou, Wuzong; Bruce, Duncan W

    2005-03-21

    Mesoporous silicates are prepared by templating on the hexagonal (H1) mesophase of surfactant bipyridine complexes of ruthenium(II) using a true liquid-crystal templating approach. On calcination, the surfactant template is removed except for the central metal ion that is oxidised, forming nanoparticles of RuO2 that deposit within the pores. RuO2 is a known oxidation catalyst and, despite its anhydrous nature in these silicates, is found to be very active in catalyzing the oxidation of water by acidic CeIV.

  18. Surfactant-assisted sacrificial template-mediated synthesis, characterization and photoluminescent properties of LaPO₄ : Eu³⁺ phosphor

    Indian Academy of Sciences (India)

    HEENA KHAJURIA; JIGMET LADOL; RAJINDER SINGH; HAQ NAWAZ SHEIKH; VINAY KUMAR

    2017-06-01

    In this paper, we report a surfactant-assisted self-sacrificing route for synthesis of Eu³⁺ doped LaPO4 nanostructures under hydrothermal conditions using the La(OH)CO₃ : Eu³⁺ precursor as a template andNH₄H₂PO₄ as the phosphate source. The synthesis was carried out in the absence and presence of surfactant [cetyltrimethyl ammonium bromide (CTAB)] and two different solvents (water and ethylene glycol). The precursor and products were characterized by powder X-ray diffraction, fourier transform infrared spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopyand photoluminescence studies. Influence of surfactant and solvents on morphology and luminescence of the final product in sacrificial template-assisted method has been investigated in detail.

  19. Tuning magnetoelectric coupling using porosity in multiferroic nanocomposites of ALD-grown Pb(Zr,Ti)O3 and templated mesoporous CoFe2O4

    Science.gov (United States)

    Chien, Diana; Buditama, Abraham N.; Schelhas, Laura T.; Kang, Hye Yeon; Robbennolt, Shauna; Chang, Jane P.; Tolbert, Sarah H.

    2016-09-01

    In this manuscript, we examine ways to create multiferroic composites with controlled nanoscale architecture. We accomplished this by uniformly depositing piezoelectric lead zirconate titanate (PZT) into templated mesoporous, magnetostrictive cobalt ferrite (CFO) thin films to form nanocomposites in which strain can be transferred at the interface between the two materials. To study the magnetoelectric coupling, the nanostructure was electrically poled ex situ prior to magnetic measurements. No samples showed a change in in-plane magnetization as a function of voltage due to substrate clamping. Out-of-plane changes were observed, but contrary to expectations based on total PZT volume fraction, mesoporous CFO samples partially filled with PZT showed more change in out-of-plane magnetization than the sample with fully filled pores. This result suggests that residual porosity in the composite adds mechanical flexibility and results in greater magnetoelectric coupling.

  20. SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

    Institute of Scientific and Technical Information of China (English)

    Jie-bin Pang; Kun-yuan Qiu; Yen Wei

    2000-01-01

    Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder Xray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m2/g) and pore volumes (e.g. 0.6 cm3/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

  1. Template free synthesis of mesoporous CuO nano architects for field emission applications.

    Science.gov (United States)

    Das, Swati; Maiti, Soumen; Saha, Subhajit; Das, Nirmalya Sankar; Chattopadhyay, Kalyan Kumar

    2013-04-01

    Cupric oxide mesospheres composed of its nanoparticles have been synthesized by a simple template free chemical route at different temperatures. Thermal aging followed by higher temperature (350 degrees C, 6 hours) annealing on these architects transformed them into hollow mesospheres consisting of sharp needle like structures with high aspect ratio (- 10(3)). A detailed analysis of field emission scanning electron microscopy confirmed a uniform registry of the prepared nanostructures. High resolution transmission electron microscopy showed that the as-grown mesospheres have hollow inner cavity with a thin outer shell. X-ray photoelectron spectroscopic analysis showed no obvious changes in the chemical composition of the nanostructures after annealing, confirming that the elements in the final products were in the proper oxidation states. Electron emission under electric field was investigated from these interesting structures. It was found that both of these nanostructures showed electron emission, but emission performance of the hollow mesospheres consisting of nanoneedles exhibited excellent performance with turn-on field as low as 2.8 V/microm and high enhancement factor (beta) - 5537.

  2. Molecular Modeling and Adsorption Properties of Ordered Silica-Templated CMK Mesoporous Carbons.

    Science.gov (United States)

    Jain, Surendra Kumar; Pellenq, Roland J-M; Gubbins, Keith E; Peng, Xuan

    2017-03-07

    Realistic molecular models of silica-templated CMK-1, CMK-3, and CMK-5 carbon materials have been developed by using carbon rods and carbon pipes that were obtained by adsorbing carbon in a model MCM-41 pore. The interactions between the carbon atoms with the silica matrix were described using the PN-Traz potential, and the interaction between the carbon atoms was calculated by the reactive empirical bond order (REBO) potential. Carbon rods and pipes with different thicknesses were obtained by changing the silica-carbon interaction strength, the temperature, and the chemical potential of carbon vapor adsorption. These equilibrium structures were further used to obtain the atomic models of CMK-1, CMK-3, and CMK-5 materials using the same symmetry as found in TEM pictures. These models are further refined and made more realistic by adding interconnections between the carbon rods and carbon pipes. We calculated the geometric pore size distribution of the different models of CMK-5 and found that the presence of interconnections results in some new features in the pore size distribution. Argon adsorption properties were investigated using GCMC simulations to characterize these materials at 77 K. We found that the presence of interconnection results greatly improves the agreement with available experimental data by shifting the capillary condensation to lower pressures. Adding interconnections also induces smoother adsorption/condensation isotherms, and desorption/evaporation curves show a sharp jump. These features reflex the complexity of the nanovoids in CMKs in terms of their pore morphology and topology.

  3. Underpotential deposition and anodic stripping voltammetry at mesoporous microelectrodes.

    Science.gov (United States)

    Sanchez, Pablo Lozano; Elliott, Joanne M

    2005-05-01

    Using the technique of liquid crystal templating a series of high surface area mesoporous platinum microelectrodes was fabricated. The underpotential deposition of metal ions at such electrodes was found to be similar to that at conventional platinum electrodes. The phenomena of underpotential deposition, in combination with the intrinsic properties of mesoporous microelectrodes (i.e. a high surface area and efficient mass transport) was exploited for the purpose of anodic stripping voltammetry. In particular the underpotential deposition of Ag(+), Pb(2+) and Cu(2+) ions was investigated and it was found that mesoporous microelectrodes were able to quantify the concentration of ions in solution down to the ppb range. The overall behaviour of the mesoporous electrodes was found to be superior to that of conventional microelectrodes and the effects of interference by surfactants were minimal.

  4. Silica-templated synthesis of ordered mesoporous tungsten carbide/graphitic carbon composites with nanocrystalline walls and high surface areas via a temperature-programmed carburization route.

    Science.gov (United States)

    Wu, Zhangxiong; Yang, Yunxia; Gu, Dong; Li, Qiang; Feng, Dan; Chen, Zhenxia; Tu, Bo; Webley, Paul A; Zhao, Dongyuan

    2009-12-01

    Ordered mesostructured tungsten carbide and graphitic carbon composites (WC/C) with nanocrystalline walls are fabricated for the first time by a temperature-programmed carburization approach with phosphotungstic acid (PTA) as a precursor and mesoporous silica materials as hard templates. The mesostructure, crystal phase, and amount of deposited graphitic carbon can be conveniently tuned by controlling the silica template (SBA-15 or KIT-6), carburizing temperature (700-1000 degrees C), the PTA-loading amount, and the carburizing atmosphere (CH(4) or a CH(4)/H(2) mixture). A high level of deposited carbon is favorable for connecting and stabilizing the WC nanocrystallites to achieve high mesostructural regularity, as well as promoting the carburization reaction. Meanwhile, large pore sizes and high mesoporosity of the silica templates can promote WC-phase formation. These novel, ordered, mesoporous WC/C nanocomposites with high surface areas (74-169 m(2) g(-1)), large pore volumes (0.14-0.17 cm(3) g(-1)), narrow pore-size distributions (centered at about 3 nm), and very good oxidation resistance (up to 750 degrees C) have potential applications in fuel-cell catalysts and nanodevices.

  5. Macroporous silica–alumina composites with mesoporous walls

    Indian Academy of Sciences (India)

    Gautam Gundiah

    2001-04-01

    Macroporous silica–alumina composites with mesopores have been prepared by employing polymethylmethacrylate beads as templates in the presence of the cationic surfactant, N-cetyl-N,N,N-trimethylammonium bromide. The Si/Al ratio in the composites has been varied between 4.5 and 48 and the occurrence of mesopores has been verified by X-ray diffraction. The surface areas of the samples vary between 676 and 1038 m2g–1, with the highest value in the sample with Si/Al = 48.

  6. Effects of adsorbed and templated nanosilver in mesoporous calcium-silicate nanoparticles on inhibition of bacteria colonization of dentin

    Directory of Open Access Journals (Sweden)

    Fan W

    2014-11-01

    Full Text Available Wei Fan,1,* Daming Wu,1,* Franklin R Tay,2 Tengjiao Ma,1 Yujie Wu,1 Bing Fan1 1The State Key Laboratory Breeding Base of Basic Science of Stomatology (Hubei-MOST and Key Laboratory of Oral Biomedicine Ministry of Education, School and Hospital of Stomatology, Wuhan University, Wuhan, People’s Republic of China; 2Department of Endodontics, Georgia Regents University, Augusta, Georgia, USA *These authors contributed equally to this work Abstract: Mesoporous calcium-silicate nanoparticles (MCSNs are advanced biomaterials for controlled drug delivery and mineralization induction. Nanosilver-incorporated MCSNs (Ag-MCSNs were prepared in the present study using both the adsorption and template methods. Both versions of Ag-MCSNs showed characteristic morphology of mesoporous materials and exhibited sustained release of ions over time. In antibacterial testing against planktonic Enterococcus faecalis, Ag-MCSNs showed significantly better antibacterial effects when compared with MCSNs (P<0.05. The Ag-MCSNs aggregated on the dentin surface of root canal walls and infiltrated into dentinal tubules after ultrasound activation, significantly inhibiting the adherence and colonization of E. faecalis on dentin (P<0.05. Despite this, Ag-MCSNs with templated nanosilver showed much lower cytotoxicity than Ag-MCSNs with adsorbed nanosilver (P<0.05. The results of the present study indicated that nanosilver could be incorporated into MCSNs using the template method. The templated nanosilver could release silver ions and inhibit the growth and colonization of E. faecalis both in the planktonic form and as biofilms on dentin surfaces as absorbed nanosilver. Templated Ag-MCSNs may be developed into a new intracanal disinfectant for root canal disinfection due to their antibacterial ability and low cytotoxicity, and as controlled release devices for other bioactive molecules to produce multifunctional biomaterials. Keywords: antibacterial effect, mesoporosity

  7. A tri-continuous mesoporous material with a silica pore wall following a hexagonal minimal surface

    KAUST Repository

    Han, Yu

    2009-04-06

    Ordered porous materials with unique pore structures and pore sizes in the mesoporous range (2-50nm) have many applications in catalysis, separation and drug delivery. Extensive research has resulted in mesoporous materials with one-dimensional, cage-like and bi-continuous pore structures. Three families of bi-continuous mesoporous materials have been made, with two interwoven but unconnected channels, corresponding to the liquid crystal phases used as templates. Here we report a three-dimensional hexagonal mesoporous silica, IBN-9, with a tri-continuous pore structure that is synthesized using a specially designed cationic surfactant template. IBN-9 consists of three identical continuous interpenetrating channels, which are separated by a silica wall that follows a hexagonal minimal surface. Such a tri-continuous mesostructure was predicted mathematically, but until now has not been observed in real materials. © 2009 Macmillan Publishers Limited. All rights reserved.

  8. Microwave synthesis of delaminated acid saponites using quaternary ammonium salt or polymer as template. Study of pH influence

    NARCIS (Netherlands)

    Gebretsadik, Fiseha B.; Mance, Deni; Baldus, Marc; Salagre, Pilar; Cesteros, Yolanda

    2015-01-01

    Mesoporous saponites were prepared at pH8 and 13 without and with template (surfactant or polymer) at 453K and autogenic pressure using microwaves or conventional oven during the hydrothermal ageing treatment. Acidity was obtained by calcination of the NH4-form. The effect of dilution (H<

  9. Microwave synthesis of delaminated acid saponites using quaternary ammonium salt or polymer as template. Study of pH influence

    NARCIS (Netherlands)

    Gebretsadik, Fiseha B.; Mance, Deni; Baldus, Marc; Salagre, Pilar; Cesteros, Yolanda

    2015-01-01

    Mesoporous saponites were prepared at pH8 and 13 without and with template (surfactant or polymer) at 453K and autogenic pressure using microwaves or conventional oven during the hydrothermal ageing treatment. Acidity was obtained by calcination of the NH4-form. The effect of dilution

  10. Self-assembled mesoporous Co and Ni-ferrite spherical clusters consisting of spinel nanocrystals prepared using a template-free approach.

    Science.gov (United States)

    Yu, Byong Yong; Kwak, Seung-Yeop

    2011-10-21

    Based on a self-assembly strategy, spherical mesoporous cobalt and nickel ferrite nanocrystal clusters with a large surface area and narrow size distribution were successfully synthesized for the first time via a template-free solvothermal process in ethylene glycol and subsequent heat treatment. In this work, the mesopores in the ferrite clusters were derived mainly from interior voids between aggregated primary nanoparticles (with crystallite size of less than 7 nm) and disordered particle packing domains. The concentration of sodium acetate is shown herein to play a crucial role in the formation of mesoporous ferrite spherical clusters. These ferrite clusters were characterized in detail using wide-angle X-ray diffraction, thermogravimetric-differential thermal analysis, (57)Fe Mössbauer spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, standard and high-resolution transmission electron microscopy, and other techniques. The results confirmed the formation of both pure-phase ferrite clusters with highly crystalline spinel structure, uniform size (about 160 nm) and spherical morphology, and worm-like mesopore structures. The BET specific surface areas and mean pore sizes of the mesoporous Co and Ni-ferrite clusters were as high as 160 m(2) g(-1) and 182 m(2) g(-1), and 7.91 nm and 6.87 nm, respectively. A model for the formation of the spherical clusters in our system is proposed on the basis of the results. The magnetic properties of both samples were investigated at 300 K, and it was found that these materials are superparamagnetic.

  11. Controllable modification of nanostructured carbon with hollow macroporous core/mesoporous shell and its application as templates in aqueous solution

    Science.gov (United States)

    Ren, Xiaona; Xia, Min; Yan, Qingzhi; Ge, Changchun

    2016-10-01

    Controllable modification of hydrophilic groups on tubular nanostructured carbon with hollow macroporous core/mesoporous shell (TNC-HMC/MS) was systematically studied and the mesoporous structure of TNC-HMC/MS has been kept. Different oxidants were used to modify the TNC-HMC/MS. Results revealed that the TNC-HMC/MS could be modified with carboxyl or hydroxy by different oxidants. More importantly, the BET/BJH results indicated that the mesoporous shell of TNC-HMC/MS has not been destroyed. In addition, water-soluble ammonium metatungstate has been encapsulated into the hollow core of TNC-HMC/MS and formed nanodot, bamboo-like and nanowire morphology.

  12. Enhanced Efficiency of Dye-Sensitized Solar Cells with Mesoporous-Macroporous TiO2 Photoanode Obtained Using ZnO Template

    Science.gov (United States)

    Pham, Trang T. T.; Mathews, Nripan; Lam, Yeng-Ming; Mhaisalkar, Subodh

    2017-06-01

    Improved light harvesting efficiency can be achieved by enhancing the optical properties of the titanium dioxide (TiO2) photoanode in dye-sensitized solar cells (DSSCs), leading to higher power conversion efficiency. By incorporating submicrometer cavities in TiO2 mesoporous film, using zinc oxide (ZnO) particles as a template, a bimodal pore size structure has been created, called a mesoporous-macroporous nanostructure. This photoanode structure consists of 20-nm TiO2 nanoparticles with two kinds of pores with size of 20 nm (mesopores) and 500 nm (macropores). Energy-dispersive x-ray spectroscopy and x-ray diffraction studies showed no trace of ZnO in the TiO2 after removal by TiCl4 treatment. Higher diffuse transmittance of this film compared with the standard transparent photoanode provides evidence of improved light scattering. When employed in a device, the incident-photon-to-current efficiency of ZnO-assisted devices showed enhancement at longer wavelengths, corresponding to the Mie light scattering effect with the macropores as scattering centers. This resulted in overall higher power conversion efficiency of the DSSC. In this work, a nonvolatile gel ionic liquid was used as the electrolyte to also demonstrate the benefit of this structure in combination with a viscous electrolyte and its promising application to prolong the stability of DSSCs.

  13. Enhanced Efficiency of Dye-Sensitized Solar Cells with Mesoporous-Macroporous TiO2 Photoanode Obtained Using ZnO Template

    Science.gov (United States)

    Pham, Trang T. T.; Mathews, Nripan; Lam, Yeng-Ming; Mhaisalkar, Subodh

    2017-02-01

    Improved light harvesting efficiency can be achieved by enhancing the optical properties of the titanium dioxide (TiO2) photoanode in dye-sensitized solar cells (DSSCs), leading to higher power conversion efficiency. By incorporating submicrometer cavities in TiO2 mesoporous film, using zinc oxide (ZnO) particles as a template, a bimodal pore size structure has been created, called a mesoporous-macroporous nanostructure. This photoanode structure consists of 20-nm TiO2 nanoparticles with two kinds of pores with size of 20 nm (mesopores) and 500 nm (macropores). Energy-dispersive x-ray spectroscopy and x-ray diffraction studies showed no trace of ZnO in the TiO2 after removal by TiCl4 treatment. Higher diffuse transmittance of this film compared with the standard transparent photoanode provides evidence of improved light scattering. When employed in a device, the incident-photon-to-current efficiency of ZnO-assisted devices showed enhancement at longer wavelengths, corresponding to the Mie light scattering effect with the macropores as scattering centers. This resulted in overall higher power conversion efficiency of the DSSC. In this work, a nonvolatile gel ionic liquid was used as the electrolyte to also demonstrate the benefit of this structure in combination with a viscous electrolyte and its promising application to prolong the stability of DSSCs.

  14. Supercritical-assistant liquid crystal template approach to synthesize mesoporous titania/multiwalled carbon nanotube composites with high visible-light driven photocatalytic performance

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Chen; Li, Youji, E-mail: bcclyj@163.com; Xu, Peng; Li, Ming; Huo, Pingxiang

    2014-12-15

    Graphical abstract: We investigate the influence of mesoporous titania content upon the visible-light driven photocatalytic performance of MPT/MWCNTs in phenol degradation. - Highlights: • MPT/MWCNTs were fabricated by liquid-crystal template in supercritical CO{sub 2}. • MPT/MWCNTs show high visible-light driven photoactivity for phenol degradation. • MPT/MWCNTs also show high reusable photoactivity under visible irradiation. • MPT content can control visible-light driven photoactivity of MPT/MWCNTs. • MPT is not easily broken away from from MPT/MWCNT composites. - Abstract: Mesoporous titania (MPT) was deposited onto multiwalled carbon nanotubes (MWCNTs) by deposition of titanium sol containing liquid-crystal template with assistant of supercritical CO{sub 2}. The products were characterized with various analytical techniques to determine their structural, morphological, optical absorption and photocatalytic properties. The results indicate that in photocatalytic degradation of phenol under visible light, the mixtures or composites of MPT and MWCNT show the high efficiency because of synergies between absorbing visible light, releasing electrons and facilitating transfer of charge carriers of MWCNTs and providing activated centers of MPT. Because of the mutual constraint between MPT and MWCNTs on the photocatalytic efficiency, the optimal loading of MPT in MPT/MWCNT-3 for phenol degradation is 48%. Because the intimate contact between MWCNTs and MPT is more beneficial to electron transformation, photoactivity of mixture is lower than that of composites with high reusable performance. The optimum conditions of phenol degradation were obtained.

  15. Templated Synthesis of Magnetic Nanoparticles through the Self-Assembly of Polymers and Surfactants

    Directory of Open Access Journals (Sweden)

    Vo Thu An Nguyen

    2014-08-01

    Full Text Available The synthesis of superparamagnetic nanoparticles (NPs for various technological applications continues to be an interesting research topic. The successful application of superparamagnetic NPs to each specific area typically depends on the achievement of high magnetization for the nanocrystals obtained, which is determined by their average size and size distribution. The size dispersity of magnetic NPs (MNPs is markedly improved when, during the synthesis, the nucleation and growth steps of the reaction are well-separated. Tuning the nucleation process with the assistance of a hosting medium that encapsulates the precursors (such as self-assembled micelles, dispersing them in discrete compartments, improves control over particle formation. These inorganic-organic hybrids inherit properties from both the organic and the inorganic materials, while the organic component can also bring a specific functionality to the particles or prevent their aggregation in water. The general concept of interest in this review is that the shape and size of the synthesized MNPs can be controlled to some extent by the geometry and the size of the organic templates used, which thus can be considered as molds at the nanometer scale, for both porous continuous matrices and suspensions.

  16. Gelatin-templated mesoporous titania for photocatalytic air treatment and application in metal chalcogenide nanoparticle-sensitized solar cells.

    Science.gov (United States)

    Stroyuk, Oleksandr L; Rayevska, Oleksandra Ye; Shvalagin, Vitaly V; Kuchmiy, Stepan Ya; Bavykin, Dmitry V; Streltsov, Eugene A; Poznyak, Sergey K

    2013-04-01

    Mesoporous titania as powders and thin films on ITO were prepared using gelatin as an available and non-expensive pore-forming agent. The mesoporous TiO2 manifested a much higher photocatalytic activity in the gas-phase air oxidation of ethanol and acetaldehyde than the commercial nanocrystalline TiO2 P25 (Degussa Corp.). The mesoporous ITO/TiO2 films exhibited 12-14% efficiency of photocurrent generation in aqueous Na2S electrolyte when illuminated by UV light. Deposition of CdS and PbS nanoparticles onto the surface of ITO/TiO2 further increases the photocurrent yields and expands the light sensitivity range of the films to 500-520 nm (CdS) and to 650-700 nm (PbS).

  17. Mesoporous TiO2 Bragg Stack Templated by Graft Copolymer for Dye-sensitized Solar Cells

    OpenAIRE

    Jung Tae Park; Won Seok Chi; Sang Jin Kim; Daeyeon Lee; Jong Hak Kim

    2014-01-01

    Organized mesoporous TiO2 Bragg stacks (om-TiO2 BS) consisting of alternating high and low refractive index organized mesoporous TiO2 (om-TiO2) films were prepared to enhance dye loading, light harvesting, electron transport, and electrolyte pore-infiltration in dye-sensitized solar cells (DSSCs). The om-TiO2 films were synthesized via a sol-gel reaction using amphiphilic graft copolymers consisting of poly(vinyl chloride) backbones and poly(oxyethylene methacrylate) side chains, i.e., PVC-g-...

  18. Fabrication of mesoporous silica for ultra-low-k interlayer dielectrics

    Science.gov (United States)

    Fujii, Nobutoshi; Kohmura, Kazuo; Nakayama, Takahiro; Tanaka, Hirofumi; Hata, Nobuhiro; Seino, Yutaka; Kikkawa, Takamaro

    2005-11-01

    We have developed sol-gel self-assembly techniques to control the pore structure and diameter of ultra-low-k interlayer dielectric (ILD) films. Porous silica films have been fabricated using cationic and nonionic surfactants as templates, resulting in 2D-hexagonal and disordered pore structures, respectively. The disordered mesoporous silica film has a worm-hole like network of pore channels having a uniform diameter. Precursors of the mesoporous silica films were synthesized by use of tetraethyl-orthosilicate (TEOS), inorganic acid, water, ethanol and various surfactants. The surfactants used were cationic alkyltrimethyl-ammonium (ATMA) chloride surfactants for 2D-hexagonal pores and nonionic tri-block copolymer for disordered structures. Dimethyldiethoxysilane (DMDEOS) was added for forming the disordered mesoporous silica. The disordered cylindrical pore structure with a uniform pore size was fabricated by controlling the static electrical interaction between the surfactant and the silica oligomer with methyl group of DMDEOS. Tetramethylcycrotetrasiloxane (TMCTS) vapor treatment was developed, which improved the mechanical strength of mesoporous silica films. The TMCTS polymer covered the pore wall surface and cross-linked to passivate the mechanical defects in the silica wall. Significant enhancement of mechanical strength was demonstrated by TMCTS vapor treatment. The porous silica film modified with a catalyst and a plasma treatment achieved higher mechanical strength and lower dielectric constant than conventional porous silica films because the TMCTS vapor treatment was more effective for mechanical reinforcement and hydrophobicity.

  19. A facile one-pot self-assembly approach to incorporate SnOx nanoparticles in ordered mesoporous carbon with soft templating for fuel cells.

    Science.gov (United States)

    Huang, Yingqiang; Zhai, Zhicheng; Luo, Zhigang; Liu, Yingju; Liang, Zhurong; Fang, Yueping

    2014-04-04

    Unique SnO(x) (x = 1,2)/ordered mesoporous carbon nanocomposites (denoted as SnO(x)/OMC) are firstly synthesized through a 'one-pot' synthesis together with the soft template self-assembly approach. The obtained SnO(x)/OMC nanocomposites with various SnO(x) contents exhibit uniform pore sizes between 3.9 and 4.2 nm, high specific surface areas between 497 and 595 m(2) g(-1), and high pore volumes between 0.39 and 0.48 cm(3) g(-1). With loading of Pt, Pt-SnO(x)/OMC with relatively low SnO(x) content exhibits superior electrocatalytic performance, long-term durability, and resistance to CO poisoning for methanol oxidation, as compared to Pt/OMC, PtRu/C and Pt-SnO(x)/C, which may be attributed not only to the synergetic effect of embedded SnO(x), but also to the highly ordered mesostructure with high specific surface areas and large pore volumes affording plenty of surface area for support of Pt nanoparticles. This work supplies an efficient way to synthesize novel ordered mesoporous carbon self-supported metallic oxide as catalyst support and its further potential application to reduce the cost of catalysts in direct methanol fuel cells.

  20. A facile one-pot self-assembly approach to incorporate SnOx nanoparticles in ordered mesoporous carbon with soft templating for fuel cells

    Science.gov (United States)

    Huang, Yingqiang; Zhai, Zhicheng; Luo, Zhigang; Liu, Yingju; Liang, Zhurong; Fang, Yueping

    2014-04-01

    Unique SnOx (x = 1,2)/ordered mesoporous carbon nanocomposites (denoted as SnOx/OMC) are firstly synthesized through a ‘one-pot’ synthesis together with the soft template self-assembly approach. The obtained SnOx/OMC nanocomposites with various SnOx contents exhibit uniform pore sizes between 3.9 and 4.2 nm, high specific surface areas between 497 and 595 m2 g-1, and high pore volumes between 0.39 and 0.48 cm3 g-1. With loading of Pt, Pt-SnOx/OMC with relatively low SnOx content exhibits superior electrocatalytic performance, long-term durability, and resistance to CO poisoning for methanol oxidation, as compared to Pt/OMC, PtRu/C and Pt-SnOx/C, which may be attributed not only to the synergetic effect of embedded SnOx, but also to the highly ordered mesostructure with high specific surface areas and large pore volumes affording plenty of surface area for support of Pt nanoparticles. This work supplies an efficient way to synthesize novel ordered mesoporous carbon self-supported metallic oxide as catalyst support and its further potential application to reduce the cost of catalysts in direct methanol fuel cells.

  1. Soft-Templated Self-Assembly of Mesoporous Anatase TiO2/Carbon Composite Nanospheres for High-Performance Lithium Ion Batteries.

    Science.gov (United States)

    Wu, Ruofei; Shen, Shuiyun; Xia, Guofeng; Zhu, Fengjuan; Lastoskie, Christian; Zhang, Junliang

    2016-08-10

    Mesoporous anatase TiO2/carbon composite nanospheres (designated as meso-ATCCNs) were successfully synthesized via a facile soft-templated self-assembly followed by thermal treatment. Structural and morphological analyses reveal that the as-synthesized meso-ATCCNs are composed of primary TiO2 nanoparticles (∼5 nm), combined with in situ deposited carbon either on the surface or between the primary TiO2 nanoparticles. When cycled in an extended voltage window from 0.01 to 3.0 V, meso-ATCCNs exhibit excellent rate capabilities (413.7, 289.7, and 206.8 mAh g(-1) at 200, 1000, and 3000 mA g(-1), respectively) as well as stable cyclability (90% capacity retention over 500 cycles at 1000 mA g(-1)). Compared with both mesoporous TiO2 nanospheres and bulk TiO2, the superior electrochemical performance of the meso-ATCCNs electrode could be ascribed to a synergetic effect induced by hierarchical structure that includes uniform TiO2 nanoparticles, the presence of hydrothermal carbon derived from phenolic resols, a high surface area, and open mesoporosity.

  2. Enhanced photocatalytic performance of mesoporous TiO{sub 2} coated SBA-15 nanocomposites fabricated through a novel approach: supercritical deposition aided by liquid-crystal template

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Chen; Lin, Xiao; Li, Youji, E-mail: bcclyj@163.com; Xu, Peng; Li, Ming; Chen, Feitai

    2016-03-15

    Highlights: • Highly uniform mesoporous TiO{sub 2} nanopartices were coated SBA-15. • MT showed smaller crystallite size, higher hydroxyl content and surface area. • MT/SBA-15 show enhanced photocatalytic activity and high reused activity. • The optimum MT loading rate and calcination temperature were obtained to be 15% and 400 °C, respectively. • Photocatalytic behaviors are discussed in terms of the Langmuir–Hinshelwood model. - Abstract: Mesoporous TiO2 coated SBA-15 (MT@S) nanocomposites were fabricated through supercritical CO{sub 2} deposition aided by liquid-crystal template. The as-prepared samples were characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, diffuse reflectance spectroscopy and so on. The results reveal that MT uniformly deposited onto silica with titania incorporated in SBA-15 channels, showed smaller crystallite size, higher hydroxyl content and surface area than nonporous TiO{sub 2} coated SBA-15 (NT@S) obtained by a similar route without template. With TiO{sub 2} loading ratio of 15 wt% and calcination temperature of 400 °C, 15%MT@S-400 showed the enhanced degradation efficiency for azo dyes (methylene blue, methyl orange, and rhodamine B) and phenol in comparsion with 15%NT@S-400, due to those improved textural and physicochemical properties. Meanwhile, the reused MT@S also showed high photoactivity. Additionally, the effects of MT content and calcination temperature have been examined as operational parameters. Photocatalytic reactions followed pseudo-first-order kinetics and are discussed in terms of the Langmuir–Hinshelwood model.

  3. Synthesis of mesoporous zeolite catalysts by in situ formation of carbon template over nickel nanoparticles

    DEFF Research Database (Denmark)

    Abildstrøm, Jacob Oskar; Kegnæs, Marina; Hytoft, Glen

    2016-01-01

    oxide, a carbon-silica composite is obtained and exploited as a combined carbon template/silica source for zeolite synthesis. This approach has several advantages in comparison with conventional carbon templating methods, where relatively complicated preparative strategies involving multistep...... impregnation procedures and rather expensive chemicals are used. Removal of the carbon template by combustion results in zeolite single crystals with intracrystalline pore volumes between 0.28 and 0.48 cm3/g. The prepared zeolites are characterized by XRD, SEM, TEM and physisorption analysis. The isomerization...

  4. Facile synthesis and application of a carbon foam with large mesopores

    KAUST Repository

    Fu, Liling

    2013-01-01

    By combining elements of hard- and soft-templating, a facile synthesis method for carbon foams with large mesopores has been demonstrated. A commercial Pluronic surfactant was used as the structure-directing agent as well as the carbon precursor. No micelle swelling agent or post treatment is necessary to enlarge mesopores. As such this method requires fewer synthesis steps and is highly scalable. The as-synthesized meso-carbons showed potential applications in the fields of carbon oxide capture and lithium-sulfur batteries. © 2013 the Owner Societies.

  5. The study of the relationship between pore structure and photocatalysis of mesoporous TiO2

    Indian Academy of Sciences (India)

    Bing Guo; Hangyan Shen; Kangying Shu; Yaowu Zeng; Wensheng Ning

    2009-05-01

    Mesoporous titania was synthesized by a sol-gel method using the surfactants Span85 and X114 as the template. The pore structure was determined by the N2 adsorption/desorption method below 73 K and calculated using the BJH model. TEM characterizations show that the pores are formed through particle accumulation. Two kinds of channels, straight channels made of cylindrical capillaries and curved channels made of slit-shaped pores, exist in the bulk materials. The influence of the pore structure of mesoporous TiO2 on its photocatalytic performance was studied. The sample with higher porosity, better textural properties and straight channels are good for photocatalytic performance.

  6. Synthesis and Characterization of Periodic Mesoporous Organosilicas as Anion-Exchance Resins for Perrhenate Adsorption.

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Byunghwan [Korea Institute of Industrial Technology, ChonAn, Korea; Im, Hee-Jung [ORNL; Luo, Huimin [ORNL; Hagaman, Edward {Ed} W [ORNL; Dai, Sheng [ORNL

    2005-01-01

    A new methodology to immobilize ionic liquids through the use of a bridged silsesquioxane N-(3-triethoxysilylpropyl), N(3)-3-trimethoxysilylpropyl-4,5-dihydroimidazolium iodide that incorporates an ionic functionality for the assembly of novel periodic mesoporous organosilica (PMO) materials has been developed. The resulting PMO materials were investigated for use as novel anion exchange resins for the separation of perrhenate anions in aqueous solution. As compared with cetyltrimethylammonium chloride, 1-hexadecane-3-methylimidazolium bromide has been demonstrated to be a more efficient surfactant template for the generation of mesopores and surface areas for such PMO materials.

  7. Dopamine functionalized tannic-acid-templated mesoporous silica nanoparticles as a new sorbent for the efficient removal of Cu2+ from aqueous solution

    Science.gov (United States)

    Gao, Junkai; Lei, Hao; Han, Zhi; Shi, Qian; Chen, Yan; Jiang, Yanjun

    2017-03-01

    A simple, environmentally friendly and cost-effective nonsurfactant template method was used to synthesize tannic-acid-templated mesoporous silica nanoparticles (TMSNs), and then dopamine functionalized TMSNs (Dop-TMSNs) which was synthesized by a facile and biomimetic coating strategy, was developed as a new sorbent for the removal of Cu2+ from aqueous solution. The Dop-TMSNs were thoroughly characterized by SEM, TEM, BET, FT-IR and TGA, and the effects of contact time, initial pH, K+ and Na+ concentrations, co-existing polyvalent metal ions and adsorption-desorption cycle times on the sorption capacity of Dop-TMSNs were studied. It was demonstrated that the maximum adsorption capacity of Cu2+ by Dop-TMSNs was 58.7 mg/g at pH 5.5, and the sorption reached equilibrium within 180 min. Moreover, the K+ and Na+ concentrations had a very slight influence on the sorption process and the adsorption capacity of the Dop-TMSNs still remained 89.2% after recycling for four times. All the results indicated that the Dop-TMSNs could be utilized as an excellent sorbent for the sequestration of Cu2+.

  8. Facile surfactant- and template-free synthesis and electrochemical properties of SnO{sub 2}/graphene composites

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jing, E-mail: xy13787103391@126.com [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Zhang, Xia, E-mail: zyx02090229@163.com [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Guo, Jianqiang; Peng, Rufang [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China); Xie, Ruishi [Analytical and Testing Center, Southwest University of Science and Technology, Mianyang 621010 (China); Huang, Yeju; Qi, Yongcheng [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010 (China)

    2016-07-25

    In this work, we demonstrate a facile and green hydrothermal process without using any surfactant or template to synthesize SnO{sub 2} nanoflowers (NFs)/graphene nanosheets (GNSs) composites as a high-performance electrode material for electric double layer capacitors (EDLCs). The crystal structure and morphology of the products were characterized by X-ray diffraction, scanning electron microscopy, and transition electron microscopy. The electrochemical properties were investigated by galvanostatic charge/discharge cycling and cycling voltammetry in a voltage range of −0.2–0.8 V. The results exhibit that the addition of GNSs did not change the tetragonal crystal structure of SnO{sub 2}, and the GNSs were successfully coated on the flower-like surface of SnO{sub 2}. The grain morphology of SnO{sub 2}@GNSs composites has a flower-like appearance suggesting excellent electrochemical properties which were confirmed by electrochemical techniques. Compared with the GNSs, the SnO{sub 2}@GNSs composites exhibit a high specific discharge capacitance of 126 F g{sup −1} at 0.2 A g{sup −1} and remains 98.2% after 2000 charge–discharge cycles. The combination of GNSs and SnO{sub 2} could significantly improve the electrical conductivity, enhance the interactions between GNSs and SnO{sub 2} NFs and provide more reaction sites, thereby resulting in improved electrochemical properties for the SnO{sub 2}@GNSs composites in contrast with the pristine GNSs sample. The high specific capacity and long stability make the SnO{sub 2}@GNSs nanocomposite as a electrode material for high-performance supercapacitors. - Highlights: • SnO{sub 2} nanoflowers (NFs)/Graphene nanosheets(GNSs) composites were prepared by a simple and rapid hydrothermal process. • The results show that the GNSs were homogeneously and tightly attached on the surface of SnO{sub 2} NFs. • The SnO{sub 2} NFs/GNSs composites electrode exhibited the enhanced capacitive performances than those of pure GNSs.

  9. Fabrication and characterization of mesoporous silica nanochannels inside the channels of anodic alumina membrane

    Directory of Open Access Journals (Sweden)

    Moataz M. Mekawy

    2016-03-01

    Full Text Available Brij type surfactants (CnEOx that have different chemical structures were used to fabricate 3D Mesoporous Silica Nanochannels (MSN inside the channels of Anodic Alumina Membrane (AAM under acidic conditions. The fabricated 3D MSN were characterized using TEM-ED, SEM, Small angle XRD, and N2 isotherm. Results revealed that the synthesis of ordered 3D cubic Im3m mesostructures can be formed with tunable pore diameters varied from 4.0 to 4.9 nm that are partially affected with the length of ethylene oxide (EO group in the template surfactant.

  10. Synthesis and characterization of surface-modified mesoporous silica materials with β-cyclodextrin

    Directory of Open Access Journals (Sweden)

    Sarker T. Mahmud

    2016-12-01

    Full Text Available Mesoporous silica materials containing microporous cavities provided by surface-bound β-cyclodextrin (CD ICS were synthesized by co-condensation of a β-CD-functionalized triethoxysilane (CD ICL with TEOS using dodecylamine, tetradecylamine, or hexadecylamine surfactants as structure directing agents. The incorporation of β-CD within the mesoporous framework was supported by IR, Raman, MALDI TOF MS, 13C solids CP-MAS NMR, and TGA results. Small-angle X-ray diffraction and nitrogen adsorption provide evidence of ordered silica mesostructured frameworks. For materials with similar CD loading, the textural properties (surface area and pore volume doubled as the surfactant changed from dodecylamine (C12 to hexadecylamine (C16. The textural properties decrease with CD loading (2 to 6%. The sorption capacity of gas phase polar and apolar species (nitrogen and methyl chloride varies along with the adsorption properties in aqueous solution toward p-nitrophenol according to the CD loading (2–6% and surfactant template employed. Along with gas adsorption of model compounds, the structural effects relate to the surfactant alkyl chain length due to the structure directing effects of the C12 to C16 surfactants. This study reveals the structural contribution of surface modification and framework incorporation of β-cyclodextrin with mesoporous silica framework materials.

  11. Characteristics and properties of a novel in situ method of synthesizing mesoporous TiO{sub 2} nanopowders by a simple coprecipitation process without adding surfactant

    Energy Technology Data Exchange (ETDEWEB)

    Yeh, Shang-Wei [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China); Department of Life Science, National University of Kaohsiung, 700 Kaohsiung University Road, Kaohsiung 811, Taiwan (China); Ko, Horng-Huey [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China); Chiang, Hsiu-Mei [Department of Cosmeceutics, China Medical University, 91 Hsueh-Shih Road, Taichung 40402, Taiwan (China); Chen, Yen-Ling, E-mail: yelichen@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China); Lee, Jian-Hong [Clean Energy and Eco-Technology Center, Industrial Technology Research Institute, 8 Gongyan Road, Tainan 734, Taiwan (China); Wen, Chiu-Ming [Department of Life Science, National University of Kaohsiung, 700 Kaohsiung University Road, Kaohsiung 811, Taiwan (China); Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80782, Taiwan (China)

    2014-11-15

    Highlights: • The TiO{sub 2} precursor powder contained anatase and 19.5% NH{sub 4}Cl. • Mesoporous anatase TiO{sub 2} nanopowders were successfully synthesized. • Uncalcined precursor powder contained the phases of type I NH{sub 4}Cl and anatase TiO{sub 2}. • Anatase size increases from 3.3 to 14.3 nm when calcined at 473–773 K for 2 h. • The average pore size between 3.80 and 14.0 nm when calcined between 473 and 773 K. - Abstract: In situ synthesis of mesoporous TiO{sub 2} nanopowders using titanium tetrachloride (TiCl{sub 4}) and NH{sub 4}OH as initial materials has been successfully fabricated by a coprecipitation process without the addition of surfactant. Characteristics and properties of the mesoporous TiO{sub 2} nanopowders were investigated using differential scanning calorimetry/thermogravimetry (DSC/TG), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) and Barrent–Joyner–Halenda (BJH) analyses, transmission electron microscopy (TEM), selected area electron diffraction (SAED) and high resolution TEM (HRTEM). The results of TG and XRD showed that the NH{sub 4}Cl decomposed between 513 and 673 K. XRD results showed that the anatase TiO{sub 2} only contained a single phase when the calcination temperature of the precursor powder was less than 673 K. Whereas phases of anatase and rutile TiO{sub 2} coexist after calcining at 773 K for 2 h. The crystalline size of the anatase and rutile TiO{sub 2} was 14.3 and 26.6 nm, respectively, when the precursor powder was calcined at 773 K for 2 h. The BET and BJH results showed a significant increase in surface area and pore volumes when the NH{sub 4}Cl was completely decomposed. The maximum values of BET specific surface area and volume were 172.8 m{sup 2}/g and 0.392 cm{sup 3}/g, respectively. The average pore sizes when calcination was at 473 and 773 K for 2 h were 3.8 and 14.0 nm, respectively.

  12. Hierarchical control of porous silica by pH adjustment: Alkyl polyamines as surfactants for bimodal silica synthesis and its carbon replica

    Science.gov (United States)

    Abellán, G.; Carrillo, A. I.; Linares, N.; Serrano, E.; García-Martínez, J.

    2009-08-01

    Bimodal macro-mesoporous silica networks have been prepared in a simple one-pot synthesis using an inexpensive tetramine surfactant and tetraethoxysilane as a silica precursor. These novel materials show high pore volumes and templated mesopores (average pore size 3.0 nm) embedded in 20 nm thick walls forming interparticle large meso/macropores. The judicious control of the pH during the silica formation allows for the precise control of the interparticle condensation, likely due to the change in the interaction between the tetramine surfactant and the silica precursors. Finally, a highly porous carbon replica with bimodal porosity was prepared by using the bimodal silica as a hard sacrificial template. The microstructure of the silica template was accurately transferred to the carbon material obtaining high surface areas (up to 1300 m 2 g -1) and total pore volumes ≥2 cm 3 g -1.

  13. Amphiphilic block-graft copolymer templates for organized mesoporous TiO2 films in dye-sensitized solar cells

    Science.gov (United States)

    Lim, Jung Yup; Lee, Chang Soo; Lee, Jung Min; Ahn, Joonmo; Cho, Hyung Hee; Kim, Jong Hak

    2016-01-01

    Amphiphilic block-graft copolymers composed of poly(styrene-b-butadiene-b-styrene) (SBS) backbone and poly(oxyethylene methacrylate) (POEM) side chains are synthesized and combined with hydrophilically preformed TiO2 (Pre-TiO2), which works as a structural binder as well as titania source. This results in the formation of crack free, 6-μm-thick, organized mesoporous TiO2 (OM-TiO2) films via one-step doctor-blading based on self-assembly of SBS-g-POEM as well as preferential interaction of POEM chains with Pre-TiO2. SBS-g-POEM with different numbers of ethylene oxide repeating units, SBS-g-POEM(500) and SBS-g-POEM(950), are used to form OM-TiO2(500) and OM-TiO2(950), respectively. The efficiencies of dye-sensitized solar cells (DSSCs) with a quasi-solid-state polymer electrolyte reach 5.7% and 5.8% at 100 mW/cm2 for OM-TiO2(500) and OM-TiO2(950), respectively. The surface area of OM-TiO2(950) was greater than that of OM-TiO2(500) but the light reflectance was lower in the former, which is responsible for similar efficiency. Both DSSCs exhibit much higher efficiency than one (4.8%) with randomly-organized particulate TiO2 (Ran-TiO2), which is attributed to the higher dye loading, reduced charge recombination and improved pore infiltration of OM-TiO2. When utilizing poly((1-(4-ethenylphenyl)methyl)-3-butyl-imidazolium iodide) (PEBII) and mesoporous TiO2 spheres as the solid electrolyte and the scattering layer, the efficiency increases up to 7.5%, one of the highest values for N719-based solid-state DSSCs.

  14. Visible-Light Degradation of Dyes and Phenols over Mesoporous Titania Prepared by Using Anthocyanin from Red Radish as Template

    OpenAIRE

    Zhiying Yan; Wenjuan Gong; Yongjuan Chen; Deliang Duan,; Junjie Li; Wei Wang; Jiaqiang Wang

    2014-01-01

    Heterogeneous photocatalysis is able to operate effectively to eliminate organic compounds from wastewater in the presence of semiconductor photocatalyst and a light source. Although photosensitization of titania by organic dyes is one of the conventional ways for visible-light utilization of titania, previous studies have not yet addressed the use of natural food coloring agents as templates in the synthesis of mesostructured materials, let alone the simultaneous achievement of highly crysta...

  15. SYNTHESIS AND CHARACTERIZATIONOF ORGANIC FUNCTIONALIZED MESOPOROUS SILICA AND EVALUATE THEIR ADSORPTIVE BEHAVIOR FOR REMOVAL OF METHYLENE BLUE FROM AQUEOUS SOLUTION

    OpenAIRE

    Sameer H. Kareem; Inaam H. Ali; M. G. Jalhoom

    2014-01-01

    Three Mesoporous Silica (MPS) with different functional groups were prepared by one-step synthesis based on the simultaneous hydrolysis and condensation of tetraethoxy silane with organo-silane in the presence of template surfactant Polydimethylsiloxane-Polyethyleneoxide (PDMS-PEO). The prepared materials were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric Analysis (TGA) and nitrogen adsorption-desorption experiments. The results indicate that the preparati...

  16. Soft-to-hard templating to well-dispersed N-doped mesoporous carbon nanospheres via one-pot carbon/silica source copolymerization

    Institute of Scientific and Technical Information of China (English)

    Qinglu Kong; Lingxia Zhang; Min Wang; Mengli Li; Heliang Yao; Jianlin Shi

    2016-01-01

    Here we report a new approach referred as "softto-hard templating" strategy via the copolymerization of carbon source (dopamine) and silica source (tetraethyl orthosilicate) for the synthesis of well dispersed N-doped mesoporous carbon nanospheres (MCNs),which exhibit high performance for electrochemical supercapacitor.This method overcomes the shortcoming of uncontrolled dispersity and complicated procedures of soft-or hard-tem-plating methods,respectively.Moreover,the synthesized MCNs feature enriched heteroatom N-doping and easy functionalization by noble-metal nanoparticles during the one-pot synthesis.All the above characters make the asprepared MCNs a promising platform in a variety of applications.To demonstrate the applicability of the synthesized nitrogen-doped MCNs,this material has been employed as an electrode for high-performance electrochemical supercapacitor,which shows a capacitance of 223 and 140 F/g at current densities of 0.5 and 10 A/g in 1 mol/L KOH electrolyte,respectively.

  17. Regenerated cellulose membrane as bio-template for in-situ growth of visible-light driven C-modified mesoporous titania.

    Science.gov (United States)

    Mohamed, Mohamad Azuwa; W Salleh, W N; Jaafar, Juhana; Mohd Hir, Zul Adlan; Rosmi, Mohamad Saufi; Abd Mutalib, Muhazri; Ismail, Ahmad Fauzi; Tanemura, Masaki

    2016-08-01

    Visible light driven C-doped mesoporous TiO2 (C-MTiO2) nanorods have been successfully synthesized through green, low cost, and facile approach by sol-gel bio-templating method using regenerated cellulose membrane (RCM) as nanoreactor. In this study, RCM was also responsible to provide in-situ carbon sources for resultant C-MTiO2 nanorods in acidified sol at low temperatures. The composition, crystallinity, surface area, morphological structure, and optical properties of C-MTiO2 nanorods, respectively, had been characterized using FTIR, XRD, N2 adsorption/desorption, TEM, UV-vis-NIR, and XPS spectroscopy. The results suggested that the growth of C-MTiO2 nanorods was promoted by the strong interaction between the hydroxyl groups of RCMs and titanium ion. Optical and XPS analysis confirmed that carbon presence in TiO2 nanorods were responsible for band-gap narrowing, which improved the visible light absorption capability. Photocatalytic activity measurements exhibited the capability of C-MTiO2 nanorods in degradation of methyl orange in aqueous solution, with 96.6% degradation percentage under visible light irradiation.

  18. Mesoporous metal oxide graphene nanocomposite materials

    Science.gov (United States)

    Liu, Jun; Aksay, Ilhan A.; Kou, Rong; Wang, Donghai

    2016-05-24

    A nanocomposite material formed of graphene and a mesoporous metal oxide having a demonstrated specific capacity of more than 200 F/g with particular utility when employed in supercapacitor applications. A method for making these nanocomposite materials by first forming a mixture of graphene, a surfactant, and a metal oxide precursor, precipitating the metal oxide precursor with the surfactant from the mixture to form a mesoporous metal oxide. The mesoporous metal oxide is then deposited onto a surface of the graphene.

