Sample records for sol-gel derived organic-inorganic

  1. Photochromic organic-inorganic composite materials prepared by sol-gel processing : properties and potentials

    Hou, Lisong; Mennig, Martin; Schmidt, Helmut K.


    The sol-gel method which features a low-temperature wet-chemical process opens vast possibilities to incorporating organic dyes into solid matrices for various optical applications. In this paper we present our experimental results on the sol-gel derived photochromic organic-inorganic composite (ORMOCER) materials follwoing an introductory description of the sol-gel process and a brief review on the state of the art of the photochromic solids prepared using this method. Our photochromic spiro...

  2. Wood-Based Nanocomposite Derived by in Situ Formation of Organic-Inorganic Hybrid Polymer within Wood via a Sol-Gel Method.

    Dong, Xiaoying; Zhuo, Xiao; Wei, Jie; Zhang, Gang; Li, Yongfeng


    Solid wood materials and wood-plastic composites as two kinds of lightweight materials are attracting great interest from academia and industry due to their green and recycling nature. However, the relatively lower specific strength limits their wider applications. In particular, solid wood is vulnerable to moisture and decay fungi in nature, resulting in its poor durability for effectively long-term utilization. Inspired from the porous structure of wood, we propose a new design to build a wood-based nanocomposite with higher specific strength and satisfactory durability by in situ generation of organic-inorganic hybrid polymer within wood via a sol-gel method. The derived composite has 50-1200% improvement of impact toughness, 56-192% improvement of tensile strength, and 110-291% improvement of flexural strength over those of typical wood-plastic composites, respectively; and even 34% improvement of specific tensile strength than that of 36A steel; 208% enhancement of hardness; and 156% enhancement of compression strength than those of compared solid wood, respectively; as well as significantly improved dimensional stability and decay resistance over those of untreated natural wood. Such materials could be potentially utilized as lightweight and high-strength materials for applications in construction and automotive industries. This method could be extended to constitute other inorganic nanomaterials for novel organic-inorganic hybrid polymer within wood.

  3. Photochromic organic-inorganic composite materials prepared by sol-gel processing: properties and potentials

    Hou, Lisong; Mennig, Martin; Schmidt, Helmut K.


    The sol-gel method which features a low-temperature wet-chemical process opens vast possibilities to incorporating organic dyes into solid matrices for various optical applications. In this paper we present our experimental results on the sol-gel derived photochromic organic- inorganic composite (Ormocer) materials following an introductory description of the sol-gel process and a brief review on the state of the art of the photochromic solids prepared using this method. Our photochromic spirooxazine-Ormocer gels and coatings possess better photochromic response and color-change speed than the corresponding photochromic polymer coatings and similar photochemical stability to the latter. Further developments are proposed as to tackle the temperature dependence problem and further tap the potentialities of the photochromic dye-Ormocer material for practical applications.

  4. Sol-gel derived sorbents

    Sigman, Michael E.; Dindal, Amy B.


    Described is a method for producing copolymerized sol-gel derived sorbent particles for the production of copolymerized sol-gel derived sorbent material. The method for producing copolymerized sol-gel derived sorbent particles comprises adding a basic solution to an aqueous metal alkoxide mixture for a pH.ltoreq.8 to hydrolyze the metal alkoxides. Then, allowing the mixture to react at room temperature for a precalculated period of time for the mixture to undergo an increased in viscosity to obtain a desired pore size and surface area. The copolymerized mixture is then added to an immiscible, nonpolar solvent that has been heated to a sufficient temperature wherein the copolymerized mixture forms a solid upon the addition. The solid is recovered from the mixture, and is ready for use in an active sampling trap or activated for use in a passive sampling trap.

  5. Organic-inorganic crosslinked and hybrid membranes derived from sulfonated poly(arylene ether sulfone)/silica via sol-gel process

    Feng, Shaoguang; Shang, Yuming; Wang, Yingzi; Xie, Xiaofeng; Mathur, V. K.; Xu, Jingming

    A series of covalently crosslinkable organic-inorganic hybrid membranes have been prepared from sulfonated poly(arylene ether sulfone) (SPAES) with pendant propenyl moiety and various amounts of vinyl substituted silica via sol-gel process which are then thermally crosslinked in the presence of benzoyl peroxide (BPO) initiator. The obtained membranes are characterized in terms of oxidative stability, thermal property, ion exchange capacity (IEC), water uptake, swelling ratio in methanol aqueous solution, proton conductivity, and methanol permeability coefficient. The results indicate that the oxidative stability and thermal stability of the hybrid membranes are improved. Moreover, introduction of silica reduces the water uptake and methanol swelling of membranes. The swelling ratio of membranes in 2 mol L -1 methanol aqueous solution at 80 °C slowly decreases from 26 to 19% with the increase of SiO 2 content from 0 to 12 wt.%. Furthermore, with the increase in silica content, the methanol permeability coefficient of the hybrid membranes decreases at first and then increases. When the silica content reaches 8 wt.%, the methanol permeability coefficient is at the minimum of 6.02 × 10 -7 cm 2 s -1, a 2.64-fold decrease compared with that of the pristine SPAES membrane. Moreover, the proton conductivity is found to be at about 95% of that of pristine polymer at that silica content.

  6. Organic-inorganic crosslinked and hybrid membranes derived from sulfonated poly(arylene ether sulfone)/silica via sol-gel process

    Feng, Shaoguang; Shang, Yuming; Wang, Yingzi; Xie, Xiaofeng; Xu, Jingming [Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing 100084 (China); Mathur, V.K. [Department of Chemical Engineering, University of New Hampshire, NH 03824 (United States)


    A series of covalently crosslinkable organic-inorganic hybrid membranes have been prepared from sulfonated poly(arylene ether sulfone) (SPAES) with pendant propenyl moiety and various amounts of vinyl substituted silica via sol-gel process which are then thermally crosslinked in the presence of benzoyl peroxide (BPO) initiator. The obtained membranes are characterized in terms of oxidative stability, thermal property, ion exchange capacity (IEC), water uptake, swelling ratio in methanol aqueous solution, proton conductivity, and methanol permeability coefficient. The results indicate that the oxidative stability and thermal stability of the hybrid membranes are improved. Moreover, introduction of silica reduces the water uptake and methanol swelling of membranes. The swelling ratio of membranes in 2 mol L{sup -1} methanol aqueous solution at 80 C slowly decreases from 26 to 19% with the increase of SiO{sub 2} content from 0 to 12 wt.%. Furthermore, with the increase in silica content, the methanol permeability coefficient of the hybrid membranes decreases at first and then increases. When the silica content reaches 8 wt.%, the methanol permeability coefficient is at the minimum of 6.02 x 10{sup -7} cm{sup 2} s{sup -1}, a 2.64-fold decrease compared with that of the pristine SPAES membrane. Moreover, the proton conductivity is found to be at about 95% of that of pristine polymer at that silica content. (author)

  7. Sol-gel derived ceramics


    The synthesis of ceramic raw materials has become an important factor in ceramic technologies. The increasing demands to the performance of ceramic compounds has caused increased activities for the preparation of tailor-made raw materials. Amongst a variety of new syntheses like flame pyrolysis, reactive spray drying, plasma or laser assisted techniques, the sol-gel process plays an important and increasing role. The process describes the building up of an inorganic (in general an oxide) netw...

  8. Sol-Gel Derived Hafnia Coatings

    Feldman, Jay D.; Stackpoole, Mairead; Blum, Yigal; Sacks, Michael; Ellerby, Don; Johnson, Sylvia M.; Venkatapathy, Ethiras (Technical Monitor)


    Sol-gel derived hafnia coatings are being developed to provide an oxidation protection layer on ultra-high temperature ceramics for potential use in turbine engines (ultra-efficient engine technology being developed by NASA). Coatings using hafnia sol hafnia filler particles will be discussed along with sol synthesis and characterization.