  19. Mesoporous film of WO3-the "sunlight" assisted decomposition of surfactant in wastewater for voltammetric determination of Pb

    Science.gov (United States)

    Krasnodębska-Ostręga, Beata; Bielecka, Agnieszka; Biaduń, Ewa; Miecznikowski, Krzysztof

    2016-12-01

    In this paper we present the application of "sunlight" assisted digestion in the presence of WO3 to the decomposition of dissolved organic matter, using the anionic surfactant sodium dodecyl sulfate (SDS) and the nonionic surfactant (1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol (Triton™X-114) in natural water samples, prior to the determination of traces residues of lead by stripping voltammetry methods. The results of the study showed firstly that the preparation of reproducible WO3 layers characterized by high mechanical and chemical resistance was possible, and secondly that it was also possible to obtain a high efficiency of decomposition, equal in efficiency to that of the reference method, which was the hydrogen peroxide oxidation assisted by UV, with evaporation nearly to dryness. The developed procedure is suggested to be a no-reagents method for the decomposition of added SDS, leading to 100% recovery of added Pb (II). The anodic stripping voltammetric curves recorded in solution after 4 h irradiation with UV assisted by WO3 were repeatable and increased linearly with standard additions, but the data finally obtained were incorrect. The curves recorded in solution after "sunlight" assisted digestion in the presence of WO3 were repeatable, and increased linearly with an increasing of concentration of standard additions (100% recovery of Pb). In the case of a nonionic surfactant, the decomposition time is at least 6 h. The advantage of the proposed method is the fact that the digestion process does not need the addition of any chemicals for the complete decomposition of organic matter.

  20. Spindle-like mesoporous α-Fe₂O₃ anode material prepared from MOF template for high-rate lithium batteries.

    Science.gov (United States)

    Xu, Xiaodong; Cao, Ruiguo; Jeong, Sookyung; Cho, Jaephil

    2012-09-12

    Spindle-like porous α-Fe(2)O(3) was prepared from an iron-based metal organic framework (MOF) template. When tested as anode material for lithium batteries (LBs), this spindle-like porous α-Fe(2)O(3) shows greatly enhanced performance of Li storage. The particle with a length and width of ∼0.8 and ∼0.4 μm, respectively, was composed of clustered Fe(2)O(3) nanoparticles with sizes of <20 nm. The capacity of the porous α-Fe(2)O(3) retained 911 mAh g(-1) after 50 cycles at a rate of 0.2 C. Even when cycled at 10 C, comparable capacity of 424 mAh g(-1) could be achieved.

  1. One-pot, template- and surfactant-free solvothermal synthesis of high-crystalline Fe3O4 nanostructures with adjustable morphologies and high magnetization

    Science.gov (United States)

    Zong, Yan; Xin, Hongna; Zhang, Jiarui; Li, Xinghua; Feng, Juan; Deng, Xia; Sun, Yong; Zheng, Xinliang

    2017-02-01

    In the present study, high-crystalline and well-defined Fe3O4 nanostructures with tunable morphologies were fabricated through a facile one-pot solvothermal approach. The morphology, crystal structure and chemical compositions of the products were characterized at the nanoscale. X-ray diffraction and selected area electron diffraction patterns indicate that the products have a pure spinel phase without the presence of any other impurity. Based on the transmission electron microscope technology, shape evolution of the products were investigated. Several morphologies including irregular particles, clusters, hollow sphere and octahedrons can be obtained by only adjusting the amount of NaOH without using any surfactant. Magnetism investigations show that all the products perform ferromagnetic behavior with high saturation magnetization at room temperature, which mainly originates from their high crystalline nature and template-free fabrication process.

  2. Dual-mesoporous ZSM-5 zeolite with highly b-axis-oriented large mesopore channels for the production of benzoin ethyl ether.

    Science.gov (United States)

    Zhou, Xiaoxia; Chen, Hangrong; Zhu, Yan; Song, Yudian; Chen, Yu; Wang, Yongxia; Gong, Yun; Zhang, Guobin; Shu, Zhu; Cui, Xiangzhi; Zhao, Jinjin; Shi, Jianlin

    2013-07-22

    Dual-mesoporous ZSM-5 zeolite with highly b axis oriented large mesopores was synthesized by using nonionic copolymer F127 and cationic surfactant CTAB as co-templates. The product contains two types of mesopores--smaller wormlike ones of 3.3 nm in size and highly oriented larger ones of 30-50 nm in diameter along the b axis--and both of them interpenetrate throughout the zeolite crystals and interconnect with zeolite microporosity. The dual-mesoporous zeolite exhibits excellent catalytic performance in the condensation of benzaldehyde with ethanol and greater than 99 % selectivity for benzoin ethyl ether at room temperature, which can be ascribed to the zeolite lattice structure offering catalytically active sites and the hierarchical and oriented mesoporous structure providing fast access of reactants to these sites in the catalytic reaction. The excellent recyclability and high catalytic stability of the catalyst suggest prospective applications of such unique mesoporous zeolites in the chemical industry.

  3. Preparation of bicontinuous mesoporous silica and organosilica materials containing gold nanoparticles by co-synthesis method

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Byunghwan [Korea Institute of Industrial Technology, ChonAn, Korea; Zhu, Haoguo [ORNL; Zhang, Zongtao [ORNL; Overbury, Steven {Steve} H [ORNL; Dai, Sheng [ORNL

    2004-01-01

    Catalytic activities of gold strongly depend on its particle size. It is necessary to have homogeneous distributions of small gold nanoparticles with diameters between 2 and 5 nm for excellent catalytic activities. In this study, gold-containing mesoporous silica materials were prepared by a co-synthesis method. The essence of this sol-gel co-synthesis method is to combine together neutral surfactant template synthesis of mesoporous silica materials with the introduction of metal ions via bifunctional silane ligands, so that the formation of mesostructures and metal-ion doping occur simultaneously. The formation of gold nanoparticles with size less than 5 nm inside mesoporous materials (HMS, MSU, and PMO) has been achieved by this co-synthesis sol-gel process. In addition, the effects of post-treatments, such as calcination and reduction, on pore structures and nanoparticle size distributions were also investigated.

  4. Precursor Mediated Synthesis of Nanostructured Silicas: From Precursor-Surfactant Ion Pairs to Structured Materials

    Directory of Open Access Journals (Sweden)

    Peter Hesemann

    2014-04-01

    Full Text Available The synthesis of nanostructured anionic-surfactant-templated mesoporous silica (AMS recently appeared as a new strategy for the formation of nanostructured silica based materials. This method is based on the use of anionic surfactants together with a co-structure-directing agent (CSDA, mostly a silylated ammonium precursor. The presence of this CSDA is necessary in order to create ionic interactions between template and silica forming phases and to ensure sufficient affinity between the two phases. This synthetic strategy was for the first time applied in view of the synthesis of surface functionalized silica bearing ammonium groups and was then extended on the formation of materials functionalized with anionic carboxylate and bifunctional amine-carboxylate groups. In the field of silica hybrid materials, the “anionic templating” strategy has recently been applied for the synthesis of silica hybrid materials from cationic precursors. Starting from di- or oligosilylated imidazolium and ammonium precursors, only template directed hydrolysis-polycondensation reactions involving complementary anionic surfactants allowed accessing structured ionosilica hybrid materials. The mechanistic particularity of this approach resides in the formation of precursor-surfactant ion pairs in the hydrolysis-polycondensation mixture. This review gives a systematic overview over the various types of materials accessed from this cooperative ionic templating approach and highlights the high potential of this original strategy for the formation of nanostructured silica based materials which appears as a complementary strategy to conventional soft templating approaches.

  5. Solution-Stable Colloidal Gold Nanoparticles via Surfactant-Free, Hyperbranched Polyglycerol-b-polystyrene Unimolecular Templates.

    Science.gov (United States)

    Iocozzia, James; Lin, Zhiqun

    2016-07-19

    Hyperbranched polyglycerol-block-polystyrene copolymers, denoted HPG-b-PS, are synthesized and employed as a new and effective unimolecular template for synthesizing colloidal gold (Au) nanoparticles. The coordination of noble metal precursors with polyether within the inner HPG core and subsequent in situ reduction enables the formation of well-dispersed and stable PS-capped Au nanoparticles. The inner HPG core is produced via ring opening multibranching polymerization (ROMBP) and subsequently converted into atom transfer radical polymerization (ATRP) macroinitiators for the controlled growth of polystyrene (PS) arms possessing low polydispersity (PDI < 1.31). An initial investigation into the templating parameters of HPG-b-PS was undertaken by producing templates with different arm numbers (98 and 117) and different PS chain lengths (i.e., molecular weight = 3500-13400 g/mol). It was found that the PS chain length and solvent conditions affect the quality of the resulting PS-capped colloidal Au nanoparticles. This work demonstrates, for the first time, a simple, lower-cost approach for templating nonpolar solvent-soluble PS-capped Au nanoparticles on the order of 10-30 nm in diameter.

  6. A study of freezing-melting hysteresis of water in different porous materials. Part II: surfactant-templated silicas.

    Science.gov (United States)

    Petrov, Oleg; Furó, István

    2011-09-28

    The freezing-melting hysteresis of water in mesoporous silicas MCM-48, MCM-41 and SBA-16 has been studied by NMR cryoporometry. The hysteresis in MCM-48 was found to exhibit nearly parallel branches, matching type H1 hysteresis that had been observed earlier in controlled pore glass. The same type of hysteresis is observed in two of three different-sized MCM-41 under study (a pore diameter of 3.6 and 3 nm), superimposed with a secondary, extremely broad, type H3 hysteresis. No hysteresis was found in the smallest MCM-41 with a pore diameter hysteresis with the freezing branch being essentially steeper than the melting one, which is attributed to a pore blockage upon freezing, similar to what we observed earlier in Vycor porous glass. The data were analyzed using the model of curvature-dependent metastability of a solid phase upon melting; the validity of this model has been discussed.

  7. Synthesis and Characterization of Bimodal Mesoporous Silica

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xiaofang; GUO Cuili; WANG Xiaoli; WU Yuanyuan

    2012-01-01

    Mesoporous silica with controllable bimodal pore size distribution was synthesized with cetyltrimethylammonium bromide (CTAB) as chemical template for small mesopores and silica gel as physical template for large mesopores.The structure of synthesized samples were characterized by Fourier transform infrared (FT-IR) spectroscopy,X-ray diffraction (XRD),scanning electron microscopy (SEM),transmission electron microscopy (TEM) and N2 adsorption-desorption measurements.The experimental results show that bimodal mesoporous silica consists of small mesopores of about 3 nm and large mesopores of about 45 nm.The small mesopores which were formed on the external surface and pore walls of the silica gel had similar characters with those of MCM-41,while large mesopores were inherited from parent silica gel material.The pore size distribution of the synthesized silica can be adjusted by changing the relative content of TEOS and silica gel or the feeding sequence of silica gel and NH4OH.

  8. Electrochemical characterisation and anodic stripping voltammetry at mesoporous platinum rotating disc electrodes.

    Science.gov (United States)

    Lozano-Sanchez, Pablo; Elliott, Joanne M

    2008-02-01

    Using the technique of liquid crystal templating a rotating disc electrode (RDE) was modified with a high surface area mesoporous platinum film. The surface area of the electrode was characterised by acid voltammetry, and found to be very high (ca. 86 cm(2)). Acid characterisation of the electrode produced distorted voltammograms was interpreted as being due to the extremely large surface area which produced a combination of effects such as localised pH change within the pore environment and also ohmic drop effects. Acid voltammetry in the presence of two different types of surfactant, namely Tween 20 and Triton X-100, suggested antifouling properties associated with the mesoporous deposit. Further analysis of the modified electrode using a redox couple in solution showed typical RDE behaviour although extra capacitive currents were observed due to the large surface area of the electrode. The phenomenon of underpotential deposition was exploited for the purpose of anodic stripping voltammetry and results were compared with data collected for microelectrodes. Underpotential deposition of metal ions at the mesoporous RDE was found to be similar to that at conventional platinum electrodes and mesoporous microelectrodes although the rate of surface coverage was found to be slower at a mesoporous RDE. It was found that a mesoporous RDE forms a suitable system for quantification of silver ions in solution.

  9. Beyond Creation of Mesoporosity: The Advantages of Polymer-Based Dual-Function Templates for Fabricating Hierarchical Zeolites

    KAUST Repository

    Tian, Qiwei

    2016-02-05

    Direct synthesis of hierarchical zeolites currently relies on the use of surfactant-based templates to produce mesoporosity by the random stacking of 2D zeolite sheets or the agglomeration of tiny zeolite grains. The benefits of using nonsurfactant polymers as dual-function templates in the fabrication of hierarchical zeolites are demonstrated. First, the minimal intermolecular interactions of nonsurfactant polymers impose little interference on the crystallization of zeolites, favoring the formation of 3D continuous zeolite frameworks with a long-range order. Second, the mutual interpenetration of the polymer and the zeolite networks renders disordered but highly interconnected mesopores in zeolite crystals. These two factors allow for the synthesis of single-crystalline, mesoporous zeolites of varied compositions and framework types. A representative example, hierarchial aluminosilicate (meso-ZSM-5), has been carefully characterized. It has a unique branched fibrous structure, and far outperforms bulk aluminosilicate (ZSM-5) as a catalyst in two model reactions: conversion of methanol to aromatics and catalytic cracking of canola oil. Third, extra functional groups in the polymer template can be utilized to incorporate desired functionalities into hierarchical zeolites. Last and most importantly, polymer-based templates permit heterogeneous nucleation and growth of mesoporous zeolites on existing surfaces, forming a continuous zeolitic layer. In a proof-of-concept experiment, unprecedented core-shell-structured hierarchical zeolites are synthesized by coating mesoporous zeolites on the surfaces of bulk zeolites. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Stabilization of mesoporous nanocrystalline zirconia with Laponite

    Institute of Scientific and Technical Information of China (English)

    LIU Xinmei; YAN Zifeng; LU Gaoqing

    2005-01-01

    The mesoporous nanocrystalline zircoina was synthesized via solid state reaction--structure directing method in the presence of Laponite. The introduction of Laponite renders the higher thermal stability and lamellar track to the zirconia. Laponite acts as inhibitor for crystal growth and also hard template for the mesostructure. The role of Laponite is attributed to the interaction between the zirconia precursors and the nano-platelets of Laponite via the bridge of hydrophilic segments of surfactant. It results in the formation of Zr-O-Mg-O-Si frameworks in the direction of Laponite layer with the condensation of frameworks during the calcination process, which contributes the higher stability and lamellar structure to the nano-sized zirconia samples.

  11. Synthesis of mesoporous TiO(2-x)N(x) spheres by template free homogeneous co-precipitation method and their photo-catalytic activity under visible light illumination.

    Science.gov (United States)

    Parida, K M; Naik, Brundabana

    2009-05-01

    The article presents preparation, characterization and catalytic activity evaluation of an efficient nitrogen doped mesoporous titania sphere photo-catalyst for degradation of methylene blue (MB) and methyl orange (MO) under visible light illumination. Nitrogen doped titania was prepared by soft chemical route i.e. template free, slow and controlled homogeneous co-precipitation from titanium oxysulfate sulfuric acid complex hydrate, urea, ethanol and water. The molar composition of TiOSO(4) to urea was varied to prepare different atomic % nitrogen doped titania. Mesoporous anatase TiO(2-x)N(x) spheres with average crystallite size of 10 nm and formation of titanium oxynitride center were confirmed from HRTEM, XRD and XPS study. UV-vis DRS showed a strong absorption in the range of 400-500 nm which supports its use in visible spectrum of light. Nitrogen adsorption-desorption study supports the porous nature of the doped material. All the TiO(2-x)N(x) samples showed higher photo-catalytic activity than Degussa P(25) and undoped mesoporous titania. Sample containing around one atomic % nitrogen showed highest activity among the TiO(2-x)N(x) samples.

  12. Effect of sulfuric acid on textural properties and catalytic performance of ruthenium-containing ordered mesoporous carbon prepared via a direct RuCl3/SBA-15 hard templated method.

    Science.gov (United States)

    Lan, Guojun; Tang, Haodong; Liu, Huazhang; Ni, Jun; Li, Ying

    2014-09-01

    Ruthenium-containing ordered mesoporous carbon (Ru-OMC) catalysts with highly dispersed Ru nanoparticles semi-embedded in carbon framework were prepared via a direct RuCl3/SBA-15 hard templated method. The effect of sulfuric acid on the texture structure and catalytic performance of Ru-OMC were studied. The status of Ru nanoparticles and mesoporous structure of Ru-OMC catalysts were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), nitrogen sorption, scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM) and CO chemisorption techniques. The addition of appropriate amount of sulfuric acid is necessary to improve the ordered mesoporous structure of Ru-OMC catalysts. The framework of carbon structure shrinks with the increase in sulfur acid contents, which is proved by a slight decrease in surface area and increase in pore diameters for Ru-OMC with different sulfur contents. The turnover frequency (TOF) for Ru-OMC reaches the highest up to 3.98 s(-1) in benzene hydrogenation with optimized sulfur acid content of 0.08 mmol/g sucrose.

  13. The applications of 3D-hexagonal mesoporous SiO2 in proton exchange membranes of fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, B.; Tang, H.; Pan, M.; Chen, L.; Liang, C. [Wuhan Univ. of Technology, Wuhan (China). State Key Laboratory of Advanced Technology for Materials Synthesis and Processing

    2010-07-01

    The advantages of 3D hexagonal ordered mesoporous silica include a homogeneous ordered pore, a large surface area, narrow pore size distribution and excellent thermal stability. Hetropolyacids (HPAs) are high conductivity solid proton conductors that can be loaded onto the channel of mesoporous silica as a carrier for the proton exchange membrane of fuel cells. In this study, an ordered 3D hexagonal structure HPW/SiO{sub 2} nano composite materials was prepared using the sol-gel method with a nonionic surfactant (Brij-76) as the template. The HPW/SiO{sub 2} composite was characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM) and N2 adsorption-desorption. The study showed that the synthesis method can effectively make the HPW disperse uniformly in mesoporous framework, ensuring that the synthesized material has ordered mesoscopic structure. Impedance analysis revealed that the HPW/silica nano-materials have good proton conductivity without humidification at room temperature.

  14. Synthesis of IV-VI Transition Metal Carbide and Nitride Nanoparticles Using a Reactive Mesoporous Template for Electrochemical Hydrogen Evolution Reaction

    KAUST Repository

    Alhajri, Nawal Saad

    2016-01-01

    Interstitial carbides and nitrides of early transition metals in Groups IV-VI exhibit platinum-like behavior which makes them a promising candidate to replace noble metals in a wide variety of reactions. Most synthetic methods used to prepare these materials lead to bulk or micron size powder which limits their use in reactions in particular in catalytic applications. Attempts toward the production of transition metal carbide and nitride nanoparticles in a sustainable, simple and cheap manner have been rapidly increasing. In this thesis, a new approach was presented to prepare nano-scale transition metal carbides and nitrides of group IV-VI with a size as small as 3 nm through the reaction of transition metal precursor with mesoporous graphitic carbon nitride (mpg-C3N4) that not only provides confined spaces for nanoparticles formation but also acts as a chemical source of nitrogen and carbon. The produced nanoparticles were characterized by powder X-ray diffraction (XRD), temperature-programmed reaction with mass spectroscopy (MS), CHN elemental analyses, thermogravimetric analyses (TGA), nitrogen sorption, X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). The effects of the reaction temperature, the ratio of the transition metal precursor to the reactive template (mpg-C3N4), and the selection of the carrier gas (Ar, N2, and NH3) on the resultant crystal phases and structures were investigated. The results indicated that different tantalum phases with cubic structure, TaN, Ta2CN, and TaC, can be formed under a flow of nitrogen by changing the reaction temperatures. Two forms of tantalum nitride, namely TaN and Ta3N5, were selectively formed under N2 and NH3 flow, respectively. Significantly, the formation of TaC, Ta2CN, and TaN can be controlled by altering the weight ratio of the C3N4 template relative to the Ta precursor at 1573 K under a flow of nitrogen where high C3N4/Ta precursor ratio generally resulted in high carbide

  15. 软模法磁性有序介孔炭的合成与表征%Synthesis and characterization of magnetic ordered mesoporous carbon materials using soft templating method

    Institute of Scientific and Technical Information of China (English)

    王加; 林汉森; 王秀芳

    2012-01-01

    Magnetic ordered mesoporous carbon is synthesized through soft templating method by using triblock-copolymer Pluronic F127 as soft template,resorcinol-formaldehyde (RF) as carbon precursor and ferric nitrate as an iron source. HC1 is used as the catalyst for RF polymerization. The resultant materials are characterized by X-ray diffraction, N2 sorption and vibrating-sample magnetometer measurements. The results show that magnetic ordered mesoporous carbons are obtained when the Fe/R ratio is 0. 025. For those with Fe/R ratios greater than this value,the ordering,the BET surface area,pore volume and pore size decrease. N2 sorption isotherms of all the samples show representative type IV curves with HI hysteresis loops, which indicates a typical mesoporous material. Magnetic hysteresis loops show that the remanent magnetization of Fe/OMC samples increases with the increase of the content of Fe. This research can provide scientific proof for the optimized synthesis and application in magnetic separation for magnetic ordered mesoporous carbons.%以三嵌段共聚物为软模,间苯二酚-甲醛为炭前躯体,硝酸铁为铁源合成了磁性有序介孔炭,用XRD、氮气吸附、磁性测试等方法对样品进行表征.结果表明,当硝酸铁与间苯二酚摩尔比为0.025、0.05及0.10时得到的介孔炭具有有序性,随着铁质量分数的增加,有序性降低,比表面积、孔容都相应减小.基本磁化曲线结果表明,随着铁质量分数的增加,饱和磁化强度随之增加(0.01~0.10 emu/g),材料具有较好的磁性,容易从溶液中分离,表现出良好的分离性能.为磁性有序介孔炭的优化合成及磁性分离应用提供科学依据.

  16. Influence of Template Removal Methods on Mesoporous Silica Nanospheres%模板剂去除方法对介孔氧化硅纳米球的影响

    Institute of Scientific and Technical Information of China (English)

    徐虹; 李延报; 陆春华; 李东旭; 许仲梓

    2011-01-01

    Hexagonal ordered mesoporous silica nanospheres (MSN) with a diameter of 100 nm were obtained by using tetraethoxysilane (TEOS) as silica source and cetyltrimethylammonium bromide (CTAB) as the template under alkaline conditions of 2 M sodium hydroxide. The CTAB templates were removed by calcination at 550℃ and by reflux extraction using HCl/EtOH solution, respectively. Thermogravimetric analysis (TGA), small angle X-ray diffractometry (SAXRD), transmission electron microscopy (TEM) and nitrogen adsorption-desorption techniques were employed to investigate the residue of CTAB and mesoporous structure of MSN. The results indicate that templates can be removed completely by calcination but only about 80% templates can be removed by reflux extraction. The pore size and pore volume of MSN increase with increasing the extraction time and repeated times of extraction. MSN obtained by extraction for 6 h with 4 repeated times to remove templates has the largest surface area (944.31m2 · g-1), pore volume (1.89cm3 · g-1) and pore diameter (2. 56nm).%以十六烷基三甲基溴化铵(CTAB)为模板剂,正硅酸四乙酯(TEOS)为硅源,在碱性条件下反应,分别采用煅烧法和酸化乙醇回流萃取法去除氧化硅中的模板剂,获得了直径为1OOnm分布均匀的六方有序的介孔氧化硅纳米球(MSN).通过热失重分析(TGA)、透射电子显微镜(TEM)、小角度X射线衍射(SAXRD)和氮气吸附-脱附对MSN中CTAB的残余量和介孔结构进行了表征.结果表明:煅烧法能够彻底去除模板剂,萃取法只能去除80%左右的模板剂;随着萃取时间的延长和萃取次数的增加,MSN的孔径和孔容有所增加,其中6h回流萃取4次去除模板剂后得到的MSN的比表面积、孔容、孔径最大,分别为944.31m2·g-1、1.89cm3·g-1和2.56nm.

  17. Challenges and Strategies in the Synthesis of Mesoporous Alumina Powders and Hierarchical Alumina Monoliths

    Directory of Open Access Journals (Sweden)

    Anne Galarneau

    2012-02-01

    Full Text Available A new rapid, very simple and one-step sol-gel strategy for the large-scale preparation of highly porous γ-Al2O3 is presented. The resulting mesoporous alumina materials feature high surface areas (400 m2 g−1, large pore volumes (0.8 mL g−1 and the ��-Al2O3 phase is obtained at low temperature (500 °C. The main advantages and drawbacks of different preparations of mesoporous alumina materials exhibiting high specific surface areas and large pore volumes such as surfactant-nanostructured alumina, sol-gel methods and hierarchically macro-/mesoporous alumina monoliths have been analyzed and compared. The most reproducible synthesis of mesoporous alumina are given. Evaporation-Induced Self-Assembly (EISA is the sole method to lead to nanostructured mesoporous alumina by direct templating, but it is a difficult method to scale-up. Alumina featuring macro- and mesoporosity in monolithic shape is a very promising material for in flow applications; an optimized synthesis is described.

  18. 双模板结构导向剂制备有序介孔炭%Synthesis of ordered mesoporous carbon with dual templates as structure directing agents

    Institute of Scientific and Technical Information of China (English)

    张煜; 王同华; 米盼盼

    2012-01-01

    Ordered mesoporous carbons were prepared by pyrolysis of polymer blends, which were formed by the organic-organic self-assembly of resorcinol-formaldehyde pre-polymers and tri-block copolymers under acidic conditions. The tri-block copolymer mixtures of F127 and P123 were used as structure-directing agents. The samples were characterized by X-ray diffraction, transmission electron microscopy and nitrogen adsorption. Results show that the degree of order of mesoporous carbons exhibits a maximum with increasing holding time from 24 to 72 h. When the molar ratio of the F127 to PI 23 is 1, the mesoporous carbon obtained has the most ordered hexagonal mesostructure (P6mm), with a typical BET surface area of 640.34 mVg, pore size of 3.68 nm and pore volume of 0.59 cmVg.

  19. Poly(ethylene-co-acrylic acid)-g-poly(ethylene glycol) graft copolymer templated synthesis of mesoporous TiO{sub 2} thin films for quasi-solid-state dye sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Rajkumar; Jung, Ye Eun; Kim, Dong Jun; Kim, Sang Jin; Kim, Jong Hak, E-mail: jonghak@yonsei.ac.kr

    2014-02-03

    An amphiphilic graft copolymer, poly(ethylene-co-acrylic acid)-graft-poly(ethylene glycol) (PEAA-g-PEG), consisting of a PEAA backbone and PEG side chains was synthesized via an esterification reaction. {sup 1}H nuclear magnetic resonance and Fourier-transformed infrared analysis demonstrated esterification between carboxylic acid of PEAA and hydroxyl group of PEG. Small angle X-ray scattering results revealed that the crystalline domain spacing of PEAA increased from 11.3 to 12.8 nm upon using a more polar solvent with a higher affinity for poly(acrylic acid), while the crystalline domain spacing of PEAA disappeared with PEG grafting, indicating structural change to an amorphous state. Mesoporous TiO{sub 2} thin films were synthesized via a sol–gel reaction using PEAA-g-PEG graft copolymer as a structure-directing agent. The hydrophilically-preformed TiO{sub 2} nanoparticles were selectively confined in the hydrophilic PEG domains of the graft copolymer, and mesoporous TiO{sub 2} thin films were formed, as confirmed by scanning electron microscopy. The morphology of TiO{sub 2} films was tunable by varying the concentrations of polymer solutions and the amount of preformed TiO{sub 2}. A quasi-solid-state dye-sensitized solar cell fabricated with PEAA-g-PEG templated TiO{sub 2} film exhibited an energy conversion efficiency of 3.8% at 100 mW/cm{sup 2}, which was greater than that of commercially-available paste (2.6%) at a similar film thickness (3 μm). The improved performance was due to the larger surface area for high dye loading and organized structure with good interconnectivity. - Highlights: • Poly(ethylene-co-acrylic acid)-g-poly(ethylene glycol) (PEAA-g-PEG) graft copolymer is synthesized. • Amphiphilic PEAA-g-PEG acts as a structure directing agent. • Mesoporous TiO{sub 2} thin films are prepared by sol–gel reaction using PEAA-g-PEG template. • Efficiency of DSSC with templated TiO{sub 2} is greater than with commercial TiO{sub 2} paste.

  20. 非表面活性剂模板溶胶-凝胶法制备磁性介孔二氧化硅实现纤维二糖酶的原位固定%In Situ Encapsulation of Cellubiase Enzyme in Magnetic Mesoporous Silica via the Nonsurfactant-templated Sol-gel Method

    Institute of Scientific and Technical Information of China (English)

    张翔; 李书润; 翟文韬; 曹莹泽; 齐宏旭; 吉岩; 危岩

    2015-01-01

    以非表面活性剂为模板,通过引入磁性纳米颗粒,制备了磁性介孔硅材料,实现了纤维二糖酶的原位固定,得到了磁性固定化酶。制备流程操作简单、原料易得、使用方便。溶胶-凝胶反应在水相、常温、中性条件下进行,适用于工业化生产。对磁性固定化酶进行了气体吸附分析、热重分析、表面形貌分析和磁性表征。结果表明,磁性固定化酶具有较大的比表面积、较窄的介孔分布和软铁磁性。与非介孔固定化酶相比,磁性固定化酶表观酶活明显提高。磁性颗粒的引入对酶活性没有显著的影响,并且可以非常方便和快速地从反应系统中回收再利用,结合磁场的可控性,非表面活性剂模板溶胶-凝胶法有望实现固定化酶的大规模可控释放与回收。%Nonsurfactant-templated sol-gel method is an advanced technology for enzyme encapsulation. The immobilized enzyme can be reused many times, so that can reduce the cost. It has a broad application prospect in biological catalysis. D-fructose is used as non-surfactant template to generate mesopores. The average diameter of the mesoporous silica is 3. 2 nm. And they significantly improve the activity of the immobilized enzyme. The best result is 70% of free enzyme. On the other hand, the mesopores are smaller than the size of cellobiase enzyme. So the enzyme will not leach out. That can help avoiding enzyme leaching. The magnetic nanoparticles can make the separation and recycle of immobilized enzyme easier and more feasi-ble. The incorporation of magnetic nanoparticles has little effect on the enzyme activity. The magnetic encap-sulated enzyme can be easily recycled by magnet force. More than 83% remained after 10 cycles. The process is simple and biocompatible as the sol-gel reaction occurs inaqueous phase and neutral pH.

  1. Synthesis of an Ionic Liquid and Its Application as Template for the Preparation of Mesoporous Material MCM-41: A Comprehensive Experiment for Undergraduate Students

    Science.gov (United States)

    Hu, Jun; Yin, Jinxiang; Lin, Tianshu; Li, Guangtao

    2012-01-01

    A new solvent-free microwave experiment to synthesize the ionic liquid 1-hexadecyl-3-methylimidazolium bromide (HDMIm-Br) in high yield is presented. The structure is confirmed by IR and [superscript 1]H NMR spectra. HDMIm-Br is then used to prepare an organic-inorganic mesoporous material MCM-41. The microscopic arrangements of mesoporous…

  2. Crystalline mesoporous metal oxide

    Institute of Scientific and Technical Information of China (English)

    Wenbo Yue; Wuzong Zhou

    2008-01-01

    Since the discovery of many types of mesoporous silicas, such as SBA-15, KIT-6, FDU-12 and SBA-16, porous crystalline transition metal oxides, such as Cr2O3, Co3O4, In2O3, NiO, CeO2, WO3, Fe2O3 and MnO2, have been synthesized using the mesoporous silicas as hard templates. Several synthetic methods have been developed. These new porous materials have high potential applications in catalysis, Li-ion rechargeable batteries and gas sensors. This article gives a brief review of the research of porous crystals of metal oxides in the last four years.

  3. Periodic Mesoporous Organosilica Nanorice

    Directory of Open Access Journals (Sweden)

    Mohanty Paritosh

    2008-01-01

    Full Text Available Abstract A periodic mesoporous organosilica (PMO with nanorice morphology was successfully synthesized by a template assisted sol–gel method using a chain-type precursor. The PMO is composed of D and T sites in the ratio 1:2. The obtained mesoporous nanorice has a surface area of 753 m2 g−1, one-dimensional channels, and a narrow pore size distribution centered at 4.3 nm. The nanorice particles have a length of ca. 600 nm and width of ca. 200 nm.

  4. 以冰晶体为模板制备蒙脱石质介孔材料及表征%Structure Characteristics of Mesoporous Montmorillonite Made by Ice-template

    Institute of Scientific and Technical Information of China (English)

    杨魁; 杨长辉; 李贞

    2011-01-01

    Mesoporous sodium montmorillonite (Na-MMT) was made with ice template. The experimental results show that its mesoporous diameter are mainly distributed between 35nm and 45nm, its shapes are wedgy under con-troling the microgel concentration of Na-MMT from 1.8% to 2.1% and its particle sizes is in the rang of 0.15-0.6μm. The macro-morphology of microgel Na-MMT prepared by frozen drying are parallel assemble regularly. Na-MMT possesses the numerous maroporous and mesoporous characteristics in its interlayer simultaneously. The d(00l) distance of the Na-MMT increases from 1.238 nm to 1.901 nm, and the surface area increases from 16.5m2/g to 213.6m2/g.%探索了以冰晶体为模板制备钠基蒙脱石质(Na-MMT)介孔材料的可行性.当蒙脱石(MMT)微凝胶分散液的浓度控制在1.8%~2.1%范围,MMT微粒在0.15~0.60μm之间时,冻干后的MMT微粒呈层状分布,且具有宏观层状组装纹理.MMT多孔结构体系中存在着介孔结构,介孔孔径主要分布在35~45nm,介孔孔隙呈现出楔形特征.其晶胞层间距d(001)由1.238nm增至1.901nm,比表面积由原始的16.5m2/g增至213.6m2/g.

  5. Robust conductive mesoporous carbon-silica composite films with highly ordered and oriented orthorhombic structures from triblock-copolymer template co-assembly

    Energy Technology Data Exchange (ETDEWEB)

    Song, Lingyan; Feng, Dan; Campbell, Casey G; Gu, Dong; Forster, Aaron M; Yager, Kevin G; Fredin, Nathaniel; Lee, Hae-Jeong; Jones, Ronald L; Zhao, Dongyuan; Vogt, Bryan D [AZU

    2012-07-11

    In this work, we describe a facile approach to improve the robustness of conductive mesoporous carbon-based thin films by the addition of silica to the matrix through the triconstituent organic-inorganic-organic co-assembly of resol (carbon precursor) and tetraethylorthosilicate (silica precursor) with triblock-copolymer Pluronic F127. The pyrolysis of the resol-silica-pluronic F127 film yields a porous composite thin film with well-defined mesostructure. X-Ray diffraction (XRD), grazing incidence small angle X-ray scattering (GISAXS), and electron microscopy measurements indicate that the obtained carbon-based thin films have a highly ordered orthorhombic mesostructure (Fmmm) with uniform large pore size (~3 nm). The orthorhombic mesostructure is oriented and the (010) plane is parallel to the silicon wafer substrate. The addition of silica to the matrix impacts the pore size, surface area, porosity, modulus and conductivity. For composite films with approximately 40 wt% silica, the conductivity is decreased by approximately an order of magnitude in comparison to a pure carbon mesoporous film, but the conductivity is comparable to typical printed carbon inks used in electrochemical sensing, {approx}10 S cm-1. The mechanical properties of these mesoporous silica-carbon hybrid films are similar to the pure carbon analogs with a Young's modulus between 10 GPa and 15 GPa, but the material is significantly more porous. Moreover, the addition of silica to the matrix appears to improve the adhesion of the mesoporous film to a silicon wafer. These mesoporous silica-carbon composite films have appropriate characteristics for use in sensing applications.

  6. Water adsorption properties controlled by coating/filling ordered mesoporous silica inside cellulose membranes.

    Science.gov (United States)

    Kimura, Tatsuo

    2013-09-28

    Porous organic membranes have been utilized as hard templates not only for replication of porous macrostructures but also for fabrication of hierarchical porous solids through infiltration of precursor solutions in ordered mesoporous materials. However, such organic membranes are usually burned out as sacrificial skeletons by calcination. In addition, replicated macropores are too big to enhance properties due to inorganic oxide frameworks. In this study, when cellulose membranes were used as organic membranes, a coating/filling technology of ordered mesoporous silicas was proposed and the water adsorption-desorption properties were directly investigated by using the composite membranes after extraction of nonionic surfactants used. The composite membranes possessed enough adsorption capacity for water, which will be potentially useful for improving total energy efficiency in heat-pump and desiccant air conditioning systems.

  7. Synthesis and Characterization of Nanoporous Carbon Materials; The Effect of Surfactant Concentrations and Salts

    Directory of Open Access Journals (Sweden)

    Shokoofeh Geranmayeh

    2011-01-01

    Full Text Available Nanoporous carbon framework was synthesized using phenol and formaldehyde as carbon precursors and triblock copolymer (pluronic F127 as soft template via evaporation induced self-assembly. Hexagonal mesoporous carbon with specific surface area of 350 m2/g through optimizing the situation was obtained. The effects of different surfactant/phenol molar ratio and presence of salts on specific surface area, pore size and pore volume for all the prepared samples were studied by means of the Brunauer-Emmett-Teller (BET formalism, powder X-ray diffraction technique and FT-IR spectroscopy.

  8. Dendrimer-surfactant interactions.

    Science.gov (United States)

    Cheng, Yiyun; Zhao, Libo; Li, Tianfu

    2014-04-28

    In this article, we reviewed the interactions between dendrimers and surfactants with particular focus on the interaction mechanisms and physicochemical properties of the yielding dendrimer-surfactant aggregates. In order to provide insight into the behavior of dendrimers in biological systems, the interactions of dendrimers with bio-surfactants such as phospholipids in bulk solutions, in solid-supported bilayers and at the interface of phases or solid-states were discussed. Applications of the dendrimer-surfactant aggregates as templates to guide the synthesis of nanoparticles and in drug or gene delivery were also mentioned.

  9. Removal of Copper-phthalocyanine from Aqueous Solution by Cationically Templated MCM-41 and MCM-48 Nanoporous Adsorbents

    Institute of Scientific and Technical Information of China (English)

    ANBIA Mansoor; MOHAMMADI Kaveh

    2008-01-01

    The effect of cationic template on the adsorption of copper-phthalocyanine-3,4',4",4'"-tetrasulfonic acid tetra-sodium salt [Cu(tsPc)-4·4Na+] in MCM-41 and MCM-48 mesoporous materials was investigated,using cetyl-trimethylammonium bromide(CTAB)as the cationic template and tetraethyl-orthosilicate as the silica source for synthesis of mesoporous materials.The properties of synthesized samples were characterized with XRD-Iow angle and scanning electron microscopy.The as-synthesized mesoporous samples were used for the separation of Cu(tsPc)tion speed,contact time,composition of adsorbents(presence or absence of surfactants)and initial analyte concen-trations.Adsorption uptakes were rapid on the adsorbents reaching equilibrium in 1/5 h for MCM-48 and 2 h for MCM-41.The materials showed excellent adsorption capacity toward copper-phthalocyanine anion(300.5 mg/g of Cu(tsPc)-4 for as-MCM48 and 285.5 mg/g for as-MCM-41).The materials without surfactant did not show signifi-cant affinity for analyte.Dominant sorption mechanisms were interactions including electrostatic,hydrophobicity,hydrogen bonding and π-π interactions.

  10. Hierarchical Mesoporous Lithium-Rich Li[Li0.2Ni0.2Mn0.6]O2 Cathode Material Synthesized via Ice Templating for Lithium-Ion Battery.

    Science.gov (United States)

    Li, Yu; Wu, Chuan; Bai, Ying; Liu, Lu; Wang, Hui; Wu, Feng; Zhang, Na; Zou, Yufeng

    2016-07-27

    Tuning hierarchical micro/nanostructure of electrode materials is a sought-after means to reinforce their electrochemical performance in the energy storage field. Herein, we introduce a type of hierarchical mesoporous Li[Li0.2Ni0.2Mn0.6]O2 microsphere composed of nanoparticles synthesized via an ice templating combined coprecipitation strategy. It is a low-cost, eco-friendly, and easily operated method using ice as a template to control material with homogeneous morphology and rich porous channels. The as-prepared material exhibits remarkably enhanced electrochemical performances with higher capacity, more excellent cycling stability and more superior rate property, compared with the sample prepared by conventional coprecipitation method. It has satisfactory initial discharge capacities of 280.1 mAh g(-1) at 0.1 C, 207.1 mAh g(-1) at 2 C, and 152.4 mAh g(-1) at 5 C, as well as good cycle performance. The enhanced electrochemical performance can be ascribed to the stable hierarchical microsized structure and the improved lithium-ion diffusion kinetics from the highly porous structure.

  11. Synthesis of ordered mesoporous U{sub 3}O{sub 8} by a nanocasting route

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Ran; Wang, Lin; Gu, Zhan-Jun; Yuan, Li-Yong; Xiao, Cheng-Liang; Zhao, Yu-Liang; Shi, Wei-Qun [Institute of High Energy Physics, Beijing (China). Key Laboratory of Nuclear Radiation and Nuclear Energy Technology; Chai, Zhi-Fang [Institute of High Energy Physics, Beijing (China). Key Laboratory of Nuclear Radiation and Nuclear Energy Technology; Soochow Univ., Suzhou (China). School of Radiological and Interdisciplinary Sciences

    2014-11-01

    Ordered mesoporous U{sub 3}O{sub 8} has been synthesized by a nanocasting route using mesoporous silica (KIT-6 and SBA-15) as templates and characterized by using XRD, SEM and nitrogen adsorption/desorption techniques.

  12. Influence of the preparation method on the morphology of templated NiCo{sub 2}O{sub 4} spinel

    Energy Technology Data Exchange (ETDEWEB)

    Cabo, Moises; Pellicer, Eva, E-mail: eva.pellicer.icn@uab.cat; Rossinyol, Emma; Solsona, Pau [Universitat Autonoma de Barcelona, Departament de Fisica, Facultat de Ciencies (Spain); Castell, Onofre [Universitat Autonoma de Barcelona, Servei de Microscopia, Facultat de Ciencies (Spain); Surinach, Santiago; Baro, Maria Dolors [Universitat Autonoma de Barcelona, Departament de Fisica, Facultat de Ciencies (Spain)

    2011-09-15

    The synthesis of NiCo{sub 2}O{sub 4} spinel by several nanocasting strategies (i.e., multi-step nanocasting, one-step nanocasting and soft-templating), in which nickel and cobalt nitrates are used as precursors and Pluronic P123 as surfactant, is explored. First, in the multi-step nanocasting, the effect of the impregnation method (evaporation, solid-liquid and two-solvent) of the SBA-15 silica template on the morphology of NiCo{sub 2}O{sub 4} replica is investigated. The evaporation method seems to be the best choice to obtain mesoporous NiCo{sub 2}O{sub 4} powder which, after calcination at 375 Degree-Sign C and subsequent template removal, displays the highest surface area (93.1 m{sup 2}/g). We have also checked the feasibility of the one-step nanoscating approach for the synthesis of ordered NiCo{sub 2}O{sub 4} arrays, though this methodology entails severe difficulties, mainly related to the different decomposition temperature of the nitrate precursors and the P123 surfactant. Finally, randomly oriented, aggregated NiCo{sub 2}O{sub 4} nanoparticles are obtained by means of P123 surfactant-assisted soft-templating approach.

  13. Synthesis of 5-hydroxymethylfurural from carbohydrates using large-pore mesoporous tin phosphate.

    Science.gov (United States)

    Dutta, Arghya; Gupta, Dinesh; Patra, Astam K; Saha, Basudeb; Bhaumik, Asim

    2014-03-01

    A large-pore mesoporous tin phosphate (LPSnP-1) material has been synthesized hydrothermally by using Pluronic P123 as the structure-directing agent. The material is composed of aggregated nanoparticles of 10-15 nm in diameter and has a BET surface area of 216 m(2)  g(-1) with an average pore diameter of 10.4 nm. This pore diameter is twice as large as that of mesoporous tin phosphate materials synthesized through the surfactant-templating pathways reported previously. LPSnP-1 shows excellent catalytic activity for the conversion of fructose, glucose, sucrose, cellobiose, and cellulose to 5-hydroxymethylfurfural (HMF) in a water/methyl isobutyl ketone biphasic solvent to give maximum yields of HMF of 77, 50, 51, 39, and 32 mol %, respectively, under microwave-assisted heating at 423 K. Under comparable reaction conditions, LPSnP-1 gives 12 % more HMF yield than a small-pore mesoporous tin phosphate catalyst that has an identical framework composition. This confirms the beneficial role of large mesopores and nanoscale particle morphology in catalytic reactions that involve bulky natural carbohydrate molecules.

  14. Hydrogen Bonding-Mediated Microphase Separation during the Formation of Mesoporous Novolac-Type Phenolic Resin Templated by the Triblock Copolymer, PEO-b-PPO-b-PEO

    Directory of Open Access Journals (Sweden)

    Wei-Cheng Chu

    2013-11-01

    Full Text Available After blending the triblock copolymer, poly(ethylene oxide-b-propylene oxide-b-ethylene oxide (PEO-b-PPO-b-PEO with novolac-type phenolic resin, Fourier transform infrared spectroscopy revealed that the ether groups of the PEO block were stronger hydrogen bond acceptors for the OH groups of phenolic resin than were the ether groups of the PPO block. Thermal curing with hexamethylenetetramine as the curing agent resulted in the triblock copolymer being incorporated into the phenolic resin, forming a nanostructure through a mechanism involving reaction-induced microphase separation. Mild pyrolysis conditions led to the removal of the PEO-b-PPO-b-PEO triblock copolymer and formation of mesoporous phenolic resin. This approach provided a variety of composition-dependent nanostructures, including disordered wormlike, body-centered-cubic spherical and disorder micelles. The regular mesoporous novolac-type phenolic resin was formed only at a phenolic content of 40–60 wt %, the result of an intriguing balance of hydrogen bonding interactions among the phenolic resin and the PEO and PPO segments of the triblock copolymer.

  15. 双功能性离子液体溶胶-凝胶法制备介孔SiO2%Bifunctional ionic liquid as template in the preparation of mesoporous silica via a sol-gel method

    Institute of Scientific and Technical Information of China (English)

    葛倪林; 张迪; 魏海兵; 丁运生

    2014-01-01

    首先合成了一种新型双功能性离子液体1-甲基-3-(3′-磺酸丙基)咪唑十二烷基磺酸盐([PMIM(SO3H)][C12SO3]),并采用FT-IR、1HNMR和13CNMR对其结构进行了表征;进一步以该离子液体为模板剂和酸源,以正硅酸乙酯(TEOS)为硅源,通过溶胶-凝胶法制备出介孔SiO2,利用TGA和FT-IR研究了介孔材料的形成过程,采用SAXRD、SEM、TEM和氮气等温吸附-脱附等手段对介孔材料的结构形貌进行了表征,并研究了其对Pb2+的吸附性能。结果显示,以[PMIM(SO3H)][C12SO3]为模板剂和酸源制备的介孔SiO2其比表面积、孔容、平均孔径大小分别为1010m2/g、0.95cm3/g、3.25nm,其对重金属Pb2+有很好的吸附性能。%A novel bifunctional ionic liquid 1-methyl-3-(3-sulfopropyl )-imidazolium n-dodecayl sulfonate ([PMIM(SO3 H)][C12 SO3 ])was conveniently synthesized,and the structure was determined by FT-IR,1 H NMR and 13 C NMR,respectively.Furthermore,mesoporous silica was prepared from ethyl silicate (TEOS)as silica source and the obtained ionic liquid as acid source and template by traditional sol-gel methods.The forma-tion of the mesoporous material was characterized by TGA and FT-IR.Several methods such as SAXRD,SEM, TEM and nitrogen adsorption-desorption isotherms were employed to characterized the morphological structure and properties of mesoporous silica.The experiment on Pb2+,one kind of heavy metal ion,adsorption was ap-plied so as to detect the property of the material.The resultant mesoporous silica material exhibited the specific surface area of 1 010 m2/g,the pore volume of 0.95 cm3/g and the average pore diameter size of 3.25 nm,re-spectively,while the mesoporous silica has a good adsorption property for heavy metal ion of Pb2+.

  16. Emulsion of aqueous-based nonspherical droplets in aqueous solutions by single-chain surfactants: templated assembly by nonamphiphilic lyotropic liquid crystals in water.

    Science.gov (United States)

    Varghese, Nisha; Shetye, Gauri S; Bandyopadhyay, Debjyoti; Gobalasingham, Nemal; Seo, JinAm; Wang, Jo-Han; Theiler, Barbara; Luk, Yan-Yeung

    2012-07-24

    Single-chain surfactants usually emulsify and stabilize oily substances into droplets in an aqueous solution. Here, we report a coassembly system, in which single types of anionic or non-ionic surfactants emulsify a class of water-soluble nonamphiphilic organic salts with fused aromatic rings in aqueous solutions. The nonamphiphilic organic salts are in turn promoted to form droplets of water-based liquid crystals (chromonic liquid crystals) encapsulated by single-chain surfactants. The droplets, stabilized against coalescence by encapsulated in a layer (or layers) of single chain surfactants, are of both nonspherical tactoid (elongated ellipsoid with pointy ends) and spherical shapes. The tactoids have an average long axis of ∼9 μm and a short axis of ∼3.5 μm with the liquid crystal aligning parallel to the droplet surface. The spherical droplets are 5-10 μm in diameter and have the liquid crystal aligning perpendicular to the droplet surface and a point defect in the center. Cationic and zwitterionic surfactants studied in this work did not promote the organic salt to form droplets. These results illustrate the complex interplay of self-association and thermodynamic incompatibility of molecules in water, which can cause new assembly behavior, including potential formation of vesicles or other assemblies, from surfactants that usually form only micelles. These unprecedented tactoidal shaped droplets also provide potential for the fabrication of new soft organic microcapsules.

  17. 模板法制备介孔VN纳米电极材料及其电容性能%Template Synthesis of Mesoporous Nanocrystalline VN Electrode Materials and Its Supercapacitive Behavior

    Institute of Scientific and Technical Information of China (English)

    高兆辉; 张浩; 曹高萍; 韩敏芳; 杨裕生

    2012-01-01

    Using hexadecyl trimethyl ammonium bromide (CTAB) as the template, mesoporous VN nanocrystalline was synthesized by NH3 reduction of precursor V2O5. The structure and surface morphology of mesoporous VN were characterized by XRD and TEM. Specific area and pore size distribution were studied by N2 absorption. The XRD result indicated that VN nanocrystalline belonged to the cubic crystal system. VN nanoparticles were in dimension of about 10 nm. N2 absorption result indicated that the surface area of VN sample was 88 m2/g, and most pores were distributed in the range of 2-6 nm. The supercapacitive behavior of VN electrode in 1 mol/L KOH electrolyte was studied by cyclic voltammetry (CV) and constant current charge-discharge measurements. The results showed that mesoporous VN electrode had both electrical double-layer capacitive properties and redox pseudoca-pacitive properties. The specific capacitance was of VN electrode 517 F/g at 1 mV/s scan rate, when the scan rate was up to 10 mV/s, its specific capacitance maintained 275 F/g.%以十六烷基三甲基溴化铵(CTAB)为模板剂,通过高温氨解还原V2O5前驱体制得了具有丰富介孔的VN纳米材料,采用XRD与TEM分析观察样品的结构和形貌,用N2吸附测试样品的比表面积和孔径分布.XRD分析表明,介孔VN纳米材料属于立方晶系的晶体结构.TEM和N2吸附测试结果表明,VN纳米材料的颗粒粒径大约为10 nm,比表面积为88 m2/g,有比较丰富的2~6 nm的介孔.在1 mol/L KOH电解液中进行循环伏安和恒流充放电测试研究其电容性能,结果显示,VN电极同时具有双电层电容性能和氧化-还原反应的准电容性能,1 mV/s的扫描速率下能获得517 F/g的比电容;当扫描速率增大到10 mV/s时,其比电容仍有275F/g.

  18. Mesoporous ethanesilica materials with bimodal and trimodal pore-size distributions synthesised in the presence of cobalt ions

    Directory of Open Access Journals (Sweden)

    Alufelwi M. Tshavhungwe

    2010-07-01

    Full Text Available Mesoporous organosilica materials containing ethane groups in their framework were formed with two and three pore sizes (i.e. bimodal and trimodal pores when synthesised by the sol-gel method in the presence of cobalt ions. The compounds 1,2-bistrimethoxysilylethane and tetraethylorthosilicate were used as silicon sources and the reactions were done in the presence of a surfactant, which served as a template. Diffuse reflectance infrared Fourier transform spectroscopy revealed that organic functional groups were incorporated into the ethanesilica. Powder X-ray diffraction and nitrogen adsorption data indicated that the mesophase and textural properties (surface area, pore volume, pore diameter of the materials were dependent on the ageing temperature, the amount/ratio of silica precursors and cobalt ion incorporation. Secondary mesopores were drastically reduced by changing the ratio of silicon precursors.

  19. TOWARDS A NEW CLASS OF MESOPOROUS MATERIALS FOR APPLICATIONS IN PETROLEUM REFINING

    Energy Technology Data Exchange (ETDEWEB)

    Conrad Ingram; Mark Mitchell

    2005-03-21

    This project focuses on the synthesis of mesoporous aluminophosphates, silicates and aluminosilicates as catalysts for applications in the conversion of large petroleum feedstock compounds to useful middle distillates and naphtha transportation fuels. Summarized herein is our research progress from September 1, 2003, to August 31, 2004. In previous reports it was demonstrated that mesoporous aluminophosphates with neutral framework (containing Al, P and O) could be synthesized, but their thermal stabilities were limited. In general, the materials' pore structure collapsed when calcined at 500-550 C in air or extracted in ethanol/HCl mixture to remove the surfactants, which were used as synthesis templates. New methods to improve the thermal stability of the materials needed to be explored. It was conceived that by adding divalent metals cations, such as Mg and Co, not only that the acid sites would be created by balancing the negatively charged framework (balanced by H{sup +}), but the thermal stability of the materials would be improved. In addition, methods to facilitate the interaction of hydrocarbon substrates with acid sites within the mesoporous are also needed. One concept towards improving this was to incorporate organic functional groups within or attached to the otherwise purely inorganic aluminophosphate (containing Co or Mg) or aluminosilicate pore walls of the mesopores. In the last report we detailed that mesoporous organosilicates were synthesized using block copolymer under acid conditions containing silica and phenylene (-C{sub 6}H{sub 4}-). Materials prepared with phenylene group among the silica pore walls was found to be thermally stable up to 550 C which is almost 100 C higher than the temperature used for the mild hydrocracking of petroleum. It was also highlighted that this area was the subject of recent intense research activities by other researchers. Building on precedence of the last report and on the results of other researchers, we

  20. Poly(ethylene oxide)-poly(butylene oxide)-poly(ethylene oxide)-templated synthesis of mesoporous alumina: effect of triblock copolymer and acid concentration.

    Science.gov (United States)

    Materna, Kelly L; Grant, Stacy M; Jaroniec, Mietek

    2012-07-25

    Mesoporous alumina was synthesized via a one-pot self-assembly of aluminum isopropoxide and poly(ethylene oxide)-poly(butylene oxide)-poly(ethylene oxide) triblock copolymer in an acidic ethanol solution. The effects of the polymer concentration and nitric acid concentration, independently, on the adsorption properties (such as surface area, pore volume, microporosity, mesoporosity, and pore width) were studied. An increase in the specific surface area and the pore volume was seen for the samples containing a polymer/aluminum isopropoxide wt. ratio up to 0.71 and a polymer/acid wt ratio of 0.88. Titania isopropoxide was also added to the synthesis to illustrate the extension of this approach to alumina-based mixed metal oxides.

  1. Mesostructured Metal Germanium Sulfide and Selenide Materials Based on the Tetrahedral [Ge 4S 10] 4- and [Ge 4Se 10] 4- Units: Surfactant Templated Three-Dimensional Disordered Frameworks Perforated with Worm Holes

    Science.gov (United States)

    Wachhold, Michael; Kasthuri Rangan, K.; Lei, Ming; Thorpe, M. F.; Billinge, Simon J. L.; Petkov, Valeri; Heising, Joy; Kanatzidis, Mercouri G.

    2000-06-01

    The polymerization of [Ge4S10]4- and [Ge4Se10]4- unit clusters with the divalent metal ions Zn2+, Cd2+, Hg2+, Ni2+, and Co2+ in the presence of various surfactant cations leads to novel mesostructured phases. The surfactants are the quaternary ammonium salts C12H25NMe3Br, C14H29NMe3Br, C16H33NMe3Br, and C18H37NMe3Br, which play the role of templates, helping to assemble a three-dimensional mesostructured metal-germanium chalcogenide framework. These materials are stoichiometric in nature and have the formula of (R-NMe3)2[MGe4Q10] (Q=S, Se). The local atomic structure was probed by X-ray diffuse scattering and pair distribution function analysis methods and indicates that the adamantane clusters stay intact while the linking metal atoms possess a tetrahedral coordination environment. A model can be derived, from the comparison of measured and simulated X-ray powder diffraction patterns, describing the structure as an amorphous three-dimensional framework consisting of adamantane [Ge4Q10]4- units that are bridged by tetrahedral coordinated M2+ cations. The network structures used in the simulations were derived from corresponding disordered structures developed for amorphous silicon. The frameworks in (R-NMe3)2[MGe4Q10] are perforated with worm hole-like tunnels, occupied by the surfactant cations, which show no long-range order. This motif is supported by transmission electron microscopy images of these materials. The pore sizes of these channels were estimated to lie in the range of 20-30 Å, depending on the appointed surfactant cation length. The framework wall thickness of ca. 10 Å is thereby independent from the surfactant molecules used. Up to 80% of the surfactant molecules can be removed by thermal degradation under vacuum without loss of mesostructural integrity. Physical, chemical, and spectroscopic properties of these materials are discussed.

  2. Metathesis depolymerizable surfactants

    Science.gov (United States)

    Jamison, Gregory M.; Wheeler, David R.; Loy, Douglas A.; Simmons, Blake A.; Long, Timothy M.; McElhanon, James R.; Rahimian, Kamyar; Staiger, Chad L.

    2008-04-15

    A class of surfactant molecules whose structure includes regularly spaced unsaturation in the tail group and thus, can be readily decomposed by ring-closing metathesis, and particularly by the action of a transition metal catalyst, to form small molecule products. These small molecules are designed to have increased volatility and/or enhanced solubility as compared to the original surfactant molecule and are thus easily removed by solvent extraction or vacuum extraction at low temperature. By producing easily removable decomposition products, the surfactant molecules become particularly desirable as template structures for preparing meso- and microstructural materials with tailored properties.

  3. Ordered mesoporous MFe(2)O(4) (M = Co, Cu, Mg, Ni, Zn) thin films with nanocrystalline walls, uniform 16 nm diameter pores and high thermal stability: template-directed synthesis and characterization of redox active trevorite.

    Science.gov (United States)

    Haetge, Jan; Suchomski, Christian; Brezesinski, Torsten

    2010-12-20

    In this paper, we report on ordered mesoporous NiFe(2)O(4) thin films synthesized via co-assembly of hydrated ferric nitrate and nickel chloride with an amphiphilic diblock copolymer, referred to as KLE. We establish that the NiFe(2)O(4) samples are highly crystalline after calcination at 600 °C, and that the conversion of the amorphous inorganic framework comes at little cost to the ordering of the high quality cubic network of pores averaging 16 nm in diameter. We further show that the synthesis method employed in this work can be readily extended to other ferrites, such as CoFe(2)O(4), CuFe(2)O(4), MgFe(2)O(4), and ZnFe(2)O(4), which could pave the way for innovative device design. While this article focuses on the self-assembly and characterization of these materials using various state-of-the-art techniques, including electron microscopy, grazing incidence small-angle X-ray scattering (GISAXS), time-of-flight secondary ion mass spectrometry (TOF-SIMS), X-ray photoelectron spectroscopy (XPS), as well as UV-vis and Raman spectroscopy, we also examine the electrochemical properties and show the benefits of combining a continuous mesoporosity with nanocrystalline films. KLE-templated NiFe(2)O(4) electrodes exhibit reasonable levels of lithium ion storage at short charging times which stem from facile pseudocapacitance.

  4. Templated Growth of Carbon Nanotubes

    Science.gov (United States)

    Siochik Emilie J. (Inventor)

    2007-01-01

    A method of growing carbon nanotubes uses a synthesized mesoporous si lica template with approximately cylindrical pores being formed there in. The surfaces of the pores are coated with a carbon nanotube precu rsor, and the template with the surfaces of the pores so-coated is th en heated until the carbon nanotube precursor in each pore is convert ed to a carbon nanotube.

  5. 一种松香基双季铵盐和CTAB共混模板介孔SiO2的制备%Preparation of mesoporous silica using a rosin-based bis-quaternary ammonium salt and CTAB as the blend template

    Institute of Scientific and Technical Information of China (English)

    韩世岩; 李淑君; 王威; 宋湛谦

    2013-01-01

    Using a mixture of a rosin-based bis-quaternary ammonium salt and CTAB as a template and tetraethyl orthosilicate as silica source,four kinds of silica materials SiA,SiB,SiC and SiD were prepared based on the alkaline hydrolysis with different proportion of the two surfactants.Their calcination temperature was 550 C,which was determined by TGA.SEM observation showed that SiC and SiD were more homogeneous-dispersed spheroidal particles without agglomeration than SiA and SiB were.According to TEM photographs,SiC and SiD were spheroidal particles with mesoporous structure.FT-IR spectrogram identified the structure of SiC and SiD before and after calcination.Nitrogen adsorption-desorption analysis showed that the pore sizes of SiC and SiD were mainly at 3.8nm,surface areas and cumulative pore volumes of SiC and SiD were 685.29m2/g,1.22cm3/g and 609.73m2/g,0.93cm3/g,respectively.%以一种松香基双季铵盐和CTAB为共混模板,正硅酸乙酯为硅源,通过调节两种表面活性剂的不同用量,在碱性条件下水解制备了SiA、SiB、SiC、SiD 4种SiO2材料.采用TGA确定煅烧温度为550℃;SEM照片分析可知SiC、SiD的微观形貌优于SiA、SiB,且为分散均匀的球形颗粒,无团聚;TEM照片分析可知,SiC、SiD为具有介孔结构的球形颗粒;FT-IR确证了SiC、SiD煅烧前后的基本结构;经氮气吸附-脱附实验分析,结果表明,SiC、SiD的孔径主要集中在3.8nm处,比表面积和累积孔体积分别为685.29m2/g、1.22cm3/g和609.73m2/g、0.93cm3/g.

  6. Macroscopically Oriented Porous Materials with Periodic Ordered Structures: From Zeolites and Metal-Organic Frameworks to Liquid-Crystal-Templated Mesoporous Materials.

    Science.gov (United States)

    Cho, Joonil; Ishida, Yasuhiro

    2017-07-01

    Porous materials with molecular-sized periodic structures, as exemplified by zeolites, metal-organic frameworks, or mesoporous silica, have attracted increasing attention due to their range of applications in storage, sensing, separation, and transformation of small molecules. Although the components of such porous materials have a tendency to pack in unidirectionally oriented periodic structures, such ideal types of packing cannot continue indefinitely, generally ceasing when they reach a micrometer scale. Consequently, most porous materials are composed of multiple randomly oriented domains, and overall behave as isotropic materials from a macroscopic viewpoint. However, if their channels could be unidirectionally oriented over a macroscopic scale, the resultant porous materials might serve as powerful tools for manipulating molecules. Guest molecules captured in macroscopically oriented channels would have their positions and directions well-defined, so that molecular events in the channels would proceed in a highly controlled manner. To realize such an ideal situation, numerous efforts have been made to develop various porous materials with macroscopically oriented channels. An overview of recent studies on the synthesis, properties, and applications of macroscopically oriented porous materials is presented. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Worm-like mesoporous TiO2 thin films templated using comb copolymer for dye-sensitized solar cells with polymer electrolyte

    Science.gov (United States)

    Lee, Jae Hun; Park, Cheol Hun; Jung, Jung Pyo; Kim, Jong Hak

    2015-12-01

    A comb copolymer consisting of hydrophobic poly(2-[3-(2H-benzotriazol-2-yl)-4-hydroxyphenyl] ethyl methacrylate) (PBEM) and hydrophilic poly(oxyethylene methacrylate) (POEM) is synthesized via one-pot free radical polymerization. The PBEM-POEM comb copolymer is used as an agent to direct the structure toward one consisting of worm-like mesoporous TiO2 (WM-TiO2) films. The selective, preferential interaction between the titania precursor and the hydrophilic POEM chains is responsible for the formation of a well-organized worm-like mesostructure. The morphology of the WM-TiO2 films is characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM). In particular, the effects of film thickness on the optical and electrochemical properties are systematically investigated. The introduction of the WM-TiO2 layer between the nanocrystalline TiO2 (NC-TiO2) layer and fluorine-doped tin oxide (FTO) glass results in increased transmittance of visible light due to an antireflective property, decreased interfacial resistance and suppressed charge recombination at the interfaces of NC-TiO2/FTO glass. As a result, the photovoltaic conversion efficiency of the dye-sensitized solar cell (DSSC) with a polymer electrolyte is improved from 5.3% to 6.6% at an optimum film thickness (310 nm). The obtained efficiency represents a higher efficiency for the N719-based DSSC with a solvent-free, polymer electrolyte.

  8. Dendrimer Templated Synthesis of One Nanometer Rh and Pt Particles Supported on Mesoporous Silica: Catalytic Activity for Ethylene and Pyrrole Hydrogenation.

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Wenyu; Kuhn, John N.; Tsung, Chia-Kuang; Zhang, Yawen; Habas, Susan E.; Yang, Peidong; Somorjai, Gabor A.

    2008-05-09

    Monodisperse rhodium (Rh) and platinum (Pt) nanoparticles as small as {approx}1 nm were synthesized within a fourth generation polyaminoamide (PAMAM) dendrimer, a hyperbranched polymer, in aqueous solution and immobilized by depositing onto a high-surface-area SBA-15 mesoporous support. X-ray photoelectron spectroscopy indicated that the as-synthesized Rh and Pt nanoparticles were mostly oxidized. Catalytic activity of the SBA-15 supported Rh and Pt nanoparticles was studied with ethylene hydrogenation at 273 and 293 K in 10 torr of ethylene and 100 torr of H{sub 2} after reduction (76 torr of H{sub 2} mixed with 690 torr of He) at different temperatures. Catalysts were active without removing the dendrimer capping but reached their highest activity after hydrogen reduction at a moderate temperature (423 K). When treated at a higher temperature (473, 573, and 673 K) in hydrogen, catalytic activity decreased. By using the same treatment that led to maximum ethylene hydrogenation activity, catalytic activity was also evaluated for pyrrole hydrogenation.

  9. Performance Enhancement of Dye-Sensitized Solar Cells Based on TiO₂ Thick Mesoporous Photoanodes by Morphological Manipulation.

    Science.gov (United States)

    Keshavarzi, Reza; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammadpoor-Baltork, Iraj

    2015-10-27

    This study is an attempt to give an account of the preparation of mesoporous TiO2 thick templated films of nonsimilar pore architecture and their use in dye-sensitized solar cells (DSSCs). Highly crystallized mesoporous titania thick templated films with four different morphologies including hexagonal, wormlike, cubic, and gridlike mesostructure, have been successfully synthesized through an evaporation-induced self-assembly (EISA) route followed by layer-by-layer deposition. Stabilization, followed by each coating, and calcinations, carried out after every five layers, were used to produce crack-free thick films. These mesoporous templated titanium dioxide samples were characterized by TEM, XRD, SEM, BET, and UV-vis measurements and used as a photoelectrode material in DSSCs. The mesostructured films with a thickness of about 7 μm demonstrated better performance in comparison to nanocrystalline TiO2 films (NC-TiO2) at a film thickness of 13 μm as the most typical films utilized in DSSCs. The findings reveal that a surfactant/Ti ratio change undergone for developing cubic mesostructures can enhance the crystallinity and roughness factor and therefore increase the energy conversion efficiency of DSSC. The cell performances derived from these mesofilms were enhanced compared to the efficiencies reported thus far. The best photovoltaic performance of 8.73% came from DSSC using the cubic mesoporous TiO2 photoelectrode with the following properties: open circuit voltage of 743 mV, short circuit photocurrent density of 16.35 mA/cm(2), and fill factor of 0.72.

  10. 模板法煤沥青基中孔炭的制备及其电化学性能%The electrochemical properties of templated and activated mesoporous carbons produced from coal pitch

    Institute of Scientific and Technical Information of China (English)

    周颖; 宋晓娜; 舒成; 邱介山

    2011-01-01

    以煤沥青质为碳源,气相法二氧化硅为模板,制备中孔炭(Mesoporous carbon,MC),通过CO2活化调变其表面结构.用TEM、N2吸附、电化学工作站及Land电池测试系统等对产品炭的微观结构及电化学性能进行研究.结果表明:在活化温度900℃、CO2气流量100mL/min条件下,随着活化时间的增加,炭产品的BET比表面积、微孔孔容均呈增加趋势.在活化时间为150min时,产品炭的BET比表面积可达1 360m2/g,比活化前的比表面积提高了约88%.产品炭作为超级电容器电极材料表现出良好的电化学性能,活化时间为120min的样品,在1000mA/g的电流密度下,材料的质量比电容为135F/g,10000次充放电循环后,比电容值保持率高达93%.%Mesoporous carbons ( MCs) were made from coal pitch derived from coal liquefaction residue with silica nanoparticles as template and CO2 as activation agent. The microstructure and electrochemical properties of the MCs were investigated with TEM, N2 adsorption, an electrochemical workstation and a Land battery test system. Results show that the specific surface area increases with activation time at 900 ℃ under a CO2 flow rate of 100 mL·min-1. The specific surface area of MC activated for 150min is 1360 m2·g-1 while that of the un-activated one is 722 m2·g-1. The specific capacitance of the MC activated for 150 min is 135 F·g-1 at a current density of 1 000 mA·g-1 and the decrease in its specific capacitance is 7% after being charged and discharged 10000 times.

  11. Synthesis, Characterization of Mesoporous Al-Mg Composite Oxide and Catalytic Performance for Oxyethylation of Fatty Alcohol

    Institute of Scientific and Technical Information of China (English)

    SONG Wei-ming; DENG Qi-gang; ZHOU De-rui; ZHAO De-feng

    2005-01-01

    A mesoporous Al-Mg composite oxide with a hexagonal structure was synthesized with aluminium nitrate and magnesium nitrate as the reagents and sodium dodecyl sulfate(SDS) as the template in the presence of ethylenediamine. The XRD, nitrogen adsorption-desorption and TEM studies indicate that the composite has a hexagonal framework structure and an average pore diameter of 2.6 nm. The TG/DTA spectra indicate that the decomposition and the removal of the occluded surfactant of the sample take place in a range of 230-550 ℃. The mesoporous Al-Mg composite oxide exhibites a highly catalytic activity for the oxyethylation of fatty alcohols. Narrow-range distributed ethoxylates are formed in the presence of the mesoporous Al-Mg composite oxide catalyst. The distribution selectivity coefficient(Cs) is 24 when the mesoporous Al-Mg composite oxide was used as a catalyst for the oxyethylation of octanol and the average adduct degree of ethoxylates is 6.4.

  12. Direct synthesis of graphitic mesoporous carbon from green phenolic resins exposed to subsequent UV and IR laser irradiations

    Science.gov (United States)

    Sopronyi, Mihai; Sima, Felix; Vaulot, Cyril; Delmotte, Luc; Bahouka, Armel; Matei Ghimbeu, Camelia

    2016-12-01

    The design of mesoporous carbon materials with controlled textural and structural features by rapid, cost-effective and eco-friendly means is highly demanded for many fields of applications. We report herein on the fast and tailored synthesis of mesoporous carbon by UV and IR laser assisted irradiations of a solution consisting of green phenolic resins and surfactant agent. By tailoring the UV laser parameters such as energy, pulse repetition rate or exposure time carbon materials with different pore size, architecture and wall thickness were obtained. By increasing irradiation dose, the mesopore size diminishes in the favor of wall thickness while the morphology shifts from worm-like to an ordered hexagonal one. This was related to the intensification of phenolic resin cross-linking which induces the reduction of H-bonding with the template as highlighted by 13C and 1H NMR. In addition, mesoporous carbon with graphitic structure was obtained by IR laser irradiation at room temperature and in very short time periods compared to the classical long thermal treatment at very high temperatures. Therefore, the carbon texture and structure can be tuned only by playing with laser parameters, without extra chemicals, as usually required.

  13. SYNTHESIS AND CHARACTERIZATIONOF ORGANIC FUNCTIONALIZED MESOPOROUS SILICA AND EVALUATE THEIR ADSORPTIVE BEHAVIOR FOR REMOVAL OF METHYLENE BLUE FROM AQUEOUS SOLUTION

    Directory of Open Access Journals (Sweden)

    Sameer H. Kareem

    2014-01-01

    Full Text Available Three Mesoporous Silica (MPS with different functional groups were prepared by one-step synthesis based on the simultaneous hydrolysis and condensation of tetraethoxy silane with organo-silane in the presence of template surfactant Polydimethylsiloxane-Polyethyleneoxide (PDMS-PEO. The prepared materials were characterized by Fourier Transform Infrared Spectroscopy (FTIR, Thermogravimetric Analysis (TGA and nitrogen adsorption-desorption experiments. The results indicate that the preparation of methyl and phenyl functionalized silica were successful. The adsorption behavior of methylene blue from aqueous systems onto these mesoporous silica has been studied. Batch experiments were carried out to measure the adsorption as a function of contact time, initial concentration (2.5-20 mg L-1 and temperature (288, 298, 308 and 318 K. The equilibrium of the process was achieved within (30-60 min. The adsorption of methylene blue on the mesoporous silica increases with increasing temperature which indicating an endothermic process. Adsorption isotherms were fitted with the Langmuir, Freundlich models. The kinetic data were analyzed using pseudo-first- order and pseudo-second-order models and intraparticle diffusion. The adsorption kinetics of methylene blue on mesoporous silica matched well with pseudo-second order kinetic model.

  14. Synthesis, characterization and photocatalytic reactions of phosphated mesoporous titania

    Indian Academy of Sciences (India)

    Pallabi Goswami; Jatindra Nath Ganguli

    2012-10-01

    Mesoporous titania nanoparticles with a well-definedmesostructure was prepared by hydrothermal process, using nonionic triblock copolymer P123 as surfactant template, modified with phosphoric acid and followed by calcination at 600°C. The sol–gel titania was modified by in situ phosphorylation using phosphoric acid and thereby incorporating phosphorous directly into the framework of TiO2. The resulting materials were characterized by XRD, SEM, TEM, nitrogen adsorption, TGA and DRS. It was found that the structural and optical properties of titania samples are strongly influenced by their phosphate modification. In case of calcined samples a positive effect on the specific surface area for the in situ phosphated sample was found. Mesoporous structure of phosphated titania did not collapse even after calcination at 600°C. The enhanced photocatalytic activity of the synthesized phosphate nanomaterials were evaluated through a study of the decomposition of fluorescein under UV light excitation and compared with undoped titania nanomaterial as well as with commercial titania.

  15. Alendronate functionalized mesoporous hydroxyapatite nanoparticles for drug delivery

    Energy Technology Data Exchange (ETDEWEB)

    Li, Dongdong, E-mail: lidongchem@sina.cn [State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 (China); Zhu, Yuntao; Liang, Zhiqiang [State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 (China)

    2013-06-01

    Highlights: ► The synthesized mesoporous hydroxyapatite has nanostructure and bioactivity. ► The materials have high surface area and amino group. ► The materials show higher drug loading and slower release rate than pure HAP. - Abstract: Mesoporous nanosized hydroxyapatite (HAP) functionalized by alendronate (ALN) was synthesized using cationic surfactant CTAB as template. The structural, morphological and textural properties were fully characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and N{sub 2} adsorption/desorption. Then the obtained materials were performed as drug delivery carriers using ibuprofen (IBU) as a model drug to investigate their drug storage/release properties in simulated body fluid (SBF). The materials showed relatively slower release rate compared with HAP due to the ionic interaction between -NH{sub 3}{sup +} on the matrix and -COO{sup −}belongs to IBU. The system provides a new concept for improving the drug loading or slowing down the release rate.

  16. Aminopropyl-modified mesoporous molecular sieves as efficient adsorbents for removal of auxins

    Energy Technology Data Exchange (ETDEWEB)

    Moritz, Michał, E-mail: michal.moritz@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemistry and Technical Electrochemistry, Berdychowo 4, 60-965 Poznań (Poland); Geszke-Moritz, Małgorzata, E-mail: Malgorzata.Geszke-Moritz@amu.edu.pl [NanoBioMedical Centre, Adam Mickiewicz University, Umultowska 85, 61-614 Poznań (Poland)

    2015-03-15

    Graphical abstract: Adsorption of indole-3-acetic acid (IAA) on aminopropyl-modified mesoporous sieves. - Highlights: • Four types of mesoporous molecular sieves were used as sorbents for removal of auxins. • SBA-15, MCF, PHTS and SBA-16 were grafted with (3-aminopropyl)triethoxysilane. • The adsorption capacity of modified materials was higher as compared to pure silicas. • Surface modification and pore volume play important role in adsorption process. - Abstract: In the present study, mesoporous siliceous materials grafted with 3-aminopropyltriethoxysilane (APTES) were examined as sorbents for removal of chosen plant growth factors (auxins) such as 1-naphthaleneacetic acid (NAA), indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA). Four different types of mesoporous molecular sieves including SBA-15, PHTS, SBA-16 and MCF have been prepared via non-ionic surfactant-assisted soft templating method. Silica molecular sieves were thoroughly characterized by nitrogen adsorption–desorption analysis, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FT-IR). The maximum adsorption capacity (Q{sub max}) for NAA, IAA and IBA was in the range from 51.0 to 140.8 mg/g and from 4.3 to 7.3 mg/g for aminopropyl-modified adsorbents and pure silicas, respectively. The best adsorption performance was observed for IAA entrapment using both APTES-functionalized SBA-15 and MCF matrices (Q{sub max} of 140.8 and 137.0 mg/g, respectively) which can be ascribed to their larger pore volumes and pore diameters. Moreover, these silicas were characterized by the highest adsorption efficiency exceeding 90% at low pollutant concentration. The experimental points for adsorption of plant growth factors onto aminopropyl-modified mesoporous molecular sieves fitted well to the Langmuir equation.

  17. 以纤维素为模板制备多孔SiO2棒%Synthesis of Mesoporous Silica Nanorod by Using the Cellulose as Template

    Institute of Scientific and Technical Information of China (English)

    张奎; 刘春华; 王平华; 范保林; 屈龙

    2011-01-01

    以2-溴丁酰溴与羟乙基纤维素的酯化产物为原子转移自由基(ATRP)聚合的天分子引发剂,在60℃引发甲基丙烯酸-N,N-二甲氨基乙酯(DMAEMA)聚合,再将PDMAEMA接枝到纤维素上.以此作为模板,在其水溶液中搅拌加入前驱体正硅酸乙酯(TEOS),水解产生二氧化硅凝胶并吸附在模板上,形成二氧化硅棒,通过红外光谱(FT-IR),热重分析(TGA)和透射电镜(TEM)对产物的结构、组成进行了表征.研究了pH值、TEOS用量、水解时间对二氧化硅棒形态的影响.实验结果表明,在pH=4,TEOS浓度为10mg/mL时,水解24 h~36 h,可以获得较好的棒状结构.%Cellulose was acylated with 2-bromobutyrylbromide at ambient temperature in ionic liquid (RTIL), 1allyi-3-methylimidazolium chloride, giving polyfunctional macroinitiators for atom transfer radical polymerization (ATRP). Copolymers were obtained via ATRP of N, N-dimethylamino-2-ethyl methacrylate (DMAEMA) with CuBr/pentamethyldiethylenetriamine (PMDETA) as catalyst and N, N-dimethylformamide (DMF) as solvent at 60 ℃. The resultant Cellulose-graft-poly (N, N-dimethylamino-2-ethyl methacrylate) (cellulose-g-PDMAEMA) was dissolved in distilled water under stirring. Mesoporous silica nanotubes were synthesized under mild conditions by applying conventional sol gel routes using tetraethyl orthosilicate (TEOS) as the precursors. The results were confirmed via FT-IR, TGA and TEM. The effect of the pH value, the concentration of TEOS and polycondensation time on the morphology of silicarod was studied. The results show that the desirable morphology of silicarod can be obtained from polycondensation of TEOS in aqueous solution with concentration of 10 mg/mL at pH= 4 for 24 h~36 h.

  18. Surface-modified Nafion membranes with mesoporous SiO 2 layers via a facile dip-coating approach for direct methanol fuel cells

    Science.gov (United States)

    Lin, Yuhan; Li, Haidong; Liu, Changpeng; Xing, Wei; Ji, Xiangling

    In this study, Nafion ® 117 membrane is surface-modified with mesoporous silica layers through in situ surfactant-templated sol-gel reaction. The reaction makes use of tetraethyl orthosilicate (TEOS) under acidic condition via dip-coating technique on both sides. Scanning electron microscopy (SEM), Fourier transformation infrared (FTIR), and thermogravimetric analysis (TGA) are employed to characterize the resultant membranes. Proton conductivity and methanol permeability of the membranes are also studied. It is determined that the aging time, along with the number of the silicon dioxide (SiO 2) layer, influence both proton conductivity and methanol permeability. Specifically, double-side modified membrane with 5 min interval of the second layer (S (5)) exhibits optimal properties on the combined criterion of conductivity and permeability. However, the application of mesoporous silica layer in modifying commercial Nafion membranes through dip-coating is proven to be a facile route in improving the said criteria simultaneously.

  19. Mesoporous composite nickel cobalt oxide/graphene oxide synthesized via a template-assistant co-precipitation route as electrode material for supercapacitors

    Science.gov (United States)

    Xu, Yanjie; Wang, Lincai; Cao, Peiqi; Cai, Chuanlin; Fu, Yanbao; Ma, Xiaohua

    2016-02-01

    A simple co-precipitation method utilizing SDS (sodium dodecyl sulfate) as template and ammonia as precipitant is successfully employed to synthesize nickel cobalt oxide/graphene oxide (NiCo2O4/GO) composite. The as-prepared composite (NCG-10) exhibits a high capacitance of 1211.25 F g-1, 687 F g-1 at the current density of 1 A g-1, 10 A g-1 and good cycling ability which renders NCG-10 as promising electrode material for supercapacitors. An asymmetric supercapacitor (ASC) (full button cell) has been constructed with NCG-10 as positive electrode and lab-made reduced graphene oxide (rGO) as negative electrode. The fabricated NCG-10//rGO with an extended stable operational voltage of 1.6 V can deliver a high specific capacitance of 144.45 F g-1 at a current density of 1 A g-1. The as-prepared NCG-10//rGO demonstrates remarkable energy density (51.36 W h kg-1 at 1 A g-1), high power density (50 kW kg-1 at 20 A g-1). The retention of capacitance is 88.6% at the current density of 8 A g-1 after 2000 cycles. The enhanced capacitive performance can be attributed to the improved specific surface area and 3D open area of NCG-10 generated by the pores and channels with the substantial function of SDS.

  20. Template-free fabrication of graphene-wrapped mesoporous ZnMn2O4 nanorings as anode materials for lithium-ion batteries

    Science.gov (United States)

    Zhou, Weiwei; Wang, Dong; Zhao, Limin; Ding, Chunyan; Jia, Xingtao; Du, Yu; Wen, Guangwu; Wang, Huatao

    2017-06-01

    We rationally designed a facile two-step approach to synthesize ZnMn2O4@G composite anode material for lithium-ion batteries (LIBs), involving a template-free fabrication of ZnMn2O4 nanorings and subsequent coating of graphene sheets. Notably, it is the first time that ring-like ZnMn2O4 nanostructure is reported. Moreover, our system has been demonstrated to be quite powerful in producing ZnMn2O4 nanorings regardless of the types of Zn and Mn-containing metal salts reactants. The well-known inside-out Ostwald ripening process is tentatively proposed to clarify the formation mechanism of the hollow nanorings. When evaluated as anode material for LIBs, the resulting ZnMn2O4@G hybrid displays significantly improved lithium-storage performance with high specific capacity, good rate capability, and excellent cyclability. After 500 cycles, the ZnMn2O4@G hybrid can still deliver a reversible capacity of 958 mAh g-1 at a current density of 200 mA g-1, much higher than the theoretical capacity of 784 mAh g-1 for pure ZnMn2O4. The outstanding electrochemical performance should be reasonably ascribed to the synergistic interaction between hollow and porous ZnMn2O4 nanorings and the three-dimensional interconnected graphene sheets.

  1. Aminopropyl-modified mesoporous molecular sieves as efficient adsorbents for removal of auxins

    Science.gov (United States)

    Moritz, Michał; Geszke-Moritz, Małgorzata

    2015-03-01

    In the present study, mesoporous siliceous materials grafted with 3-aminopropyltriethoxysilane (APTES) were examined as sorbents for removal of chosen plant growth factors (auxins) such as 1-naphthaleneacetic acid (NAA), indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA). Four different types of mesoporous molecular sieves including SBA-15, PHTS, SBA-16 and MCF have been prepared via non-ionic surfactant-assisted soft templating method. Silica molecular sieves were thoroughly characterized by nitrogen adsorption-desorption analysis, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FT-IR). The maximum adsorption capacity (Qmax) for NAA, IAA and IBA was in the range from 51.0 to 140.8 mg/g and from 4.3 to 7.3 mg/g for aminopropyl-modified adsorbents and pure silicas, respectively. The best adsorption performance was observed for IAA entrapment using both APTES-functionalized SBA-15 and MCF matrices (Qmax of 140.8 and 137.0 mg/g, respectively) which can be ascribed to their larger pore volumes and pore diameters. Moreover, these silicas were characterized by the highest adsorption efficiency exceeding 90% at low pollutant concentration. The experimental points for adsorption of plant growth factors onto aminopropyl-modified mesoporous molecular sieves fitted well to the Langmuir equation.

  2. Facile Preparation, Structural Control and Spheroidization of Mesoporous Car-bons Using Hydrolyzed Water Glass as a Template%中孔炭的水玻璃模板法制备、结构调控及球形功能化

    Institute of Scientific and Technical Information of China (English)

    张川; 王际童; 李旭; 龙东辉; 乔文明; 凌立成

    2015-01-01

    Mesoporous carbons (MC) with controlled pore structure were synthesized using hydrolyzed water glass (sodium silicate) as hard template precursor. The mixture of carbon precursor (resorcinol-formaldehyde) sol and silica sol followed by Sol-Gel process generated a polymer/silica dual hydrogels. After ambient drying, carboniza-tion and HF etching, mesoporous carbons with developed mesoporous structure were obtained. The hydrolysis conditions of water glass including hydrolysis temperature and hydrolysis time, and the weight ratio of RF polymer to silica were studied respectively to investigate their effects on the mesoporous structure. The microstructures of the mesoporous carbons were characterized by N2 adsorption, SEM and TEM observations. It was found that as-prepared mesoporous carbons displayed disordered mesoporous channels which replicated from the initial colloidal silica networks. The average mesopore size could be precisely adjusted in the range from 6 nm to 12 nm by tuning the hydrolysis time and hydrolysis temperature, while the total porosity could be controlled by changing the weight ratio of polymer precursor to silica. Furthermore, with the assistant of suspension polymerization and spray drying technologies, spherical mesoporous carbons with millimetre and micrometer-sized particles were drying technologies, spherical mesoporous carbons with millimetre and micrometer-sized particles were produced, respectively. The present work provides a low-cost approach for deliberately controlling the mesoporous structure and spherical morphology to mesoporous carbons that can be extended to many different applications.%以廉价水玻璃为原料,通过控制水解条件,合成出具有不同尺寸的 SiO2溶胶,并与间苯二酚-甲醛(RF)溶胶形成均相的凝胶复合物,经常压干燥、炭化、酸洗,得到具有可控结构的中孔炭材料。考察了水解温度、水解时间和反应物组成对孔结构的影响,并通过氮气吸

  3. Morphology control of ordered mesoporous carbons for high capacity lithium sulfur batteries

    Energy Technology Data Exchange (ETDEWEB)

    Schuster, Joerg David

    2011-06-07

    The focus of this thesis concerns the morphology control of ordered mesoporous carbon (OMC) materials. Ordered mesoporous carbons with diverse morphologies, that are thin films, fibers - embedded in anodic alumina membranes and free-standing - or spherical nanoparticles, have been successfully prepared by soft-templating procedures. The mechanisms of structure formation and processing were investigated with in-situ SAXS measurements and their application in high capacity lithium-sulfur batteries was successfully tested in cooperation with Guang He and Linda Nazar from the University of Waterloo in Canada. The Li-S batteries receive increasing attention due to their high theoretical energy density which is 3 to 5 times higher than from lithium-ion batteries. For this type of battery the specific pore volume is crucial for the content of the active component (sulfur) in the cathode and therefore correlates with the capacity and gravimetric energy density of the battery. At first, mesoporous thin films with 2D-hexagonal structure were obtained through organic-organic self-assembly of a preformed oligomeric resol precursor and the triblock copolymer template Pluronic P123. The formation of a condensed-wall material through thermopolymerization of the precursor oligomers resulted in mesostructured phenolic resin films. Subsequent decomposition of the surfactant and partial carbonization were achieved through thermal treatment in inert atmosphere. The films were crack-free with tunable homogenous thicknesses, and showed either 2D-hexagonal or lamellar mesostructure. An additional, yet unknown 3D-mesostructure was also found. In the second part, cubic and circular hexagonal mesoporous carbon phases in the confined environment of tubular anodic alumina membrane (AAM) pores were obtained by self-assembly of the mentioned resol precursor and the triblock copolymer templates Pluronic F127 or P123, respectively. Casting and solvent-evaporation were also followed by

  4. BITEMPLATE SYNTHESIS OF MESOPOROUS SILICAS WITH THIOUREA GROUPS

    Directory of Open Access Journals (Sweden)

    O. I. Gona

    2009-06-01

    Full Text Available Mesoporous silicas with the thiourea functional group ≡Si(CH23NHC(SNHC2H5 have been synthesized by monotemplate and bitemplate route (bitemplate is cetylpyridinium chloride as micelle-forming surfactant and monoethanolamide of saturated n-aliphatic acid as non-micelle-forming surfactant. The infl uence of a number of factors on mesoporous silicas structure has been studied: alkoxysilanes and surfactants concentration, and as well as the nature of medium in hydrothermal treatment of mesophases. The optimum conditions under which functionalized mesoporous silicas have possessing highly ordered hexagonal structure have been found. The surface area of mesoporous silicas synthesized using optimum bitemplate solubilization composition reaches 1055-1350 m2/g and sorption volume and pore diameter are 0.75-0.95 cm3/g and 2.5-2.9 nm respectively.

  5. Ordered mesoporous silica: microwave synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Fantini, M.C.A. [IF-USP, CP 66318, 05315-970, Sao Paulo, SP (Brazil)]. E-mail: mfantini@if.usp.br; Matos, J.R. [IQ-USP, CP 26077, 05599-970, Sao Paulo, SP (Brazil); Silva, L.C. Cides da [IQ-USP, CP 26077, 05599-970, Sao Paulo, SP (Brazil); Mercuri, L.P. [IQSC-USP, CP 780, 13560-970, Sao Carlos, SP (Brazil); Chiereci, G.O. [IQSC-USP, CP 780, 13560-970, Sao Carlos, SP (Brazil); Celer, E.B. [Department of Chemistry, Kent State University, Kent, OH 44240 (United States); Jaroniec, M. [Department of Chemistry, Kent State University, Kent, OH 44240 (United States)

    2004-09-25

    Ordered mesoporous silicas, FDU-1, synthesized by using triblock copolymer, EO{sub 39}BO{sub 47}EO{sub 39}, as template were hydrothermally treated in a microwave oven at 373 K for different periods of time. The structural and morphological properties of these silicas were investigated by X-ray diffraction and nitrogen adsorption and compared with those for the FDU-1 samples prepared by conventional hydrothermal treatment at 373 K. All samples were calcined at 813 K in N{sub 2} and air. This procedure succeeded in producing ordered cage-like mesoporous structures even after 15 min of the microwave treatment. The best sample was obtained after 60 min of the microwave treatment, which is reflected by narrow pore size distribution, uniform pore size entrances and thick mesopore walls. Longer time of the microwave treatment increased nonuniformity of the pore entrance sizes as evidenced by changes in the hysteresis loops of nitrogen adsorption isotherms.

  6. Synthesis of Length Controllable Ordered Mesoporous Rodslike SBA-15 by Co-surfactant Method%长度可控杆状SBA-15的合成

    Institute of Scientific and Technical Information of China (English)

    王敏; 李冬; 蔡文京; 姜男哲

    2014-01-01

    SBA-15 rods with different lengths( from hexagonal paticials to short rods, and to longer rods) were synthesized via triblock copolymer P123 as a structure-directing agent and chitosan as a co-surfactant. The results show that chitosan is indispensable for tuning the length of SBA-15 rods. Addition of chitosan could improve the periodicity of the SBA-15 and the specific surface area and total proe volume are increased to 1157 cm2/g and 1.53 cm3/g, respectively.%以三嵌段共聚物P123为结构导向剂,天然高聚物壳聚糖为添加剂,合成出分散性较好的杆状结构SBA-15.通过调节体系中壳聚糖的含量,可以实现对产物形貌的控制,即从颗粒到短杆状,最后到长杆状.壳聚糖的加入不仅使SBA-15的介孔结构更加长程有序,同时也提高了其比表面积和孔容,其最高值分别达到1157 m2/g和1.53 cm3/g.

  7. Tuning the optical properties of mesoporous TiO2 films by nanoscale engineering.

    Science.gov (United States)

    Schwenzer, Birgit; Wang, Liang; Swensen, James S; Padmaperuma, Asanga B; Silverman, Gary; Korotkov, Roman; Gaspar, Daniel J

    2012-07-03

    The optical properties of spin-coated titanium dioxide films have been tuned by introducing mesoscale pores into the inorganic matrix. Differently sized pores were templated using Pluronic triblock copolymers as surfactants in the sol-gel precursor solutions and adjusted by varying the process parameters, such as the polymer concentration, annealing temperature, and time. The change in refractive index observed for different mesoporous anatase films annealed at 350, 400, or 450 °C directly correlates with changes in the pore size. Additionally, the index of refraction is influenced by the film thickness and the density of pores within the films. The band gap of these films is blue-shifted, presumably due to stress the introduction of pores exerts on the inorganic matrix. This study focused on elucidating the effect different templating materials (Pluronic F127 and P123) have on the pore size of the final mesoporous titania film and on understanding the relation of varying the polymer concentration (taking P123 as an example) in the sol-gel solution to the pore density and size in the resultant titania film. Titania thin film samples or corresponding titanium dioxide powders were characterized by X-ray diffraction, cross-section transmission electron microscopy, nitrogen adsorption, ellipsometery, UV/vis spectrometry, and other techniques to understand the interplay between mesoporosity and optical properties.

  8. Enantioselectively controlled release of chiral drug (metoprolol) using chiral mesoporous silica materials

    Science.gov (United States)

    Guo, Zhen; Du, Yu; Liu, Xianbin; Ng, Siu-Choon; Chen, Yuan; Yang, Yanhui

    2010-04-01

    Chiral porous materials have attracted burgeoning attention on account of their potential applications in many areas, such as enantioseparation, chiral catalysis, chemical sensors and drug delivery. In this report, chiral mesoporous silica (CMS) materials with various pore sizes and structures were prepared using conventional achiral templates (other than chiral surfactant) and a chiral cobalt complex as co-template. The synthesized CMS materials were characterized by x-ray diffraction, nitrogen physisorption, scanning electron microscope and transmission electron microscope. These CMS materials, as carriers, were demonstrated to be able to control the enantioselective release of a representative chiral drug (metoprolol). The release kinetics, as modeled by the power law equation, suggested that the release profiles of metoprolol were remarkably dependent on the pore diameter and pore structure of CMS materials. More importantly, R- and S-enantiomers of metoprolol exhibited different release kinetics on CMS compared to the corresponding achiral mesoporous silica (ACMS), attributable to the existence of local chirality on the pore wall surface of CMS materials. The chirality of CMS materials on a molecular level was further substantiated by vibrational circular dichroism measurements.

  9. Enantioselectively controlled release of chiral drug (metoprolol) using chiral mesoporous silica materials

    Energy Technology Data Exchange (ETDEWEB)

    Guo Zhen; Liu Xianbin; Ng, Siu-Choon; Chen Yuan; Yang Yanhui [School of Chemical and Biomedical Engineering, Nanyang Technological University, Singapore 637459 (Singapore); Du Yu, E-mail: du_yu@jlu.edu.cn, E-mail: yhyang@ntu.edu.sg [College of Electronic Science and Engineering, Jilin University, Changchun 130012 (China)

    2010-04-23

    Chiral porous materials have attracted burgeoning attention on account of their potential applications in many areas, such as enantioseparation, chiral catalysis, chemical sensors and drug delivery. In this report, chiral mesoporous silica (CMS) materials with various pore sizes and structures were prepared using conventional achiral templates (other than chiral surfactant) and a chiral cobalt complex as co-template. The synthesized CMS materials were characterized by x-ray diffraction, nitrogen physisorption, scanning electron microscope and transmission electron microscope. These CMS materials, as carriers, were demonstrated to be able to control the enantioselective release of a representative chiral drug (metoprolol). The release kinetics, as modeled by the power law equation, suggested that the release profiles of metoprolol were remarkably dependent on the pore diameter and pore structure of CMS materials. More importantly, R- and S-enantiomers of metoprolol exhibited different release kinetics on CMS compared to the corresponding achiral mesoporous silica (ACMS), attributable to the existence of local chirality on the pore wall surface of CMS materials. The chirality of CMS materials on a molecular level was further substantiated by vibrational circular dichroism measurements.

  10. Adsorption of L-phenylalanine onto mesoporous silica

    Energy Technology Data Exchange (ETDEWEB)

    Goscianska, Joanna; Olejnik, Anna; Pietrzak, Robert, E-mail: pietrob@amu.edu.pl

    2013-11-01

    Mesoporous silica materials, such as SBA-3, SBA-15, SBA-16 and KIT-6 were synthesized using tetraethyl orthosilicate as the silica source and different surfactants as templates. The products were characterised by a number of techniques, including low-temperature nitrogen sorption, X-ray diffraction and transmission electron microscopy. Results of the studies confirmed the ordered mesoporous structures of all silica samples obtained. Adsorption of L-phenylalanine on various mesoporous adsorbents was studied from solutions with different pH (5.6–9.4). Maximum sorption capacity was observed at pH 5.6, which is close to the isoelectric point of L-phenylalanine (pI = 5.48). Above this pH value, the amount of adsorbed amino acid decreased. In the range of equilibrium concentration (pH 5.6), the adsorption capacities of ordered silica samples decreased in the following order: KIT-6 (420 μmol g{sup −1}) > SBA-15 (389 μmol g{sup −1}) > SBA-16 (357 μmol g{sup −1}) > SBA-3 (219 μmol g{sup −1}). The lowest sorption capacity towards L-phenylalanine was found for SBA-3 despite the fact that it showed the largest surface area, which can be explained assuming that part of the pores in SBA-3 can be inaccessible to L-phenylalanine molecules. Large pore size of KIT-6 and SBA-15 permitted the amino acid molecule to enter into the pores of these mesoporous molecular sieves. - Highlights: • SBA-3, SBA-15, SBA-16, KIT-6 materials were prepared by hydrothermal method. • Ordered mesoporous silicas are promising as adsorbents of L-phenylalanine. • Adsorption of L-phenylalanine was studied from solutions with different pH. • Sorption capacities decrease in the following order: KIT-6 > SBA-15 > SBA-16 > SBA-3. • Large pore size of KIT-6 and SBA-15 permit the amino acid to enter into the pores.