  9. Sol-gel Process in Preparation of Organic-inorganic Hybrid Materials

    Macan, J


    Full Text Available Organic-inorganic hybrid materials are a sort of nanostructured material in which the organic and inorganic phases are mixed at molecular level. The inorganic phase in hybrid materials is formed by the sol-gel process, which consists of reactions of hydrolysis and condensation of metal (usually silicon alkoxides. Flexibility of sol-gel process enables creation of hybrid materials with varying organic and inorganic phases in different ratios, and consequently fine-tuning of their properties. In order to obtain true hybrid materials, contact between the phases should be at molecular level, so phase separation between thermodynamically incompatible organic and inorganic phases has to be prevented. Phase interaction can be improved by formation of hydrogen or covalent bonds between them during preparation of hybrid materials. Covalent bond can be introduced by organically modified silicon alkoxides containing a reactive organic group (substituent capable of reacting with the organic phase. In order to obtain hybrid materials with desired structures, a detailed knowledge of hydrolysis and condensation mechanism is necessary. The choice of catalyst, whether acid or base, has the most significant influence on the structure of the inorganic phase. Other important parameters are alkoxide concentration, water: alkoxide ratio, type of alkoxide groups, solvent used, temperature, purity of chemicals used, etc. Hydrolysis and condensation of organically modified silicon alkoxides are additionally influenced by nature and size of the organic supstituent.

  10. Novel hybrid organic-inorganic sol-gel materials based on highly efficient heterocyclic push-pull chromophores

    Abbotto, Alessandro; Bozio, Renato; Brusatin, Giovanna; Facchetti, Antonio; Guglielmi, Massimo; Innocenzi, Plinio; Meneghetti, Moreno; Pagani, Giorgio A.; Signorini, Raffaella


    We report the synthesis of sol-gel materials based on highly efficient heterocycle-based push-pull chromophores showing second- and third-order nonlinear optical activity. We show the proper functionalization of the best performing chromophores and their incorporation into a hybrid organic- inorganic sol-gel matrix. Different types of functionalization of the active molecule have been considered, including hydroxyl and alkoxysilyl end-groups. The functionalization strategy responded to different criteria such as stability and synthetic availability of the final molecular precursors, their solubility, and the used synthetic approach to the sol-gel material. The synthesis of the sol-gel materials has been tuned in order to preserve molecular properties and control important factors such as final concentration of the active dye in the matrix. Both acid- and base-catalyzed sol-gel synthesis has been taken into account. 3-Glycidoxypropyltrimethoxysilane and 3- aminopropyltriethoxysilane have been used as the organically modified alkoxides to prepare the hybrid organic-inorganic matrix. Characterization of the spectroscopic properties of the sol-gel materials is presented.


    Hong-xia Xi; Zhong Li; Zhao-xi Liang


    A new organic/inorganic hybrid nonlinear optical (NLO) material was developed by the sol-gel process of an alkoxysilane dye with tetraethoxysilane. A NLO moiety based on 4-nitro-4′-hydroxy azobenzene was covalently bonded to the triethoxysilane derivative, i.e. γ-isocyanatopropyl triethoxysilane. The preparation process and properties of the sol-gel derived NLO polymer were studied and characterized by SEM, FTIR, 1H-NMR, UV-Vis, DSC and second harmonic generation (SHG) measurement. The results indicated that the chemical bonding of the chromophores to the inorganic SiO2 networks induces Iow dipole alignment relaxation and preferable orientational stability. The SHG measurements also showed that the bonded polymer film containing 75 wt% of the akoxysilane dye has a high electro-optic coefficient (r33) of7. 1 pm/V at 1.1 μm wavelength, and exhibit good SHG stability, the r33 values can maintain about 92.7% of its initial value at room temperature for 90 days, and can maintain about 59.3% at 100℃ for 300 min.``

  12. Germania-based, sol-gel hybrid organic-inorganic coatings for capillary microextraction and gas chromatography.

    Fang, Li; Kulkarni, Sameer; Alhooshani, Khalid; Malik, Abdul


    Germania-based, sol-gel hybrid organic-inorganic coatings were developed for capillary microextraction and gas chromatography (GC). Being an isostructural analogue of SiO2, GeO2 is compatible with the silica network. Because of this similarity, germania-based materials possess great potential for being used in the areas of chromatographic separation and sample preparation. These possibilities, however, remain practically unexplored. To our knowledge, this is the first instance that a germania-based hybrid sol-gel material is used as a sorbent in analytical sample preparation or chromatographic separation. Tetramethoxygermane was used as a precursor to create a sol-gel network via hydrolytic polycondensation reactions performed within a fused-silica capillary. The growing sol-gel germania network was simultaneously reacted with an organic ligand that contained sol-gel-active sites in its chemical structure. Three different sol-gel-active ligands were used: (a) hydroxy-terminated poly(dimethylsiloxane), (b) hydroxy-terminated poly(dimethyldiphenylsiloxane), and (c) 3-aminopropyltrimethoxysilane. Sol-gel germania-coated capillaries of desired polarity and extraction selectivity were prepared by using an appropriately selected sol-gel-active ligand in the sol solution. These capillaries were further used to extract trace concentrations of polycyclic aromatic hydrocarbons, aldehydes, ketones, alcohols, phenols, and free fatty acids from aqueous samples. The extracted solutes were further analyzed by GC-FID. The new germania-based coatings showed excellent stability under harsh operation conditions involving extreme pH values, high temperatures, and aggressive solvents. Our preliminary results also indicate that sol-gel hybrid germania coatings have the potential to offer great analytical performance as GC stationary phases.

  13. Sol-gel-derived silicate nano-hybrids for biomedical applications.

    Tsuru, Kanji; Shirosaki, Yuki; Hayakawa, Satoshi; Osaka, Akiyoshi


    Organic-inorganic hybrids of poly(dimethyl siloxane), gelatin, and chitosan with such silanes as tetraethoxysilane and 3-glycidoxytriethoxysilane are derived via the sol-gel routes. Their biomedical applications are discussed from biomimetic deposition of bone-like apatite, cell culture, and in vivo behavior.

  14. Synthesis of an imprinted hybrid organic-inorganic polymeric sol-gel matrix toward the specific binding and isotherm kinetics investigation of creatinine.

    Chang, Yong-Sheun; Ko, Ting-Hsien; Hsu, Ting-Jung; Syu, Mei-Jywan


    Hybrid organic-inorganic polymeric sol-gel materials imprinted with creatinine template molecules were synthesized for the specific binding of creatinine. Creatinine is a metabolite from creatine and is the final product from kidney metabolism. Therefore, creatinine can be an important index to estimate the function of the kidney. It was then chosen as the target molecule in this work. To achieve the specific binding toward creatinine, molecular imprinting was used to create a polymeric matrix for the regarding purpose. Sol-gel was further added to create a rigid network structure for the absorption of creatinine. An inorganic precursor, tetraethoxysilane (TEOS), was mixed with an organic functional monomer, 2-acrylamido-2-methylpropane-sulfonic acid (AMPS), and the creatinine template to form a hybrid organic-inorganic imprinted polymer. The chemical functionality was achieved as well as a confined matrix via the polymerization and the hydrolysis-condensation of the sol-gel. The imprinting effect from the hybrid materials against the corresponding nonimprinted was investigated. BET (Brunauer-Emmett-Teller) analysis was carried out for the imprinted and the nonimprinted materials. The specificity of the hybrid materials was further examined by capping the surface silanol groups with chloro-trimethylsilane (CTMS) and 1,1,1,3,3,3-hexamethyldisilazane (HMDS), respectively. The capping effect was compared and discussed from the binding results. Selectivity of the materials toward creatinine was obtained using mixture solutions in the presence of creatinine and its analogues. Reutilization and storage stability of the hybrid organic-inorganic imprinted material were also studied. Additionally, the affinity distribution of the hybrid imprinted materials derived from the allosteric model was also analyzed from the adsorption isotherm data.

  15. Synthesis and characterization of polymer-silica hybrid latexes and sol-gel-derived films

    Petcu, Cristian; Purcar, Violeta; Ianchiş, Raluca; Spătaru, Cătălin-Ilie; Ghiurea, Marius; Nicolae, Cristian Andi; Stroescu, Hermine; Atanase, Leonard-Ionuţ; Frone, Adriana Nicoleta; Trică, Bogdan; Donescu, Dan