  11. Template-mediated synthesis of periodic membranes for improved liquid-phase separations

    Energy Technology Data Exchange (ETDEWEB)

    Groger, H. [American Research Corp. of Virginia, Radford, VA (United States)

    1997-10-01

    Solid/liquid separations of particulates in waste streams will benefit from design and development of ultrafiltration (UF) membranes with uniform, tailorable pore size and chemical, thermal, and mechanical stability. Such membranes will perform solid/liquid separations with high selectivity, permeance, lifetime, and low operating costs. Existing organic and inorganic membrane materials do not adequately meet all these requirements. An innovative solution to the need for improved inorganic membranes is the application of mesoporous ceramics with narrow pore-size distributions and tailorable pore size (1.5 to 10 nm) that have recently been shown to form with the use of organic surfactant molecules and surfactant assemblies as removable templates. This series of porous ceramics, designated MCM-41, consists of silica or aluminosilicates distinguished by periodic arrays of uniform channels. In this Phase I Small Business Innovation Research program, American Research Corporation of Virginia will demonstrate the use of supported MCM-41 thin films deposited by a proprietary technique, as UF membranes. Technical objectives include deposition in thin, defect-free periodic mesoporous MCM-41 membranes on porous supports; measurement of membrane separation factors, permeance, and fouling; and measurement of membrane lifetime as part of an engineering and economic analysis.

  12. Improving the quality of patchouli oil by adsorption process using surfactant modified of natural zeolite

    Science.gov (United States)

    Kuntari, Purbaningtias, Tri Esti; Wiyantoko, Bayu; Kurniawati, Puji; Prasetyoko, Didik; Suprapto

    2017-03-01

    This research concerns with the development of natural material i.e. natural zeolite. Natural zeolite were modified by surfactant treatment. Material modification has been done using cetyltrimethyllammonium bromide as cationic surfactant for mesopore template. The physicochemical characters of natural material modified and unmodified was investigated by using XRD, FTIR, nitrogen physisorption, and SEM-EDX. The XRD was used to show crystallinity structure of natural material modified and unmodified. Surfactant treatment caused decreasing crystallinity of natural zeolite. The FTIR spectra showed characteristic peaks for natural zeolite modified and unmodified, the bands around 3400-3500 cm-1 and 1635-1641 cm-1 correspond to adsorbed water and bands around finger print area were characteristic for silica and alumina. Meanwhile physisorption nitrogen profiles gave information that the pore modification by surfactant. The morphologies of natural material modified and unmodified as well as chemical composition of the particles were shown by SEM-EDX. The usage of modified material decrease acidity number into 19.47% than unmodified material, which is 7,62%. The GC analysis showed that percentage of patchouli alcohol increases and new peaks were not identified indicated there was not any reaction appeared.

  13. Diffusion effects on formation process of mesoporous molecular sieve MCM-41

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The regular mesoporous molecular sieve MCM-41 has been investigated at different stages during its formation,using high resolution transmission electron microscopy and powder X-ray diffraction.The results not only support the liquid-crystal templating mechanism previously postulated,but allow the extension fo its scope to discribe ditails of MCM-41 formation.It has been observed that formation of the hexagonal liquid crystal phase on the one hand and of silica aggregates on the other,occurs simultaneously at the inception of gel formation and throughout the crystallisation.This process is most probably affected by diffusion of both the surfactant molecules and the oligomeric silicate ions.With this postulate it becomes possible to explain several experimental observation(both old and new)and to develop a multi-step synthesis method to grow large particles of MCM-41 using small calcined crystals of MCM-41 as seeds.

  14. Performance of a Novel Hydrophobic Mesoporous Material for High Temperature Catalytic Oxidation of Naphthalene

    Directory of Open Access Journals (Sweden)

    Guotao Zhao

    2014-01-01

    Full Text Available A high surface area, hydrophobic mesoporous material, MFS, has been successfully synthesized by a hydrothermal synthesis method using a perfluorinated surfactant, SURFLON S-386, as the single template. N2 adsorption and TEM were employed to characterize the pore structure and morphology of MFS. Static water adsorption test indicates that the hydrophobicity of MFS is significantly higher than that of MCM-41. XPS and Py-GC/MS analysis confirmed the existence of perfluoroalkyl groups in MFS which led to its high hydrophobicity. MFS was used as a support for CuO in experiments of catalytic combustion of naphthalene, where it showed a significant advantage over MCM-41 and ZSM-5. SEM was helpful in understanding why CuO-MFS performed so well in the catalytic combustion of naphthalene. Experimental results indicated that MFS was a suitable support for catalytic combustion of large molecular organic compounds, especially for some high temperature catalytic reactions when water vapor was present.

  15. A multifunctional mesoporous Fe{sub 3}O{sub 4}/SiO{sub 2}/CdTe magnetic-fluorescent composite nanoprobe

    Energy Technology Data Exchange (ETDEWEB)

    Yin, Naiqiang; Wu, Ping; Liang, Guo; Cheng, Wenjing [Shangqiu Normal University, School of Physics and Electrical Information, Shangqiu, Henan (China)

    2016-03-15

    A multifunctional mesoporous, magnetic and fluorescent Fe{sub 3}O{sub 4}/SiO{sub 2}/CdTe nanoprobe with well-defined core-shell nanostructures was prepared. This multifunctional nanoprobe was synthesized through a novel method mainly including two steps. The first step involved the controlled growth of mesoporous silica layer onto the surface of Fe{sub 3}O{sub 4} nanoparticle using tetraethyl orthosilicate as silica source, cationic surfactant cetyltrimethylammonium bromide as template, and 1,3,5-triisopropylbenzene as pore swelling agents. The second step involved the layer-by-layer assembly of 3-aminopropyltrimethoxysilane and fluorescent CdTe quantum dots with the mesoporous Fe{sub 3}O{sub 4}/SiO{sub 2} nanoparticles. The well-designed nanoprobe exhibits strong excitonic photoluminescence and superparamagnetism at room temperature. In attention, the mesoporous silica layer of the nanoprobe with great loading capacity makes it a promising candidate as targeted drug delivery platform. (orig.)

  16. Shape-controlled Synthesis of Activated Bio-chars by Surfactant-templated Ionothermal Carbonization in Acidic Ionic Liquid and Activation with Carbon Dioxide

    Directory of Open Access Journals (Sweden)

    Feng Guo

    2014-04-01

    Full Text Available Shape-controlled bio-chars were synthesized in two steps: (i ionothermal carbonization of biomass (e.g., glucose, cellulose, lignin, and bamboo at low temperatures (150 to 180 °C in an acidic ionic liquid (IL, and (ii subsequent activation with carbon dioxide at higher temperature (500 °C. Acidic IL was used as both the medium and catalyst for advanced carbon materials production. During the first step the primary structures of spherical particles were obtained. The surfactants sodium dodecyl sulfonate (SDS, ethylene glycol (EG, and sodium oleate (SO were also used to modify the surface morphology of bio-chars and activated bio-chars. After the second step, the primary structures of bio-chars were still preserved or improved. The Brunauer-Emmett-Teller surface area and the pore diameter of activated bio-chars were 289 to 469 m2/g and 3.5 to 3.6 nm, respectively. Scanning electron microscope and transmission electron microscope images show that after modification of bio-chars with SDS, EG, and SO, activated bio-char particles agglomerated into rod-like (~200 nm diameter, nano-membrane (~70 nm thickness, and spherical (~200 nm morphologies, respectively. The morphology of activated bio-chars was easily controlled during the synthesis, which is important for the exploitation of their peculiar properties and unique applications.

  17. Synthesis and photo-catalytic activity of mesoporous TiO2 fiber using collagen fiber as a template%胶原纤维为模板制备介孔TiO2纤维及光催化活性研究

    Institute of Scientific and Technical Information of China (English)

    蔡莉

    2013-01-01

    以胶原纤维为模板,硫酸钛为钛源,通过 Ti (Ⅳ)与胶原纤维发生配位反应,将其负载于胶原纤维上,经过煅烧除去胶原纤维模板而获得具有介孔结构的TiO2纤维.通过场发射扫描电镜、N2吸附-脱附、广角XRD衍射、分子荧光光谱等分析手段对所制备的TiO2纤维的表面结构、孔结构和晶体结构等进行表征.实验结果表明,硫酸钛与胶原纤维质量比及煅烧温度明显影响TiO2纤维的表面形貌和孔结构.当硫酸钛与胶原纤维质量比为8∶5,煅烧温度为600℃,所制备的TiO2纤维能较完整地保留天然胶原纤维的形貌和有序的介孔结构,孔径分布集中在4.3 nm.酸性橙Ⅱ的光催化降解实验表明,具有介孔结构的 TiO2纤维的光催化活性明显高于无介孔结构的 Degussa P25.%Mesoporous TiO2 fiber was prepared using collagen fiber as the template and Ti(SO4 )2 as the titanium source.The Ti(Ⅳ)was loaded on collagen fiber by chelation reaction,and then the mesoporous TiO2 fiber was obtained after heat-treatment to remove the template of collagen fiber.The surface morphology and pore struc-ture of the as-prepared mesoporous TiO2 fiber were characterized by means of field emission scanning electron microscopy,N2 absorption-desorption isothermal method,wide angle XRD and photoluminescence spectra (PL).The experimental results indicated that the mass ratio of Ti(SO4 )2 to collagen fiber and calcination tem-perature significantly influenced the surface morphology and mesoporous structure of TiO2 fiber.When the mass ratio was 8∶5 and calcination temperature was 600 ℃,the morphology of nature collagen fiber was well preserved in the as-prepared mesoporous TiO2 fiber,and the mesoporous structure was in ordered and the pore size distribution was centered in 4.3 nm.The photo-catalytic degradation of acid orange Ⅱ experiments indicated that the photo-catalytic activity of the as-prepared mesoporous TiO2 fiber was much higher

  18. Catalytic abatement of CO and volatile organic compounds in waste gases by gold catalysts supported on ceria-modified mesoporous titania and zirconia

    Institute of Scientific and Technical Information of China (English)

    Vasko Idakiev; Dimitar Dimitrov; Tatyana Tabakova; Krasimir Ivanov; Zhong-Yong Yuan; Bao-Lian Su

    2015-01-01

    Mesoporous oxides TiO2 and ZrO2, synthesized by surfactant templating via a neutral C13(EO)6–Zr(OC3H7)4 assembly pathway, and ceria‐modified TiO2 and ZrO2, prepared by a deposi‐tion–precipitation (DP) method, featuring high surface areas and uniform pore size distributions were used as supports for gold catalysts. The supported gold catalysts were assessed for the cata‐lytic abatement of air pollutants, i.e., CO, CH3OH, and (CH3)2O. The gold was supported on the mes‐oporous oxides by a DP method. The supports and catalysts were characterized by powder X‐ray diffraction, high‐resolution transmission electron microscopy, N2 adsorption–desorption analysis, and temperature‐programmed reduction technique. A high degree of synergistic interaction be‐tween ceria and mesoporous ZrO2 and TiO2 as well as a positive modification of the structural and catalytic properties by ceria was observed. The ceria additive interacts with the mesoporous oxides and induces a strong effect on the reducibility of the supports. The catalytic behavior of the catalysts was discussed to determine the role of the ceria modifying additive and possible interaction be‐tween the gold nanoparticles and ceria‐mesoporous oxide supports. The gold catalysts supported on ceria‐modified mesoporous ZrO2 displayed superior catalytic activity (~100%conversion of CO at 10 °C and CH3OH at 60 °C). The high catalytic activity can be attributed to the ability of the sup‐port to assist oxygen vacancies formation. The studies indicate that the ceria‐modified mesoporous oxide supports have potential as supports for gold‐based catalysts.

  19. Yttrium deposition on mesoporous TiO2: textural design and UV decolourization of organic dyes

    Indian Academy of Sciences (India)

    M L Ojeda; C Velasquez; V Renteria; A Campero; M A García-Sánchez; F Rojas

    2015-02-01

    This study discusses about the photochemical, topological and textural properties of yttrium-doped titanium dioxide (TiO2) photocatalysts. The mesoporous yttrium-doped TiO2 substrates prepared in this research work operate efficiently via low-cost commercial 13-W UV lamps. A quantity of 2 wt% yttrium deposition on TiO2 accelerates methyl orange UV decolourization kinetics. When Y content increases to 8 wt%, besides anatase, rutile is formed from 600°C. The Y2Ti2O7 photoinactive compound emerges at 800°C. The P-123 surfactant mesopore templating treatment of TiO2 xerogels (when concurrent with the sol–gel Y-doping of Ti alkoxides) features the following two correlated phenomena: (i) The surface area increases while the access to the inner porosity of the substrate becomes much easier, so that a larger portion of the surface is made accessible to the dye molecules as well as to the yttrium dopant; (ii) the inclusion of tubular instead of ink-bottle pores facilitates the transport of organic species in and out of the pore structure. The most active mesoporous substrate resulted to be made of 2 wt% Y; contrastingly, when Y= 8 wt%, photoinactivity arose because of Y2Ti2O7 formation. The involvement of P123 was not the sole factor influencing the efficiency of TiO2 mesoporous photocatalysts. There were additional key factors, such as the surging of co-ordination and nucleophilic species, during the dye photodegradation process, which were also induced by the presence of Y species on the surface of these substrates.

  20. TiO2/palygorskite composite nanocrystalline films prepared by surfactant templating route: synergistic effect to the photocatalytic degradation of an azo-dye in water.

    Science.gov (United States)

    Stathatos, E; Papoulis, D; Aggelopoulos, C A; Panagiotaras, D; Nikolopoulou, A

    2012-04-15

    Microfibrous palygorskite clay mineral and nanocrystalline TiO(2) are incorporating in the preparation of nanocomposite films on glass substrates via sol-gel route at 500°C. The synthesis involves a simple chemical method employing nonionic surfactant molecule as pore directing agent along with the acetic acid-based sol-gel route without direct addition of water molecules. Drying and thermal treatment of composite films lead to the elimination of organic material while ensure the formation of TiO(2) nanoparticles homogeneously distributed on the surface of the palygorskite microfibers. TiO(2) nanocomposite films without cracks consisted of small crystallites in size (12-16 nm) and anatase crystal phase was found to cover palygorskite microfibers. The composite films were characterized by microscopy techniques, UV-vis, IR spectroscopy, and porosimetry methods in order to examine their structural properties. Palygorskite/TiO(2) composite films with variable quantities of palygorskite (0-2 w/w ratio) were tested as new photocatalysts in the photo-discoloration of Basic Blue 41 azo-dye in water. These nanocomposite films proved to be very promising photocatalysts and highly effective to dye's discoloration in spite of the small amount of immobilized palygorskite/TiO(2) catalyst onto glass substrates. 3:2 palygorskite/TiO(2) weight ratio was finally the most efficient photocatalyst while reproducible discoloration results of the dye were obtained after three cycles with same catalyst. It was also found that palygorskite showed a positive synergistic effect to the TiO(2) photocatalysis.

  1. A Reliable Method for the Preparation of Multiporous Alumina Monoliths by Ice-Templating

    Directory of Open Access Journals (Sweden)

    Jérémy Dhainaut

    2016-03-01

    Full Text Available Alumina supports presenting a bimodal porosity are generally advantageous for the conversion of bulky molecules such as found in biomass, refining, and petrochemistry. However, shaping of such materials, while controlling pores size and orientation, proves to be hard. This problem can be tackled by using a simple method involving sol-gel chemistry, surfactant self-assembly, and ice-templating. Herein, a systematic study of the formulation and process parameters’ influence on the final material properties is presented. This protocol results in the repeatable preparation of centimeter-sized alumina monoliths presenting a uni-directional macroporosity and structured mesopores. These monoliths should be of particular interest in high flow rate catalytic applications.

  2. Synthesis of High Surface Area and Well Crystallized Mesoporous WC at Low Temperature with a Pore Structure Collapsed Replication Route

    Institute of Scientific and Technical Information of China (English)

    LI Hua; SHI Jianlin; CHEN Hangrong; ZHANG Lingxia; LI Lei

    2011-01-01

    An approach named "pore structure collapsed replication route" has been developed to prepare mesoporous WC materials with a high surface area (105 m2/g) and crystallized framework at a temperature as low as 700 ℃. The XRD, TEM, EDS, and BET characterizations were conducted to analyze the effects of the synthesis parameters and the template types on the structure of mesoporous WC. The compaction on the templates is the key to form mesoporous structure of WC while the templates help to control the size of crystalline. At a content of 7 wt% for the precursor of WC, the mesoporous WC could be formed with well ordered structure.

  3. Template synthesis of monodisperse carbon nanodots

    Science.gov (United States)

    Kurdyukov, D. A.; Eurov, D. A.; Stovpiaga, E. Yu.; Kirilenko, D. A.; Konyakhin, S. V.; Shvidchenko, A. V.; Golubev, V. G.

    2016-12-01

    Monodisperse carbon nanodots in pores of mesoporous silica particles are obtained by template synthesis. This method is based on introducing a precursor (organosilane) into pores, its thermal decomposition with formation of carbon nanodots, and the template removal. Structural analysis of the nanomaterial has been performed, which showed that carbon nanodots have an approximately spherical form and a graphite-like structure. According to dynamic light scattering data, the size of carbon nanodots is 3.3 ± 0.9 nm.

  4. 同步合成模板炭化法制备双电层电容器电极用中孔炭材料的研究%New mesoporous carbons prepared by a simultaneous synthetic template carbonization method for electric double layer capacitors

    Institute of Scientific and Technical Information of China (English)

    侯朝辉; 李新海; 刘恩辉; 何则强; 邓凌峰

    2004-01-01

    以正硅酸乙酯为模板硅源,间苯二酚-甲醛凝胶为炭前驱体,采用同步合成模板炭化(SSTCM)法制备了具有可控结构的中孔炭材料.炭材料的比表面积可达1 500 m2/g,平均孔径在3 nm~10 nm之间.经过酸催化水解预处理的二氧化硅模板前驱体溶液与间苯二酚-甲醛溶液混合,碱性条件下使两者的溶胶凝胶反应同步发生,得到有机/无机凝胶混合物.再经炭化、HF去模,制得SSTCM炭材料.N2等温吸脱附研究表明,与炭前驱体聚合物同步合成的结构可调的二氧化硅模板,导致了SSTCM炭材料可控中孔结构的形成.循环伏安研究表明,采用这种同步合成模板炭化法制备的SSTCM炭材料质量比容量达270 F/g,炭材料具有的典型中孔结构使其可能成为一种理想的双电层电容器电极材料.%A simultaneous synthetic template carbonization method (SSTCM), where tetraethoxy silane (TEOS) was used as the source of the silica template and resorcinol-formaldehyde gel as the carbon precursor, was suggested for the preparation of mesoporous carbons with a controllable pore structure. A precursor solution of the silica template prepared by prehydrolysis of TEOS in an acid medium was blended with resorcinol-formaldehyde solution. The two sol-gel reactions proceeded simultaneously under basic conditions in a sealed vessel and resulted in the formation of organic/inorganic hybrids. A new mesoporous SSTCM carbon was obtained by dissolving the silica template with HF in the hybrid after carbonization, followed by drying. N2 adsorption isotherms at -196 ℃ suggested that the silica template synthesized simultaneously with the carbon precursor polymer resulted in the controllable mesoporous structure of the resultant carbons. Cyclic voltammetry measurements show that the as-prepared SSTCM carbons exhibit a high mass-specific capacitance up to 270 F/g. Their typical mesoporous structure makes these carbons promising materials for electric

  5. Synthesis and Characterization of Zirconia Nanocrystallites by Cationic Surfactant and Anionic Surfactant

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Study on nanomaterials has attracted great interests in recent years. In this article,zirconia nanocrystallites of different structures have been successfully synthesized via hydrothermal methods with cationic surfactant (CTAB) and anionic surfactant (SDS), respectively. Differential Scanning Calorimeter (DSC-TG), X-ray Diffractometer (XRD), Transmission Electron Microscope (TEM), Ultraviolet-Visible (UV-vis) and N2 adsorption-desorption analyses are used for their structure characteristics. The results show that the cationic surfactant has a distinctive direction effect on the formation of zirconia nanocrystallites, while the anionic surfactant has a self-assembly synergistic effect on them. The sample synthesized with the cationic surfactant presents good dispersion with the main phase of tetragonal zirconia, and the average nanocryst al size is around 15nm after calcination at 500 ℃. While the sample synthesized with the anionic surfactant exhibits a worm-like mesoporous structure with pure tetragonal phase after calcination at 500 ℃ and with good thermal stability.

  6. Hard template synthesis of metal nanowires

    Directory of Open Access Journals (Sweden)

    Go eKawamura

    2014-11-01

    Full Text Available Metal nanowires (NWs have attracted much attention because of their high electron conductivity, optical transmittance and tunable magnetic properties. Metal NWs have been synthesized using soft templates such as surface stabilizing molecules and polymers, and hard templates such as anodic aluminum oxide, mesoporous oxide, carbon nanotubes. NWs prepared from hard templates are composites of metals and the oxide/carbon matrix. Thus, selecting appropriate elements can simplify the production of composite devices. The resulting NWs are immobilized and spatially arranged, as dictated by the ordered porous structure of the template. This avoids the NWs from aggregating, which is common for NWs prepared with soft templates in solution. Herein, the hard template synthesis of metal NWs is reviewed, and the resulting structures, properties and potential applications are discussed.

  7. Morphology control of ordered mesoporous carbons for high capacity lithium sulfur batteries

    Energy Technology Data Exchange (ETDEWEB)

    Schuster, Joerg David

    2011-06-07

    The focus of this thesis concerns the morphology control of ordered mesoporous carbon (OMC) materials. Ordered mesoporous carbons with diverse morphologies, that are thin films, fibers - embedded in anodic alumina membranes and free-standing - or spherical nanoparticles, have been successfully prepared by soft-templating procedures. The mechanisms of structure formation and processing were investigated with in-situ SAXS measurements and their application in high capacity lithium-sulfur batteries was successfully tested in cooperation with Guang He and Linda Nazar from the University of Waterloo in Canada. The Li-S batteries receive increasing attention due to their high theoretical energy density which is 3 to 5 times higher than from lithium-ion batteries. For this type of battery the specific pore volume is crucial for the content of the active component (sulfur) in the cathode and therefore correlates with the capacity and gravimetric energy density of the battery. At first, mesoporous thin films with 2D-hexagonal structure were obtained through organic-organic self-assembly of a preformed oligomeric resol precursor and the triblock copolymer template Pluronic P123. The formation of a condensed-wall material through thermopolymerization of the precursor oligomers resulted in mesostructured phenolic resin films. Subsequent decomposition of the surfactant and partial carbonization were achieved through thermal treatment in inert atmosphere. The films were crack-free with tunable homogenous thicknesses, and showed either 2D-hexagonal or lamellar mesostructure. An additional, yet unknown 3D-mesostructure was also found. In the second part, cubic and circular hexagonal mesoporous carbon phases in the confined environment of tubular anodic alumina membrane (AAM) pores were obtained by self-assembly of the mentioned resol precursor and the triblock copolymer templates Pluronic F127 or P123, respectively. Casting and solvent-evaporation were also followed by

  8. Synthesis of hydrothermally stable, hierarchically mesoporous aluminosilicate Al-SBA-1 and their catalytic properties

    Science.gov (United States)

    Li, Na; Wang, Jin-Gui; Xu, Jian-Xiong; Liu, Jin-Yu; Zhou, Hui-Jing; Sun, Ping-Chuan; Chen, Tie-Hong

    2012-03-01

    Hydrothermally stable mesoporous aluminosilicates Al-SBA-1 with hierarchical pore structure have been successfully synthesized under alkaline condition at 120 °C by employing organic mesomorphous complexes of polyelectrolyte (poly(acrylic acid) (PAA)) and cationic surfactant (hexadecyl pyridinium chloride (CPC)) as template. The Si/Al ratio could be as high as 5 and the incorporation of Al into the silica framework did not disturb the well-ordered cubic Pm3&cmb.macr;n mesostructure. Meanwhile, the incorporation of Al could greatly increase the specific surface area and pore volume of the samples. The Al-SBA-1 materials exhibited a high hydrothermal stability and remained stable even after being treated in boiling water for 10 days. The catalytic activity of the Al-SBA-1 materials was investigated by employing the Friedel-Crafts alkylation of toluene with benzyl alcohol as a model reaction and they exhibited excellent catalytic property due to the incorporated acid sites and the hierarchically mesoporous structure.

  9. Adsorptive desulfurization of diesel with mesoporous aluminosilicates

    Institute of Scientific and Technical Information of China (English)

    TANG Huang; LI Wang-Liang; LIU Qing-Fen; GUAN Li-Li; SONG Jia-Qing; XING dian-Min; LIU Hui-Zhou

    2009-01-01

    Mesoporous aluminosilicates (MAS) bearing microporous zeolite units and mesoporous structures were synthesized by the hydrothermal method. Adsorptive desulfurization ability of model oil and hy-drotreated diesel was studied. The effects of template concentration, crystalization time and calcination time were investigated. The desulfurization ability of adsorbents was improved by transitional metal ion-exchanging. The adsorptive desulfurization of diesel was carried out on a fixed-bed system. The results show that the adsorptive capacity is MASMCM-41NaY. The improvement of desulfurization ability of MAS by Cu+ is more significant than that of Ag+.

  10. Synthesis and characterization of mesoporous hydrocracking catalysts

    Science.gov (United States)

    Munir, D.; Usman, M. R.

    2016-08-01

    Mesoporous catalysts have shown great prospective for catalytic reactions due to their high surface area that aids better distribution of impregnated metal. They have been found to contain more adsorption sites and controlled pore diameter. Hydrocracking, in the presence of mesoporous catalyst is considered more efficient and higher conversion of larger molecules is observed as compared to the cracking reactions in smaller microporous cavities of traditional zeolites. In the present study, a number of silica-alumina based mesoporous catalysts are synthesized in the laboratory. The concentration and type of surfactants and quantities of silica and alumina sources are the variables studied in the preparation of catalyst supports. The supports prepared are well characterized using SEM, EDX, and N2-BET techniques. Finally, the catalysts are tested in a high pressure autoclave reactor to study the activity and selectivity of the catalysts for the hydrocracking of a model mixture of plastics comprising of LDPE, HDPE, PP, and PS.

  11. Preparation of magnetic core-mesoporous shell microspheres with C8-modified interior pore-walls and their application in selective enrichment and analysis of mouse brain peptidome.

    Science.gov (United States)

    Liu, Shasha; Li, Yan; Deng, Chunhui; Mao, Yu; Zhang, Xiangmin; Yang, Pengyuan

    2011-12-01

    In this paper, magnetic mesoporous silica microspheres with C8-modified interior pore-walls were prepared through a facile one-pot sol-gel coating strategy, and were successfully applied for selective enrichment of endogenous peptides in mouse brain for peptidome analysis. Through the one-pot sol-gel approach with surfactant (CTAB) as a template, tetraethyl orthosilicate (TEOS) and n-ctyltriethoxysilane (C8TEOS) as the precursors, C8-modified magnetic mesoporous microspheres (C8-Fe(3)O(4)@mSiO(2)) consisting magnetic core and mesoporous silica shell with C8-groups exposed in the mesopore channels were synthesized. The obtained microspheres possess highly open mesopores of 3.4 nm, high surface area (162.5 m(2)/g), large pore volume (0.17 cm(3)/g), excellent magnetic responsivity (56.3 emu/g) and good dispersibility in aqueous solution. Based on the abundant surface silanol groups, functional C8 groups and the strong magnetic responsivity of the core-shell C8-Fe(3) O(4) @mSiO(2) microspheres, efficient and fast enrichment of peptides was achieved. Additionally, the C8-Fe(3)O(4)@mSiO(2) microspheres exhibit excellent performance in selective enrichment of endogenous peptides from complex samples that are consist of peptides, large proteins and other compounds, including human serum and mouse brain followed by automated nano-LC-ESI-MS/MS analysis. These results indicate C8-Fe(3)O(4)@mSiO(2) microspheres would be a potential candidate for endogenous peptides enrichment and biomarkers discovery in peptidome analysis.

  12. Direct coating of mesoporous titania on CTAB-capped gold nanorods

    Science.gov (United States)

    Zhao, Junwei; Xu, Pengyu; Li, Yue; Wu, Jian; Xue, Junfei; Zhu, Qiannan; Lu, Xuxing; Ni, Weihai

    2016-03-01

    We demonstrate a CTAB-templated approach towards direct coating of mesoporous titania on gold nanorods in aqueous solutions. The formation of the mesoporous shell is found to be closely correlated with CTAB concentration and the amount of the titania precursor. This approach can be readily extended to form mesoporous titania shells on other CTAB-capped nanoparticles.We demonstrate a CTAB-templated approach towards direct coating of mesoporous titania on gold nanorods in aqueous solutions. The formation of the mesoporous shell is found to be closely correlated with CTAB concentration and the amount of the titania precursor. This approach can be readily extended to form mesoporous titania shells on other CTAB-capped nanoparticles. Electronic supplementary information (ESI) available: Experimental details including chemicals, sample preparation, and characterization methods. UV-Vis extinction spectra, SEM images, and TEM images of AuNR@mTiO2 nanostructures. See DOI: 10.1039/c5nr05692f

  13. Biodegradation-tunable mesoporous silica nanorods for controlled drug delivery.

    Science.gov (United States)

    Park, Sung Bum; Joo, Young-Ho; Kim, Hyunryung; Ryu, WonHyoung; Park, Yong-il

    2015-05-01

    Mesoporous silica in the forms of micro- or nanoparticles showed great potentials in the field of controlled drug delivery. However, for precision control of drug release from mesoporous silica-based delivery systems, it is critical to control the rate of biodegradation. Thus, in this study, we demonstrate a simple and robust method to fabricate "biodegradation-tunable" mesoporous silica nanorods based on capillary wetting of anodic aluminum oxide (AAO) template with an aqueous alkoxide precursor solution. The porosity and nanostructure of silica nanorods were conveniently controlled by adjusting the water/alkoxide molar ratio of precursor solutions, heat-treatment temperature, and Na addition. The porosity and biodegradation kinetics of the fabricated mesoporous nanorods were analyzed using N2 adsorption/desorption isotherm, TGA, DTA, and XRD. Finally, the performance of the mesoporous silica nanorods as drug delivery carrier was demonstrated with initial burst and subsequent "zero-order" release of anti-cancer drug, doxorubicin.

  14. Mesoporous zeolite and zeotype single crystals synthesized in fluoride media

    DEFF Research Database (Denmark)

    Egeblad, Kresten; Kustova, Marina; Klitgaard, Søren Kegnæs

    2007-01-01

    We report the synthesis and characterization of a series of new mesoporous zeolite and zeotype materials made available by combining new and improved procedures for directly introducing carbon into reaction mixtures with the fluoride route for conventional zeolite synthesis. The mesoporous...... characterized by XRPD, SEM, TEM and N-2 physisorption measurements. For the zeolite materials it A as found that mesoporous MFI and MEL structured single crystals could indeed be crystallized from fluoride media using an improved carbon-templating approach. More importantly, it was found that mesoporous BEA......-type single crystals could be crystallized from fluoride media by a newly developed procedure presented here. Thus, we here present the only known route to mesoporous BEA-type single crystals, since crystallization of this framework structure from basic media is known to give only nanosized crystals...

  15. Recovery of silica from electronic waste for the synthesis of cubic MCM-48 and its application in preparing ordered mesoporous carbon molecular sieves using a green approach

    Science.gov (United States)

    Liou, Tzong-Horng

    2012-07-01

    The electronics industry is one of the world's fastest growing manufacturing industries. However, e-waste has become a serious pollution problem. This study reports the recovery of e-waste for preparing valuable MCM-48 and ordered mesoporous carbon for the first time. Specifically, this study adopts an alkali-extracted method to obtain sodium silicate precursors from electronic packaging resin ash. The influence of synthesis variables such as gelation pH, neutral/cationic surfactant ratio, hydrothermal treatment temperature, and calcination temperature on the mesophase of MCM-48 materials is investigated. Experimental results confirm that well-ordered cubic MCM-48 materials were synthesized in strongly acidic and strongly basic media. The resulting mesoporous silica had a high surface area of 1,317 m2/g, mean pore size of about 3.0 nm, and a high purity of 99.87 wt%. Ordered mesoporous carbon with high surface area (1,715 m2/g) and uniform pore size of CMK-1 type was successfully prepared by impregnating MCM-48 template using the resin waste. The carbon structure was sensitive to the sulfuric acid concentration and carbonization temperature. Converting e-waste into MCM-48 materials not only eliminates the disposal problem of e-waste, but also transforms industrial waste into a useful nanomaterial.

  16. Crystallization of CaCO3 Induced by Mixed Template of Polymer and Surfactant%聚合物与表面活性剂混合模板调控碳酸钙结晶

    Institute of Scientific and Technical Information of China (English)

    丁红霞; 尹晓爽; 杨文忠

    2011-01-01

    以聚乙烯醇(PVA)和聚苯乙烯磺酸钠(PSSS)分别与十六烷基三甲基溴化铵(CTAB)组成混合模板,在CaCl2、Na2CO3体系中调控合成CaCO3晶体.考察了不同CTAB浓度及结晶温度对碳酸钙晶体的影响.通过扫描电子显微镜(SEM)、红外光谱(FT-IR)及X射线衍射(XRD)等技术对晶体的形貌和结构进行了表征,并对不同形貌碳酸钙的形成机理进行了探讨.结果表明:在PVA和CTAB模板中,5℃为方解石椭球状聚集体,25℃时为菊花状、立方状的方解石和球霰石的混晶,90℃时得到针状文石晶簇.以PSSS和CTAB模板调控下的碳酸钙,5℃时为球状的方解石和球霰石的混晶,25℃为颗粒均匀的球形球霰石,90℃时得到了花朵状文石.不同形貌及晶型碳酸钙的生成源自聚合物与CTAB组成复合物结构的差异.%Calcium carbonate was prepared by the Na2CO3 with CaCl2 in the mixed templates of polymer (PVA/PSSS) and surfactant (CTAB) at different temperatures and concentrations of CTAB. The products were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD). The results showed that in the PVA/CTAB system the ellipsoid aggregates of calcite could be prepared at 5 ℃ and rosette type and cubic aggregates of calcite and vaterite at 25 ℃ while druses of needle-like aragonite crystals were obtained at 90 ℃. In the PSSS/CTAB system, spherical precipitation of calcite and vaterite could be obtained at 5 ℃, uniform size of spherical vaterite were obtained at 25 ℃. At the temperature of 90 ℃, flower-like aragonite was precipitated. The different complex of polymer and CTAB resulted in the different morphology and crystal form of calcium carbonate

  17. Functional-template directed self-assembly (FTDSA) of mesostructured organic-inorganic hybrid materials

    Institute of Scientific and Technical Information of China (English)

    LI LeLe; SUN LingDong; ZHANG YaWen; YAN ChunHua

    2009-01-01

    Since the discovery of a surfactant directed self-assembly approach for the fabrication of mesoporous silica in 1992,increasing attention has been focused on the design and synthesis of mesostructured functional materials.Organic functionalization is becoming a major topic in this research field,since highly ordered mesostructured organic-inorganic hybrids offer novel functionalities and enhanced performance over their individual components.We begin with a brief overview of the three fundamental methods (post-synthetic grafting technique,co-condensation method,and preparation of periodic mesoporous organosilicas) for the preparation of organically functionalized mesostructured silica,and focus on one of the most promising approaches,which herein was named as functional-template directed self-assembly (FTDSA) approach,and in the eyes of the authors it has a special position in the preparation of this class of hybrid materials.A comprehensive overview of the state of research in the area of FTDSA and its potential applications will be given.

  18. Poly(vinyl chloride)-g-poly(2-(dimethylamino)ethyl methacrylate) graft copolymers templated synthesis of mesoporous TiO{sub 2} thin films for dye-sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Rajkumar; Ahn, Sung Hoon; Seo, Jin Ah; Kim, Sang Jin; Kim, Jong Hak, E-mail: jonghak@yonsei.ac.kr [Yonsei University, Department of Chemical and Biomolecular Engineering (Korea, Republic of)

    2012-07-15

    A poly(vinyl chloride) (PVC) main chain was grafted with poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA) containing a quaternary amine group using atom transfer radical polymerization. The successful synthesis of a PVC-g-PDMAEMA graft copolymer was confirmed by Fourier transform infrared, nuclear magnetic resonance, thermogravimetric analysis, and transmission electron microscopy. The PVC-g-PDMAEMA graft copolymer was used as a structure-directing agent (SDA) for the fabrication of a mesoporous thin film containing a titanium dioxide (TiO{sub 2}) layer. To control the porosity of the resultant inorganic layer, the ratio of SDA to TTIP as well as the concentration of the sol-gel was varied. The structure and porosity of the mesoporous film were characterized by XRD and SEM analysis. The mesoporous TiO{sub 2} film fabricated on the FTO surface was used as a photoanode for the dye-sensitized solar cell (DSSC). DSSC performance was the greatest when using TiO{sub 2} film with a higher porosity and lower interfacial resistance. The highest energy conversion efficiency reached 3.2 % at 100 mW/cm{sup 2}, which was one of the highest reported values for a quasi-solid-state DSSC with 600-nm-thick TiO{sub 2} film.

  19. Synthesis of periodic mesoporous organosilicas functionalized with different amine-organoalkoxysilanes via direct co-condensation

    Energy Technology Data Exchange (ETDEWEB)

    Suriyanon, Nakorn [International Postgraduate Programs in Environmental Management, Graduate School, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand); Center of Excellence for Environmental and Hazardous Waste Management (EHWM), Pathumwan, Bangkok 10330 (Thailand); Punyapalakul, Patiparn [Center of Excellence for Environmental and Hazardous Waste Management (EHWM), Pathumwan, Bangkok 10330 (Thailand); Department of Environmental Engineering, Faculty of Engineering, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand); Ngamcharussrivichai, Chawalit, E-mail: Chawalit.Ng@Chula.ac.th [Fuels Research Center, Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand); Center of Excellence on Petrochemical and Materials Technology (PETROMAT), Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand)

    2015-01-15

    A series of amine-functionalized periodic mesoporous organosilicas (PMOs) were synthesized from bis(triethoxysilyl)ethane via surfactant-templating using supramolecular assemblies of hexadecyltrimethylammonium chloride under basic conditions. Functionalization of the PMO materials was performed via direct co-condensation in the presence of mono-, di- or tri-amine-organoalkoxysilanes. The effect of the type and concentration of the added organosilanes on the physicochemical properties of the functionalized PMOs were investigated. Thermogravimetric/differential thermal analysis (TG/DTA) and Fourier transform infrared spectroscopy (FTIR) confirmed the presence of the inorganic–organic hybrid framework functionalized with the amine groups. The total nitrogen content of the functionalized PMOs ranged from 0.26 to 1.27 mmol/g. The materials possessed a hexagonal lattice with the highly ordered mesostructure being preserved after the amine-functionalization as evidenced by X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM). The N{sub 2} adsorption–desorption measurement revealed that the materials had high specific surface areas (963–1252 m{sup 2}/g) and a relatively high total pore volume (0.52–0.85 cm{sup 3}/g). The mesopore size and wall thickness of these materials varied in relation with the molecular size and the loading of the organosilanes. Moreover, the morphology of the PMO materials was increasingly transformed from irregular shaped particles to spheres with increasing amounts of amine-functional groups or with organo-functional groups with several amine units. - Highlights: • Periodic mesoporous organosilicas (PMOs) were functionalized via co-condensation. • Long-chain organosilane with three amine units was employed a precursor. • Hexagonal mesostructure of PMO was preserved at a 40 mol% loading level. • Amine-functionalized PMOs had a high surface area and total pore volume. • Their morphology depended on the

  20. Aluminum-rich mesoporous MFI - type zeolite single crystals

    DEFF Research Database (Denmark)

    Kustova, Marina; Kustov, Arkadii; Christensen, Christina Hviid

    2005-01-01

    . With this technique, only zeolites with relatively low Al contents were reported (Si/Al ratio about 100). In this work, the preparation of aluminum-rich mesoporous MFI-type zeolite single crystals (Si/Al similar to 16-50) using aluminum isopropoxide as the aluminum Source is reported for the first time. All samples......Zeolitcs are crystalline materials, which are widely used as solid acid catalysts and supports in many industrial processes. Recently, mesoporous MFI-type zeolite single crystals were synthesized by use of carbon particles as a mesopore template and sodium aluminate as the aluminum Source...

  1. Aluminum-rich mesoporous MFI - type zeolite single crystals

    DEFF Research Database (Denmark)

    Kustova, Marina; Kustov, Arkadii; Christensen, Christina Hviid

    2005-01-01

    Zeolitcs are crystalline materials, which are widely used as solid acid catalysts and supports in many industrial processes. Recently, mesoporous MFI-type zeolite single crystals were synthesized by use of carbon particles as a mesopore template and sodium aluminate as the aluminum Source...... are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), ammonia temperature programmed desorption (NH3-TPD), and N-2 adsorption measurements. The obtained zeolites combine the high crystallinity and the characteristic micropores of zeolites with an intracrystalline mesopore system...

  2. Synthesis of Mesoporous Silica and Ti-containing Molecular Sieves via A Novel Assembly

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Thermally stable mesoporous silica and Ti-containing molecular sieves have been synthesized at mild temperature using low-cost and biodegradable---amphoteric tetradecyl betaine as template. The physicochemical characterizations proved that Ti(Ⅳ) could be incorporated in the mesoporous struture.

  3. A highly ordered cubic mesoporous silica/graphene nanocomposite

    Science.gov (United States)

    Lee, Chang-Wook; Roh, Kwang Chul; Kim, Kwang-Bum

    2013-09-01

    A highly ordered cubic mesoporous silica (KIT-6)/graphene nanocomposite and 2D KIT-6 nanoflakes were synthesized using a novel synthesis methodology. The non-ionic triblock copolymer, P123, played a dual role as a structure-directing agent in the formation of the cubic mesoporous structure and as a cross-linking agent between mesoporous silica and graphene. The prepared (KIT-6)/graphene nanocomposite could act as a template for the preparation of mesoporous material/graphene nanocomposites.A highly ordered cubic mesoporous silica (KIT-6)/graphene nanocomposite and 2D KIT-6 nanoflakes were synthesized using a novel synthesis methodology. The non-ionic triblock copolymer, P123, played a dual role as a structure-directing agent in the formation of the cubic mesoporous structure and as a cross-linking agent between mesoporous silica and graphene. The prepared (KIT-6)/graphene nanocomposite could act as a template for the preparation of mesoporous material/graphene nanocomposites. Electronic supplementary information (ESI) available: S1: TEM images of disordered mesoporous silica/graphene nanocomposite; S2: TEM images of KIT-6/GO nanocomposite; S3: Thermogravimetric analysis of KIT-6/GO and KG-400-700; S4: SEM and TEM images of KIT-6; S5: Low angle XRD, Raman spectra, N2 adsorption isotherms, pore size distribution and photographic images of the prepared samples; S6: TEM image and N2 adsorption isotherms of mesoporous carbon/graphene nanocomposite; S7: XPS C1s spectra of the prepared samples. See DOI: 10.1039/c3nr03108j

  4. Preparation and characterization of mesoporous indium oxide

    Institute of Scientific and Technical Information of China (English)

    ZHAO Yi-zhe; CHENG Zhi-xuan; PAN Qing-yi; DONG Xiao-wen; ZHANG Jian-cheng; PAN Ling-li

    2009-01-01

    Indium oxide nanocrystals with mesoporous structure were successfully synthesized by using triblock copolymer as a template,and characterized by thermogravimetry-differential scanning calorimeter (TG-DSC),X-ray powder diffraction (XRD),high resolution transmission electron microscopy (HRTEM) and N2 adsorption.A high EO/PO ratio is thought to be the key point to prepare mesoporous In2O3.The results show that the average pore diameter of the products is 6 nm,the BET surface area is 54.78 m2/g,and the adsorbing pore volume is 0.345 cm3/g.After comparing with normal indium oxide nanoparticles by BET test,mesoporous indium oxide demonstrates a large difference in adsorbing pore volume and average pore diameters from normal ones.

  5. Improvement of surface acidity and structural regularity of Zr-modified mesoporous MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Chen, L.F. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico)]. E-mail: chenlf2001@yahoo.com; Norena, L.E. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico); Navarrete, J. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Wang, J.A. [Laboratorio de Catalisis y Materiales, SEPI-ESIQIE, Instituto Politecnico Nacional, Av. Politecnico S/N, Col. Zacatenco, 07738 Mexico D.F. (Mexico)

    2006-06-10

    This work reports the synthesis and surface characterization of a Zr-modified mesoporous MCM-41 solid with an ordered hexagonal arrangement, prepared through a templated synthesis route, using cetyltrimethylammonium chloride as the template. The surface features, crystalline structure, textural properties and surface acidity of the materials were characterized by in situ Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), N{sub 2} physisorption isotherms, {sup 29}Si MAS-NMR and in situ FT-IR of pyridine adsorption. It is evident that the surfactant cations inserted into the network of the solids during the preparation could be removed by calcination of the sample above 500 deg. C. The resultant material showed a large surface area of 680.6 m{sup 2} g{sup -1} with a uniform pore diameter distribution in a very narrow range centered at approximately 2.5 nm. Zirconium incorporation into the Si-MCM-41 framework, confirmed by {sup 29}Si MAS-NMR analysis, increased not only the wall thickness of the mesopores but also the long-range order of the periodically hexagonal structure. Both, Lewis and Broensted acid sites, were formed on the surface of the Zr-modified MCM-41 solid. Compared to Si-MCM-41 on which only very weak Lewis acid sites were formed, the densities of both Lewis and Broensted acid sites and the strength of the acidity on the Zr-modified sample were significantly increased, indicating that the incorporation of zirconium greatly enhances the acidity of the material.

  6. 碱法纳米纤维素模板剂合成介孔TiO2及其性能%Synthesis and Properties of Mesoporous TiO2 Using Nano-cellulose Template Prepared by Alkali Method

    Institute of Scientific and Technical Information of China (English)

    陈孝云; 陈星; 洪时伟; 陈筱; 黄彪

    2011-01-01

    Mesoporous TiO2 was synthesized by a hydrolysis-precipitation method using biological renewable resources of nano-cellulose as template and using TiCl4 as precursor. The photocatalytic activity of TiO2 was investigated by the degradation of phenol under ultraviolet light irradiation. Transmission electron microscopy, X-ray diffraction, thermogravimetry-differential thermal analysis, and N2 adsorp tion-desorption were used for catalyst characterization. The results showed that TiO2 synthesized with alkali nano-cellulose template exhib ited high activity under UV irradiation. The material had average size of about 13.5 nm in diameter and exhibited mesoporous structure with specific area of 176 m2/g and average pore size of 6.17 nm. The addition of alkali nano-cellulose template can retard phase transformation. The higher photocatalytic activity was attributed to the small grain size, more pores, and higher specific surface area of the catalyst.%以生物可再生资源碱法纳米纤维素为模板剂,TiCl4为钛源,采用液相水解-沉淀法合成了具有介孔结构的TiO2光催化剂,采用透射电镜、X射线衍射、热重差热、低温N2物理吸附-脱附等技术对催化剂进行了表征,并以苯酚为模型物,考察了介孔TiO2的光催化活性.结果表明,所得TiO2催化剂具有良好的孔隙结构,平均孔径6.17 nm、比表面积176.3 m2/g、平均晶粒尺寸13.5 nm.碱法纳米纤维素的加入在一定程度上提高了锐钛矿相向金红石相转变的温度.该TiO2晶粒小、孔隙较多、比表面积大、吸附性能强,因此表现出较高的光催化活性.

  7. Mesoporous carbon materials

    Science.gov (United States)

    Dai, Sheng; Fulvio, Pasquale Fernando; Mayes, Richard T.; Wang, Xiqing; Sun, Xiao-Guang; Guo, Bingkun

    2014-09-09

    A conductive mesoporous carbon composite comprising conductive carbon nanoparticles contained within a mesoporous carbon matrix, wherein the conductive mesoporous carbon composite possesses at least a portion of mesopores having a pore size of at least 10 nm and up to 50 nm, and wherein the mesopores are either within the mesoporous carbon matrix, or are spacings delineated by surfaces of said conductive carbon nanoparticles when said conductive carbon nanoparticles are fused with each other, or both. Methods for producing the above-described composite, devices incorporating them (e.g., lithium batteries), and methods of using them, are also described.

  8. Recycle of silicate waste into mesoporous materials.

    Science.gov (United States)

    Kim, Jung Ho; Kim, Minwoo; Yu, Jong-Sung

    2011-04-15

    Template synthesis of porous carbon materials usually requires selective removal of template silica from the carbon/silica composites. It not only involves waste of valuable chemicals, but also poses significant environmental concerns including high waste treatment cost. Recycling of silicates released from such nanocasting methods is successfully performed for the first time to regenerate valuable mesoporous MCM and SBA type silica materials, which will not only help in saving valuable chemicals, but also in decreasing chemical waste, contributing in improvement of our environmental standards. This approach can thus improve cost effectiveness for the mass production of nanostructured carbon and others utilizing silica directed nanocasting method by recycling otherwise silicate waste into highly desirable valuable mesoporous silica.

  9. Preliminary Synthesis and Characterization of Mesoporous Nanocrystalline Zirconia

    Institute of Scientific and Technical Information of China (English)

    Xinmei Liu; Gaoqing Lu; Zifeng Yan

    2003-01-01

    A novel method to prepare mesoporous nano-zirconia was developed. The synthesis was carried out in the presence of PEO surfactants via a solid-state reaction. The materials exhibit a strong diffraction peak at low 2θ angle and their nitrogen adsorption/desorption isotherms are typical of type Ⅳ with H1 hysteresis loops. The pore structure imaged by TEM can be described as wormhole domains.The tetragonal zirconia nanocrystals are uniform in size (around 1.5 nm) and their mesopores focus on around 4.6 nm. The zirconia nanocrystal growth is tentatively postulated to be the result of an aggregation mechanism. This study also reveals that the PEO surfactants can interact with the Zr-O-Zr framework to reinforce the thermal stability of zirconia. The ratio of NaOH to ZrOC12, crystallization and calcination temperature play an important role in the synthesis of mesoporous nano-zirconia.

  10. Large-scale, three-dimensional, free-standing, and mesoporous metal oxide networks for high-performance photocatalysis.

    Science.gov (United States)

    Bai, Hua; Li, Xinshi; Hu, Chao; Zhang, Xuan; Li, Junfang; Yan, Yan; Xi, Guangcheng

    2013-01-01

    Mesoporous nanostructures represent a unique class of photocatalysts with many applications, including splitting of water, degradation of organic contaminants, and reduction of carbon dioxide. In this work, we report a general Lewis acid catalytic template route for the high-yield producing single- and multi-component large-scale three-dimensional (3D) mesoporous metal oxide networks. The large-scale 3D mesoporous metal oxide networks possess large macroscopic scale (millimeter-sized) and mesoporous nanostructure with huge pore volume and large surface exposure area. This method also can be used for the synthesis of large-scale 3D macro/mesoporous hierarchical porous materials and noble metal nanoparticles loaded 3D mesoporous networks. Photocatalytic degradation of Azo dyes demonstrated that the large-scale 3D mesoporous metal oxide networks enable high photocatalytic activity. The present synthetic method can serve as the new design concept for functional 3D mesoporous nanomaterials.

  11. Large-Scale, Three-Dimensional, Free-Standing, and Mesoporous Metal Oxide Networks for High-Performance Photocatalysis

    Science.gov (United States)

    Bai, Hua; Li, Xinshi; Hu, Chao; Zhang, Xuan; Li, Junfang; Yan, Yan; Xi, Guangcheng

    2013-07-01

    Mesoporous nanostructures represent a unique class of photocatalysts with many applications, including splitting of water, degradation of organic contaminants, and reduction of carbon dioxide. In this work, we report a general Lewis acid catalytic template route for the high-yield producing single- and multi-component large-scale three-dimensional (3D) mesoporous metal oxide networks. The large-scale 3D mesoporous metal oxide networks possess large macroscopic scale (millimeter-sized) and mesoporous nanostructure with huge pore volume and large surface exposure area. This method also can be used for the synthesis of large-scale 3D macro/mesoporous hierarchical porous materials and noble metal nanoparticles loaded 3D mesoporous networks. Photocatalytic degradation of Azo dyes demonstrated that the large-scale 3D mesoporous metal oxide networks enable high photocatalytic activity. The present synthetic method can serve as the new design concept for functional 3D mesoporous nanomaterials.

  12. Preparation of Hierarchical Mesoporous TiO2 Nanosheet Using China Rose Petal as Template%以花瓣为模板制备TiO2分层介孔纳米片

    Institute of Scientific and Technical Information of China (English)

    赵晓兵; 王芳; 钱君超

    2012-01-01

    Hierarchical mesoporous TiO2 nanosheets were prepared using China rose petal as biotemplate through facile infiltration and thermal decomposition. For characterization of texture, X-ray diffraction spec-troscopy( XRD) , field emission scanning electron microscopy ( FESEM), transmission electron microscopy (TEM) , UV-Vis diffuse reflectance spectra(UV-Vis/DRS) and nitrogen adsorption-desorption measurements were adopted. The results demonstrate that the biomorphic structure of anatase TiO2 nanosheets with the thickness of ca. 4 nm is obtained. There exist mesopores with pore size of about 4 nm on the surface of the TiO2 nanosheets. Hierarchical mesoporous TiO2 nanosheets exhibit a clear red shift(20 nm) comparing with Degus-sa P25, which could be excited by visible irradiation and enhance the visible activity. Hierarchical mesoporous TiO2 nanosheets display the superior photocatalytic activity for the degradation of methylene blue under sunlight irradiation, with a which degradation rate as high as 98%.%以月季花花瓣为模板,经钛盐溶液浸渍后煅烧,合成了新型TiO2分层介孔纳米片.采用X射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、环境扫描电子显微镜(ESEM)、透射电子显微镜(TEM)、紫外-可见漫反射光谱(UV-Vis/DRS)和氮气吸附-脱附曲线分析等手段对样品进行了表征.结果表明,所得样品由厚度约4 nm的具有生物形态结构的锐钛矿型TiO2纳米片组成.TiO2薄层表面存在大量介孔,其孔径集中分布于4 nm左右.由紫外-可见漫反射吸收光谱可知,材料的吸收边较纳米TiO2(P25)红移了约20 nm,因而具有更高的可见光光催化活性.TiO2分层介孔纳米片在阳光下表现出较强的光催化活性,在90 min内对亚甲基蓝的降解率可达98%,远高于TiO2纳米粉.

  13. Multifunctional mesoporous silica catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Victor Shang-Yi; Tsai, Chih-Hsiang; Chen, Hung-Ting; Pruski, Marek; Kobayashi, Takeshi

    2015-03-31

    The present invention provides bifunctional silica mesoporous materials, including mesoporous silica nanoparticles ("MSN"), having pores modified with diarylammonium triflate and perfluoroaryl moieties, that are useful for the acid-catalyzed esterification of organic acids with organic alcohols.

  14. Progress of the Application of Mesoporous Silica-Supported Heteropolyacids in Heterogeneous Catalysis and Preparation of Nanostructured Metal Oxides

    Directory of Open Access Journals (Sweden)

    Heyong He

    2010-01-01

    Full Text Available Mesoporous silica molecular sieves are a kind of unique catalyst support due to their large pore size and high surface area. Several methods have been developed to immobilize heteropolyacids (HPAs inside the channels of these mesoporous silicas. The mesoporous silica-supported HPA materials have been widely used as recyclable catalysts in heterogeneous systems. They have shown high catalytic activities and shape selectivities in some reactions, compared to the parent HPAs in homogeneous systems. This review summarizes recent progress in the field of mesoporous silica-supported HPAs applied in the heterogeneous catalysis area and preparation of nanostructured metal oxides using HPAs as precursors and mesoporous silicas as hard templates.

  15. Triply Periodic Multiply Continuous Lyotropic Liquid Crystals Derived from Gemini Surfactants

    Science.gov (United States)

    Sorenson, Gregory P.

    A subtle balance of non-covalent interactions directs the self-assembly of small molecule amphiphiles in aqueous media into supramolecular assemblies known as aqueous lyotropic liquid crystals (LLCs). Aqueous LLCs form many intricate, ordered nanoscale morphologies comprising distinct and structurally periodic hydrophobic and hydrophilic domains. Triply periodic multiply continuous (TPMC) LLC morphologies, which exhibit continuous hydrophobic and aqueous domains that percolate in three-dimensions, are of particular interest by virtue of their potentially wide ranging technological applications including advanced membranes for electrical energy storage and utilization, therapeutic delivery, and templates for new organic and inorganic mesoporous materials. However, robust molecular design criteria for amphiphiles that readily form TMPC morphologies are notably lacking in the literature. Recent reports have described the increased propensity for quaternary ammonium and phosphonium gemini surfactants, derived from dimerization of traditional single-tail surfactants at or near the hydrophilic headgroups through a hydrophobic linker, to stabilize TMPC mesophases. The generality of this surfactant design strategy remains untested in other amphiphiles classes bearing different headgroup chemistries. In this thesis, we describe the unusual aqueous LLC phase behavior of series of gemini dicarboxylate amphiphiles as a function of the alkyl tail length, hydrophobic linker length, and the charge-compensating counterion. These dicarboxylate surfactants unexpectedly exhibit a strong propensity to form TPMC LLCs over amphiphile concentration windows as wide as 20 wt% over a temperature range T = 25--100 °C. Through systematic modifications of the length of the hydrophobic linker and alkyl tails, we use small-angle X-ray scattering to demonstrate that these surfactants adopt new LLC mesophases including the first report of a single-gyroid phase (I4132 symmetry) and a new

  16. Luminescent Organic–Inorganic Hybrids of Functionalized Mesoporous Silica SBA-15 by Thio-Salicylidene Schiff Base

    Directory of Open Access Journals (Sweden)

    Li Ying

    2010-01-01

    Full Text Available Abstract Novel organic–inorganic mesoporous luminescent hybrid material N, N′-bis(salicylidene-thiocarbohydrazide (BSTC-SBA-15 has been obtained by co-condensation of tetraethyl orthosilicate and the organosilane in the presence of Pluronic P123 surfactant as a template. N,N′-bis(salicylidene-thiocarbohydrazide (BSTC grafted to the coupling agent 3-(triethoxysilyl-propyl isocyanate (TESPIC was used as the precursor for the preparation of mesoporous materials. In addition, for comparison, SBA-15 doped with organic ligand BSTC was also synthesized, denoted as BSTC/SBA-15. This organic–inorganic hybrid material was well-characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy (HRTEM, and photoluminescence spectra, which reveals that they all have high surface area, uniformity in the mesostructure. The resulting materials (BSTC-SBA-15 and BSTC/SBA-15 exhibit regular uniform microstructures, and no phase separation happened for the organic and the inorganic compounds was covalently linked through Si–O bonds via a self-assemble process. Furthermore, the two materials have different luminescence range: BSTC/SBA-15 presents the strong dominant green luminescence, while BSTC-functionalized material BSTC-SBA-15 shows the dominant blue emission.

  17. Ordered mesoporous NiO with thin pore walls and its enhanced sensing performance for formaldehyde.

    Science.gov (United States)

    Lai, Xiaoyong; Shen, Guoxin; Xue, Ping; Yan, Bingqin; Wang, Hong; Li, Peng; Xia, Weitao; Fang, Junzhuo

    2015-03-07

    A class of formaldehyde (HCHO) gas sensors with a high response were developed based on ordered mesoporous NiO, which were synthesized via the nanocasting route by directly using mesoporous silica as the hard template. A series of mesoporous NiO with different textural parameters such as specific surface area, pore size, pore wall thickness were achieved by selecting mesoporous silica with different pore sizes as templates. The gas sensing properties for formaldehyde (HCHO) of the NiO specimens were examined. The results show that this mesoporous NiO possesses a much higher response to HCHO even at low concentration levels than the bulk NiO, and a larger specific surface area and pore size as well as thinner pore walls would be beneficial for enhancing the sensing properties of NiO.

  18. Switchable Surfactants

    National Research Council Canada - National Science Library

    Yingxin Liu; Philip G. Jessop; Michael Cunningham; Charles A. Eckert; Charles L. Liotta

    2006-01-01

    .... We report that long-chain alkyl amidine compounds can be reversibly transformed into charged surfactants by exposure to an atmosphere of carbon dioxide, thereby stabilizing water/alkane emulsions...

  19. Formation of monodisperse mesoporous silica microparticles via spray-drying.

    Science.gov (United States)

    Waldron, Kathryn; Wu, Winston Duo; Wu, Zhangxiong; Liu, Wenjie; Selomulya, Cordelia; Zhao, Dongyuan; Chen, Xiao Dong

    2014-03-15

    In this work, a protocol to synthesize monodisperse mesoporous silica microparticles via a unique microfluidic jet spray-drying route is reported for the first time. The microparticles demonstrated highly ordered hexagonal mesostructures with surface areas ranging from ~900 up to 1500 m(2)/g and pore volumes from ~0.6 to 0.8 cm(3)/g. The particle size could be easily controlled from ~50 to 100 μm from the same diameter nozzle via changing the initial solute content, or changing the drying temperature. The ratio of the surfactant (CTAB) and silica (TEOS), and the amount of water in the precursor were found to affect the degree of ordering of mesopores by promoting either the self-assembly of the surfactant-silica micelles or the condensation of the silica as two competing processes in evaporation induced self-assembly. The drying rate and the curvature of particles also affected the self-assembly of the mesostructure. The particle mesostructure is not influenced by the inlet drying temperature in the range of 92-160 °C, with even a relatively low temperature of 92 °C producing highly ordered mesoporous microparticles. The spray-drying derived mesoporous silica microparticles, while of larger sizes and more rapidly synthesized, showed a comparable performance with the conventional mesoporous silica MCM-41 in controlled release of a dye, Rhodamine B, indicating that these spray dried microparticles could be used for the immobilisation and controlled release of small molecules.

  20. Comparative studies of Zr-based MCM-41 and MCM-48 mesoporous molecular sieves: Synthesis and physicochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Chen, L.F. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico)]. E-mail: chenlf2001@yahoo.com; Zhou, X.L. [Petroleum Processing Research Center, East China University of Science and Technology, 200237 Shanghai (China); Norena, L.E. [Departamento de Ciencias Basicas, Universidad Autonoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 Mexico D.F. (Mexico)]. E-mail: lnf@correo.azc.uam.mx; Wang, J.A. [Laboratorio de Catalisis y Materiales, SEPI-ESIQIE, Instituto Politecnico Nacional, Av. Politecnico S/N, Col. Zacatenco, 07738 Mexico D.F. (Mexico); Navarrete, J. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Salas, P. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Montoya, A. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Del Angel, P. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Llanos, M.E. [Grupo de Molecular Ingenieria, Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico)

    2006-12-30

    Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using different Si sources but keeping the same zirconium precursor (zirconium-n-propoxide). When fumed silica was used as Si precursor, a Zr-MCM-48 material of cubic structure was formed with a surface area of 654.8 m{sup 2}/g and an unimodal pore diameter distribution. It shows low stability: after calcination at 600 deg. C, the ordered structure was transformed into a relatively disordered worm-like mesostructure with many defects and silanol groups. The use of tetraethyl orthosilicate as Si source led to the formation of a Zr-MCM-41 mesoporous solid, which had good thermal stability and a highly ordered hexagonal arrangement, with a surface area 677.9 m{sup 2}/g and an uniform pore diameter distribution. Fourier transform infrared (FT-IR) characterization and {sup 29}Si NMR analysis confirm that zirconium ions indeed incorporated into the framework of the solid. The in situ FT-IR spectroscopy of pyridine adsorption reveals that both, Lewis and Broensted acid sites, were formed on the surface of these mesoporous materials. The strength and number of the Broensted acid sites of the Zr-MCM-48 solid were greater than those of the Zr-MCM-41, due to a lower degree of condensation reaction during the synthesis that led to more structural defects in the framework and more silanol groups stretching from the solid surface.

  1. Improvement of the activation of lipase from Candida rugosa following physical and chemical immobilization on modified mesoporous silica.

    Science.gov (United States)

    Wang, Chunfeng; Li, Yanjing; Zhou, Guowei; Jiang, Xiaojie; Xu, Yunqiang; Bu, Zhaosheng

    2014-12-01

    Lipase from Candida rugosa (CRL) was chemically and physically immobilized onto four types of rod-shaped mesoporous silica (RSMS). RSMS prepared using surfactant P123 and poly(ethylene glycol) as co-templates was functionalized with (3-aminopropyl)triethoxysilane (APTES) to obtain P-RSMS by post-synthesis grafting. Tetraethoxysilane was hydrothermally co-condensed with APTES to obtain C-RSMS. A two-step process using APTES and glutaraldehyde was also performed to obtain G-RSMS. The effects of modification methods (including post-synthesis grafting and co-condensation) and glutaraldehyde on the mesoscopic order, interplanar spacing d100, cell parameter a0, mesoporous structure, and wall thickness of RSMS were studied in detail. Results showed that all samples were mesoporous materials with 2D mesostructures (p6mm). Pore size and d100 decreased, whereas the wall thickness increased after different modifications. CRL was used as a model enzyme to determine the effect of physical and chemical adsorption on loading amount and enzymatic activity. The possible mechanism of CRL immobilization on G-RSMS by chemical adsorption was systematically investigated. The chemical immobilization of CRL on G-RSMS increased the loading amount, hydrolytic activity, thermal stability, and reusability. Moreover, immobilized CRL was employed to catalyze the resolution of 2-octanol by esterification with caprylic acid. The enantiomeric excess of 2-octanol was 45.8% when the reaction was catalyzed by G-RSMS-CRL and decreased to about 38%-39% using the physically immobilized CRL, after 48 h of reaction in hexane. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Synthesis of mesoporous Beta and Sn-Beta zeolites and their catalytic performances.

    Science.gov (United States)

    Jin, Junjiang; Ye, Xinxin; Li, Yongsheng; Wang, Yanqin; Li, Liang; Gu, Jinlou; Zhao, Wenru; Shi, Jianlin

    2014-06-14

    Mesoporous Beta zeolite has been successfully prepared through hydrothermal synthesis in the presence of cationic ammonium-modified chitosan as the meso-template. Through a subsequent solid-gas reaction between highly dealuminated mesoporous Beta zeolite and SnCl4 steam at an elevated temperature, mesoporous Sn-Beta has been facilely obtained. It was revealed that the addition of cationic chitosan induced the nanocrystal aggregation to particle sizes of ∼300 nm, giving rise to the intercrystalline/interparticle mesoporosity. In the Sn-implanting procedure, Sn species were demonstrated to be doped into the framework of the resulting mesoporous Beta zeolite in a tetrahedral environment without structural collapse. Due to the micro/mesoporous structures, both mesoporous Beta and Sn-Beta exhibited superior performances in α-pinene isomerization, Baeyer-Villiger oxidation of 2-adamantanone by hydrogen peroxide and the isomerization of glucose in water, respectively.

  3. Synthesis, characterization and catalytic activity of a novel mesoporous ZSM-5 zeolite

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Yuanyuan [College of Chemistry, Jilin University, Changchun 130023 (China); Key Laboratory of Fine Chemicals of College of Heilongjiang Province, Qiqihar University, Qiqihar 161006 (China); Hu, Jing [College of Chemistry, Jilin University, Changchun 130023 (China); Jia, Lihua [Key Laboratory of Fine Chemicals of College of Heilongjiang Province, Qiqihar University, Qiqihar 161006 (China); Li, Zhifang [College of Chemistry, Jilin University, Changchun 130023 (China); Kan, Qiubin, E-mail: catalysischina@yahoo.com.cn [College of Chemistry, Jilin University, Changchun 130023 (China); Wu, Shujie, E-mail: wusj@jlu.edu.cn [College of Chemistry, Jilin University, Changchun 130023 (China)

    2013-05-15

    Highlights: ► Mesoporous ZSM-5 zeolites. ► The strong acidic intensity. ► High activity for the alkylation of phenol and tert-butyl alcohol. ► Remarkable hydrothermal stability. - Abstract: A novel mesoporous ZSM-5 zeolite was hydrothermally synthesized using glucose as a template. Characterizations by XRD, TEM and nitrogen isotherms indicated that ZSM-5 possessed worm-like mesoporous. {sup 27}Al-MAS-NMR and NH{sub 3}-TPD showed that the mesoporous ZSM-5 preserved tetrahedral coordination aluminum and stronger acidity than conventional mesoporous material. As-prepared mesoporous ZSM-5 was successfully used in alkylation reaction of phenol with tert-butanol and exhibited significantly high phenol conversion and 2,4-DTBP selectivity. In addition, the hydrothermal stability was also studied by boiling in water for 7 days and displayed good results.

  4. Synthesis and characterization of surface-modified mesoporous silica materials with β-cyclodextrin

    OpenAIRE

    Sarker T. Mahmud; Lee D. Wilson

    2016-01-01

    Mesoporous silica materials containing microporous cavities provided by surface-bound β-cyclodextrin (CD ICS) were synthesized by co-condensation of a β-CD-functionalized triethoxysilane (CD ICL) with TEOS using dodecylamine, tetradecylamine, or hexadecylamine surfactants as structure directing agents. The incorporation of β-CD within the mesoporous framework was supported by IR, Raman, MALDI TOF MS, 13C solids CP-MAS NMR, and TGA results. Small-angle X-ray diffraction and nitrogen adsorption...

  5. Salt-free vesicle-phases and their template effect

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Researches on the construction, structure, and formation of vesicles formed from surfactants have attracted great attention from colloid and interface chemists. The vesicles formed from salt-free cationic-anionic surfactant systems are very different from those with excess salts, having many particular properties. In this paper, we introduce the properties of vesicles prepared from salt-free surfactant systems, according to our own results, especially the vesicles formed from surfactants with divalent metal ions as counterions in aqueous solutions and room temperature ionic liquids. Moreover, the primary results on template effect of the metal-ligand vesicles have also been summarized.

  6. Synthesis and Photocatalytic Activity of Mesoporous TiO2 Using Nano-Cellulose Template Prepared by Acid Method%酸法纳米纤维素模板剂合成介孔TiO2及光催化活性

    Institute of Scientific and Technical Information of China (English)

    陈孝云; 陆东芳; 陈彦; 谭非

    2013-01-01

    Mesoporous TiO2 was synthesized by a hydrolysis-precipitation method using a renewable biological resource of nano-cellulose as the template and TiCl4 as the precursor. The photocatalytic activity of TiO2 was evaluated using the degradation of methyl orange under ultraviolet light irradiation as a model reaction. N2 adsorption-desorption, transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetry-differential Scanning Calorimetry (TG/DSC), fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) were used for catalyst characterization. The results show that TiO2 synthesized with acid nano-cellulose template exhibits high activity under UV irradiation. The material exhibits mesoporous structure with specific area of 192 m2·g-1, average pore size of 5.03 nm, and pore volume of 0.35 cm3·g-1. The addition of acid nano-cellulose template can reduce the amount of surface OH- of TiO2, hydroxyl groups of long-chain cellulose and surface hydroxyl groups of TiO2 bonding can inhibit the TiO2 precursor growth and aggregation, and inhibit the phase transformation from anatase to rutile.%以生物可再生资源的酸法纳米纤维素为模板剂,四氯化钛为钛源,采用液相水解-沉淀法制备了具有介孔结构的TiO2光催化剂.采用低温N2物理吸附-脱附、透射电镜(TEM)、X射线衍射(XRD)、热重-量热扫描(TG/DSC)、傅里叶变换红外(FTIR)、X射线光电子能谱(XPS)等对介孔TiO2进行了表征,并以甲基橙为模型物,考察了介孔TiO2光催化活性.结果表明,以酸法纳米纤维素为模板剂合成的TiO2光催化活性显著提高,且具有良好的孔隙结构,平均孔径5.03 nm、总孔容积0.35 cm3·g-1、比表面积192m2· g-1;纤维素模板剂合成的TiO2表面羟基数量降低;纤维素长链分子结构之间的羟基与TiO2表面羟基的键合,可有效限制TiO2前驱体的生长和团聚,并抑制锐钛矿相TiO2向金红石相转变.

  7. SYNTHESIS AND COATING OF ORDERED MESOPOROUS SILICA

    Institute of Scientific and Technical Information of China (English)

    Wei Guo; Guangsheng Luo; Yujun Wang

    2003-01-01

    1,3,5-trimethyl benzene (TMB) was used as organic swelling agent in O/W emulsions to template ultra-large mesoporous materials using the hydrothermal method. The silicas with well-defined mesopores and hydrothermally robust framework were characterized by X-ray diffraction, transmission electron microscopy and BET surface area analysis. The influence of the quantity of TMB during preparation was studied. It has been found that the TMB/CTAB ratio must be controlled for producing high pore volume materials. Polysulfone (PSU), as the usual extraction agent, was coated on the silicas with the solvent evaporation method to produce a solid separation medium. The adsorptivity and the surface area of the coated MCM were determined: 10% PSU coated MCM adsorbed twice as much phenol as the uncoated material, reaching 0.5 mg/g silica. It was found that the surface area of the coated material decreased rapidly with an increase of the PSU loading.

  8. Preparation of Mesoporous Hollow Spheres of Silica and Titania Using Melamine Formaldehyde Microspheres as Templates%以三聚氰胺甲醛微球为模板制备介孔二氧化硅和二氧化钛空心微球

    Institute of Scientific and Technical Information of China (English)

    房洪杰; 刘慧; 闫芳; 李洪亮

    2015-01-01

    以聚合物三聚氰胺甲醛(MF)微球为模板,十六烷基三甲基溴化铵(CTAB)为致孔剂,经溶胶–凝胶和高温煅烧两步法,制备了SiO2和TiO2介孔结构的空心微球。以亚甲基蓝水溶液为模型物,分别评价了SiO2和TiO2微球的吸附性能和光催化活性。对空心微球的结构、形貌和光谱性质进行了表征。结果表明:两种微球的粒径为300 nm 左右,具有完整的球形空腔、较高的比表面积和介孔结构壳层;SiO2空心微球具有良好的吸附性能,而 TiO2空心微球在紫外光照射下有高效的光催化活性。%Mesoporous hollow spheres consisting of SiO2 or TiO2 were prepared with melamine formaldehyde microspheres as a core template and hexadecyl trimethyl ammonium bromide as a pore directing agent via a sol-gel process and subsequent calcination. The adsorption property of SiO2 hollow spheres and photocatalytic degradation activity of TiO2 hollow spheres to methylene blue (MB) were investigated, respectively.The structure, morphology, composition and optical properties of the resultant hollow sphere were characterized. The results show that the hollow spheres with the diameter of 300 nm, the relative large specific surface area and the mesoporous shell can be obtained. The SiO2 hollow spheres show an intensive adsorption performance to MB. The TiO2 hollow spheres have the superior photocatalytic degradation property under an ultraviolet light equipped.

  9. Organized thiol functional groups in mesoporous core shell colloids

    Energy Technology Data Exchange (ETDEWEB)

    Marchena, Martin H. [Gerencia Quimica, Centro Atomico Constituyentes, Comision Nacional de Energia Atomica (CNEA), Avda. Gral. Paz 1499, B1650KNA Buenos Aires (Argentina); Granada, Mara [Centro Atomico Bariloche-CNEA, 8400 San Carlos de Bariloche (Argentina); Instituto Balseiro-Centro Atomico Bariloche-CNEA, San Carlos de Bariloche 8400 (Argentina); Bordoni, Andrea V. [Gerencia Quimica, Centro Atomico Constituyentes, Comision Nacional de Energia Atomica (CNEA), Avda. Gral. Paz 1499, B1650KNA Buenos Aires (Argentina); Joselevich, Maria [Asociacion Civil Expedicion Ciencia, Cabrera 4948, C1414BGP Buenos Aires (Argentina); Troiani, Horacio [Centro Atomico Bariloche-CNEA, 8400 San Carlos de Bariloche (Argentina); Instituto Balseiro-Centro Atomico Bariloche-CNEA, San Carlos de Bariloche 8400 (Argentina); Williams, Federico J. [DQIAQyF-INQUIMAE FCEN, Universidad de Buenos Aires, Ciudad Universitaria, Pabellon II, C1428EHA Buenos Aires (Argentina); Wolosiuk, Alejandro, E-mail: wolosiuk@cnea.gov.ar [Gerencia Quimica, Centro Atomico Constituyentes, Comision Nacional de Energia Atomica (CNEA), Avda. Gral. Paz 1499, B1650KNA Buenos Aires (Argentina)

    2012-03-15

    The co-condensation in situ of tetraethoxysilane (TEOS) and mercaptopropyltrimethoxysilane (MPTMS) using cetyltrimethylammonium bromide (CTAB) as a template results in the synthesis of multilayered mesoporous structured SiO{sub 2} colloids with 'onion-like' chemical environments. Thiol groups were anchored to an inner selected SiO{sub 2} porous layer in a bilayered core shell particle producing different chemical regions inside the colloidal layered structure. X-Ray Photoelectron Spectroscopy (XPS) shows a preferential anchoring of the -SH groups in the double layer shell system, while porosimetry and simple chemical modifications confirm that pores are accessible. We can envision the synthesis of interesting colloidal objects with defined chemical environments with highly controlled properties. - Graphical abstract: Mesoporous core shell SiO{sub 2} colloids with organized thiol groups. Highlights: Black-Right-Pointing-Pointer Double shell mesoporous silica colloids templated with CTAB. Black-Right-Pointing-Pointer Sequential deposition of mesoporous SiO{sub 2} layers with different chemistries. Black-Right-Pointing-Pointer XPS shows the selective functionalization of mesoporous layers with thiol groups.

  10. A NEW CLASS MESOPOROUS ALUMINOPHOSPHATES AS POTENTIAL CATALYSTS IN THE UPGRADING PETROLEUM FEEDSTOCKS

    Energy Technology Data Exchange (ETDEWEB)

    Conrad Ingram; Mark Mitchell

    2005-08-31

    A comprehensive investigation was conducted towards the synthesis and catalytic evaluation of high surface areas, uniform pore size, mesoporous aluminophosphates (AlPO{sub 4}) as potential catalysts for the upgrading of heavy petroleum feedstock, such as heavy crudes and petroleum residuum. The influence of several synthesis variables (including, the nature of the reactants, chemical composition of reaction mixtures, time and temperature) on the synthesis and physicochemical characteristics of the resulting products was explored. Phosphoric acid and three different aluminum sources, namely, aluminum hydroxide, aluminum isopropoxide and psuedobohemite alumina, were used as the inorganic precursors. Cetyltrimethylammonium chloride (C{sub 16}TACl) surfactant was used as charge compensating cation and structure directing agent in the surfactant-micellar-mediated synthesis pathway employed. Synthesis were conducted from reaction mixtures within the following typical molar composition range: xAl{sub 2}O{sub 3}:P{sub 2}O{sub 5}:yC{sub 16}TMACl: zTHMAOH: wH{sub 2}O, where x = 0.29-2.34, y = 0.24-0.98, z = 0.34-1.95, w = 86-700. Selected materials were evaluated for the conversion of isopropylbenzene (cumene) in order to understand the nature of any acid sites created. The synthesis products obtained depended strongly on the molar composition of the synthesis mixture. A lamellar (layered) phase was favored by synthesis mixtures comprised of low Al/P ratios (<0.33), low TMAOH content, high C{sub 16}TACl concentrations and high synthesis temperature (110 C). Formation of the desired hexagonal (tubular) phase was favored by higher Al/P ratios and TMAOH content, pH range between 8-10, low C{sub 16}TACl concentration and ambient temperature. The aluminum source had significant influence on the products obtained. With aluminum hydroxide (A1(OH){sub 3}) as the hydroxide source, the resulting hexagonal phase in the ''as-synthesized'' form demonstrated well

  11. Synthesis of ordered mesoporous uranium dioxide by a nanocasting route

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Ran; Wang Lin; Shi, Wei-Qun [Chinese Academy of Sciences, Beijing (China). Laboratory of Nuclear Energy Chemistry and Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety; Chai, Zhi-Fang [Chinese Academy of Sciences, Beijing (China). Laboratory of Nuclear Energy Chemistry and Key Laboratory for Biomedical Effects of Nanomaterials and Nanosafety; Soochow Univ., Suzhou (China). School of Radiological and Interdisciplinary Sciences and Collaborative Innovation Center

    2016-11-01

    Ordered mesoporous UO{sub 2} with 3-D structure (for UO{sub 2}-KIT-6) and nanowire bundles (for UO{sub 2}-SBA-15) was synthesized for the first time by a nanocasting route using different ordered mesoporous silica (KIT-6 and SBA-15, respectively) as templates and uranyl nitrate hexahydrate as the metal precursor. The uranyl nitrate was impregnated into the mesopore of the silica template and was converted to U{sub 3}O{sub 8} after the first step. The synthesis of ordered UO{sub 2} mesostructure was achieved by reducing the mesoporous U{sub 3}O{sub 8} with silica composites under 5% H{sub 2}/Ar atmosphere at 700 C, followed by a template removal process. The as-prepared UO{sub 2}-KIT-6 had a particle size of several millimeters, and was constructed with uncoupled subframework mesostructure and crystalline walls, while UO{sub 2}-SBA-15 possessed a rope-like morphology and consisted of nanowire arrays. The surface area and pore volume of ordered UO{sub 2} mesostructure are 47.2 m{sup 2} g{sup -1} and 0.23 cm{sup 3} g{sup -1} for the UO{sub 2}-KIT-6, and 54.4 m{sup 2} g{sup -1} and 0.28 cm{sup 3} g{sup -1} for the UO{sub 2}-SBA-15, respectively.

  12. Effects of Fe-doping on the photocatalytic activity of mesoporous TiO2 powders prepared by an ultrasonic method.

    Science.gov (United States)

    Zhou, Minghua; Yu, Jiaguo; Cheng, Bei

    2006-10-11

    Highly photoactive nanocrystalline mesoporous Fe-doped TiO(2) powders were prepared by the ultrasonic-induced hydrolysis reaction of tetrabutyl titanate (Ti(OC(4)H(9))(4)) in a ferric nitrate aqueous solution (pH 5) without using any templates or surfactants. The as-prepared samples were characterized by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), N(2) adsorption-desorption measurements, UV-visible adsorbance spectra (UV-vis) and X-ray photoelectron spectroscopy (XPS). The photocatalytic activities were evaluated by the photocatalytic oxidation of acetone in air. The results showed that all the Fe-doped TiO(2) samples prepared by ultrasonic methods were mesoporous nanocrystalline. A small amount of Fe(3+) ions in TiO(2) powders could obviously enhance their photocatalytic activity. The photocatalytic activity of Fe-doped TiO(2) powders prepared by this method and calcined at 400 degrees C exceeded that of Degussa P25 (P25) by a factor of more than two times at an optimal atomic ratio of Fe to Ti of 0.25. The high activities of the Fe-doped TiO(2) powders could be attributed to the results of the synergetic effects of Fe-doping, large BET specific surface area and small crystallite size.

  13. Research on the biological activity and doxorubicin release behavior in vitro of mesoporous bioactive SiO2-CaO-P2O5 glass nanospheres

    Science.gov (United States)

    Wang, Xiang; Wang, Gen; Zhang, Ying

    2017-10-01

    Mesoporous bioactive glass (MBG) nanospheres have been synthesized by a facile method of sacrificing template using cetyl trimethyl ammonium bromide (CTAB) as surfactant. The prepared MBG nanospheres possess high specific surface area (632 m2 g-1) as well as uniform size (∼100 nm). In addition, MBG nanospheres exhibited a quick in vitro bioactive response in simulated body fluids (SBF) and excellent bioactivity of inducing hydroxyapatite (HA) forming on the surface of MBG nanospheres. Furthermore, MBG nanospheres can sustain release of doxorubicin (DOX) with a higher encapsulation efficiency (63.6%) and show distinct degradation in PBS by releasing Si and Ca ions. The encapsulation efficiency and DOX release of MBG nanospheres could be controlled by mesoporous structure and local pH environment. The greater surface area and pore volumes of prepared MBG nanospheres are conducive to bioactive response and drug release in vitro. The amino groups in DOX can be easily protonated at acidic medium to become positively charged NH+3, which allow these drug molecules to be desorbed from the surface of MBG nanospheres via electrostatic effect. Therefore, the synthesized MBG nanospheres have a pH-sensitive drug release capability. In addition, the cytotoxicity of MBG nanospheres was assessed using a cell counting kit-8 (CCK-8), and results showed that the synthesized MBG nanospheres had no significant cytotoxicity to MC3T3 cells. These all indicated that as-prepared MBG nanospheres are promising candidates for bone tissue engineering.

  14. Container effect in nanocasting synthesis of mesoporous metal oxides.

    Science.gov (United States)

    Sun, Xiaohong; Shi, Yifeng; Zhang, Peng; Zheng, Chunming; Zheng, Xinyue; Zhang, Fan; Zhang, Yichi; Guan, Naijia; Zhao, Dongyuan; Stucky, Galen D

    2011-09-21

    We report a general reaction container effect in the nanocasting synthesis of mesoporous metal oxides. The size and shape of the container body in conjunction with simply modifying the container opening accessibility can be used to control the escape rate of water and other gas-phase byproducts in the calcination process, and subsequently affect the nanocrystal growth of the materials inside the mesopore space of the template. In this way, the particle size, mesostructure ordering, and crystallinity of the final product can be systemically controlled. The container effect also explain some of the problems with reproducibility in previously reported results.

  15. Mesoporous NiO-Samaria doped ceria fuel cell materials.

    Science.gov (United States)

    Eom, Tae Wook; Kim, Kyung Hwan; Kim, Jong Sung; Jo, Myung-Chan; Yoon, Hyon Hee; Park, Sang Joon

    2009-02-01

    The mesoporous NiO-SDC was synthesized using a cationic surfactant (cetyl-trimethylammonium bromide; CTAB) for obtaining wide triple-phase boundary (TPB) in solid oxide fuel cells (SOFCs). The microstructure of mesoporous NiO-SDC was characterized by XRD, SEM, BET, and HRTEM and the results showed that the mesoporous NiO-SDC with 6.3 nm pores could be obtained. After calcined at 600 degrees C, the surface area of NiO-SDC was 206 m2/g, which was sufficiently high for providing large TPB in SOFC anode. In addition, FT-IR measurements revealed that Ni(OH)2 and SDC were incorporated with amine group of CTAB.

  16. Adsorption characterization of gaseous volatile organic compound on mesoporous silica particles prepared from spent diatomaceous earth.

    Science.gov (United States)

    Bei, Lei-Lei; Tao, Hong; Ma, Chih-Ming; Shiue, Angus; Chang, Chang-Tang

    2014-04-01

    This study used spent diatomaceous earth (SDE) from drink processing as source of Si and cationic surfactant (CTAB) as a template for the synthesis of mesoporous silica Materials (MSM) through hydrothermal method. The MSM was characterized by Small-angle X-ray Diffraction (SXRD), Scanning Electron Microscopy (SEM), Thermo Gravimetric Analysis (TGA), Fourier Transform Infrared (FT-IR) spectroscopy and N2 adsorption-desorption analyzer. The results showed that the surface area, pore volume and pore size was roughly ranged from 880 to 1060 m2 g(-1), 1.05 cm3 g(-1) and 4.0 nm, respectively. The properties of the synthesized MSM were also compared with those prepared from pure silica sources (MCM-41) and got almost the same characteristics. The synthesized MSM was used as adsorbent at 25 degrees C with carrier gas of air. The adsorption equilibrium revealed that adsorption capacity of MSM was 59.6, 65.7, 69.6, 84.9 mg g(-1) while the acetone concentration was 600, 800, 1000 ppm, 1600 ppm respectively. Results showed that breakthrough curves correlate to the challenge vapor concentration, adsorbent loading, and the flow rate. The results obtained in the present work demonstrated that it was feasibility of using the SDE as a potential source of silica to prepare MSM.

  17. 5-Azacytidine delivered by mesoporous silica nanoparticles regulates the differentiation of P19 cells into cardiomyocytes

    Science.gov (United States)

    Cheng, Jin; Ding, Qian; Wang, Jia; Deng, Lin; Yang, Lu; Tao, Lei; Lei, Haihong; Lu, Shaoping

    2016-01-01

    Heart disease is one of the deadliest diseases causing mortality due to the limited regenerative capability of highly differentiated cardiomyocytes. Stem cell-based therapy in tissue engineering is one of the most exciting and rapidly growing areas and raises promising prospects for cardiac repair. In this study, we have synthesized FITC-mesoporous silica nanoparticles (FMSNs) based on a sol-gel method (known as Stöber's method) as a drug delivery platform to transport 5-azacytidine in P19 embryonic carcinoma stem cells. The surfactant CTAB is utilized as a liquid crystal template to self-aggregate into micelles, resulting in the synthesis of MSNs. Based on the cell viability assay, treatment with FMSNs + 5-azacytidine resulted in much more significant inhibition of the proliferation than 5-azacytidine alone. To study the mechanism, we have tested the differentiation genes and cardiac marker genes in P19 cells and found that these genes have been up-regulated in P19 embryonic carcinoma stem cells treated with FMSNs + 5-azacytidine + poly(allylamine hydrochloride) (PAH), with the changes of histone modifications on the regulatory region. In conclusion, with FMSNs as drug delivery platforms, 5-azacytidine can be more efficiently delivered into stem cells and can be used to monitor and track the transfection process in situ to clarify their effects on stem cell functions and the differentiation process, which can serve as a promising tool in tissue engineering and other biomedical fields.

  18. Synthesis of Hydrophobic Mesoporous Material MFS and Its Adsorption Properties of Water Vapor

    Directory of Open Access Journals (Sweden)

    Guotao Zhao

    2014-01-01

    Full Text Available Fluorine-containing hydrophobic mesoporous material (MFS with high surface area is successfully synthesized with hydrothermal synthesis method by using a perfluorinated surfactant SURFLON S-386 template. The adsorption properties of water vapor on the synthesized MFS are also investigated by using gravimetric method. Results show that SEM image of the MFS depicted roundish morphology with the average crystal size of 1-2 μm. The BET surface area and total pore volume of the MFS are 865.4 m2 g−1 and 0.74 cm3 g−1 with a narrow pore size distribution at 4.9 nm. The amount of water vapor on the MFS is about 0.41 mmol g−1 at 303 K, which is only 52.6% and 55.4% of MCM-41 and SBA-15 under the similar conditions, separately. The isosteric adsorption heat of water on the MFS is gradually about 27.0–19.8 kJ mol−1, which decreases as the absorbed water vapor amount increases. The value is much smaller than that on MCM-41 and SBA-15. Therefore, the MFS shows more hydrophobic surface properties than the MCM-41 and SBA-15. It may be a kind of good candidate for adsorption of large molecule and catalyst carrier with high moisture resistance.

  19. Impact of film thickness on the morphology of mesoporous carbon films using organic-organic self-assembly.

    Science.gov (United States)

    Vogt, Bryan D; Chavez, Vicki L; Dai, Mingzhi; Arreola, M Regina Croda; Song, Lingyan; Feng, Dan; Zhao, Dongyuan; Perera, Ginusha M; Stein, Gila E

    2011-05-03

    Mesoporous polymer and carbon thin films are prepared by the organic-organic self-assembly of an oligomeric phenolic resin with an amphiphilic triblock copolymer template, Pluronic F127. The ratio of resin to template is selected such that a body-centered cubic (Im3m) mesostructure is formed in the bulk. However, well-ordered mesoporous films are not always obtained for thin films (body-centered cubic symmetry with a preferential orientation of the closest-packed (110) plane parallel to the substrate. Film thickness and initial composition of the carbonizable precursors in the template are critical factors in determining the morphology of mesoporous carbon films. These results provide insight into why difficulties have been reported in producing ultrathin ordered mesoporous carbon films using cooperative organic-organic self-assembly.

  20. Removal of Hg (II and Mn (II from aqueous solution using nanoporous carbon impregnated with surfactants

    Directory of Open Access Journals (Sweden)

    Mansoor Anbia

    2016-09-01

    Full Text Available Mesoporous carbons were impregnated with the anionic and cationic surfactants to increase adsorbing capacity for heavy metal ions. Prepared samples were characterized by X-ray diffraction (XRD and nitrogen adsorption–desorption isotherms. Batch adsorption studies were carried out to study the effect of various parameters like contact time, pH, metal ion concentration and agitation speed. The mercury removal by cationic surfactant cetyltrimethyl ammonium bromide (CTAB, anionic surfactant sodium dodecyl sulfate (SDS modified mesoporous carbon and unmodified mesoporous carbon were found to be 94%, 81.6% and 54.5%, respectively while the manganese removal for these adsorbents were found to be 82.2%, 70.5% and 56.8%, respectively. The sorption data were fit better with the Langmuir adsorption isotherm than Freundlich isotherm.

  1. Formation of pyridine N-oxides using mesoporous titanium silicalite-1

    DEFF Research Database (Denmark)

    Mielby, Jerrik Jørgen; Abildstrøm, Jacob Oskar; Perez-Ferreras, Susana

    2014-01-01

    Mesoporous titanium silicalite-1 (TS-1) prepared by carbon-templating is significantly more active than conventional TS-1 for the oxidation of pyridine derivatives using aqueous hydrogen peroxide as oxidant. The catalytic activity is increased by the system of mesopores that helps to overcome...... the configurational diffusion limitations within the microporous catalyst. The use of a carbon-template for generation of secondary porosity is more effective than desilication. The desilicated catalyst is slightly more active than conventional TS-1, probably due to a decrease of the mean diffusion path length....... In contrast, carbon-templated mesopores provides an efficient transport throughout the zeolite, thus preventing deactivation due to product confinement. All catalysts were characterised by X-ray powder diffraction, scanning electron microscopy, UV-Vis spectroscopy and nitrogen physisorption. The results...

  2. Ordered mesoporous carbide-derived carbon as new high performance electrode material in supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Korenblit, Yair; Yushin, Gleb [Georgia Inst. of Technology, Atlanta, GA (United States); Rose, Marcus; Kockrick, Emanuel; Borchardt, Lars; Kaskel, Stefan [Technische Univ. Dresden (Germany); Kvit, Alexander [Wisconsin Univ., Madison, WI (United States)

    2010-07-01

    The preparation and application of templated ordered mesoporous CDC overcome the present limitations of slow intraparticle ion transport and poor control over the biomodal pore size distribution in the carbons currently used, and shows a route for further performance enhancement. The ordered mesoporous channels in SiC CDC serve as ion-highways and allow for very fast ionic transport into the bulk of the CDC particles, thus leading to an excellent frequency response and outstanding capacitance retention at high current densities. The ordered mesopores in SiC allow for a greatly increased specific surface area and specific capacitance of SiC CDC, nearly doubling the previously reported values. The use of CDC produced from other carbides, including mesoporous TiC or VC is expected to further enhance the energy storage characteristics of EDLC electrodes, while optimization of the mesopore size is expected to enhance the power characteristics of EDLC. (orig.)

  3. Enantioselective recognition at mesoporous chiral metal surfaces

    Science.gov (United States)

    Wattanakit, Chularat; Côme, Yémima Bon Saint; Lapeyre, Veronique; Bopp, Philippe A.; Heim, Matthias; Yadnum, Sudarat; Nokbin, Somkiat; Warakulwit, Chompunuch; Limtrakul, Jumras; Kuhn, Alexander

    2014-02-01

    Chirality is widespread in natural systems, and artificial reproduction of chiral recognition is a major scientific challenge, especially owing to various potential applications ranging from catalysis to sensing and separation science. In this context, molecular imprinting is a well-known approach for generating materials with enantioselective properties, and it has been successfully employed using polymers. However, it is particularly difficult to synthesize chiral metal matrices by this method. Here we report the fabrication of a chirally imprinted mesoporous metal, obtained by the electrochemical reduction of platinum salts in the presence of a liquid crystal phase and chiral template molecules. The porous platinum retains a chiral character after removal of the template molecules. A matrix obtained in this way exhibits a large active surface area due to its mesoporosity, and also shows a significant discrimination between two enantiomers, when they are probed using such materials as electrodes.

  4. Synergistic effects of graphene quantum dot sensitization and nitrogen doping of ordered mesoporous TiO2 thin films for water splitting photocatalysis(Conference Presentation)

    Science.gov (United States)

    Islam, Syed Z.; Wanninayake, Namal; Reed, Allen D.; Kim, Doo-Young; Rankin, Stephen E.

    2016-10-01

    The optical and electronic properties of TiO2 thin films provide tremendous opportunities in several applications including photocatalysis, photovoltaics and photoconductors for energy production. Despite many attractive features of TiO2, critical challenges include the innate inability of TiO2 to absorb visible light and the fast recombination of photoexcited charge carriers. In this study, we prepared ordered mesoporous TiO2 films co-modified by graphene quantum dot sensitization and nitrogen doping (GQD-N-TiO2) for hydrogen production from photoelectrochemical water splitting under visible light irradiation. First, cubic ordered mesoporous TiO2 films were prepared by a surfactant templated sol-gel method. Then, TiO2 films were treated with N2/Ar plasma for the incorporation of substitutional N atoms into the lattice of TiO2. GQDs were prepared by chemically oxidizing carbon nano-onions. The immobilization of GQDs was accomplished by reacting carboxyl groups of GQDs with amine groups of N-TiO2 developed by the prior immobilization of (3-aminopropyl)triethoxysilane (APTES). Successful immobilization of GQDs onto N-TiO2 was probed by UV-Vis, FT-IR, and scanning electron microscopy. Further, zeta potential and contact angle measurements showed enhanced surface charge and hydrophilicity, confirming the successful immobilization of GQDs. The GQD-N-TiO2, N-TiO2 and GQD-TiO2 films showed 400 times, 130 times and 8 times photocurrent enhancement, respectively, compared to TiO2 films for water splitting with a halogen bulb light source. This outstanding enhancement is attributed to the high surface area of mesoporous films and synergistic effects of nitrogen doping and GQD sensitization resulting in enhanced visible light absorption, efficient charge separation and transport.

  5. CO2-assisted synthesis of mesoporous carbon/C-doped ZnO composites for enhanced photocatalytic performance under visible light.

    Science.gov (United States)

    Wang, Fangxiao; Liang, Lin; Shi, Lei; Liu, Mengshuai; Sun, Jianmin

    2014-11-21

    Visible-light-responsive mesoporous carbon/C-doped ZnO (mC/C-ZnO) composites were fabricated using a facile, fast, one-step process in CO2-expanded ethanol solution. It is a green and sustainable process that does not need tedious pretreatment, surfactants or precipitants. CO2 played triple roles in the synthesis of mC/C-ZnO composites; the first was to provide a simple physical expansion to evenly dope the carbon in the ZnO; the second was to offer some chemical groups such as CO3(2-) and HCO3(-), facilitating the uniform and complete deposition through the coordination of a metallic cation with these anions; and the third was to offer CO3(2-) acting as a template for the formation of mesoporosity in the carbon. When used as a photocatalyst for the photodegradation of RhB and the organic pollutant phenol, the mC/C-ZnO composites with glucose content at 22 wt% (mC/C-ZnO-CE-2) synthesized in CO2-expanded ethanol exhibited better recycling stability and photodegradation rate than the corresponding sample synthesized in pure ethanol. Such improved photocatalytic performance was attributed to the well-mixing of the mesoporous carbon and the small sized C-doped ZnO particles in the mC/C-ZnO-CE-2 composites. The facile and fast synthesis method could be extended to other mesoporous carbon/C-doped metal oxide composites, which are expected to be good photocatalyst candidates, or in other application fields.