    Sol-gel derived organic-inorganic hybrid systems were obtained by applying alkaline-catalyzed co-hydrolysis and copolycondensation reactions of tetraethoxysilane (TEOS), methyltriethoxysilane (MTES), isobutyltriethoxysilane (IBTES), diethoxydimethylsilane (DMDES), and vinyltriethoxysilane (VTES), respectively, into a polymer latex functionalized with vinyltriethoxysilane (VTES). The properties of the latex hybrid materials were analyzed by FTIR, water contact angle, environmental scanning electron microscopy (ESEM), TEM and AFM analysis, respectively. FT-IR spectra confirmed that the chemical structures of the sol-gel derived organic-inorganic materials are changed as function of inorganic precursor and Sisbnd Osbnd Si networks are formed during the co-hydrolysis and copolycondensation reactions. The water contact angle on the sol-gel latex film containing TEOS + VTES increased to 135° ± 2 compared to 65° ± 5 for the blank latex, due VTES incorporation into latex material. TGA curves of hybrid sample modifies against neat polymer, the thermal stability being influenced by the presence of the inorganic partner. ESEM analysis showed that the latex hybrid films prepared with different inorganic precursors were formed and the Si-based polymers were distributed on the surface of the dried sol-gel hybrid films. TEM and AFM photos revealed that the latex emulsion morphology was modified due to the VTES incorporation into system.

  16. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    Seyyal, Emre; Malik, Abdul


    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C12) and phenethyl (PhE) ligands. Here, the ability of the PF-C12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L(-1) limit of detections (LOD

  17. Effect of chromophore-chromophore electrostatic interactions in the NLO response of functionalized organic-inorganic sol-gel materials

    Reyes-Esqueda, J.; Darracq, B.; García-Macedo, J.; Canva, M.; Blanchard-Desce, M.; Chaput, F.; Lahlil, K.; Boilot, J. P.; Brun, A.; Lévy, Y.


    In the last years, important non-linear optical (NLO) results on sol-gel and polymeric materials have been reported, with values comparable to those found in crystals. These new materials contain push-pull chromophores either incorporated as guest in a high Tg polymeric matrix (doped polymers) or grafted onto the polymeric matrix. These systems present several advantages, however they require significant improvement at the molecular level—by designing optimized chromophores with very large molecular figure of merit, specific to each application targeted. Besides, it was recently stated in polymers that the chromophore-chromophore electrostatic interactions, which are dependent of chromophore concentration, have a strong effect into their NLO properties. This has not been explored at all in sol-gel systems. In this work, the sol-gel route was used to prepare hybrid organic-inorganic thin films with different NLO chromophores grafted into the skeleton matrix. Combining a molecular engineering strategy for getting a larger molecular figure of merit and by controlling the intermolecular dipole-dipole interactions through both: the tuning of the push-pull chromophore concentration and the control of tetraethoxysilane concentration, we have obtained a r33 coefficient around 15 pm/V at 633 nm for the classical DR1 azo-chromophore and a r33 around 50 pm/V at 831 nm for a new optimized chromophore structure.

  18. Shape control synthesis of spheroid and rod-like silver nanostructures in organic-inorganic sol-gel composite

    Saraidarov, T.; Levchenko, V.; Popov, I.; Reisfeld, R.


    The synthesis of a variety of spheroid and rod-like silver nanoparticles in hybrid organic-inorganic sol-gel composite films was examined. The sol-gel matrix used in this work involves urethane terminated silica network which acts as a stabilizing and coupling agent and can complex with silver atoms through its secondary amine functionality and form stable colloid dispersions. The parameters determining the particles size and shape are the starting concentrations of silver ions, the coordination and reduction abilities of the solvent and the reaction kinetics and temperature. In this work the reduction process of silver ion was performed by DMF in sol-gel polyurethane precursor solution at two reaction temperatures: (a) 40 ∘C and (b) reflux at boiling temperature. The effects of concentration and temperature of solution on the morphology and uniformity of silver nanorods were investigated by UV-VIS spectroscopy, SEM and TEM. Spheroid nanoparticles size was as 10-12 nm. Electron diffraction shows that all nanoparticles have a silver face-centered cubic crystal lattice. The silver nanoparticles obtained in composite films exhibit a strong characteristic extinction peak, due to surface plasmon resonance occurring nearly 420-440 nm.