  6. Mesoporous tin-doped indium oxide thin films: effect of mesostructure on electrical conductivity

    Directory of Open Access Journals (Sweden)

    Till von Graberg, Pascal Hartmann, Alexander Rein, Silvia Gross, Britta Seelandt, Cornelia Röger, Roman Zieba, Alexander Traut, Michael Wark, Jürgen Janek and Bernd M Smarsly

    2011-01-01

    Full Text Available We present a versatile method for the preparation of mesoporous tin-doped indium oxide (ITO thin films via dip-coating. Two poly(isobutylene-b-poly(ethyleneoxide (PIB-PEO copolymers of significantly different molecular weight (denoted as PIB-PEO 3000 and PIB-PEO 20000 are used as templates and are compared with non-templated films to clarify the effect of the template size on the crystallization and, thus, on the electrochemical properties of mesoporous ITO films. Transparent, mesoporous, conductive coatings are obtained after annealing at 500 °C; these coatings have a specific resistance of 0.5 Ω cm at a thickness of about 100 nm. Electrical conductivity is improved by one order of magnitude by annealing under a reducing atmosphere. The two types of PIB-PEO block copolymers create mesopores with in-plane diameters of 20–25 and 35–45 nm, the latter also possessing correspondingly thicker pore walls. Impedance measurements reveal that the conductivity is significantly higher for films prepared with the template generating larger mesopores. Because of the same size of the primary nanoparticles, the enhanced conductivity is attributed to a higher conduction path cross section. Prussian blue was deposited electrochemically within the films, thus confirming the accessibility of their pores and their functionality as electrode material.

  7. Studies on Supercapacitor Electrode Material from Activated Lignin-Derived Mesoporous Carbon

    Energy Technology Data Exchange (ETDEWEB)

    Saha, Dipendu [ORNL; Li, Yunchao [ORNL; Bi, Zhonghe [ORNL; Chen, Jihua [ORNL; Keum, Jong Kahk [ORNL; Hensley, Dale K [ORNL; Grappe, Hippolyte A. [Oak Ridge Institute for Science and Education (ORISE); Meyer III, Harry M [ORNL; Dai, Sheng [ORNL; Paranthaman, Mariappan Parans [ORNL; Naskar, Amit K [ORNL

    2014-01-01

    We synthesized mesoporous carbon from pre-cross-linked lignin gel impregnated with a surfactant as the pore-forming agent, and then activated the carbon through physical and chemical methods to obtain activated mesoporous carbon. The activated mesoporous carbons exhibited 1.5- to 6-fold increases in porosity with a maximum BET specific surface area of 1148 m2/g and a pore volume of 1.0 cm3/g. Slow physical activation helped retain dominant mesoporosity; however, aggressive chemical activation caused some loss of the mesopore volume fraction. Plots of cyclic voltammetric data with the capacitor electrode made from these carbons showed an almost rectangular curve depicting the behavior of ideal double-layer capacitance. Although the pristine mesoporous carbon exhibited the same range of surface-area-based capacitance as that of other known carbon-based supercapacitors, activation decreased the surface-area-based specific capacitance and increased the gravimetric-specific capacitance of the mesoporous carbons. Surface activation lowered bulk density and electrical conductivity. Warburg impedance as a vertical tail in the lower frequency domain of Nyquist plots supported good supercapacitor behavior for the activated mesoporous carbons. Our work demonstrated that biomass-derived mesoporous carbon materials continue to show potential for use in specific electrochemical applications.

  8. Bimetallic Nanocatalysts in Mesoporous Silica for Hydrogen Production from Coal-Derived Fuels

    Energy Technology Data Exchange (ETDEWEB)

    Kuila, Debasish [North Carolina Agricultural & Technical State Univ., Greensboro, NC (United States); Ilias, Shamsuddin [North Carolina Agricultural & Technical State Univ., Greensboro, NC (United States)

    2013-02-13

    In steam reforming reactions (SRRs) of alkanes and alcohols to produce H2, noble metals such as platinum (Pt) and palladium (Pd) are extensively used as catalyst. These metals are expensive; so, to reduce noble-metal loading, bi-metallic nanocatalysts containing non-noble metals in MCM-41 (Mobil Composition of Material No. 41, a mesoporous material) as a support material with high-surface area were synthesized using one-pot hydrothermal procedure with a surfactant such as cetyltrimethylammonium bromide (CTAB) as a template. Bi-metallic nanocatalysts of Pd-Ni and Pd-Co with varying metal loadings in MCM-41 were characterized by x-ray diffraction (XRD), N2 adsorption, and Transmission electron microscopy (TEM) techniques. The BET surface area of MCM-41 (~1000 m2/g) containing metal nanoparticles decreases with the increase in metal loading. The FTIR studies confirm strong interaction between Si-O-M (M = Pd, Ni, Co) units and successful inclusion of metal into the mesoporous silica matrix. The catalyst activities were examined in steam reforming of methanol (SRM) reactions to produce hydrogen. Reference tests using catalysts containing individual metals (Pd, Ni and Co) were also performed to investigate the effect of the bimetallic system on the catalytic behavior in the SRM reactions. The bimetallic system remarkably improves the hydrogen selectivity, methanol conversion and stability of the catalyst. The results are consistent with a synergistic behavior for the Pd-Ni-bimetallic system. The performance, durability and thermal stability of the Pd-Ni/MCM-41 and Pd-Co/MCM-41 suggest that these materials may be promising catalysts for hydrogen production from biofuels. A part of this work for synthesis and characterization of Pd-Ni-MCM-41 and its activity for SRM reactions has been published (“Development of Mesoporous Silica Encapsulated Pd-Ni Nanocatalyst for Hydrogen Production” in “Production and Purification of Ultraclean

  9. Versatility of Evaporation-Induced Self-Assembly (EISA Method for Preparation of Mesoporous TiO2 for Energy and Environmental Applications

    Directory of Open Access Journals (Sweden)

    Luther Mahoney

    2014-03-01

    Full Text Available Evaporation-Induced Self-Assembly (EISA method for the preparation of mesoporous titanium dioxide materials is reviewed. The versatility of EISA method for the rapid and facile synthesis of TiO2 thin films and powders is highlighted. Non-ionic surfactants such as Pluronic P123, F127 and cationic surfactants such as cetyltrimethylammonium bromide have been extensively employed for the preparation of mesoporous TiO2. In particular, EISA method allows for fabrication of highly uniform, robust, crack-free films with controllable thickness. Eleven characterization techniques for elucidating the structure of the EISA prepared mesoporous TiO2 are discussed in this paper. These many characterization methods provide a holistic picture of the structure of mesoporous TiO2. Mesoporous titanium dioxide materials have been employed in several applications that include Dye Sensitized Solar Cells (DSSCs, photocatalytic degradation of organics and splitting of water, and batteries.

  10. Versatility of Evaporation-Induced Self-Assembly (EISA) Method for Preparation of Mesoporous TiO2 for Energy and Environmental Applications

    Science.gov (United States)

    Mahoney, Luther; Koodali, Ranjit T.

    2014-01-01

    Evaporation-Induced Self-Assembly (EISA) method for the preparation of mesoporous titanium dioxide materials is reviewed. The versatility of EISA method for the rapid and facile synthesis of TiO2 thin films and powders is highlighted. Non-ionic surfactants such as Pluronic P123, F127 and cationic surfactants such as cetyltrimethylammonium bromide have been extensively employed for the preparation of mesoporous TiO2. In particular, EISA method allows for fabrication of highly uniform, robust, crack-free films with controllable thickness. Eleven characterization techniques for elucidating the structure of the EISA prepared mesoporous TiO2 are discussed in this paper. These many characterization methods provide a holistic picture of the structure of mesoporous TiO2. Mesoporous titanium dioxide materials have been employed in several applications that include Dye Sensitized Solar Cells (DSSCs), photocatalytic degradation of organics and splitting of water, and batteries. PMID:28788590

  11. STUDY OF THE FORMATION OF MESOPOROUS TiO2 USING ISOPROPOXIDE PRECURSORS UNDER LESS WATER CONDITIONS

    Directory of Open Access Journals (Sweden)

    Indriana Kartini

    2010-06-01

    Full Text Available The role of the synthesis parameters (the molar ratio of template, isopropyl alcohol, acetylacetone, and water with respect to titanium(IV tetraisopropoxide has been thoroughly investigated to understand their effects on the mesostructures and the formation of crystalline phases of mesoporous titania xerogels in less water condition (no added water at 60 oC. The resultant mesoporous titania are more likely to have worm-hole like structure as the dominant stable structure. The template appears to play no significant role in structure directing at mesophase level. However, increasing the amount of the template delays the formation of anatase crystalline phase   Keywords: mesoporous titania, templating synthesis, anatase, evaporation-induced self-assembly

  12. Influence of surfactant concentration on nanohydroxyapatite growth

    Indian Academy of Sciences (India)

    D Gopi; J Indira; S Nithiya; L Kavitha; U Kamachi Mudali; K Kanimozhi

    2013-10-01

    Nanohydroxyapatite particles with different morphologies were synthesized through a microwave coupled hydrothermal method using CTAB as a template. A successful synthesis of nanosized HAP spheres, rods and fibres is achieved through this method by controlling the concentration of the surfactant. The concentration of the surfactant was tuned in such a way that the desired HAP nanostructures were obtained. The resultant powders were sintered at 900 °C in order to obtain phase pure HAP particles. The results obtained by Fourier transform infrared spectroscopy (FT–IR), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques have substantiated the formation of nanosized HAP spheres and fibres.

  13. Mesoporous Carbon-based Materials for Alternative Energy Applications

    Science.gov (United States)

    Cross, Kimberly Michelle

    Increasing concerns for the escalating issues activated by the effect of carbon dioxide emissions on the global climate from extensive use of fossil fuels and the limited amount of fossil resources has led to an in-depth search for alternative energy systems, primarily based on nuclear or renewable energy sources. Recent innovations in the production of more efficient devices for energy harvesting, storage, and conversion are based on the incorporation of nanostructured materials into electrochemical systems. The aforementioned nano-electrochemical energy systems hold particular promise for alternative energy transportation related technologies including fuel cells, hydrogen storage, and electrochemical supercapacitors. In each of these devices, nanostructured materials can be used to increase the surface area where the critical chemical reactions occur within the same volume and mass, thereby increasing the energy density, power density, electrical efficiency, and physical robustness of the system. Durable corrosion resistant carbon support materials for fuel cells have been designed by adding conductive low cost carbon materials with chemically robust ceramic materials. Since a strict control of the pore size is mandatory to optimize properties for improved performance, chemical activation agents have been utilized as porogens to tune surface areas, pore size distributions, and composition of carbon-based mesoporous materials. Through the use of evaporative self-assembly methods, both randomly disordered and surfactant-templated, ordered carbon-silica nanocomposites have been synthesized with controlled surface area, pore volume, and pore size ranging from 50-800 m2/g, 0.025-0.75 cm3/g, and 2-10 nm, respectively. Multi-walled carbon nanotubes (MWNTs) ranging from 0.05-1.0 wt. % were added to the aforementioned carbon-silica nanocomposites, which provided an additional increase in surface area and improved conductivity. Initially, a conductivity value of 0.0667 S

  14. Continuous microwave flow synthesis of mesoporous hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini [Department of Chemistry, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Lintang, Hendrik O. [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia)

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca{sup 2+} ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA.

  15. Photochromic mesoporous hybrid coatings

    Science.gov (United States)

    Raboin, L.; Matheron, M.; Gacoin, T.; Boilot, J.-P.

    2008-09-01

    Spirooxazine (SO) photochromic molecules were trapped in sol-gel matrices. In order to increase the colourability and improve mechanical properties of sol-gel photochromic films, we present an original strategy in which SO photochromic molecules were dispersed in mesoporous organized films using the impregnation technique. Well-ordered organosilicate mesoporous coatings with the 3D-hexagonal symmetry were prepared by the sol-gel technique. These robust mesoporous films, which contain high amounts of hydrophobic methyl groups at the pore surface, offer optimized environments for photochromic dyes dispersed by impregnation technique. After impregnation by a spirooxazine solution, the photochromic response is only slightly slower when compared with mesostructured or soft sol-gel matrices, showing that mesoporous organized hybrid matrix are good host for photochromic dyes. Moreover, the molecular loading in films is easily adjustable in a large range using multi-impregnation procedure and increasing the film thickness leading to coatings for optical switching devices.

  16. A spectroscopic study on the adsorption of cationic dyes into mesoporous AlMCM-41 materials

    Science.gov (United States)

    Zanjanchi, M. A.; Ebrahimian, A.; Alimohammadi, Z.

    2007-03-01

    Mesoporous materials loaded with dyes are of interest with respect to novel optical applications. The spectral behaviors of some dyes in these materials are considerably affected by the presence of surfactants. A comparative study has been carried out on the adsorption of the methylene blue, rhodamine 6G and thionine dyes into a surfactant-free and surfactant-containing mesoporous AlMCM-41. The ion exchange method has been employed for incorporation of the dye molecules into the structure of MCM-41. The exchangeable sites in the MCM-41 were generated prior to dye loading by isomorphous substitution of aluminum for silicon in the structure of the mesoporous material during the synthesis procedure. Diffuse reflectance measurements indicate adsorption of methylene blue and rhodamine 6G dye molecules into AlMCM-41 taken place via ion exchange at room temperature. The spectra show presence of monomer and dimer aggregates of the dyes established into the pores and surface of AlMCM-41. The ratio of dimer to monomer forms of rhodamine 6G incorporated in the surfactant-free and surfactant-containing AlMCM-41 is about one which is higher than those observed in aqueous solutions. The surfactant-containing AlMCM-41 induced destabilization and decomposition of methylene blue while uploading the dye. Degradation of this dye produces intermediate species identified as demethylated forms of methylene blue adsorbed on AlMCM-41. Our experiments revealed that kinetics of ion exchange for thionine dye is very slow at room temperature, but it become faster at higher temperatures. The spectral properties of thionine in AlMCM-41 are close to that of thionine in an aqueous solution, possibly due to high pore space in a mesoporous molecular sieve. No adsorption of thionine was observed for surfactant-containing AlMCM-41 even at higher temperatures.

  17. Synthesis and characterization of molybdenum incorporated mesoporous aluminophosphate

    Science.gov (United States)

    Ho, Li-Ngee; Ikegawa, Tasuku; Nishiguchi, Hiroyasu; Nagaoka, Katsutoshi; Takita, Yusaku

    2006-07-01

    A synthesis of molybdenum incorporated mesoporous aluminophosphate with long-chain n-alkylamine as template material had been prepared under non-aqueous condition. These materials were extensively characterized by using X-ray diffraction (XRD), nitrogen sorption isotherms, nuclear magnetic resonance of 27Al and 31P (NMR), inductive coupled plasma (ICP), electron spin resonance (ESR), Fourier transform infrared (FTIR) and thermogravimetric-differential thermal analysis (TG-DTA). Morphology of the materials had been observed by using transmission electron microscope (TEM) that revealed the mesoporous materials possessed wormhole-like structures. Alkaline solvent extraction using n-butylamine/ethanol had been efficiently removed the n-alkylamine from the mesoporous samples which yielded BET surface areas around 550-730 m 2/g. BJH analysis showed a narrow pore size distribution which increased with increasing of the carbon chain length of alkylamine (template). Valence state and coordination of the molybdenum in the obtained samples were investigated by using ESR and FTIR where it was found that Mo 4+ and Mo 6+ molybdenum species existed in the molybdenum incorporated mesoporous aluminophosphate in tetrahedral coordination.

  18. Low-cost preparation of mesoporous silica with high pore volume

    Institute of Scientific and Technical Information of China (English)

    Shuling Shen; Wei Wu; Kai Guo; Jianfeng Chen

    2007-01-01

    Mesoporous silica materials with high pore volume were successfully prepared by the chemical precipitation method, with water glass and a biodegradable nonionic surfactant polyethylene glycol (PEG). The obtained materials were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), thermo gravimetric analyzer and differential scanning calorimetry (TG-DSC), nitrogen adsorption-desorption measurements, and X-ray diffraction (XRD). The results showed that the changes of the pore parameters depended on both the surfactant content and heat treatment temperature. When the content of PEG was 10wt% and the obtained PEG/SiO2 composite was heated at 600℃, the mesoporous silica with a pore volume of 2.2 cm3/g, a BET specific surface area of 361.55 m2/g, and a diameter of 2-4 μm could be obtained. The obtained mesoporous silica materials have potential applications in the fields of paint and plastic, as thickening, reinforcing, and flatting agents.

  19. Stable Tetrahedral Aluminum Sites in Hexagonal Mesoporous Aluminosilicates

    Institute of Scientific and Technical Information of China (English)

    韩宇; 刘宪春; 等

    2002-01-01

    A unique templating approach for the synthesis of hexagonal mesoporous aluminosilicates via self-assembly of pre-formed aluminosilcate nacoclusters with the templating micella formed by cetyltrimethylammonium bromide (CTAB) is described ,The obtained materials of MAS-5 are hydrothermally stable,which is shown by X-ray diffraction (XRD) analysis,Further-more,as charaacterized by NMR technique ,MAS-5 has taable tetrahedral aluminum sites that is the major contributions to the acidity of aluminosilicate molecular sieve ,and on non-frame-work aluminium species in the saples was observed.

  20. Stable Tetrahedral Aluminum Sites in Hexagonal Mesoporous Aluminosilicates

    Institute of Scientific and Technical Information of China (English)

    HAN,Yu(韩宇); YU,Yi(于沂); XU,Xian-Zhu(许宪祝); XIAO,Feng-Shou(肖丰收); LIU,Xian-Chun(刘宪春); HAN,Xiu-Wen(韩秀文); BAO,Xin-He(包信和)

    2002-01-01

    A unique templating approach for the synthesis of hexagonal mesoporous aluminosilicates via self-assembly of pre-formed aluminosilcate nanoclusters with the templating micella formed by cetyltrimethylammonium bromide (CTAB) is described.The obtained materials of MAS-5 are hydrothermally stable,which is shown by X-ray diffraction (XRD) analysis. Furthermore, as characterized by NMR technique, MAS-5 has stable tetrahedral aluminum sites that is the major contributions to the acidity of aluminosilicate molecular sieve, and on non-framework aluminium species in the samples was observed.

  1. Synthesis and characterization of submicron-sized mesoporous aluminosilicate spheres

    Indian Academy of Sciences (India)

    Gautam Gundiah; M Eswaramoorthy; S Neeraj; Srinivasan Natarajan; C N R Rao

    2001-06-01

    Me soporous a luminosilicate spheres of 0 3-0 4 m diameter, with different Si/Al ratios, have been prepared by surfactant templating. Surface area of these materials is in the 510-970 m2g-1 range and pore diameter in the 15-20 Å range.

  2. Surfactant-free hydrothermal synthesis of lithium aluminate microbricks and nanorods from aluminium oxide nanoparticles.

    Science.gov (United States)

    Joshi, Upendra A; Chung, Soo Hyun; Lee, Jae Sung

    2005-09-21

    Beta-LiAlO2 microbricks and rectangular nanorods have been successfully synthesized from Al2O3 nanoparticles by a simple hydrothermal process without any surfactant or template, by simply changing the Li/Al molar ratio.

  3. Fabrication and Characterization of Inorganic Silver and Palladium Nanostructures within Hexagonal Cylindrical Channels of Mesoporous Carbon

    Directory of Open Access Journals (Sweden)

    Jheng-Guang Li

    2014-06-01

    Full Text Available In this study, we prepared a mesoporous carbon with hexagonally packed mesopores through evaporation-induced self-assembly (EISA—with the diblock copolymer poly(ethylene oxide-b-ε-caprolactone (PEO-b-PCL as the template (EO114CL84, phenolic resin as the carbon precursor, hexamethylenetetramine (HMTA as the curing agent, and star octakis-PEO-functionalized polyhedral oligomeric silsesquioxane (PEO–POSS as the structure modifier—and subsequent carbonization. We then took the cylindrical mesoporous carbon as a loading matrix, with AgNO3 and Pd(NO32 as metal precursors, to fabricate Ag nanowire/mesoporous carbon and Pd nanoparticle/mesoporous carbon nanocomposites, respectively, through an incipient wetness impregnation method and subsequent reduction under H2. We used transmission electron microscopy, electron diffraction, small-angle X-ray scattering, N2 isotherm sorption experiment, Raman spectroscopy, and power X-ray diffraction to investigate the textural properties of these nanometal/carbon nanocomposites. Most notably, the Raman spectra of the cylindrical mesoporous carbon, Ag/mesoporous carbon, and Pd/mesoporous carbon revealed interesting phenomena in terms of the ratios of the intensities of the D and G bands (ID/IG, the absolute scattering intensities, and the positions of the D bands.

  4. Mesoporous high surface area Ce0.9Gd0.1O1.95 synthesized by spray drying

    DEFF Research Database (Denmark)

    Lundberg, Mats; Wang, Hsiang-Jen; Blennow Tullmar, Peter;

    2011-01-01

    Mesoporous gadolinium doped cerium dioxide with high surface area was produced by spray drying using Pluronic 123 as surfactant. The powder, when calcined at 400 °C, had a BET surface area of 136 m2 g−1 and was polycrystalline as confirmed by XRD and TEM. XEDS confirmed Ce, Gd and O, as the only......, corresponding to the crystallite size calculated from XRD data. The similar size range of the mesopores and the observed crystallite size indicates that the porosity is partly formed from intergranular mesoporosity. Using the spray drying method of a surfactant assisted liquid precursor solution it can...

  5. Ordered Mesoporous Carbons as Novel and Efficient Adsorbent for Dye Removal from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Phuong T. Dang

    2016-01-01

    Full Text Available Ordered mesoporous carbons (OMCs were successfully synthesized by using hard template and soft template methods. These materials were characterized by XRD, TEM, and N2 adsorption-desorption Brunauer-Emmett-Teller (BET. From the obtained results, it is revealed that the obtained OMCs samples showed high surface area (>1000 m2/g with high pore volume, mainly mesopore volume (1.2–2.4 cm3/g. Moreover, OMCs samples had similar structure of the SBA-15 silica and exhibited high MB adsorption capacity with qm of 398 mg·g−1 for OMCs synthesis with hard template and 476 mg·g−1 for OMCs synthesis with soft template, respectively. From kinetics investigation, it is confirmed that MB adsorption from aqueous solution obeys the pseudo-second-order kinetic equation.

  6. Synthesis and Textural Characterization of Mesoporous and Meso-/Macroporous Silica Monoliths Obtained by Spinodal Decomposition

    Directory of Open Access Journals (Sweden)

    Anne Galarneau

    2016-04-01

    Full Text Available Silica monoliths featuring either mesopores or flow-through macropores and mesopores in their skeleton are prepared by combining spinodal phase separation and sol-gel condensation. The macroporous network is first generated by phase separation in acidic medium in the presence of polyethyleneoxides while mesoporosity is engineered in a second step in alkaline medium, possibly in the presence of alkylammonium cations as surfactants. The mesoporous monoliths, also referred as aerogels, are obtained in the presence of alkylpolyethylene oxides in acidic medium without the use of supercritical drying. The impact of the experimental conditions on pore architecture of the monoliths regarding the shape, the ordering, the size and the connectivity of the mesopores is comprehensively discussed based on a critical appraisal of the different models used for textural analysis.

  7. Mesoporous Structure Control of Silica in Room-Temperature Synthesis under Basic Conditions

    Directory of Open Access Journals (Sweden)

    Jeong Wook Seo

    2015-01-01

    Full Text Available Various types of mesoporous silica, such as continuous cubic-phase MCM-48, hexagonal-phase MCM-41, and layer-phase spherical silica particles, have been synthesized at room temperature using cetyltrimethylammonium bromide as a surfactant, ethanol as a cosurfactant, tetraethyl orthosilicate as a silica precursor, and ammonia as a condensation agent. Special care must be taken both in the filtering of the resultant solid products and in the drying process. In the drying process, further condensation of the silica after filtering was induced. As the surfactant and cosurfactant concentrations in the reaction mixture increased and the NH3 concentration decreased, under given conditions, continuous cubic MCM-48 and layered silica became the dominant phases. A cooperative synthesis mechanism, in which both the surfactant and silica were involved in the formation of mesoporous structures, provided a good explanation of the experimental results.

  8. Code Generation with Templates

    CERN Document Server

    Arnoldus, Jeroen; Serebrenik, A

    2012-01-01

    Templates are used to generate all kinds of text, including computer code. The last decade, the use of templates gained a lot of popularity due to the increase of dynamic web applications. Templates are a tool for programmers, and implementations of template engines are most times based on practical experience rather than based on a theoretical background. This book reveals the mathematical background of templates and shows interesting findings for improving the practical use of templates. First, a framework to determine the necessary computational power for the template metalanguage is presen

  9. Template-Free Synthesis of Hierarchical Porous Metal-Organic Frameworks

    Energy Technology Data Exchange (ETDEWEB)

    Yue, Yanfeng [ORNL; Qiao, Zhen-an [University of Tennessee, Knoxville (UTK); Fulvio, Pasquale F [ORNL; Dai, Sheng [ORNL; Binder, Andrew J [ORNL; Tian, Chengcheng [ORNL; Nelson, Kimberly M [ORNL; Zhu, Xiang [ORNL

    2013-01-01

    A template-free synthesis of a hierarchical microporous-mesoporous metal-organic framework (MOF) of Zn(II)-2,5-dihydroxy-1,4-benzenedicarboxylate, namely Zn-MOF-74, is reported. The surface morphology and porosity of the bimodal materials can be modified by etching the pore walls with the synthesis solvent under different reaction times and different solvents. This template-free strategy allows for the preparation of stable frameworks with mesopores exceeding 15 nm, which was previously unattained by the synthesis of MOFs by ligand exten-sion method.

  10. The development of chiral nematic mesoporous materials.

    Science.gov (United States)

    Kelly, Joel A; Giese, Michael; Shopsowitz, Kevin E; Hamad, Wadood Y; MacLachlan, Mark J

    2014-04-15

    Cellulose nanocrystals (CNCs) are obtained from the sulfuric acid-catalyzed hydrolysis of bulk cellulose. The nanocrystals have diameters of ~5-15 nm and lengths of ~100-300 nm (depending on the cellulose source and hydrolysis conditions). This lightweight material has mostly been investigated to reinforce composites and polymers because it has remarkable strength that rivals carbon nanotubes. But CNCs have an additional, less explored property: they organize into a chiral nematic (historically referred to as cholesteric) liquid crystal in water. When dried into a thin solid film, the CNCs retain the helicoidal chiral nematic order and assemble into a layered structure where the CNCs have aligned orientation within each layer, and their orientation rotates through the stack with a characteristic pitch (repeating distance). The cholesteric ordering can act as a 1-D photonic structure, selectively reflecting circularly polarized light that has a wavelength nearly matching the pitch. During CNC self-assembly, it is possible to add sol-gel precursors, such as Si(OMe)4, that undergo hydrolysis and condensation as the solvent evaporates, leading to a chiral nematic silica/CNC composite material. Calcination of the material in air destroys the cellulose template, leaving a high surface area mesoporous silica film that has pore diameters of ~3-10 nm. Importantly, the silica is brilliantly iridescent because the pores in its interior replicate the chiral nematic structure. These films may be useful as optical filters, reflectors, and membranes. In this Account, we describe our recent research into mesoporous films with chiral nematic order. Taking advantage of the chiral nematic order and nanoscale of the CNC templates, new functional materials can be prepared. For example, heating the silica/CNC composites under an inert atmosphere followed by removal of the silica leaves highly ordered, mesoporous carbon films that can be used as supercapacitor electrodes. The composition

  11. A Review of Recent Developments of Mesoporous Materials.

    Science.gov (United States)

    Suib, Steven L

    2017-06-29

    This personal account concerns novel recent discoveries in the area of mesoporous materials. Most of the papers discussed have been published within the last two to three years. A major emphasis of most of these papers is the synthesis of unique mesoporous materials by a variety of synthetic methods. Many of these articles focus on the control of the pore sizes and shapes of mesoporous materials. Synthetic methods of various types have been used for such control of porosity including soft templating, hard templating, nano-casting, electrochemical methods, surface functionalization, and trapping of species in pores. The types of mesoporous materials range from carbon materials, metal oxides, metal sulfides, metal nitrides, carbonitriles, metal organic frameworks (MOFs), and composite materials. The vast majority of recent publications have centered around biological applications with a majority dealing with drug delivery systems. Several other bio-based articles on mesoporous systems concern biomass conversion and biofuels, magnetic resonance imaging (MRI) studies, ultrasound therapy, enzyme immobilization, antigen targeting, biodegradation of inorganic materials, applications for improved digestion, and antitumor activity. Numerous nonbiological applications of mesoporous materials have been pursued recently. Some specific examples are photocatalysis, photo-electrocatalysis, lithium ion batteries, heterogeneous catalysis, extraction of metals, extraction of lanthanide and actinide species, chiral separations and catalysis, capturing and the mode of binding of carbon dioxide (CO2 ), optical devices, and magneto-optical devices. Of this latter class of applications, heterogeneous catalysis is predominant. Some of the types of catalytic reactions being pursued include hydrogen generation, selective oxidations, aminolysis, Suzuki coupling and other coupling reactions, oxygen reduction reactions (ORR), oxygen evolution reactions (OER), and bifunctional catalysis. For

  12. Studies on supercapacitor electrode material from activated lignin-derived mesoporous carbon.

    Science.gov (United States)

    Saha, Dipendu; Li, Yunchao; Bi, Zhonghe; Chen, Jihua; Keum, Jong K; Hensley, Dale K; Grappe, Hippolyte A; Meyer, Harry M; Dai, Sheng; Paranthaman, M Parans; Naskar, A K

    2014-01-28

    We synthesized mesoporous carbon from pre-cross-linked lignin gel impregnated with a surfactant as the pore-forming agent and then activated the carbon through physical and chemical methods to obtain activated mesoporous carbon. The activated mesoporous carbons exhibited 1.5- to 6-fold increases in porosity with a maximum Brunauer-Emmett-Teller (BET) specific surface area of 1148 m(2)/g and a pore volume of 1.0 cm(3)/g. Both physical and chemical activation enhanced the mesoporosity along with significant microporosity. Plots of cyclic voltammetric data with the capacitor electrode made from these carbons showed an almost rectangular curve depicting the behavior of ideal double-layer capacitance. Although the pristine mesoporous carbon exhibited a range of surface-area-based capacitance similar to that of other known carbon-based supercapacitors, activation decreased the surface-area-based specific capacitance and enhanced the gravimetric specific capacitance of the mesoporous carbons. A vertical tail in the lower-frequency domain of the Nyquist plot provided additional evidence of good supercapacitor behavior for the activated mesoporous carbons. We have modeled the equivalent circuit of the Nyquist plot with the help of two constant phase elements (CPE). Our work demonstrated that biomass-derived mesoporous carbon materials continue to show potential for use in specific electrochemical applications.

  13. Synthesis of highly phosphonic acid functionalized benzene-bridged periodic mesoporous organosilicas for use as efficient dye adsorbents.

    Science.gov (United States)

    Deka, Juti Rani; Liu, Chia-Ling; Wang, Tzu-Hua; Chang, Wei-Chieh; Kao, Hsien-Ming

    2014-08-15

    Periodic mesoporous organosilicas (PMOs) with benzene bridging groups in the silica wall were functionalized with a tunable content of phosphonic acid groups. These bifunctional materials were synthesized by co-condensation of two different organosilane precursors, that is, 1,4-bis(triethoxysilyl)benzene (BTEB) and sodium 3-(trihydroxysilyl)propyl methyl phosphate (SPMP), under acidic conditions using nonionic surfactant Brij-S10 as template. The materials exhibited well-ordered mesostructures and were characterized by X-ray diffraction, nitrogen sorption, TEM, TGA, FTIR, and solid-state NMR measurements. The materials thus obtained were employed as adsorbents to remove different types of dyes, for example, cationic dyes methylene blue and phenosafranine, anionic orange II, and amphoteric rhodamine B, from aqueous solutions. The materials exhibited a remarkably high adsorption capacity than activated carbon due to their ordered mesostructures, a large number of phosphonic acid groups, and high surface areas. The adsorption was mainly governed by electrostatic interaction, but also involved π-π stacking interaction as well as hydrogen bonding. The adsorption kinetics can be better fitted by the pseudo-second order model. The adsorption process was controlled by the mechanisms of external mass transfer and intraparticle diffusion. The materials retained more than 97% dye removal efficiency after use for five consecutive cycles.

  14. Tunable solar-heat shielding property of transparent films based on mesoporous Sb-doped SnO₂ microspheres.

    Science.gov (United States)

    Li, Yusheng; Liu, Jie; Liang, Jie; Yu, Xibin; Li, Dongjia

    2015-04-01

    In this paper, mesoporous antimony doped tin oxide (ATO) microspheres are synthesized via a solvothermal method from a methanol system with the surfactant followed by a thermal treatment process. Morphology studies reveal that the spherical products obtained by polyvinylpyrrolidone (PVP) templating result in a higher uniformity in size. Such obtained ATO microspheres with a secondary particle size ranging between 200 and 800 nm consist of packed tiny nanocrystals and have high specific surface area (∼98 m(2) g(-1)). The effect of Sb doping on the structural and electrical properties of SnO2 microspheres is studied. Because of the substitution of Sn(4+) with Sb(5+) accompanied by forming a shallow donor level close to the conduction band of SnO2, a lower resistivity of powder pellet can be achieved, which corresponds to the spectrally selective property of films. The application of ATO microspheres provides an example of transparent coatings; depending on Sb concentration in SnO2 and solid content of coatings, transparent films with tunable solar-heat shielding property are obtained.

  15. 胶原纤维为模板TiO2、Lax/TiO2纳米纤维的制备、表征及光催化活性研究%Collagen fiber as a template for mesoporous TiO2 and Lax/TiO2 nano-fibers:synthesis,characterization and photocatalytic activities

    Institute of Scientific and Technical Information of China (English)

    蔡莉

    2014-01-01

    以胶原纤维为模板分别负载钛(Ti4+)或钛(Ti4+)和镧(La3+),经高温煅烧制得介孔 TiO 2和Lax/TiO 2纳米纤维.通过场发射扫描电镜(FESEM)、N2吸附-脱附等温线、X 射线衍射(XRD)、分子荧光光谱(PL)和紫外-可见吸收光谱(UV-Vis)等对这2类纳米纤维的结构和物理性能进行了表征.结果表明胶原纤维的纤维状结构能被较好地保留在TiO 2和 Lax/TiO 2纳米纤维中.TiO 2和 Lax/TiO 2纳米纤维的 N2吸附-脱附等温线属于典型的Ⅳ型,表明其具有介孔结构.XRD 分析表明,La3+的掺杂减小了 TiO 2的晶粒尺寸.与 Degussa P25相比,介孔TiO 2和 Lax/TiO 2(x ≤0.02)纳米纤维的紫外-可见吸收光谱红移,分子荧光光谱强度明显减弱.以孔雀石绿的光催化降解为模型反应,在可见光和紫外光激发下,介孔 TiO 2和 Lax/TiO 2纳米纤维的光催化活性均高于 Degussa P25.此外,Lax/TiO 2在可见光激发下的光催化活性高于未掺杂的 TiO 2纳米纤维.%Mesoporous TiO 2 and Lax/TiO 2 nano-fiber were prepared by loading titanium (Ti4+ ),or titanium (Ti4+ )and lanthanum (La3 + )on collagen fiber template,respectively,and then heat treated.The physico-chemical properties of these nano-fibers were fully characterized by means of field emission scanning electron microscopy (FESEM),N2 adsorption-desorption,X-ray diffraction (XRD),photoluminescence spectra (PL) and UV-Vis absorption spectra.It was found that the fibrous morphology of collagen fiber was well preserved in the TiO 2 and La0.02/TiO 2 nano-fibers.The N2 adsorption-desorption isotherms of TiO 2 and Lax/TiO 2 nano-fi-bers were the typical type Ⅳ,which associated with the characteristics of mesoporous materials.XRD analysis showed that La3 + doped into TiO 2 has a significant influence on crystal size of TiO 2 .Compared with Degussa P25,the TiO 2 and Lax/TiO 2 (x ≤0.02)nano-fibers showed a red-shift in their UV-Vis absorption spectra,and their PL spectra intensity

  16. Synthesis, characterization, and application of surface-functionalized ordered mesoporous nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Po-Wen [Iowa State Univ., Ames, IA (United States)

    2009-01-01

    The dissertation begins with Chapter 1, which is a general introduction of the fundamental synthesis of mesoporous silica materials, the selective functionlization of mesoporous silica materials, and the synthesis of nanostructured porous materials via nanocasting. In Chapter 2, the thermo-responsive polymer coated mesoporous silica nanoparticles (MSN) was synthesized via surface-initated polymerization and exhibited unique partition activities in a biphasic solution with the thermally induced change. In Chapter 3, the monodispersed spherical MSN with different mesoporous structure (MCM-48) was developed and employed as a template for the synthesis of mesoporous carbon nanoparticles (MCN) via nanocasting. MCN was demonstrated for the delivery of membrane impermeable chemical agents inside the cells. The cellular uptake efficiency and biocompabtibility of MCN with human cervical cancer cells were also investigated. In addition to the biocompabtibility of MCN, MCN was demonstrated to support Rh-Mn nanoparticles for catalytic reaction in Chapter 4. Owing to the unique mesoporosity, Rh-Mn nanoparticles can be well distributed inside the mesoporous structure and exhibited interesting catalytic performance on CO hydrogenation. In Chapter 5, the synthesis route of the aforementioned MCM-48 MSN was discussed and investigated in details and other metal oxide nanoparticles were also developed via nanocasting by using MCM-48 MSN as a template. At last, there is a general conclusion summarized in Chapter 6.

  17. Supported mesoporous carbon ultrafiltration membrane and process for making the same

    Science.gov (United States)

    Strano, Michael; Foley, Henry C.; Agarwal, Hans

    2004-04-13

    A novel supported mesoporous carbon ultrafiltration membrane and process for producing the same. The membranes comprise a mesoporous carbon layer that exists both within and external to the porous support. A liquid polymer precursor composition comprising both carbonizing and noncarbonizing templating polymers is deposited on the porous metal support. The coated support is then heated in an inert-gas atmosphere to pyrolyze the polymeric precursor and form a mesoporous carbon layer on and within the support. The pore-size of the membranes is dependent on the molecular weight of the noncarbonizing templating polymer precursor. The mesoporous carbon layer is stable and can withstand high temperatures and exposure to organic chemicals. Additionally, the porous metal support provides excellent strength properties. The composite structure of the membrane provides novel structural properties and allows for increased operating pressures allowing for greater membrane flow rates. The invention also relates to the use of the novel ultrafiltration membrane to separate macromolecules from solution. An example is shown separating bovine serum albumin from water. The membrane functions by separating and by selective adsorption. Because of the membrane's porous metal support, it is well suited to industrial applications. The unique properties of the supported mesoporous carbon membrane also allow the membrane to be used in transient pressure or temperature swing separations processes. Such processes were not previously possible with existing mesoporous membranes. The present invention, however, possesses the requisite physical properties to perform such novel ultrafiltration processes.

  18. Highly-branched mesoporous Au-Pd-Pt trimetallic nanoflowers blooming on reduced graphene oxide as an oxygen reduction electrocatalyst.

    Science.gov (United States)

    Huang, Liang; Han, Yujie; Dong, Shaojun

    2016-07-05

    Herein, we develop a one-pot, two surfactant-assisted synthesis of highly-branched mesoporous Au-Pd-Pt trimetallic nanoflowers blooming on rGO with superior electrochemical performance for the ORR. Similarly to the interaction between Pluronic F127 and hexadecylpyridinium chloride (HDPC), this method may be extended to other nonionic/ionic surfactants to synthesize all-metal branched porous nanoparticles, and shows promising applications in electrochemistry and catalysis.

  19. Thermally cleavable surfactants

    Science.gov (United States)

    McElhanon, James R.; Simmons, Blake A.; Zifer, Thomas; Jamison, Gregory M.; Loy, Douglas A.; Rahimian, Kamyar; Long, Timothy M.; Wheeler, David R.; Staiger, Chad L.

    2006-04-04

    Two new surfactant molecules are reported which contain thermally labile Diels-Alder adducts connecting the polar and non-polar sections of each molecule. The two surfactants possess identical non-polar dodecyl tail segments but exhibit different polar headgroups. The surfactants become soluble in water when anionic salts are formed through the deprotonation of the surfactant headgroups by the addition of potassium hydroxide. When either surfactant is exposed to temperature above about 60.degree. C., the retro Diels-Alder reaction occurs, yielding hydrophilic and hydrophobic fragments and the aqueous solutions of the surfactants subsequently exhibit loss of all surface-active behavior.

  20. Thermally cleavable surfactants

    Energy Technology Data Exchange (ETDEWEB)

    McElhanon, James R. (Manteca, CA); Simmons, Blake A. (San Francisco, CA); Zifer, Thomas (Manteca, CA); Jamison, Gregory M. (Albuquerque, NM); Loy, Douglas A. (Albuquerque, NM); Rahimian, Kamyar (Albuquerque, NM); Long, Timothy M. (Urbana, IL); Wheeler, David R. (Albuquerque, NM); Staiger, Chad L. (Albuquerque, NM)

    2009-09-29

    Two new surfactant molecules are reported which contain thermally labile Diels-Alder adducts connecting the polar and non-polar sections of each molecule. The two surfactants possess identical non-polar dodecyl tail segments but exhibit different polar headgroups. The surfactants become soluble in water when anionic salts are formed through the deprotonation of the surfactant headgroups by the addition of potassium hydroxide. When either surfactant is exposed to temperature above about 60.degree. C., the retro Diels-Alder reaction occurs, yielding hydrophilic and hydrophobic fragments or the aqueous solutions of the surfactants subsequently exhibit loss of all surface-active behavior.

  1. Thermally cleavable surfactants

    Energy Technology Data Exchange (ETDEWEB)

    McElhanon, James R. (Manteca, CA); Simmons, Blake A. (San Francisco, CA); Zifer, Thomas (Manteca, CA); Jamison, Gregory M. (Albuquerque, NM); Loy, Douglas A. (Albuquerque, NM); Rahimian, Kamyar (Albuquerque, NM); Long, Timothy M. (Urbana, IL); Wheeler, David R. (Albuquerque, NM); Staiger, Chad L. (Albuquerque, NM)

    2009-11-24

    Two new surfactant molecules are reported which contain thermally labile Diels-Alder adducts connecting the polar and non-polar sections of each molecule. The two surfactants possess identical non-polar dodecyl tail segments but exhibit different polar headgroups. The surfactants become soluble in water when anionic salts are formed through the deprotonation of the surfactant headgroups by the addition of potassium hydroxide. When either surfactant is exposed to temperature above about 60.degree. C., the retro Diels-Alder reaction occurs, yielding hydrophilic and hydrophobic fragments or the aqueous solutions of the surfactants subsequently exhibit loss of all surface-active behavior.

  2. Synthesis of hierarchical zeolites using an inexpensive mono-quaternary ammonium surfactant as mesoporogen.

    Science.gov (United States)

    Zhu, Xiaochun; Rohling, Roderigh; Filonenko, Georgy; Mezari, Brahim; Hofmann, Jan P; Asahina, Shunsuke; Hensen, Emiel J M

    2014-12-04

    A simple amphiphilic surfactant containing a mono-quaternary ammonium head group (N-methylpiperidine) is effective in imparting substantial mesoporosity during synthesis of SSZ-13 and ZSM-5 zeolites. Highly mesoporous SSZ-13 prepared in this manner shows greatly improved catalytic performance in the methanol-to-olefins reaction compared to bulk SSZ-13.

  3. Nanocasting Process to Pore-Expanded Ordered Mesoporous Carbons with 2D Hexagonal Mesostructure

    Directory of Open Access Journals (Sweden)

    Chongwen Jiang

    2014-01-01

    Full Text Available Pore-expanded ordered mesoporous carbons with 2D hexagonal mesostructure were synthesized by a simple nanocasting process. We adopted sucrose as carbon precursors, mesoporous silica materials SBA-15 as the hard templates, and hexane as micelle swelling agents. The pore size distribution of OMCs was narrow and centered at 5.4 nm, which is larger than the upper limit of pore diameters typically reported for CMK-3. The BET surface area and mesopore volume of PE-CMK-3 can reach to 1213.47 m2/g and 1.56 cm3/g, respectively, indicating that choosing large pore size materials as template is good for preparation of high performance of OMCs.

  4. Tuning the iridescence of chiral nematic cellulose nanocrystals and mesoporous silica films by substrate variation.

    Science.gov (United States)

    Nguyen, Thanh-Dinh; Hamad, Wadood Y; MacLachlan, Mark J

    2013-12-14

    We have discovered that the self-assembly of cellulose nanocrystals (CNCs) into chiral nematic phases varies significantly with the substrate and evaporation rate. These variables allow the reflectance peak of iridescent chiral nematic films of CNCs and mesoporous silica templated from CNCs to be tuned over a wide range of wavelengths.

  5. Functional mesoporous materials for energy applications: solar cells, fuel cells, and batteries.

    Science.gov (United States)

    Ye, Youngjin; Jo, Changshin; Jeong, Inyoung; Lee, Jinwoo

    2013-06-07

    This feature article presents recent progress made in the synthesis of functional ordered mesoporous materials and their application as high performance electrodes in dye-sensitized solar cells (DSCs) and quantum dot-sensitized solar cells (QDSCs), fuel cells, and Li-ion batteries. Ordered mesoporous materials have been mainly synthesized using two representative synthetic methods: the soft template and hard template methods. To overcome the limitations of these two methods, a new method called CASH was suggested. The CASH method combines the advantages of the soft and hard template methods by employing a diblock copolymer, PI-b-PEO, which contains a hydrophilic block and an sp(2)-hybridized-carbon-containing hydrophobic block as a structure-directing agent. After discussing general techniques used in the synthesis of mesoporous materials, this article presents recent applications of mesoporous materials as electrodes in DSCs and QDSCs, fuel cells, and Li-ion batteries. The role of material properties and mesostructures in device performance is discussed in each case. The developed soft and hard template methods, along with the CASH method, allow control of the pore size, wall composition, and pore structure, providing insight into material design and optimization for better electrode performances in these types of energy conversion devices. This paper concludes with an outlook on future research directions to enable breakthroughs and overcome current limitations in this field.

  6. Preparation of mesoporous carbon/polypyrrole composite materials and their supercapacitive properties

    Directory of Open Access Journals (Sweden)

    WU-JUN ZOU

    2011-08-01

    Full Text Available We synthesized mesoporous carbons/polypyrrole composites, using a chemical oxidative polymerization and calcium carbonate as a sacrificial template. N2 adsorption-desorption method, Fourier infrared spectroscopy, and transmission electron microscopy were used to characterize the structure and morphology of the composites. The measurement results indicated that as-synthesized carbon with the disordered mesoporous structure and a pore size of approximately 5 nm was uniformly coated by polypyrrole. The electrochemical behavior of the resulting composite was examined by cyclic voltammetry and cycle life measurements, and the obtained results showed that the specific capacitance of the resulting composite electrode was as high as 313 F g−1, nearly twice the capacitance of pure mesoporous carbon electrode (163 F g–1. This reveals that the electrochemical performance of these materials is governed by a combination of the electric double layer capacitance of mesoporous carbon and pseudocapacitance of polypyrrole.

  7. Synthesis of mesoporous hollow carbon hemispheres as highly efficient Pd electrocatalyst support for ethanol oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Zaoxue; Meng, Hui; Li, Zihui; Shen, Pei Kang [The Key Laboratory of Low-carbon Chemistry and Energy Conservation of Guangdong Province, The State Key Laboratory of Optoelectronic Materials and Technologies, Sun Yat-Sen University, Guangzhou, 510275 (China); Shi, Lei [Changling Catalyst Division, Sinopec Group, Yueyang 414012 (China)

    2010-05-15

    The synthesis procedure of the highly mesoporous hollow carbon hemispheres (HCHs) using glucose as carbon source and solid core mesoporous shell silica (SCMSS) as template and the formation mechanism of the HCHs have been presented. The HCHs show an ultrahigh surface area of 1095.59 m{sup 2} g{sup -1} and an average mesopore size of 9.38 nm. The hemispherical structure with large mesopores also results in the improvement in the mass transfer and therefore more concentrated ethanol solution can be used to increase the energy density. The additional advantage of the HCHs compared to the hollow carbon spheres is that they can provide the similar surface area at reduced volume. The current densities of ethanol oxidation on Pd nanoparticles supported on HCH (Pd/HCH) electrocatalyst are three times as many as on Pd/C at the same Pd loadings. (author)

  8. SYNTHESIS AND BIOTECHNOLOGICAL APPLICATIONS OF VINYL POLYMER-INORGANIC HYBRID AND MESOPOROUS MATERIALS

    Institute of Scientific and Technical Information of China (English)

    Yen Wei; Kun-yuan Qiu

    2000-01-01

    We describe the sol-gel synthesis of a new family of organic-inorganic hybrid materials, in which various vinyl polymers are covalently bonded to and uniformly distributed in inorganic oxide matrices. The materials can be tailored to have both good toughness and hardness while maintaining excellent optical transparency. Doping the sol-gel metal oxides with optically active compounds such as D-glucose results in new optical rotatory composite materials. Removal of the dopant compounds from the composites affords mesoporous oxide materials, which represents a new, nonsurfactant-templated route to mesoporous molecular sieves. We have successfully immobilized a series of enzymes and other bioactive agents in mesoporous materials. Catalytical activities of the enzyme encapsulated in mesoporous materials were found to be much higher than those encapsulated in microporous materials.

  9. Polymer templated nickel cobaltate for energy storage★

    Directory of Open Access Journals (Sweden)

    Albohani Shaymaa

    2017-01-01

    Full Text Available In order to take advantage of the increasing sophistication of technology for harnessing renewable energy resources, serious attention must be paid to how to store and re-access this energy. Electrochemical storage, in the guise of batteries, supercapacitors and pseudocapacitors, has attracted much attention as a viable option for enhanced energy storage applications. But in order for these technologies to be implemented successfully we need to find materials that perform better and are relatively easy to synthesise. Bimetallic transition metal oxides are materials that are readily synthesised and may be multifunctional, i.e. have a role at the electrochemical atomic level as well as the device level. In order for these materials to work efficiently in new generation systems based on sodium and lithium they also need to be mesoporous. This can be achieved by trying to find synthetic techniques that produce specific, highly regulated nanostructures or by adding a ‘templating’ agent during the bulk synthesis step. We have investigated the simple hydrothermal preparation of a number of nickel cobaltate (NiCo2O4 materials using polymer templates, eggshell membrane (ESM and poly methyl methacrylate (PMMA, as potential electrode materials for supercapacitors. The ESM was expected to act as a fibrous, random polymeric template while the PMMA should produce a much more ordered material. Electrochemical testing showed that the different templates have led to changes in material morphology and these have resulted in a difference in electrochemical properties. Templated materials increased specific capacitance compared to non-templated and the choice of template could influence the capacitance by as much as 30%.

  10. Thermal and hydrothermal stability of ZrMCM-41 mesoporous molecular sieves obtained by microwave irradiation

    Indian Academy of Sciences (India)

    T S Jiang; Y H Li; X P Zhou; Q Zhao; H B Yin

    2010-05-01

    ZrMCM-41 mesoporous molecular sieves were synthesized by using the zirconium sulfate as zirconium source and using cetyltrimethyl ammonium bromide as a template under microwave irradiation condition. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), inductive coupled plasma (ICP) technique, Fourier transform infrared spectroscopy (FT-IR) and N2 physical adsorption, respectively. The effect of the different initial ZrO2 : SiO2 molar ratio, the different thermal treatment temperature and hydrothermal treatment time on textural property was investigated. The results show that the obtained products possess a typical mesoporous structure of MCM-41 and have specific surface areas in the range of 598.1 ∼ 971.4 m2/g and average pore sizes in the range of ca. 2.46 ∼ 3.43 nm. On the other hand, the BET specific surface area and pore volume of the synthesized ZrMCM-41 mesoporous molecular sieve decrease with the increased amount of zirconium incorporated in the starting material, the rise of thermal treatment temperature and the prolonging of hydrothermal treatment time, the mesoporous ordering deteriorates. The mesoporous structure of the ZrMCM-41 mesoporous molecular sieve still retains after calcination at 750°C for 3 h or hydrothermal treatment at 100°C for 6 days, however, the mesoporous ordering is poor.

  11. Three-dimensional ordered mesoporous Co3O4 enhanced by Pd for oxygen evolution reaction

    Science.gov (United States)

    Qu, Qing; Zhang, Jian-Hua; Wang, Jing; Li, Qing-Yu; Xu, Chang-Wei; Lu, Xihong

    2017-01-01

    Considerable efforts have been devoted recently to design and fabrication of high performance and low cost electrocatalysts for oxygen evolution reaction (OER). However, catalytic activity of current electrocatalysts is usually restricted by high onset potential and limited active sites. Herein, we fabricated three-dimensional (3D) highly ordered mesoporous Pd-Co3O4 composite materials as excellent electrocatalysts for OER in alkaline solution with high activity and stability. Three-dimensional highly ordered mesoporous Co3O4 material was firstly synthesized using mesoporous silica KIT-6 as hard template. Then, Pd-Co3O4 nanomaterials were prepared by a simple reduction method. The as-prepared 3D mesoporous Pd-Co3O4 catalysts have ordered mesoporous structure with a high surface area of 81.0 m2 g‑1. Three-dimensional highly ordered mesoporous structure can facilitate diffusion and penetration of electrolyte and oxygen. Moreover, the catalysts can also keep catalyst particles in a well dispersed condition with more catalytic active sites. Electrochemical measurements reveal that the 3D mesoporous Pd-Co3O4 catalysts exhibit superior performance in alkaline solution with low onset potential (0.415 V vs. SCE) and excellent long-duration cycling stability.

  12. Study of CO2 adsorption capacity of mesoporous carbon and activated carbon modified by triethylenetetramine (TETA)

    Science.gov (United States)

    Sulistianti, I.; Krisnandi, Y. K.; Moenandar, I.

    2017-04-01

    Mesoporous carbon was synthesized by soft template method using phloroglucinol and formaldehyde as a carbon source; and Pluronic F-127 as a mesoporous template. The synthesized mesoporous carbon and commercial activated carbon were modified with triethylenetetramine (TETA) to increase CO2 adsorption capacity. Based on FTIR characterization, the synthesized mesoporous carbon and the activated carbon without modification process has similarity pattern. After the modification, both of them showed absorption peaks in the area around 1580 to 1650 cm-1 which is known as N-H bending vibration and absorption peaks in the area around 3150 to 3380 cm-1 which is known as N-H stretching vibration. The XRD results showed two peaks at 2θ = 24.21° and 2θ = 43.85°, according to JCPDS index No. 75-1621 those peak are the typical peaks for hexagonal graphite carbon. In BET analysis, the synthesized mesoporous carbon and activated carbon modified TETA have surface area, pore volume and pore diameter lower than without modification process. In carbon dioxide adsorption testing, the synthesized mesoporous carbon showed better performance than the commercial activated carbon for CO2 adsorption both without modification and by modification. The synthesized mesoporous carbon obtained CO2 adsorption of 9.916 mmol/g and the activated carbon of 3.84 mmol/g for on 3.5 hours of adsorption. It is three times better than activated carbon for adsorption of carbon dioxide. The modified mesoporous carbon has the best performance for adsorption of gas CO2 if compared by unmodified.

  13. Application of mesoporous carbon and modified mesoporous carbon for treatment of DMF sewage

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Fang, E-mail: liufangfw@163.com; Gao, Ya; Zhang, Shuang; Yan, Xi; Fan, Fengtao; Zhao, Chaocheng; Sun, Juan [China University of Petroleum(East China), Department of Chemical Engineering (China)

    2016-02-15

    Mesoporous carbon (MC) was prepared in soft template, and potassium ferricyanide was added into MC to prepare the modified mesoporous carbon (MMC). TEM, SEM, FT-IR, and N{sub 2} adsorption–desorption were used to characterize the textural properties of mesoporous materials. The BET specific surface area, pore volume, and the pore size of MC and MMC were 607.6321 and 304.7475 m{sup 2}/g, 0.313552 and 0.603573 cm{sup 3}/g, and 5.4356 and 7.9227 nm, respectively. The adsorption capabilities of MC and MMC were compared with the silica mesoporous material MCM-41. The influences of different adsorption conditions were optimized. For MC, the optimums of adsorbent dose, DMF initial concentration, rotating speed, and pH were 0.002 mg/50 mL, 200 mg/L, 200 r/min, and 4, respectively. MMC showed the highest DMF adsorption capacity at adsorbent dose 0.002 g/50 mL, DMF initial concentration 1000 mg/L, rotating speed 1000 r/min, pH more than 9, and contact time of less than 20 min. Meanwhile for MC, MMC, Pseudo-second-order equation was used to fit adsorption kinetics data. And adsorption process could be well fitted by Langmuir and Freundlich adsorption isotherms of MC, MMC. The results showed that MMC was a perfect adsorbent for DMF, and it was easy to separation and recycle. The recycling property of MMC was still relatively better than other two adsorbents.

  14. Double-Mesopore V-MSU-X Silica and its Pure Siliceous Derivative Prepared by One Synthesis System

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Non-ionically templated organo-modified MSU-2 mesoporous silicas have been prepared in neutral medium by co-condensation TEOS and vinyltriexoylsiloxane (VTES) and exhibit highly symmetric bimodal mesopore systems. A bromination reaction of V-MSU-2 provides evidence for attachment of most vinyl groups to the accessible surface within the channels. Further, siliceous MSU-2 materials with double pore size have been obtained from calcination of so-produced organo-modified MSU-2 and demonstrate the immense flexibility of the non-ionic templating system.

  15. Mesoporous hydroxyapatite: Preparation, drug adsorption, and release properties

    Energy Technology Data Exchange (ETDEWEB)

    Gu, Lina; He, Xiaomei; Wu, Zhenyu, E-mail: zhenyuwuhn@sina.com

    2014-11-14

    Mesoporous hydroxyapatite (HA) was synthesized through gas–liquid chemical precipitation method at ambient temperature without any template. Structure, morphology and pore size distribution of HA were analyzed via X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, high-resolution electron microscopy and N{sub 2} adsorption/desorption. The chemotherapeutic agent doxorubicin (DOX) was used to investigate the drug adsorption and release behavior of HA. The kinetics of DOX adsorption on HA followed the pseudo-second-order rate expression. Adsorption isotherms at various temperatures were obtained, and the equilibrium data fitted the Langmuir model. The values of thermodynamic parameters (Gibbs free energy, entropy, and enthalpy changes) demonstrated that the adsorption process was spontaneous and endothermic. In vitro pH-responsive (pH = 7.4, 5.8) controlled release was investigated. DOX-loaded HA showed a slow, long-term, and steady release rate. The release rate at pH5.8 was larger than that at pH7.4. Consequently, the as-prepared mesoporous HA has potential applications in controlled drug delivery systems. - Highlights: • Mesoporous HA was synthesized by a simple precipitation method without any template. • The kinetics of adsorption followed the pseudo-second-order rate expression. • Thermodynamics investigation showed that adsorption was spontaneous and endothermic. • DOX-loaded HA showed a long-term, steady, and pH-controlled release rate.

  16. N-doped mesoporous alumina for adsorption of carbon dioxide

    Institute of Scientific and Technical Information of China (English)

    Jayshri A.Thote; Ravikrishna V.Chatti; Kartik S.Iyer; Vivek Kumar; Arti N.Valechha; Nitin K.Labhsetwar; Rajesh B.Biniwale; M.K.N.Yenkie; Sadhana S.Rayalu

    2012-01-01

    N-doped mesoporous alumina has been synthesized using chitosan as the biopolymer template.The adsorbent has been thoroughly investigated for the adsorption of CO2 from a simulated flue gas stream (15% CO2 balanced with N2) and compared with commercially available mesoporous alumina procured from SASOL,Germany.CO2 adsorption was studied under different conditions of pretreatment and adsorption temperature,inlet CO2 concentration and in the presence of oxygen and moisture.The adsorption capacity was determined to be 29.4 mg CO2/g of adsorbent at 55℃.This value was observed to be 4 times higher in comparison to that of commercial mesoporous alumina at a temperature of 55℃.Basicity of alumina surface coupled with the presence of nitrogen in template in synthesized sample is responsible for this enhanced CO2 adsorption.Adsorption capacity for CO2 was retained in the presence of oxygen; however moisture had a deteriorating effect on the adsorption capacity reducing it to nearly half the value.

  17. One-pot synthesis of amino functionalized mesoporous silica materials: using simulations to understand transitions between different structures

    NARCIS (Netherlands)

    patti, A; Mackie, A.D.; Zelenak, V.; Siperstein, F.R.

    2008-01-01

    The rich phase behavior of surfactants can be exploited to design materials with a given desired structure and properties. One example includes amino functionalized mesoporous silicas, which can be used in different environmental applications, including removal of heavy metals from water and CO2

  18. Synthesis and characterization of highly ordered functional mesoporous silica thin films with positively chargeable -NH2 groups.

    Science.gov (United States)

    Liu, Nanguo; Assink, Roger A; Smarsly, Bernd; Brinker, C Jeffrey

    2003-05-21

    Highly ordered mesoporous organic-inorganic hybrid silica thin films with covalently bonded, positively chargeable -NH2 terminal groups were synthesized by evaporation induced self-assembly of tetraethoxysilane, 3-aminopropyl-triethoxysilane, and a nonionic surfactant under acid conditions and characterized using TEM, GISAXS, FTIR, SAW-based N2 sorption, and TGA.

  19. C60-PMO: periodic mesoporous buckyballsilica.

    Science.gov (United States)

    Whitnall, Wesley; Cademartiri, Ludovico; Ozin, Geoffrey A

    2007-12-19

    Here we report the first documented synthesis of a periodic mesoporous organosilica (PMO), that contains a multiply bonded C60 moiety integrated into the silica channel walls of the material, dubbed C60-PMO. This is accomplished through the acid-catalyzed co-assembly, of C60(NHCH2CH2CH2Si(OEt)3)x and tetraethylorthosilicate (TEOS) with a polyethyleneoxide-polylpropyleneoxide-polyethyleneoxide triblock copolymer template. The percentage of C60 in the final material was estimated to be a minimum of 63 vol %, but potentially as high as 91 vol %. The effects of the synthesis conditions on the mesostructure of the resulting materials are examined. In particular, we demonstrate that the C60 is uniformly distributed throughout the entire sample by the use of energy dispersive X-ray fluorescence (EDX) analysis and an OsO4 label bonded to the C60.

  20. Incorporation of anti-inflammatory agent into mesoporous silica

    Science.gov (United States)

    Rodrigues Braz, Wilson; Lamec Rocha, Natállia; de Faria, Emerson H.; Silva, Márcio L. A. e.; Ciuffi, Katia J.; Tavares, Denise C.; Furtado, Ricardo Andrade; Rocha, Lucas A.; Nassar, Eduardo J.

    2016-09-01

    The unique properties of macroporous, mesoporous, and microporous systems, including their ability to accommodate molecules of different sizes inside their pores and to act as drug delivery systems, have been the object of extensive studies. In this work, mesoporous silica with hexagonal structure was obtained by template synthesis via the sol-gel process. The resulting material was used as support to accommodate the anti-inflammatory agent indomethacin. The alkaline route was used to prepare the mesoporous silica; cetyltrimethylammonium bromide was employed as porogenic agent. The silica particles were functionalized with 3-aminopropyltriethoxysilane alkoxide (APTES) by the sol-gel post-synthesis method. Indomethacin was incorporated into the silica functionalized with APTES and into non-functionalized silica. The resulting systems were characterized by x-ray diffraction (XRD), specific area, infrared spectroscopy, and thermal analyses (TGA). XRD attested to formation of mesoporous silica with hexagonal structure. This structure remained after silica functionalization with APTES and incorporation of indomethacin. Typical infrared spectroscopy vibrations and organic material decomposition during TGA confirmed silica functionalization and drug incorporation. The specific surface area and pore volume of the functionalized material incorporated with indomethacin decreased as compared with the specific surface area and pore volume of the non-functionalized silica containing no drug, suggesting both the functionalizing agent and the drug were present in the silica. Cytotoxicity tests conducted on normal fibroblasts (GM0479A) cells attested that the silica matrix containing indomethacin was less toxic than the free drug.

  1. Mesopore quality determines the lifetime of hierarchically structured zeolite catalysts

    Science.gov (United States)

    Milina, Maria; Mitchell, Sharon; Crivelli, Paolo; Cooke, David; Pérez-Ramírez, Javier

    2014-05-01

    Deactivation due to coking limits the lifetime of zeolite catalysts in the production of chemicals and fuels. Superior performance can be achieved through hierarchically structuring the zeolite porosity, yet no relation has been established between the mesopore architecture and the catalyst lifetime. Here we introduce a top-down demetallation strategy to locate mesopores in different regions of MFI-type crystals with identical bulk porous and acidic properties. In contrast, well-established bottom-up strategies as carbon templating and seed silanization fail to yield materials with matching characteristics. Advanced characterization tools capable of accurately discriminating the mesopore size, distribution and connectivity are applied to corroborate the concept of mesopore quality. Positron annihilation lifetime spectroscopy proves powerful to quantify the global connectivity of the intracrystalline pore network, which, as demonstrated in the conversions of methanol or of propanal to hydrocarbons, is closely linked to the lifetime of zeolite catalysts. The findings emphasize the need to aptly tailor hierarchical materials for maximal catalytic advantage.

  2. Colloidal suspensions of functionalized mesoporous silica nanoparticles.

    Science.gov (United States)

    Kobler, Johannes; Möller, Karin; Bein, Thomas

    2008-04-01

    The synthesis and characterization of colloidal mesoporous silica (CMS) functionalized with vinyl-, benzyl-, phenyl-, cyano-, mercapto-, aminopropyl- or dihydroimidazole moieties is reported. Uniform mesoporous particles ranging in size from 40 to 150 nm are generated in a co-condensation process of tetraethylorthosilicate (TEOS) and organotriethoxysilanes (RTES) in alkaline aqueous media containing triethanolamine (TEA) in combination with cetyltrimethylammonium chloride (CTACl) serving as a structure-directing agent. The materials are obtained as colloidal suspensions featuring long-term stability after template removal by ion exchange with an ethanolic solution of ammonium nitrate or HCl. The spherical particles exhibit a wormlike pore system with defined pore sizes and high surface areas. Samples are analyzed by a number of techniques including TEM, SEM, DLS, TGA, Raman, and cross-polarized (29)Si-MAS NMR spectroscopy, as well as nitrogen sorption measurements. We demonstrate that co-condensation and grafting methods result in similar changes in the nitrogen adsorption behavior, indicating a successful internal lining of the pores with functional groups through both procedures.

  3. Continuous microwave flow synthesis of mesoporous hydroxyapatite.

    Science.gov (United States)

    Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

    2015-11-01

    We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution.

  4. General synthesis of magnetic mesoporous FeNi/graphitic carbon nanocomposites and their application for dye adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yangang, E-mail: ygwang8136@gmail.com; Yao, Mingcui; Chen, Yuting; Zuo, Yuanhui; Zhang, Xiaodong; Cui, Lifeng, E-mail: lifeng.cui@gmail.com

    2015-04-05

    Graphical abstract: Magnetic mesoporous FeNi alloy/graphitic carbon nanocomposites with different Fe/Ni molar ratios have been synthesized through a simple nanocasting method using mesoporous silica SBA-15 as the template. It was observed that high content of magnetic FeNi alloy nanoparticles with the sizes of 3–6 nm were well dispersed into the walls of graphitic mesoporous carbon matrix, and the obtained magnetic nanocomposites with uniform mesostructure and high surface areas can be used as efficient and recycled adsorbents in the removal of dye from wastewater. - Highlights: • Novel magnetic mesoporous FeNi alloy/graphitic carbon nanocomposites were synthesized. • The synthesis was achieved by a simple nanocasting method using mesoporous silica SBA-15 as the template. • Highly dispersed FeNi alloy nanocrystals were well embedded in the graphitic mesoporous carbon walls. • The obtained magnetic mesoporous nanocomposites have high surface areas and saturation magnetization. • The nanocomposites can be used as efficient and recycled adsorbents in the removal of dye from wastewater. - Abstract: A series of magnetic mesoporous FeNi/graphitic carbon nanocomposites have been synthesized through a simple nanocasting method using mesoporous silica SBA-15 as the template. Metal nitrates and natural soybean oil are respectively used as the magnetic particle precursors and carbon source, which can be infiltrated into the silica template after impregnation, grinding mix and heat treatment. X-ray diffraction, nitrogen adsorption–desorption, inductively coupled plasma mass spectrometry, transmission electron microscopy, vibrating-sample magnetometry and thermogravimetric analysis techniques are used to characterize the samples. It is observed that high content of magnetic FeNi alloy nanocrystals with the sizes of about 3–6 nm are well homodispersed into the walls of graphitic mesoporous carbon matrix, and the resulting nanocomposites have a uniform

  5. 胶原纤维为模板介孔TiO_2和Pt掺杂TiO_2纤维的制备及光催化降解黑液(英文)%Preparation of Mesoporous TiO2 and Pt-Doped TiO2 Fibers with Collagen Fiber as a Template and Their Performance for Photocatalytic Degradation of Black Liquor

    Institute of Scientific and Technical Information of China (English)

    蔡莉

    2012-01-01

    以胶原纤维为模板,Ti(SO4)2为钛源,合成了新型光催化剂—介孔TiO2和Pt掺杂TiO2纤维。通过场发射扫描电镜(FESEM)、比表面积和孔径分析、紫外–可见光谱和分子荧光光谱等检测手段对两种介孔TiO2纤维的结构和物理性能进行了表征。FESEM分析表明,胶原纤维的表面结构能被较好地保留在介孔TiO2和Pt掺杂TiO2纤维中。N2吸附–脱附等温线为IV型,表明TiO2和Pt掺杂TiO2纤维具有介孔结构。基于结构的特点,在可见光和UV-A激发下,介孔TiO2和Pt掺杂TiO2纤维表现出强于商品级纳米TiO2(Degussa P25)的总有机碳(TOC)脱除率。此外,Pt的掺杂能明显改善介孔TiO2的光催化活性。光催化实验表明,Pt掺杂TiO2纤维(1.0g L–1)在可见光照射420 min后,黑液的TOC脱除率为37%;UV-A(360 nm)照射300min后,TOC脱除率为51%。因此,制备的介孔TiO2和Pt掺杂TiO2纤维作为一类性能优异的光催化剂,能用于黑液的光催化降解,并在其他类似的反应条件下具有潜在的应用前景。%The mesoporous TiO2 and Pt-doped TiO2 fibers as a catalyst were prepared with collagen fiber as a template and Ti(SO4)2 as a titanium source.Their structure and physical properties were characterized by field emission scanning electron microscopy(FESEM),specific surface area analysis,UV–Vis absorption spectra and photoluminescence spectra(PL) as well.The FESEM analysis indicated that the well-defined surface morphology of natural collagen fiber was mostly preserved in TiO2 and Pt-doped TiO2 fibers.The N2 adsorption/desorption isotherms of TiO2 and Pt-doped TiO2 fibers were typical type IV due to the characteristics of mesoporous materials.The mesoporous TiO2 and Pt-doped TiO2 fibers revealed a higher total organic carbon(TOC) removal rate of black liquor under visible light and UV-A light irradiation,compared to commercial nano-TiO2(Degussa P25).In addition,the photocatalytic activity of mesoporous

  6. Mesoporous cobalt oxide for largely improved lithium storage properties

    Institute of Scientific and Technical Information of China (English)

    Mai Xia Ma

    2012-01-01

    We report the microstructure,application for lithium-ion batteries of mesoporous Co3O4 prepared by modified KIT-6 template method.The sample was characterized by XRD,TEM,HRTEM and nitrogen adsorption.Their electrochemical behaviors as electrode reactants for lithium ion batteries were evaluated by cyclic voltammograms and static charge-discharge.A direct comparison of electrochemical behaviors between mesoporous nanostructure and bulk reflects interesting "nanostructure effect",which is reasonably discussed in terms of how the 3D nanostructures of Co3O4 materials function in tuning their electrochemistry.The results demonstrate that further improvement of electrochemical performance in transition metal-oxide-based anode materials can be realized via the design of multiporous nanostructured materials.

  7. SAXS andalysis of interface in organo—modified mesoporous silica

    Institute of Scientific and Technical Information of China (English)

    ZhiHongLi; YanJunGong; DongWu; YuHanSun; JunWang; YiLiu; BaozhongDon

    2001-01-01

    A small-angle x-ray scattering(SAXS)technique using synchrotron radiation as the x-ray source has been employed to characterize the microstructure of mesoporous silica prepared by one-pot template-directed synthesis methodology.The scattering of pure silica agreed with Porod’s law.the scattering of organomodified mesoporous silica showed a negative deviation from Porod’s law,suggesting that an interfacial layer exists between the pores and silica matrix.It was the organic groups comprising the interface,as shown by 29Si cross-polarization magic-angle spinning nuclear magnetic resonance imaging (29Si cp MAS/NMR) and Fourier transform infrared spectroscopy(FTIR),that caused this negative deviation of SAXS intensity from Porod’s law,and the average thichness of the interfacial layer could be deduced from this negative deviation.Copyright 2001 john Wiley and Sons,Ltd.

  8. Carbon aerogel with 3-D continuous skeleton and mesopore structure for lithium-ion batteries application

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Xiaoqing, E-mail: yxq-886@163.com [School of Materials and Energy, Guangdong University of Technology, Guangzhou 510006 (China); Huang, Hong [Instrumental Analysis and Research Center, Sun Yat-sen University, Guangzhou 510275 (China); Zhang, Guoqing; Li, Xinxi [School of Materials and Energy, Guangdong University of Technology, Guangzhou 510006 (China); Wu, Dingcai [Materials Science Institute, PCFM Laboratory, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Fu, Ruowen, E-mail: cesfrw@mail.sysu.edu.cn [Materials Science Institute, PCFM Laboratory, School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China)

    2015-01-15

    Carbon aerogel (CA) with 3-D continuous skeleton and mesopore structure was prepared via a microemulsion-templated sol–gel polymerization method and then used as the anode materials of lithium-ion batteries. It was found that the reversible specific capacity of the as-prepared CAs could stay at about 470 mA h g{sup −1} for 80 cycles, much higher than the theoretical capacity of commercial graphite (372 mAh g{sup −1}). In addition, CA also showed a better rate capacity compared to commercial graphite. The good electrochemical properties could be ascribed to the following three factors: (1) the large BET surface area of 620 m{sup 2} g{sup −1}, which can provide more lithium ion insertion sites, (2) 3-D continuous skeleton of CAs, which favors the transport of the electrons, (3) 3-D continuous mesopore structure with narrow mesopore size distribution and high mesopore ratio of 87.3%, which facilitates the diffusion and transport of the electrolyte and lithium ions. - Highlights: • Carbon aerogel (CA) was prepared via a microemulsion-templated sol–gel method. • The CA presents high surface area, 3D continuous skeleton and mesopore structure. • The reversible capacity of CA is much higher than that of graphite.

  9. Preparation, Characterization and Photocatalytic Activity of Lanthanum Doped Mesoporous Titanium Dioxide

    Institute of Scientific and Technical Information of China (English)

    Zhong-liang Shi; Hong Lai; Shu-hua Yao; Shao-feng Wang

    2012-01-01

    Lanthanum doped mesoporous titanium dioxide photocatalysts with different La content were synthesized by template method using tetrabutyltitanate (Ti(OC4H9)4) as precursor and Pluronic P123 as template.The catalysts were characterized by thermogravimetric differential thermal analysis,N2 adsorption-desorption measurements,X-ray diffraction,and UV-Vis adsorption spectroscopy.The effect of La3+ doping concentration from 0.1% to 1%on the photocatalytic activity of mesoporous TiO2 was investigated.The characterizations indicated that the photocatalysts possessed a homogeneous pore diameter of about 10 nm with high surface area of 165 m2/g.X-ray photoelectron spectroscopy measurements indicated the presence of C in the doped samples in addition to La.Compared with pure mesoporous TiO2,the La-doped samples extended the photoabsorption edge into the visible light region.The results of phenol photodecomposition showed that La-doped mesoporous TiO2 exhibited higher photocatalytic activities than pure mesoporous TiO2 under UV and visible light irradiation.

  10. Synthesis and Electrochemical Properties of Semicrystalline Gyroidal Mesoporous MnO2

    Institute of Scientific and Technical Information of China (English)

    ZHOU, Qin; LI, Xiang; LI, Yan-Guang; TIAN, Bo-Zhi; ZHAO, Dong-Yuan; JIANG, Zhi-Yu

    2006-01-01

    Mesoporous silica KIT-6 has novel three-dimensional gyroidal channel structure, space group of Ia-3d, and ordered tunable pores up to 10 nm. In this paper, such mesostructured silica was employed as hard template to prepare semicrystalline gyroidal mesoporous MnO2. The structure was investigated by XRD, TEM and HRTEM, and found to be of high quality Ia-3d symmetry, in good accordance with the template structure. The material has a BET surface of 118 m2·g-1 and pore volume of 0.35 cm3·g-1 after eliminating template. Mesoporous MnO2 has shown good electrochemical property as supercapacitor material in 1 mol·L-1 Na2SO4 and 1 mol·L-1 LiClO4 solutions, but interesting pseudocapacitance behavior was observed in the case of 6 mol·L-1 KOH. It was found that mesoporous MnO2 performed stable reversible electrochemical behavior with capacitance of 220 F·g-1 in a potential range of -0.1-0.55 V vs. Hg/HgO in alkaline solution, demonstrating that it is a promising novel electrode material for the fabrication of electrochemical capacitors.

  11. Synthesis of 2D Nitrogen-Doped Mesoporous Carbon Catalyst for Oxygen Reduction Reaction

    Directory of Open Access Journals (Sweden)

    Zhipeng Yu

    2017-02-01

    Full Text Available 2D nitrogen-doped mesoporous carbon (NMC is synthesized by using a mesoporous silica film as hard template, which is then investigated as a non-precious metal catalyst for the oxygen reduction reaction (ORR. The effect of the synthesis conditions on the silica template and carbon is extensively investigated. In this work, we employ dual templates—viz. graphene oxide and triblock copolymer F127—to control the textural features of a 2D silica film. The silica is then used as a template to direct the synthesis of a 2D nitrogen-doped mesoporous carbon. The resultant nitrogen-doped mesoporous carbon is characterized by transmission electron microscopy (TEM, nitrogen ad/desorption isotherms, X-ray photoelectron spectroscopy (XPS, cyclic voltammetry (CV, and rotating disk electrode measurements (RDE. The electrochemical test reveals that the obtained 2D-film carbon catalyst yields a highly electrochemically active surface area and superior electrocatalytic activity for the ORR compared to the 3D-particle. The superior activity can be firstly attributed to the difference in the specific surface area of the two catalysts. More importantly, the 2D-film morphology makes more active sites accessible to the reactive species, resulting in a much higher utilization efficiency and consequently better activity. Finally, it is noted that all the carbon catalysts exhibit a higher ORR activity than a commercial Pt catalyst, and are promising for use in fuel cells.

  12. Synthesis of 2D Nitrogen-Doped Mesoporous Carbon Catalyst for Oxygen Reduction Reaction

    Science.gov (United States)

    Yu, Zhipeng; Piao, Jinhua; Liang, Zhenxing

    2017-01-01

    2D nitrogen-doped mesoporous carbon (NMC) is synthesized by using a mesoporous silica film as hard template, which is then investigated as a non-precious metal catalyst for the oxygen reduction reaction (ORR). The effect of the synthesis conditions on the silica template and carbon is extensively investigated. In this work, we employ dual templates—viz. graphene oxide and triblock copolymer F127—to control the textural features of a 2D silica film. The silica is then used as a template to direct the synthesis of a 2D nitrogen-doped mesoporous carbon. The resultant nitrogen-doped mesoporous carbon is characterized by transmission electron microscopy (TEM), nitrogen ad/desorption isotherms, X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), and rotating disk electrode measurements (RDE). The electrochemical test reveals that the obtained 2D-film carbon catalyst yields a highly electrochemically active surface area and superior electrocatalytic activity for the ORR compared to the 3D-particle. The superior activity can be firstly attributed to the difference in the specific surface area of the two catalysts. More importantly, the 2D-film morphology makes more active sites accessible to the reactive species, resulting in a much higher utilization efficiency and consequently better activity. Finally, it is noted that all the carbon catalysts exhibit a higher ORR activity than a commercial Pt catalyst, and are promising for use in fuel cells. PMID:28772558

  13. Low temperature synthesis and photocatalytic properties of mesoporous TiO{sub 2} nanospheres

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Hua, E-mail: hutang79@yahoo.com.cn [School of Materials Science and Engineering, Jiangsu University, Key Laboratory of High-End Structural Materials of Jiangsu Province, Zhenjiang 212013 (China); Zhang, Du [School of Materials Science and Engineering, Jiangsu University, Key Laboratory of High-End Structural Materials of Jiangsu Province, Zhenjiang 212013 (China); Tang, Guogang [School of Materials Science and Engineering, Jiangsu University, Key Laboratory of High-End Structural Materials of Jiangsu Province, Zhenjiang 212013 (China); Department of Chemical Engineering, Zhenjiang College, Zhenjiang 212003 (China); Ji, Xiaorui [School of Materials Science and Engineering, Jiangsu University, Key Laboratory of High-End Structural Materials of Jiangsu Province, Zhenjiang 212013 (China); Li, Changsheng [School of Materials Science and Engineering, Jiangsu University, Key Laboratory of High-End Structural Materials of Jiangsu Province, Zhenjiang 212013 (China); Department of Chemical Engineering, Zhenjiang College, Zhenjiang 212003 (China); Yan, Xuehua [School of Materials Science and Engineering, Jiangsu University, Key Laboratory of High-End Structural Materials of Jiangsu Province, Zhenjiang 212013 (China); Wu, Qiong, E-mail: wuqiong9918@126.com [Department of Material Science and Engineering, Liaoning University of Technology, Jinzhou 121001 (China)

    2014-04-05

    Highlights: • Uniform mesoporous TiO{sub 2} nanospheres were prepared by a simple method. • The possible formation mechanism of the mesoporous TiO{sub 2} nanospheres was discussed. • The materials exhibit excellent photocatalytic activity. -- Abstract: Facile one-step synthetic method for the fabrication of uniform mesoporous TiO{sub 2} nanospheres was reported on the basis of template-directed deposition and in situ template-sacrificial dissolution, in which SiO{sub 2} nanospheres was employed as the template and (NH{sub 4}){sub 2}TiF{sub 6} was used as the precursor. The deposition of TiO{sub 2} nanoparticles on the surface of template is accompanied with the dissolution of SiO{sub 2} spherical cores by HF generated during the hydrolysis of (NH{sub 4}){sub 2}TiF{sub 6} in the reaction. The obtained products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), N{sub 2} adsorption–desorption analysis, and UV–visible diffuse reflectance spectroscopy. Furthermore, the photocatalytic activity of samples was evaluated by photocatalytic decolorization of three typical dyes (methyl orange, methylene blue, and rhodamine B) at ambient temperature under UV illumination. The results indicate mesoporous TiO{sub 2} nanospheres exhibited good photocatalytic activity for the degradation of different dyes. These monodisperse mesoporous TiO{sub 2} nanospheres should find various potential applications in photocatalysis, catalysis, solar cell, separation and purification processes.

  14. Gyroidal mesoporous carbon materials and methods thereof

    Energy Technology Data Exchange (ETDEWEB)

    Wiesner, Ulrich B.; Werner, Joerg G.

    2017-07-25

    The present invention relates to, inter alia, gyroidal mesoporous carbon materials and methods of use and manufacture thereof. In one embodiment, the present invention relates to a mesoporous carbon composition comprising a gyroidal mesoporous carbon having an ordered gyroidal structure and mesopores having a pore size of greater than 2 nanometers (nm) in diameter, and more particularly greater than 11 nm in diameter.

  15. The Correlation of Pore Size and Bioactivity of Spray-Pyrolyzed Mesoporous Bioactive Glasses

    Directory of Open Access Journals (Sweden)

    Yu-Jen Chou

    2017-05-01

    Full Text Available SiO2–CaO–P2O5-based mesoporous bioactive glasses (MBGs were synthesized by spray pyrolysis in this study. Three commonly used non-ionic tri-block copolymers (L121, P123, and F127 with various lengths of hydrophilic chains were applied as structural templates to achieve different pore sizes. A mesoporous structure was observed in each as-prepared specimen, and the results showed that the L121-treated MBG had the largest pore size. The results of bioactivity tests indicated that the growth of hydroxyapatite is related to the pore size of the materials.

  16. Surfactants in tribology

    CERN Document Server

    Biresaw, Girma

    2014-01-01

    Surface science and tribology play very critical roles in many industries. Manufacture and use of almost all consumer and industrial products rely on the application of advanced surface and tribological knowledge. The fourth in a series, Surfactants in Tribology, Volume 4 provides an update on research and development activities connecting surfactants and tribological phenomena. Written by renowned subject matter experts, the book demonstrates how improved design of surfactants can be harnessed to control tribological phenomena. Profusely illustrated and copiously referenced, the chapters also

  17. Comparison among Different pH Values of Rhodamine B Solution Impregnated into Mesoporous Silica

    Directory of Open Access Journals (Sweden)

    Juliana Jorge

    2013-05-01

    Full Text Available We studied the behavior of different pH values of Rhodamine B solution impregnated into pores of mesoporous silica, through structural characterization techniques, such as scanning electron microscopy and porosity measurements, and spectroscopic characterization techniques, such as infrared and luminescence spectroscopy; in order to applications in luminescence. Because, Rhodamine B is an interesting xanthene dye whose optical properties depend of many factors, dye concentration and pH values. MSU-4 type mesoporous silica has been synthesized with Tween 60 surfactant as directing-structure agent and tetraethyl orthosilicate (Si(OEt4, TEOS as silica source. The mesoporous structures doped with dyes are promissory materials for several applications, for example, optical sensors and biomarkers.

  18. POLYMERIC SURFACTANT STRUCTURE

    Institute of Scientific and Technical Information of China (English)

    P.M. Saville; J.W. White

    2001-01-01

    Polymeric surfactants are amongst the most widespread of all polymers. In nature, proteins and polysaccharides cause self organization as a result of this surfactancy; in industry, polymeric surfactants play key roles in the food, explosives and surface coatings sectors. The generation of useful nano- and micro-structures in films and emulsions as a result of polymer amphiphilicity and the application of mechanical stress is discussed. The use of X-ray and neutron small angle scattering and reflectivity to measure these structures and their dynamic properties will be described. New results on linear and dendritic polymer surfactants are presented.

  19. Superior electrode performance of mesoporous hollow TiO2 microspheres through efficient hierarchical nanostructures

    Science.gov (United States)

    Zhang, Feng; Zhang, Yu; Song, Shuyan; Zhang, Hongjie

    2011-10-01

    Mesoporous hollow TiO2 microspheres with controlled size and hierarchical nanostructures are designed from a process employing in suit template-assisted and hydrothermal methods. The results show that the hollow microspheres composed of mesoporous nanospheres possess very stable reversible capacity of 184 mAh g-1 at 0.25C and exhibit extremely high power of 122 mAh g-1 at the high rate of 10C. The superior high-rate and high-capacity performance of the sample is attributed to the efficient hierarchical nanostructures. The hollow structure could shorten the diffusion length for lithium ion in the microspheres. The large mesoporous channels between the mesoporous nanospheres provide an easily-accessed system which facilitates electrolyte transportation and lithium ion diffusion within the electrode materials. The electrolyte, flooding the mesoporous channels, can also lead to a high electrolyte/electrode contact area, facilitating transport of lithium ions across the electrolyte/electrode interface. The small mesopores in the meosporous nanospheres can make the electrolyte and lithium ion further diffuse into the interior of electrode materials and increase electrolyte/electrode contact area. The small nanoparticles can also ensure high reversible capacity.

  20. Post-treatment-free synthesis of highly mesoporous carbon for high-performance supercapacitor in aqueous electrolytes

    Science.gov (United States)

    Li, Wenqi; Liu, Simin; Pan, Ning; Zeng, Fanjun; Liu, Yingliang; Zheng, Mingtao; Liang, Yeru

    2017-07-01

    Exploring well-defined pore structure with high porosity has been a long-pursued goal for the development of porous carbon as high-performance supercapacitor electrodes. The pursuit of high surface area while maintaining uniform pore size remains a formidable challenge because their current template-directed synthetic processes are quite complex and time consuming. Here, we report herein a facile and post-treatment-free approach for synthesis of carbon materials with simultaneously high surface area and uniform mesopore size. The key to this preparation strategy is utilization of polytetrafluoroethylene that can in-situ generate hydrofluoric acid to etch out the silica templates during carbonization process. This strategy not only reduces synthesis procedure by combining post-silica-removal and carbonization in a single step, but also eliminates the direct usage of hazardous hydrofluoric acid or corrosive sodium hydroxide. The as-synthesized disordered mesoporous carbon presents higher Langmuir surface area (3257 m2 g-1), Brunauer-Emmett-Teller surface area (2302 m2 g-1) and mesopore rate (99.6%) when compared to traditional mesoporous carbon. With combination of high surface area and uniform mesopore size, the mesoporous carbon exhibits attractive capacitive properties in aqueous electrolytes, including large capacitance of 201 F g-1, high energy density of 28.3 Wh kg-1 and excellent cycling stability.

  1. Surfactant Sector Needs Urgent Readjustment

    Institute of Scientific and Technical Information of China (English)

    Huang Hongzhou

    2007-01-01

    @@ Surfactant industrial system has been basically established After 50 years' development, China has already established a surfactant industrial system with a relatively complete product portfolio and can produce 4714 varieties of surfactants in cationic,anionic, nonionic and amphoteric categories.

  2. Characterization of a chiral nematic mesoporous organosilica using NMR

    Science.gov (United States)

    Manning, Alan; Shopsowitz, Kevin; Giese, Michael; MacLachlan, Mark; Dong, Ronald; Michal, Carl

    2012-10-01

    Using templation with nanocrystalline cellulose, a mesoporous organosilica film with a chiral nematic pore structure has recently been developed. [1] We have used a variety of Nuclear Magnetic Resonance (NMR) techniques to characterize the pore structure. The pore size distribution has been found by analyzing the freezing point depression of absorbed water via NMR cryoporometry. The effective longitudinal and transverse pore diameters for diffusing water were investigated with Pulsed-Field Gradient (PFG) NMR and compared to a 1-D connected-pore model. Preliminary data on testing imposed chiral ordering in absorbed liquid crystals is also presented. [4pt] [1] K.E. Shopsowitz et al. JACS 134(2), 867 (2012)

  3. Mesoporous tertiary oxides via a novel amphiphilic approach

    Energy Technology Data Exchange (ETDEWEB)

    Bennett, Natasha; Hall, Simon R., E-mail: simon.hall@bristol.ac.uk, E-mail: Annela.Seddon@bristol.ac.uk [Bristol Centre for Functional Nanomaterials, Centre for Nanoscience and Quantum Information, Tyndall Avenue, Bristol BS8 1FD, United Kingdom and Complex Functional Materials Group, School of Chemistry, University of Bristol, Bristol BS8 1TS (United Kingdom); Seddon, Annela M., E-mail: simon.hall@bristol.ac.uk, E-mail: Annela.Seddon@bristol.ac.uk; Hallett, James E. [H.H. Wills Physics Laboratory, University of Bristol, Tyndall Avenue, Bristol BS8 1TL (United Kingdom); Kockelmann, Winfried [STFC Rutherford Appleton Laboratory, Chilton OX11 0QX (United Kingdom); Ting, Valeska P. [Department of Chemical Engineering, University of Bath, Bath BA2 7AY (United Kingdom); Sadasivan, Sajanikumari; Tooze, Robert P. [Sasol Technology (UK) Ltd, Purdie Building, North Haugh, St Andrews, Fife KY16 9ST (United Kingdom)

    2016-01-01

    We report a facile biomimetic sol-gel synthesis using the sponge phase formed by the lipid monoolein as a structure-directing template, resulting in high phase purity, mesoporous dysprosium- and gadolinium titanates. The stability of monoolein in a 1,4-butanediol and water mixture complements the use of a simple sol-gel metal oxide synthesis route. By judicious control of the lipid/solvent concentration, the sponge phase of monoolein can be directly realised in the pyrochlore material, leading to a porous metal oxide network with an average pore diameter of 10 nm.

  4. Mesoporous Metal-Containing Carbon Nitrides for Improved Photocatalytic Activities

    OpenAIRE

    Jie Luo; Zhao-Jie Cui; Guo-Long Zang

    2013-01-01

    Graphitic carbon nitrides (g-C3N4) have attracted increasing interest due to their unusual properties and promising applications in water splitting, heterogeneous catalysis, and organic contaminant degradation. In this study, a new method was developed for the synthesis of mesoporous Fe contained g-C3N4 (m-Fe-C3N4) photocatalyst by using SiO2 nanoparticles as hard template and dicyandiamide as precursor. The physicochemical properties of m-Fe-C3N4 were thoroughly investigated. The XRD and XP...

  5. Preparation and characterization of mesoporous tetragonal sulfated zirconia

    Institute of Scientific and Technical Information of China (English)

    Chun Xia He; Bin Yue; Ji Fang Cheng; Wei Ming Hua; Ying Hong Yue; He Yong He

    2009-01-01

    Mesoporous tetragonal sulfated zirconia with high surface area and narrow pore-size distribution was prepared using Zr(O-nPr)4 as zirconium precursor, sulfuric acid as sulfur source and triblock copolymer poly(ethylene glycol)-poly(propylene glycol)poly(ethylene glycol) (P123) as the template. The samples were characterized by X-ray diffraction, N2 sorption, TEM, and NH3TPD. A phase transformation from monoclinic sulfated zirconia to tetragonal sulfated zirconia is observed. The product shows strong acidity.

  6. Preparation, characterization and selective recognition for vanillic acid imprinted mesoporous silica polymers

    Energy Technology Data Exchange (ETDEWEB)

    Li, Hui, E-mail: lihuijsdx@163.com [College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000 (China); Key laboratory of plant resource and utilization, Jishou University, Hunan Jishou 416000 (China); Xu, Miaomiao; Wang, Susu; Lu, Cuimei; Li, Zhiping [College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000 (China)

    2015-02-15

    Highlights: • Preparation of a vanillic acid imprinted mesoporous silica polymers. • Improved selectivity and adsorption capability of this MIPs. • Excellent mass transfer dynamics for the MIPs. • High solid phase extraction applicability toward real sample. - Abstract: A vanillic acid imprinted mesoporous silica polymer (MIPs) was prepared by copolymerizing a modified mesoporous silica molecular sieve with template molecule, functional monomer and cross-linker in present work. Interaction between the template and functional monomer was investigated by ultraviolet/visible spectrophotometry. These MIPs were characterized by Fourier transmission infrared spectrometry (FTIR) and scanning electron microscopy (SEM). Adsorption dynamics and thermodynamic behavior of MIPs was explored and the selective recognition capability evaluated. Also, the applicability for the MIPs as solid phase extraction media was tested. Results indicated the 1:1 (mole ratio) complex of vanillic acid-4-vinylpyridine might predominate in the pre-polymerization mixture and the MIPs obtained possessed rapid binding dynamics and higher affinity toward template molecules, reaching adsorption equilibrium within 230 min with the highest adsorption amount of 50.7 mg g{sup −1}. Freundlich model was shown best to describe isotherm adsorption for the MIPs. The MIPs could selectively bind template molecule with selectivity coefficients of 1.36–1.50. In addition, a higher enrichment capability when using it for gathering target compound from methanol extract of Artemisia stelleriana and a good reusability during adsorption–desorption recycling use could be observed.

  7. Photoactive perylenediimide-bridged silsesquioxane functionalized periodic mesoporous organosilica thin films (PMO-SBA15): synthesis, self-assembly, and photoluminescent and enhanced mechanical properties.

    Science.gov (United States)

    Wahab, M Abdul; Hussain, H; He, Chaobin

    2009-04-21

    Well-organized periodic mesoporous organosilica thin films (designated as PMO-SBA15), having covalently bonded perylene-bridged silesquioxane (PTCDBS) inside their pore channels, are successfully synthesized via sol-gel self-assembly of 1,2-bis(triethoxysilyl)ethane and perylene-bridged silsesquioxane, using micelles of pluronic surfactant (P123) as a template for the first time. The surfactant is successfully removed from the pore channels of PMO-SBA15 by an acidic solvent extraction procedure. The final PMO-SBA15 thin films are characterized by high resolution X-ray diffraction (HRXRD), transmission electron microcopy (TEM), solid-state 29Si and 13C NMR CP/MAS NMR spectroscopy, nitrogen adsorption-desorption measurements, photoluminescence (PL) spectroscopy, and nanoindentation. HRXRD data reveal the formation of well-organized hexagonal channels in the pure PMO-SBA15 films. The intensity of the diffracted X-ray, however, systematically attenuates after incorporation of the perylene functionality inside the hexagonal channels. This is attributed to the low X-ray scattering contrast between the mesostructured organosilica walls and organic moieties (perylene) inside the channels, suggesting the successful incorporation of the photoactive perylene molecules inside the nanochannels. This was further confirmed by photoluminescence spectroscopy and nitrogen adsorption-desorption measurements. Additionally, the mechanical hardness of the functionalized PMO-SBA15 thin films, measured by nanoindentation, is significantly enhanced as compared with that of the pure PMO film. Thermogravimetric analysis (TGA) and elemental analysis suggested the functionalized PMO-SBA15 materials with PTCDBS.

  8. Benzylation of Toluene over Iron Modified Mesoporous Ceria

    Directory of Open Access Journals (Sweden)

    K.J. Rose Philo

    2012-12-01

    Full Text Available Green chemistry has been looked upon as a sustainable science which accomplishes both economical and environmental goals, simultaneously.With this objective, we developed an alternative process to obtain the industrially important benzyl aromatics by benzylation of aromatics using benzyl chloride, catalysed by mesoporous solid acid catalysts. In this work mesoporous ceria is prepared using neutral surfactant which helped the calcination possible at a lower temperature enabling a higher surface area. Mesoporous ceria modified with Fe can be successfully utilized for the selective benzylation of toluene to more desirable product methyl diphenyl methane with 100% conversion and selectivity in 2 hours using only 50mg of the catalyst under milder condition. The reusability, regenerability, high selectivity, 100% conversion, moderate reaction temperature and absence of solvent, etc. make these catalysts to be used in a truly heterogeneous manner and make the benzylation reaction an environment friendly one. Copyright © 2012 by BCREC UNDIP. All rights reservedReceived: 30th June 2012; Revised: 7th November 2012; Accepted: 10th November 2012[How to Cite: K.J. Rose Philo, S. Sugunan. (2012. Benzylation of Toluene over Iron Modified Mesoporouxs Ceria. Bulletin of Chemical Reaction Engineering & Catalysis, 7(2: 158-164. (doi:10.9767/bcrec.7.2.3759.158-164][How to Link / DOI: http://dx.doi.org/10.9767/bcrec.7.2.3759.158-164 ] | View in 

  9. General solution growth of mesoporous NiCo2O4 nanosheets on various conductive substrates as high-performance electrodes for supercapacitors.

    Science.gov (United States)

    Zhang, Genqiang; Lou, Xiong Wen David

    2013-02-20

    Mesoporous NiCo(2) O(4) nanosheets can be directly grown on various conductive substrates, such as Ni foam, Ti foil, stainless-steel foil and flexible graphite paper, through a general template-free solution method combined with a simple post annealing treatment. As a highly integrated binder- and conductive-agent-free electrode for supercapacitors, the mesoporous NiCo(2) O(4) nanosheets supported on Ni foam deliver ultrahigh capacitance and excellent high-rate cycling stability.

  10. SYNTHESIS OF MULTI-WALL CARBON NANOTUBES USING Fe-LOADED MESOPOROUS MOLECULAR SIEVE AS CATALYTIC TEMPLATE%采用负载铁的介孔分子筛催化模板剂合成多壁碳纳米管

    Institute of Scientific and Technical Information of China (English)

    姜廷顺; 李梅; 李艳慧; 李萌; 殷恒波

    2009-01-01

    用水热法合成纯硅介孔分子筛(mesoporous molecular sieves,MCM-41.用浸渍法将MCM-41负载不同量铁制得负载铁的介孔分子筛(Fe-loading mesoporous molecular sieve,Fe/MCM-41).以Fe/MCM-41作为催化剂催化热解乙醇制备碳纳米管.用N2物理吸附、Raman光谱、透射电镜和高分辨透射电镜等手段对样品进行了表征.结果表明:制备出了多壁碳纳米管,并且随着催化剂中Fe负载量的增加,所生成碳纳米管的管径增加.

  11. Core/shell magnetic mesoporous silica nanoparticles with radially oriented wide mesopores

    Directory of Open Access Journals (Sweden)

    Nikola Ž. Knežević

    2014-06-01

    Full Text Available Core/shell nanoparticles, containing magnetic iron-oxide (maghemite core and mesoporous shell with radial porous structure, were prepared by dispersing magnetite nanoparticles and adding tetraethylorthosilicate to a basic aqueous solution containing structure-templating cetyltrimethylammonium bromide and a pore-swelling mesithylene. The material is characterized by SEM and TEM imaging, nitrogen sorption and powder X-ray diffraction. Distinctive features of the prepared material are its high surface area (959 m2/g, wide average pore diameter (12.4 nm and large pore volume (2.3 cm3/g. The material exhibits radial pore structure and the high angle XRD pattern characteristic for maghemite nanoparticles, which are obtained upon calcination of the magnetite-containing material. The observed properties of the prepared material may render the material applicable in separation, drug delivery, sensing and heterogeneous catalysis.

  12. SURFACTANTS IN LUBRICATION

    Science.gov (United States)

    Surfactants are one of the most widely applied materials by consumers and industry. The application areas for surfactants span from everyday mundane tasks such as cleaning, to highly complex processes involving the formulation of pharmaceuticals, foods, pesticides, lubricants, etc. Even though sur...

  13. Dynamic covalent surfactants

    NARCIS (Netherlands)

    Minkenberg, C.B.

    2012-01-01

    In this thesis the development of surfactant aggregates with fast exchange dynamics between the aggregated and non-aggregated state is described. Dynamic surfactant exchange plays an important role in natural systems, for instance in cell signaling, cell division, and uptake and release of cargo. Re

  14. Self-templated chemically stable hollow spherical covalent organic framework

    Science.gov (United States)

    Kandambeth, Sharath; Venkatesh, V.; Shinde, Digambar B.; Kumari, Sushma; Halder, Arjun; Verma, Sandeep; Banerjee, Rahul

    2015-04-01

    Covalent organic frameworks are a family of crystalline porous materials with promising applications. Although active research on the design and synthesis of covalent organic frameworks has been ongoing for almost a decade, the mechanisms of formation of covalent organic frameworks crystallites remain poorly understood. Here we report the synthesis of a hollow spherical covalent organic framework with mesoporous walls in a single-step template-free method. A detailed time-dependent study of hollow sphere formation reveals that an inside-out Ostwald ripening process is responsible for the hollow sphere formation. The synthesized covalent organic framework hollow spheres are highly porous (surface area ~1,500 m2 g-1), crystalline and chemically stable, due to the presence of strong intramolecular hydrogen bonding. These mesoporous hollow sphere covalent organic frameworks are used for a trypsin immobilization study, which shows an uptake of 15.5 μmol g-1 of trypsin.

  15. Nanoconfinement in activated mesoporous carbon of calcium borohydride for improved reversible hydrogen storage.

    Science.gov (United States)

    Comănescu, Cezar; Capurso, Giovanni; Maddalena, Amedeo

    2012-09-28

    Mesoporous carbon frameworks were synthesized using the soft-template method. Ca(BH(4))(2) was incorporated into activated mesoporous carbon by the incipient wetness method. The activation of mesoporous carbon was necessary to optimize the surface area and pore size. Thermal programmed absorption measurements showed that the confinement of this borohydride into carbon nanoscaffolds improved its reversible capacity (relative to the reactive portion) and performance of hydrogen storage compared to unsupported borohydride. Hydrogen release from the supported hydride started at a temperature as low as 100 °C and the dehydrogenation rate was fast compared to the bulk borohydride. In addition, the hydrogen pressure necessary to regenerate the borohydride from the dehydrogenation products was reduced.

  16. Preparation of Mesoporous SnO2 by Electrostatic Self-Assembly

    Directory of Open Access Journals (Sweden)

    Yang Jing

    2014-01-01

    Full Text Available We report a simple and scalable strategy to synthesize mesoporous SnO2 with tin dioxide nanoparticles of 5-6 nm crystalline walls and 3-4 nm pore diameter with the assistance of Mo7O246- as templating agent at room temperature. The samples were characterized by XRD, TEM, UV-DRS, XPS, and BET. The product has a moderately high surface area of 132 m2 g−1 and a narrow mesoporous structure with an average pore diameter of 3.5 nm. The photocatalytic activities of the mesoporous SnO2 were evaluated by the degradation of methyl orange (MO in aqueous solution under UV light irradiation.

  17. Hollow carbonated hydroxyapatite microspheres with mesoporous structure: hydrothermal fabrication and drug delivery property.

    Science.gov (United States)

    Guo, Ya-Jun; Wang, Ying-Ying; Chen, Ting; Wei, Yi-Ting; Chu, Lian-Feng; Guo, Ya-Ping

    2013-08-01

    Hollow carbonated hydroxyapatite microspheres with mesoporous structure (HCHAs) have been fabricated by using calcium carbonated microspheres as sacrificial templates according to the following routes: (i) the in situ deposit of carbonated hydroxyapatite on the surfaces of CaCO3 microspheres by hydrothermal method and (ii) the removal of CaCO3 by chemical etching. The HCHAs consist of a hollow core and a mesoporous shell. Interestingly, the shell of the microspheres is constructed by carbonated hydroxyapatite nanoplates as building blocks. Moreover, these nanoplates are composed of many smaller nanoparticles with different crystal orientations, and the mesopores exist among these nanoparticles. The HCHAs exhibit the high drug-loading capacity and sustained drug release property, suggesting that the hierarchically porous microspheres have great potentials for bone-implantable drug-delivery applications. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Copper benzene tricarboxylate metal-organic framework with wide permanent mesopores stabilized by Keggin polyoxometallate ions.

    Science.gov (United States)

    Wee, Lik H; Wiktor, Christian; Turner, Stuart; Vanderlinden, Willem; Janssens, Nikki; Bajpe, Sneha R; Houthoofd, Kristof; Van Tendeloo, Gustaaf; De Feyter, Steven; Kirschhock, Christine E A; Martens, Johan A

    2012-07-04

    Porous solids with organized multiple porosity are of scientific and technological importance for broadening the application range from traditional areas of catalysis and adsorption/separation to drug release and biomedical imaging. Synthesis of crystalline porous materials offering a network of uniform micro- and mesopores remains a major scientific challenge. One strategy is based on variation of synthesis parameters of microporous networks, such as, for example, zeolites or metal-organic frameworks (MOFs). Here, we show the rational development of an hierarchical variant of the microporous cubic Cu(3)(BTC)(2) (BTC = 1,3,5-benzenetricarboxylate) HKUST-1 MOF having strictly repetitive 5 nm wide mesopores separated by uniform microporous walls in a single crystal structure. This new material coined COK-15 (COK = Centrum voor Oppervlaktechemie en Katalyse) was synthesized via a dual-templating approach. Stability was enhanced by Keggin type phosphotungstate (HPW) systematically occluded in the cavities constituting the walls between the mesopores.

  19. Hierarchical mesoporous/microporous carbon with graphitized frameworks for high-performance lithium-ion batteries

    Directory of Open Access Journals (Sweden)

    Yingying Lv

    2014-11-01

    Full Text Available A hierarchical meso-/micro-porous graphitized carbon with uniform mesopores and ordered micropores, graphitized frameworks, and extra-high surface area of ∼2200 m2/g, was successfully synthesized through a simple one-step chemical vapor deposition process. The commercial mesoporous zeolite Y was utilized as a meso-/ micro-porous template, and the small-molecule methane was employed as a carbon precursor. The as-prepared hierarchical meso-/micro-porous carbons have homogeneously distributed mesopores as a host for electrolyte, which facilitate Li+ ions transport to the large-area micropores, resulting a high reversible lithium ion storage of 1000 mA h/g and a high columbic efficiency of 65% at the first cycle.

  20. Synthesis and Physicochemical Characterization of Mesoporous SiO2 Nanoparticles

    Directory of Open Access Journals (Sweden)

    Dharani Das

    2014-01-01

    Full Text Available There exists a knowledge gap in understanding potential toxicity of mesoporous silica nanoparticles. A critical step in assessing toxicity of these particles is to have a wide size range with different chemistries and physicochemical properties. There are several challenges when synthesizing mesoporous silica nanoparticles over a wide range of sizes including (1 nonuniform synthesis protocols using the same starting materials, (2 the low material yield in a single batch synthesis (especially for particles below 60–70 nm, and (3 morphological instability during surfactant removal process and surface modifications. In this study, we synthesized a library of mesoporous silica nanoparticles with approximate particle sizes of 25, 70, 100, 170, and 600 nm. Surfaces of the silica nanoparticles were modified with hydrophilic-CH2–(CH22–COOH and relatively hydrophobic-CH2–(CH210–COOH functional groups. All silica nanoparticles were analysed for morphology, surface functionality, surface area/pore volume, surface organic content, and dispersion characteristics in liquid media. Our analysis revealed the synthesis of a spectrum of monodisperse bare and surface modified mesoporous silica nanoparticles with a narrow particle size distribution and devoid of cocontaminants critical for toxicity studies. Complete physicochemical characterization of these synthetic mesoporous silica nanoparticles will permit systematic toxicology studies for investigation of structure-activity relationships.

  1. Mesoporous titanium phosphates and related molecular sieves: Synthesis, characterization and applications

    Indian Academy of Sciences (India)

    Asim Bhaumik

    2002-08-01

    Titanium (IV) phosphates TCM-7 and -8 with mesoporous cationic framework topologies using both cationic and anionic surfactants have been synthesized. Experimental data suggest the stabilization of the tetrahedral state of Ti in TCM-7/8 (O-P-O-Ti-O-, at Ti/P = 1:1) vis-à-vis the most stable octahedral state of Ti in the rutile/anatase or pure mesoporous TiO2. Mesoporous TCM-7 and -8 show anion exchange capacity due to the framework phosphonium cation and cation exchange capacity due to defective P-OH groups. Grafting the organic functionality in the surface or bridging the organic moiety in between the inorganic phosphorus precursors can enhance hydrophobicity of these materials similar to that of mesoporous silica materials. The high catalytic activity in the liquid phase partial oxidation of cyclohexene over such organically surface modified mesoporous titanium phosphate using a dilute H2O2 oxidant supports the tetrahedral coordination of Ti in these materials. These materials also show excellent photocatalytic activity in the production of H2 by photo-reduction of water under UV light irradiation.

  2. Adsorption Of Water And Benzene Vapour In Mesoporous Materials

    Directory of Open Access Journals (Sweden)

    Paulina Taba

    2008-11-01

    Full Text Available Mesoporous materials have attracted the attention of many researchers due to the potential applications promised by the materials. This article discusses adsorption of water and benzene vapour in mesoporous materials (mesoporous silica: MCM-41, MCM-48 and their modification. MCM-41 and MCM-48 were synthesized hydrothermally at 100 oC using cethyltrimethylammonium chloride or dodecyltrimethylammonium bromide for MCM-41 (C16 or MCM-41 (C12 respectively and a mixture of cethyltrimethylammonium bromide and Triton X-100 for MCM-48 as templates. Their modifications were conducted by silylation of MCM-41 (C16 and MCM-48 with trimethylchloro silane (MCM16-TMCS and MCM48-TMCS and t-butyldimethylchloro silane (MCM16-TBDMCS and MCM48-TBDMCS. Results showed that MCM-41 and MCM-48 materials had hydrophobic features which were shown in the small amount of water adsorption at low P/P0. The hydrophobicity of samples used in this study decrease in the sequence: MCM-41 (C16 > MCM-48 > MCM-41 (C12. The hydrophobicity increased when MCM-41 and MCM-48 were silylated with TMCS or TBDMCS. All unsilylated MCM materials show higher affinity to benzene at low P/P0 than the silylated samples. The results of water and benzene adsorption showed that silylated samples are promising candidates as selective adsorbents for organic compounds.

  3. Mesoporous Metal-Containing Carbon Nitrides for Improved Photocatalytic Activities

    Directory of Open Access Journals (Sweden)

    Jie Luo

    2013-01-01

    Full Text Available Graphitic carbon nitrides (g-C3N4 have attracted increasing interest due to their unusual properties and promising applications in water splitting, heterogeneous catalysis, and organic contaminant degradation. In this study, a new method was developed for the synthesis of mesoporous Fe contained g-C3N4 (m-Fe-C3N4 photocatalyst by using SiO2 nanoparticles as hard template and dicyandiamide as precursor. The physicochemical properties of m-Fe-C3N4 were thoroughly investigated. The XRD and XPS results indicated that Fe was strongly coordinated with the g-C3N4 matrix and that the doping and mesoporous structure partially deteriorated its crystalline structure. The UV-visible absorption spectra revealed that m-Fe-C3N4 with a unique electronic structure displays an increased band gap in combination with a slightly reduced absorbance, implying that mesoporous structure modified the electronic properties of g-Fe-C3N4. The photocatalytic activity of m-Fe-C3N4 for photodegradation of Rhodamine B (RhB was much higher than that of g-Fe-C3N4, clearly demonstrating porous structure positive effect.

  4. Mesoporous Calcium Silicate Nanoparticles with Drug Delivery and Odontogenesis Properties.

    Science.gov (United States)

    Huang, Ching-Yuang; Huang, Tsui-Hsien; Kao, Chia-Tze; Wu, Yuan-Haw; Chen, Wan-Chen; Shie, Ming-You

    2017-01-01

    Calcium silicate (CS) -based materials play an important role in the development of endodontic materials that induce bone/cementum tissue regeneration and inhibit bacterial viability. The aim of this study was to prepare novel mesoporous CS (MesoCS) nanoparticles that have osteogenic, drug delivery, and antibacterial characteristics for endodontic materials and also have an excellent ability to develop apatite mineralization. The MesoCS nanoparticles were prepared using sol-gel methods. In addition, the mesoporous structure, specific surface area, pore volume, and morphology of the MesoCS nanoparticles were analyzed. The apatite mineralization ability, in vitro odontogenic differentiation, drug delivery, and antibacterial properties of the MesoCS nanoparticles were further investigated. The results indicate that the 200-nm-sized MesoCS nanoparticles synthesized using a facile template method exhibited a high specific surface area and pore volume with internal mesopores (average pore size = 3.05 nm). Furthermore, the MesoCS nanoparticles can be used as drug carriers to maintain sustained release of gentamicin and fibroblast growth factor-2 (FGF-2). The MesoCS-loaded FGF-2 might stimulate more odontogenic-related protein than CS because of the FGF-2 release. Based on this work, it can be inferred that MesoCS nanoparticles are potentially useful endodontic materials for biocompatible and osteogenic dental pulp tissue regenerative materials. Copyright © 2016 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

  5. Kinetically Controlled Synthesis of Pt-Based One-Dimensional Hierarchically Porous Nanostructures with Large Mesopores as Highly Efficient ORR Catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Shaofang; Zhu, Chengzhou; Song, Junhua; Engelhard, Mark H.; Xia, Haibing; Du, Dan; Lin, Yuehe

    2016-12-28

    Rational design and construction of Pt-based porous nanostructures with large mesopores have triggered significant considerations because of their high surface area and more efficient mass transport. Hydrochloric acid-induced kinetic reduction of metal precursors in the presence of soft template F-127 and hard template tellurium nanowires has been successfully demonstrated to construct one-dimensional hierarchical porous PtCu alloy nanostructures with large mesopores. Moreover, the electrochemical experiments demonstrated that the resultant PtCu hierarchically porous nanostructures with optimized composition exhibit enhanced electrocatalytic performance for oxygen reduction reaction.

  6. Surfactants in the environment.

    Science.gov (United States)

    Ivanković, Tomislav; Hrenović, Jasna

    2010-03-01

    Surfactants are a diverse group of chemicals that are best known for their wide use in detergents and other cleaning products. After use, residual surfactants are discharged into sewage systems or directly into surface waters, and most of them end up dispersed in different environmental compartments such as soil, water or sediment. The toxic effects of surfactants on various aquatic organisms are well known. In general, surfactants are present in the environment at levels below toxicity and in Croatia below the national limit. Most surfactants are readily biodegradable and their amount is greatly reduced with secondary treatment in wastewater treatment plants. The highest concern is the release of untreated wastewater or wastewater that has undergone primary treatment alone. The discharge of wastewater polluted with massive quantities of surfactants could have serious effects on the ecosystem. Future studies of surfactant toxicities and biodegradation are necessary to withdraw highly toxic and non-biodegradable compounds from commercial use and replace them with more environmentally friendly ones.

  7. Pulmonary surfactant and lung transplantation

    NARCIS (Netherlands)

    Erasmus, Michiel Elardus

    1997-01-01

    Pulmonary surfactant lowers the surface tension at the air-water interface inside the alveolus. This is achieved by adsorption of surfactant phospholipids at the air-water interface, a process controlled by surfactant-associated proteins, such as SP-A. In this way, surfactant prevents collapse of th

  8. Fundamentals of tri-block copolymer self-assembly in solutions, and its relation to nano-templating

    NARCIS (Netherlands)

    Denkova, A.G.

    2009-01-01

    The purpose of this thesis is to obtain a better understanding of the formation mechanism of mesoporous silica materials, such as SBA-15 that use block copolymers as templating agents. Despite the fact that these materials are now extensively synthesized, the fundamental role of the different synthe

  9. Mesoporous Pt and Pt/Ru alloy electrocatalysts for methanol oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Franceschini, Esteban A. [Grupo de Celdas de Combustible, Departamento de Fisica de la Materia Condensada, Centro Atomico Constituyentes, CNEA. Av. General Paz 1499 (1650), San Martin, Buenos Aires (Argentina); Planes, Gabriel A. [Departamento de Quimica, Facultad de Ciencias Exactas, Fisicoquimicas y Naturales, Universidad Nacional de Rio Cuarto, Agencia Postal No 3, 5800, Rio Cuarto (Argentina); Williams, Federico J. [Departamento de Quimica Inorganica, Analitica y Quimica-Fisica, INQUIMAE CONICET, Facultad Ciencias Exactas y Naturales, Pabellon 2, Ciudad Universitaria, Buenos Aires (Argentina); Soler-Illia, Galo J.A.A. [Gerencia de Quimica, Centro Atomico Constituyentes, CNEA. Av. General Paz 1499 (1650), San Martin, Buenos Aires (Argentina); Corti, Horacio R. [Grupo de Celdas de Combustible, Departamento de Fisica de la Materia Condensada, Centro Atomico Constituyentes, CNEA. Av. General Paz 1499 (1650), San Martin, Buenos Aires (Argentina); Departamento de Quimica Inorganica, Analitica y Quimica-Fisica, INQUIMAE CONICET, Facultad Ciencias Exactas y Naturales, Pabellon 2, Ciudad Universitaria, Buenos Aires (Argentina)

    2011-02-15

    Mesoporous Pt and Pt/Ru catalysts with 2D-hexagonal mesostructure were synthesized using a triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) copolymer (Pluronic F127 {sup registered}) template, on a gold support. Large electrochemical surface areas were observed for the catalysts prepared at high overpotentials. Compared to the Pt catalyst, the Pt/Ru alloy containing 3 at% of Ru exhibited lower onset potential and more than three times the limit mass activity for methanol oxidation. This behavior is assigned to the larger pore size of the mesoporous Pt and Pt/Ru catalysts obtained with this template that seems to improve the methanol accessibility to the active sites compared to those obtained using lyotropic liquid crystals. (author)

  10. A novel fabrication of meso-porous silica film by sol-gol of TEOS

    Institute of Scientific and Technical Information of China (English)

    殷明志; 姚熹; 张良莹

    2004-01-01

    A homogeneous crack-free nano- or meso-porous silica films on silicon was fabricated by colloidal silica sol derived by hydrolyzing tetraethyl orthosilicate (TEOS) catalyzing with (C4H9)4N+OH- in water medium. The solution with ratio of H2O/TEOS≥15, R4N+ and glycerol as templates, combining with the hydrolyzed intermediate, controlled the silica aggregating; the templated silica film with heterostructure was developed into homogeneous nano-porous then meso-porous silica films after being annealed from 750 ℃ to 850 ℃; the formation mechanism of the porous silica films was discussed; morphologies of the silica films were characterized. The refractive indexes of the porous silica films were 1.256-1.458, the thermal conductivity < 0.7 W/m/K. The fabricating procedure and the sequence had not been reported before.

  11. Facile synthesis and unique physicochemical properties of three-dimensionally ordered macroporous magnesium oxide, gamma-alumina, and ceria-zirconia solid solutions with crystalline mesoporous walls.

    Science.gov (United States)

    Li, Huining; Zhang, Lei; Dai, Hongxing; He, Hong

    2009-05-18

    Three-dimensionally (3D) ordered macroporous (3DOM) MgO, gamma-Al(2)O(3), Ce(0.6)Zr(0.4)O(2), and Ce(0.7)Zr(0.3)O(2) with polycrystalline mesoporous walls have been successfully fabricated with the triblock copolymer EO(106)PO(70)EO(106) (Pluronic F127) and regularly packed monodispersive polymethyl methacrylate (PMMA) microspheres as the template and magnesium, aluminum, cerium and zirconium nitrate(s), or aluminum isopropoxide as the metal source. The as-synthesized metal oxides were characterized by means of techniques such as X-ray diffraction (XRD), thermogravimetric analysis/differential scanning calorimetry (TGA/DSC), Fourier transform infrared (FT-IR), high-resolution scanning electron microscopy (HRSEM), high-resolution transmission electron microscopy/selected area electron diffraction (HRTEM/SAED), BET, carbon dioxide temperature-programmed desorption (CO(2)-TPD), and hydrogen temperature-programmed reduction (H(2)-TPR). It is shown that the as-fabricated MgO, gamma-Al(2)O(3), Ce(0.6)Zr(0.4)O(2), and Ce(0.7)Zr(0.3)O(2) samples possessed single-phase polycrystalline structures and displayed a 3DOM architecture; the MgO, Ce(0.6)Zr(0.4)O(2), and Ce(0.7)Zr(0.3)O(2) samples exhibited worm-hole-like mesoporous walls, whereas the gamma-Al(2)O(3) samples exhibited 3D ordered mesoporous walls. The solvent (ethanol or water) nature and concentration, metal precursor, surfactant, and drying condition have an important impact on the pore structure and surface area of the final product. The introduction of surfactant F127 to the synthesis system could significantly enhance the surface areas of the 3DOM metal oxides. With PMMA and F127 in a 40% ethanol solution, one can generate well-arrayed 3DOM MgO with a surface area of 243 m(2)/g and 3DOM Ce(0.6)Zr(0.4)O(2) with a surface area of 100 m(2)/g; with PMMA and F127 in an ethanol-HNO(3) solution, one can obtain 3DOM gamma-Al(2)O(3)with a surface area of 145 m(2)/g. The 3DOM MgO and 3DOM gamma-Al(2)O(3) samples showed

  12. Breakthroughs in Mesoporous Composite Materials

    Institute of Scientific and Technical Information of China (English)

    2012-01-01

    Mesoporous materials have attracted a great deal of attention due to their extremely high surface area, uniform and tunable pore structure (2-50nm in diameter), and have been investigated extensively since its invention. Unfortunately,their catalytic properties are far away from the expectation due to their amorphous and inert framework and poor stability. This research project is aimed at the design and synthesis of mesoporous-

  13. Amino acid-based surfactants – do they deserve more attention?

    Science.gov (United States)

    Bordes, Romain; Holmberg, Krister

    2015-08-01

    The 20 standard amino acids (together with a few more that are not used in the biosynthesis of proteins) constitute a versatile tool box for synthesis of surfactants. Anionic, cationic and zwitterionic amphiphiles can be prepared and surfactants with several functional groups can be obtained by the proper choice of starting amino acid. This review gives examples of procedures used for preparation and discusses important physicochemical properties of the amphiphiles and how these can be taken advantage of for various applications. Micelles with a chiral surface can be obtained by self-assembly of enantiomerically pure surfactants and such supramolecular chirality can be utilized for asymmetric organic synthesis and for preparation of mesoporous materials with chiral pores. Surfactants based on amino acids with two carboxyl groups are effective chelating agents and can be used as collectors in mineral ore flotation. A surfactant based on cysteine readily oxidizes into the corresponding cystine compound, which can be regarded as a gemini surfactant. The facile and reversible cysteine-cystine transformation has been taken advantage of in the design of a switchable surfactant. A very attractive aspect of surfactants based on amino acids is that the polar head-group is entirely natural and that the linkage to the hydrophobic tail, which is often an ester or an amide bond, is easily cleaved. The rate of degradation can be tailored by the structure of the amphiphile. The ester linkage in betaine ester surfactants is particularly susceptible to alkaline hydrolysis and this surfactant type can be used as a biocide with short-lived action. This paper is not intended as a full review on the topic. Instead it highlights concepts that are unique to amino acid-based surfactants and that we believe can have practical implications.

  14. Synthesis of high-quality mesoporous silicon particles for enhanced lithium storage performance

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Chundong, E-mail: apcdwang@hust.edu.cn [School of Optical and Electronic Information, Huazhong University of Science and Technology, Wuhan 430074 (China); Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China); Ren, Jianguo [Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China); Chen, Hao [Department of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou (China); Zhang, Yi [School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan, 430073 (China); Ostrikov, Kostya [School of Chemistry, Physics, and Mechanical Engineering, Queensland University of Technology, Brisbane 4000, QLD (Australia); Manufacturing Flagship, CSIRO, P. O. Box 218, Lindfield, NSW 2070 (Australia); Zhang, Wenjun [Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China); Li, Yi, E-mail: liyi@suda.edu.cn [Department of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou (China); Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China)

    2016-04-15

    Silicon has been considered as one of the most promising anode materials for high-capacity lithium-ion batteries (LIBs) due to its ultrahigh theoretical capacity, abundance, and environmentally benign nature. Nonetheless, the severe break during the prolonged cycling results in poor electrochemical performance, which hinders its practical application. Herein, we report the synthesis of novel mesoporous silicon particles with a facile template method by using a magnesiothermic reduction for LIBs. The obtained silicon nanoparticles are highly porous with densely porous cavities (20–40 nm) on the wall, of which it presents good crystallization. Electrochemical measurements showed that the mesoporous silicon nanoparticles delivered a high reversible specific capacity of 910 mA h g{sup −1} at a high current density of 1200 mA g{sup −1} over 50 cycles. The specific capacity at such high current density is still over twofold than that of commercial graphite anode, suggesting that the nanoporous Si architectures is suitable for high-performance Si-based anodes for lithium ion batteries in terms of capacity, cycle life, and rate capacity. - Highlights: • Silica nanotubes were prepared with a facile template method. • Novel mesoporous silicon particles were obtained by magnesiothermic reduction. • High-Performance LIBs were achieved by using mesoporous Si particle Electrodes.

  15. Highly mesoporous metal-organic framework assembled in a switchable solvent

    Science.gov (United States)

    Peng, Li; Zhang, Jianling; Xue, Zhimin; Han, Buxing; Sang, Xinxin; Liu, Chengcheng; Yang, Guanying

    2014-07-01

    The mesoporous metal-organic frameworks are a family of materials that have pore sizes ranging from 2 to 50 nm, which have shown promising applications in catalysis, adsorption, chemical sensing and so on. The preparation of mesoporous metal-organic frameworks usually needs the supramolecular or cooperative template strategy. Here we report the template-free assembly of mesoporous metal-organic frameworks by using CO2-expanded liquids as switchable solvents. The mesocellular metal-organic frameworks with large mesopores (13-23 nm) are formed, and their porosity properties can be easily adjusted by controlling CO2 pressure. Moreover, the use of CO2 can accelerate the reaction for metal-organic framework formation from metal salt and organic linker due to the viscosity-lowering effect of CO2, and the product can be recovered through CO2 extraction. The as-synthesized mesocellular metal-organic frameworks are highly active in catalysing the aerobic oxidation of benzylic alcohols under mild temperature at atmospheric pressure.

  16. The Trouble With Templates

    CERN Document Server

    Sampson, Laura; Yunes, Nicolas

    2013-01-01

    Waveform templates are a powerful tool for extracting and characterizing gravitational wave signals, acting as highly restrictive priors on the signal morphologies that allow us to extract weak events buried deep in the instrumental noise. The templates map the waveform shapes to physical parameters, thus allowing us to produce posterior probability distributions for these parameters. However, there are attendant dangers in using highly restrictive signal priors. If strong field gravity is not accurately described by General Relativity (GR), then using GR templates may result in fundamental bias in the recovered parameters, or even worse, a complete failure to detect signals. Here we study such dangers, concentrating on three distinct possibilities. First, we show that there exist modified theories compatible with all existing tests that would fail to be detected by the LIGO/Virgo network using searches based on GR templates, but which would be detected using a one parameter post-Einsteinian extension. Second...

  17. E3 Charter Template

    Science.gov (United States)

    This is a charter template which includes decisions made during the project planning phase, as well as local project goals, a communication strategy, an outreach strategy, distribution of responsibilities and a schedule.

  18. images_template

    Data.gov (United States)

    National Aeronautics and Space Administration — Images for the website template go here. It will not change their names or locations, but will hopefully help to organize them. Oh, but for a directory structure...

  19. Synthesis of highly phosphonic acid functionalized benzene-bridged periodic mesoporous organosilicas for use as efficient dye adsorbents

    Energy Technology Data Exchange (ETDEWEB)

    Deka, Juti Rani; Liu, Chia-Ling; Wang, Tzu-Hua; Chang, Wei-Chieh; Kao, Hsien-Ming, E-mail: hmkao@cc.ncu.edu.tw

    2014-08-15

    Highlights: • Synthesis of highly phosphonic acid functionalized benzene-bridged PMOs. • Phosphonic acid loaded PMOs as adsorbent for cationic and anionic dyes. • Due to electrostatic interaction the adsorbent has high dye adsorption capacity. • π–π stacking interaction between benzene and dye enhances adsorption capacity. • Intraparticle diffusion played a dominant role in the adsorption process. - Abstract: Periodic mesoporous organosilicas (PMOs) with benzene bridging groups in the silica wall were functionalized with a tunable content of phosphonic acid groups. These bifunctional materials were synthesized by co-condensation of two different organosilane precursors, that is, 1,4-bis(triethoxysilyl)benzene (BTEB) and sodium 3-(trihydroxysilyl)propyl methyl phosphate (SPMP), under acidic conditions using nonionic surfactant Brij-S10 as template. The materials exhibited well-ordered mesostructures and were characterized by X-ray diffraction, nitrogen sorption, TEM, TGA, FTIR, and solid-state NMR measurements. The materials thus obtained were employed as adsorbents to remove different types of dyes, for example, cationic dyes methylene blue and phenosafranine, anionic orange II, and amphoteric rhodamine B, from aqueous solutions. The materials exhibited a remarkably high adsorption capacity than activated carbon due to their ordered mesostructures, a large number of phosphonic acid groups, and high surface areas. The adsorption was mainly governed by electrostatic interaction, but also involved π–π stacking interaction as well as hydrogen bonding. The adsorption kinetics can be better fitted by the pseudo-second order model. The adsorption process was controlled by the mechanisms of external mass transfer and intraparticle diffusion. The materials retained more than 97% dye removal efficiency after use for five consecutive cycles.

  20. Effect of the Si/Zr molar ratio on the synthesis of Zr-based mesoporous molecular sieves

    Energy Technology Data Exchange (ETDEWEB)

    Salas, P. [Centro de Fisica Aplicada y Tecnologia Avanzada, Universidad Nacional Autonoma de Mexico, Apartado Postal 1-1010, Queretaro 76000 (Mexico)], E-mail: psalas@fata.unam.mx; Wang, J.A. [Escuela Superior de Ingenieria Quimica e Industrias Extractivas, Instituto Politecnico Nacional, Av. Politecnico S/N, Col. Zacatenco, 07738 Mexico D.F. (Mexico); Armendariz, H.; Angeles-Chavez, C. [Instituto Mexicano del Petroleo, Eje Lazaro Cardenas 152, 07730 Mexico D.F. (Mexico); Chen, L.F. [Escuela Superior de Ingenieria Quimica e Industrias Extractivas, Instituto Politecnico Nacional, Av. Politecnico S/N, Col. Zacatenco, 07738 Mexico D.F. (Mexico)

    2009-03-15

    Highly ordered Zr-based mesoporous molecular sieves were synthesized via a surfactant-templated method and the effect of the Si/Zr molar ratio on the crystalline structure, textural properties and surface acidity were studied by XRD, FTIR, TEM and {sup 29}Si MAS-NMR techniques. FTIR spectra show that the intensity of the band around 890 cm{sup -1} which corresponds to the vibration of Si-O-Zr bond was increased with increasing of the zirconium content, therefore, this band may be used as an indicator of the degree of the zirconium incorporation into the Si-framework. When the zirconium content increased in the materials, the Q{sup 3}/Q{sup 4} value obtained from {sup 29}Si MAS-NMR was linearly increased, whereas, the intensity the XRD peaks was gradually reduced; as a result, the pore wall thickness of the resultant materials was gradually increased, the surface area and the structural regularity were diminished. In order to obtain Zr-MCM-41 with highly ordered mesostructure and large surface area, proper Si/Zr molar ratio is a key factor, e.g., Si/Zr should be no less than 10. It was also found that the Bronsted acid sites which resulted from charge unbalance or local structure deformation due to the Zr{sup 4+} incorporation into the vicinity of the hydroxyls carrying silicon were created on the surface of the Zr-MCM-41 solids; strong Bronsted acidity could be formed on the solid with high zirconium content.

  1. Surfactant-free synthesis, luminescent properties, and drug-release properties of LaF3 and LaCO3F hollow microspheres.

    Science.gov (United States)

    Lv, Ruichan; Gai, Shili; Dai, Yunlu; He, Fei; Niu, Na; Yang, Piaoping

    2014-01-21

    Uniform LaF3 and LaCO3F hollow microspheres were successfully synthesized through a surfactant-free route by employing La(OH)CO3 colloidal microspheres as a sacrificial template and NaBF4 as the fluorine source. The synthetic process consists of two steps: the preparation of a La(OH)CO3 precursor via a facile urea-based precipitation and the following formation of lanthanide fluoride hollow microspheres under aqueous conditions at low temperature (50 °C) and short reaction time (3 h), without using any surfactant and catalyst. The formation of hollow spheres with controlled size can be assigned to the Kirkendall effect. It is found that the phase and structure of the products can be simply tuned by changing the pH values of the solution. Time-dependent experiments were employed to study the possible formation process. N2 adsorption/desorption results indicate the mesoporous nature of LaF3 hollow spheres. Yb(3+)/Er(3+) (Ho(3+)) and Yb(3+)/Tm(3+)-doped LaF3 hollow spheres exhibit characteristic up-conversion (UC) emissions of Er(3+) (Ho(3+)) and Tm(3+) under 980 nm laser-diode excitation, and Ce(3+)/Tb(3+)-doped LaF3 and LaCO3F emit bright yellow-green and near-white light under UV irradiation, respectively. In particular, LaF3:Yb/Er and LaCO3F:Ce/Tb hollow microspheres exhibit obvious sustained and pH-dependent doxorubicin release properties. The luminescent properties of the carriers allow them to be tracked or monitored during the release or therapy process, suggesting their high potential in the biomedical field.

  2. Synthesis of inorganic mesopore materials and their application to control chemical reactions; Muki meso kukan zairyo no gosei to kagaku hannoba to shite no riyo gijutsu ni kansuru kenkyu

    Energy Technology Data Exchange (ETDEWEB)

    Ohashi, F.; Tomura, S.; Maeda, M.; Inukai, K.; Suzuki, M.; Okazaki, M.; Konishi, Y.; Toriyama, K. [National Industrial Research Institute of Nagoya,Nagoya (Japan)

    2000-10-25

    Materials enabling 'intelligent humidity control' were synthesized by using fumed silica, tetraethylorthotitanate, and a surfactant (alkyltrimethylammonium bromides (C{sub n}H{sub 2n+1}(CH{sub 3}){sub 3}N{sup +} (center dot) Br{sup -}, n=10 - 16) as a liquid-crystal template) under a hydrothermal condition. A homogeneous hexagonal structure of SiO{sub 2}-TiO{sub 2} was confirmed from X-ray diffraction analysis and TEM observation. These products had a high BET surface area of 540-863m{sup 2}/g and auniform pore diameter of 1.5-3nm, both of which were controlled by varyingthe size of the organic template molecule. A sharp increase in water adsorption was observed when the relative pressure (P/Po) increased in the range 0.4 - 0.6. Over this region, the weight % of water came in the range 20 - 50mass%. The water vapor adsorption isotherm was classified as type V in the IUPAC notation, which is characteristic of an unusually large hysteresis. This large hysteresis can be explained from the fact that the contact angle depends on whether water is being adsorbed or desorbed. High durability in their humidity-control ability was confirmed from repeated observation of the isotherm. As a characteristic of the chemical structure upon titanium incorporation, a wider distributionof the Si-O-Si angles in the SiO{sub 4} tetrahedra was indicated from the broad Q{sup 4} {sup 29}Si-MAS/NMR spectra with a small peak shift. To clarify the formation process of these mesoporous materials in the template-synthesis, we accumulated the basic parameters of micelles from the product-yield-detected ESR observations. In addition, as a model of the chemical reaction in the mesoporous material, we observed the reaction dynamics in a spherical micelle with the same technique Based on these preliminary experiments we designed a column reactor packed with a me soporous material to control the liquid phase reaction. (author)

  3. Engineered monodisperse mesoporous materials

    Energy Technology Data Exchange (ETDEWEB)

    Saunders, R.S.; Small, J.H.; Lagasse, R.R.; Schroeder, J.L.; Jamison, G.M.

    1997-08-01

    Porous materials technology has developed products with a wide variety of pore sizes ranging from 1 angstrom to 100`s of microns and beyond. Beyond 15{angstrom} it becomes difficult to obtain well ordered, monodisperse pores. In this report the authors describe efforts in making novel porous material having monodisperse, controllable pore sizes spanning the mesoporous range (20--500 {angstrom}). They set forth to achieve this by using unique properties associated with block copolymers--two linear homopolymers attached at their ends. Block copolymers phase separate into monodisperse mesophases. They desired to selectively remove one of the phases and leave the other behind, giving the uniform monodisperse pores. To try to achieve this the authors used ring-opening metathesis polymerization to make the block copolymers. They synthesized a wide variety of monomers and surveyed their polymers by TGA, with the idea that one phase could be made thermally labile while the other phase would be thermally stable. In the precipitated and sol-gel processed materials, they determined by porosimetry measurements that micropores, mesopores, and macropores were created. In the film processed sample there was not much porosity present. They moved to a new system that required much lower thermal treatments to thermally remove over 90% of the labile phase. Film casting followed by thermal treatment and solvent extraction produced the desired monodisperse materials (based solely on SEM results). Modeling using Density Functional Theory was also incorporated into this project. The modeling was able to predict accurately the domain size and spacing vs. molecular weight for a model system, as well as accurate interfacial thicknesses.

  4. Template-directed hydrothermal synthesis of hydroxyapatite as a drug delivery system for the poorly water-soluble drug carvedilol

    Energy Technology Data Exchange (ETDEWEB)

    Zhao Qinfu [Department of Pharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Wang Tianyi [Department of Clinical Pharmacy, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Wang Jing [Department of Physical Chemistry, School of Basic Science, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Zheng Li; Jiang, Tongying; Cheng Gang [Department of Pharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China); Wang Siling, E-mail: silingwang@syphu.edu.cn [Department of Pharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No.103, Wenhua Road, Shenyang 110016 (China)

    2011-09-15

    In order to improve the dissolution rate and increase the bioavailability of a poorly water-soluble drug, intended to be administered orally, the biocompatible and bioactive mesoporous hydroxyapatite (HA) was successfully synthesized. In the present study, mesoporous HA nanoparticles were produced using Pluronic block co-polymer F127 and cetyltrimethylammonium bromide (CTAB) as templates by the hydrothermal method. The obtained mesoporous HA was employed as a drug delivery carrier to investigate the drug storage/release properties using carvedilol (CAR) as a model drug. Characterizations of the raw CAR powder, mesoporous HA and CAR-loaded HA were carried out by the scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, N{sub 2} adsorption/desorption, thermogravimetric analysis (TGA), and UV-VIS spectrophotometry. The results demonstrated that CAR was successfully incorporated into the mesoporous HA host. In vitro drug release studies showed that mesoporous HA had a high drug load efficiency and provided immediate release of CAR compared with micronized raw drug in simulated gastric fluid (pH 1.2) and intestinal fluid (pH 6.8). Consequently, mesoporous HA is a good candidate as a drug carrier for the oral delivery of poorly water-soluble drugs.

  5. Phosphine oxide surfactants revisited.

    Science.gov (United States)

    Stubenrauch, Cosima; Preisig, Natalie; Laughlin, Robert G

    2016-04-01

    This review summarizes everything we currently know about the nonionic surfactants alkyl dimethyl (C(n)DMPO) and alkyl diethyl (C(n)DEPO) phosphine oxide (PO surfactants). The review starts with the synthesis and the general properties (Section 2) of these compounds and continues with their interfacial properties (Section 3) such as surface tension, surface rheology, interfacial tension and adsorption at solid surfaces. We discuss studies on thin liquid films and foams stabilized by PO surfactants (Section 4) as well as studies on their self-assembly into lyotropic liquid crystals and microemulsions, respectively (Section 5). We aim at encouraging colleagues from both academia and industry to take on board PO surfactants whenever possible and feasible because of their broad variety of excellent properties.

  6. Effect of polyvinylpyrrolidone on mesoporous silica morphology and esterification of lauric acid with 1-butanol catalyzed by immobilized enzyme

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jinyu; Zhou, Guowei, E-mail: guoweizhou@hotmail.com; Jiang, Bin; Zhao, Minnan; Zhang, Yan

    2014-05-01

    Mesoporous silica materials with a range of morphology evolution, i.e., from curved rod-shaped mesoporous silica to straight rod-shaped mesoporous silica, were successfully prepared using polyvinylpyrrolidone (PVP) and triblock copolymer as dual template. The effects of PVP molecular weight and concentration on mesoporous silica structure parameters were studied. Results showed that surface area and pore volume continuously decreased with increased PVP molecular weight. Mesoporous silica prepared with PVP K30 also possessed larger pore diameter, interplanar spacing (d{sub 100}), and cell parameter (a{sub 0}) than that prepared with PVP K15 and PVP K90. In addition, with increased PVP concentration, d{sub 100} and a{sub 0} continuously decreased. The mechanism of morphology evolution caused by the change in PVP concentration was investigated. The conversion rate of lauric acid with 1-butanol catalyzed by immobilized Porcine pancreatic lipase (PPL) was also evaluated. Results showed that PPL immobilized on amino-functionalized straight rod-shaped mesoporous silica maintained 50% of its esterification conversion rate even after five cycles of use with a maximum conversion rate was about 90.15%. - Graphical abstract: Curved rod-shaped mesoporous silica can be obtained at low and the highest PVP concentration, while straight rod-shaped mesoporous silica can be obtained at higher PVP concentration. - Highlights: • Mesoporous silica with morphology evolution from CRMS to SRMS were prepared. • Effects of PVP molecular weight and concentration on silica morphology were studied. • A possible mechanism for the formation of morphology evolution SiO{sub 2} was proposed. • Esterification of lauric acid with 1-butanol catalyzed by immobilized PPL.

  7. Structure and functionalization of mesoporous bioceramics for bone tissue regeneration and local drug delivery.

    Science.gov (United States)

    Vallet-Regí, María; Izquierdo-Barba, Isabel; Colilla, Montserrat

    2012-03-28

    This review article describes the importance of structure and functionalization in the performance of mesoporous silica bioceramics for bone tissue regeneration and local drug delivery purposes. Herein, we summarize the pivotal features of mesoporous bioactive glasses, also known as 'templated glasses' (TGs), which present chemical compositions similar to those of conventional bioactive sol-gel glasses and the added value of an ordered mesopore arrangement. An in-depth study concerning the possibility of tailoring the structural and textural characteristics of TGs at the nanometric scale and their influence on bioactive behaviour is discussed. The highly ordered mesoporous arrangement of cavities allows these materials to confine drugs to be subsequently released, acting as drug delivery devices. The functionalization of mesoporous silica walls has been revealed as the cornerstone in the performance of these materials as controlled release systems. The synergy between the improved bioactive behaviour and local sustained drug release capability of mesostructured materials makes them suitable to manufacture three-dimensional macroporous scaffolds for bone tissue engineering. Finally, this review tackles the possibility of covalently grafting different osteoinductive agents to the scaffold surface that act as attracting signals for bone cells to promote the bone regeneration process.

  8. Preparation and photochromism of Keggin-type molybdphosphoric acid/silica mesoporous composite thin films

    Institute of Scientific and Technical Information of China (English)

    ZHANG XueAo; WU WenJian; MAN YaHui; TIAN Tian; TIAN XiaoZhou; WANG JianFang

    2007-01-01

    Using tetraethoxysilane and 3-aminopropyltriethoxysilane as the silica sources, amino-functionalized organic/inorganic hybrid mesoporous silica thin films with 2-dimensional hexagonal structure have been synthesized by evaporation induced self-assembly process in the presence of cetyltrimethyl ammonium bromide templates under acid conditions. The Keggin-type molybdphosphoric acid (PMo) is incorporated into the mesoporous silica thin films with amino-groups by wetness impregnation, and the PMo/silica mesoporous composite thin films are obtained. The results of X-ray diffraction (XRD),high resolution transmission electron microscopy (HRTEM), and Fourier transform infrared (FTIR)spectra indicate the PMo molecules maintain Keggin structure and are homogeneously distributed inside mesopores. The composite thin films possess excellent reversible photochromic properties, and change from colorless to blue under ultraviolet irradiation. The photochromic mechanism of the composite thin films is studied by ultraviolet-visible (UV-vis), electron spin resonance (ESR) and X-ray photoelectron spectroscopy (XPS) spectra. It is shown that intervalence charge transfer (IVCT) and ligand-to-metal charge transfer (LMCT) are the main reasons of photochromism. PMo anions interact strongly with amino-groups of the mesoporous suface via hydrogen bond and electrostatic force. After ultraviolet irradiation, the charge transfer occurs by reduction of heteropolyanions accompanying the formation of heteropolyblues with multivalence Mo(Ⅵ, Ⅴ), and the bleaching process of composite thin films is closely related to the presence of oxygen.

  9. Preparation and photochromism of Keggin-type molybdphosphoric acid/silica mesoporous composite thin films

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Using tetraethoxysilane and 3-aminopropyltriethoxysilane as the silica sources, amino-functionalized organic/inorganic hybrid mesoporous silica thin films with 2-dimensional hexagonal structure have been synthesized by evaporation induced self-assembly process in the presence of cetyltrimethyl ammonium bromide templates under acid conditions. The Keggin-type molybdphosphoric acid (PMo) is incorporated into the mesoporous silica thin films with amino-groups by wetness impregnation, and the PMo/silica mesoporous composite thin films are obtained. The results of X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), and Fourier transform infrared (FTIR) spectra indicate the PMo molecules maintain Keggin structure and are homogeneously distributed inside mesopores. The composite thin films possess excellent reversible photochromic properties, and change from colorless to blue under ultraviolet irradiation. The photochromic mechanism of the composite thin films is studied by ultraviolet-visible (UV-vis), electron spin resonance (ESR) and X-ray photoelectron spectroscopy (XPS) spectra. It is shown that intervalence charge transfer (IVCT) and ligand-to-metal charge transfer (LMCT) are the main reasons of photochromism. PMo anions interact strongly with amino-groups of the mesoporous suface via hydrogen bond and electrostatic force. After ultraviolet irradiation, the charge transfer occurs by reduction of heteropolyanions accompanying the formation of heteropolyblues with multivalence Mo(VI, V), and the bleaching process of composite thin films is closely related to the presence of oxygen.

  10. Hybrid Mesoporous Silicas and Microporous POSS-Based Frameworks Incorporating Evaporation-Induced Self-Assembly

    Directory of Open Access Journals (Sweden)

    Jheng-Guang Li

    2015-06-01

    Full Text Available We fabricated a series of mesoporous silicas and mesoporous organosilicates with hierarchical porosity through evaporation-induced self-assembly using Pluronic F127 as a template in this study. We could tailor the mesophase of each mesoporous silica sample by varying the weight ratio of its two silica sources: tetraethyl orthosilicate (TEOS and triethoxysilane hydrosilylated octavinyl polyhedral oligomeric silsesquioxane (OV-POSS-SILY. The mesophases ranged from an ordered body-centered cubic (bcc structure (TEOS alone to ordered face-centered cubic (fcc structure (10 and 20 wt.% of OV-POSS-SILY and finally to disordered spherical pores (≥30 wt.% of OV-POSS-SILY. We used small-angle X-ray scattering (SAXS and transmission electron microscopy (TEM to study the transformations of these mesophases, while N2 isotherm sorption curves revealed the porosities of these mesoporous silicate samples. Moreover, 29Si CP/MAS solid state nuclear magnetic resonance spectroscopy allowed us to analyze the compositions of the POSS-containing silic