  19. Filmogen organic-inorganic hybrids obtained by sol-gel in the presence of cationic polymer

    Donescu, Dan; Serban, Sever; Uricanu, Violeta; Duits, Michel; Perichaud, Alain; Olteanu, Mihaela; Spiroiu, Manuela; Vasilescu, Marilena


    Self-standing and coated-on-glass films were prepared from polymer-inorganic ormosils, using the cationic polymer poly(methacrylamide propyl quaternarydimethyldodecyl bromide). The inorganic compound was grown in sol-gel reactions based on methyltriethoxysilane (MeTES), with or without addition of t

  20. E-Beam Synthesis of Optical Organic-Inorganic Waveguide Film, prepared by Sol-gel Processing Method

    Kim, Sung Eun; Chon, Jina; Cho, Byung Gun; Noh, Seung Ju; Kwon, Yong Ku [Inha Univ., Incheon (Korea, Republic of)


    Optical organic-inorganic waveguide materials were synthesized by non-hydrolytic sol-gel reaction. To synthesize an alkoxysilane precursor, 3-glycidoxypropyl trimethoxysilane was reacted with azo-type materials at elevated temperature. This precursor was then reacted with 4.4-diphenol to synthesize the organic-inorganic hybrids by sol-gel reaction. The reaction mixture was then heat-treated for thermal condensation and methanol as a byproduct was also eliminated. After product has added 2.2-dimethoxy-2-phenylacetophenone for using UV-curing, the thin film was prepared by spin coating or bulk dropwise methode on the ITO substrate. It was cured by UV-curing methode and their patterned morphology and electro-optical properties were precisely measured. Also, E-beam process was used another cuing methode. This process was more efficient curing method than UV-curing methode. Because E-beam was very short curing time and very strong irradiation power. The detail results will be given in the meeting.

  1. Porphyrinosilica and metalloporphyrinosilica: hybrid organic-inorganic materials prepared by sol-gel processing



    Full Text Available New materials porphyrinosilica and metalloporphyrinosilica template have been obtained by a sol-gel processing where functionalyzed porphyrins and metalloporphyrins "building blocks" were assembled into a three-dimensional silicate network. The optimized conditions for preparation of these materials are revised. The monomer precursors porphyrinopropylsilyl and metalloporphyrinopropylsilyl preparation reactions and subsequent one pot sol-gel processing with tetraethoxysilane are discussed. In the case of metalloporphyrins the nitrogen base coordinates to the central metal and acts as a template in the molecular imprinting technique. UV-visible absorption spectroscopy, thermogravimetric analysis, electron paramagnetic resonance, nuclear magnetic spectra, infrared spectra, luminescence spectra, surface area and electron spectroscopy imaging of the materials are used to characterize the prepared materials. The catalytic activities of these metalloporphyrinosilica- template are compared.

  2. Coatings for mechanical and chemical protection based on organic-inorganic sol-gel nanocomposites

    Schmidt, Helmut K.; Kasemann, Reiner


    The sol-gel process opens the possibility of combining inorganic and organic units on a molecular or nanosized level. The flexible chemical approach of tailoring inorganic structures as well as organic polymeric structures in combination with the new concept of incorporation of nanoscaled metal oxide particles (in general boehmite) opens the possibility of achieving new multifunctional materials like extremely high scratch resistance, antisoiling properties, antifogging properties and corrosi...

  3. Coatings for mechanical and chemical protection based on organic-inorganic sol-gel nanocomposites

    Schmidt, Helmut K.; Kasemann, Reiner


    The sol-gel process opens the possibility of combining inorganic and organic units on a molecular or nanosized level. The flexible chemical approach of tailoring inorganic structures as well as organic polymeric structures in combination with the new concept of incorporation of nanoscaled metal oxide particles (in general boehmite) opens the possibility of achieving new multifunctional materials like extremely high scratch resistance, antisoiling properties, antifogging properties and corrosi...

  4. Improvement of photofatigue resistance of spirooxazine entrapped in organic-inorganic composite synthesized via the sol-gel process

    Hou, Lisong; Mennig, Martin; Schmidt, Helmut K.


    A photochromic dye, spirooxazine (SO), was incorporated in organic-inorganic composite (OIC) materials by the advantages of sol-gel processing. It has been found that the photochromic response is high enough and the fading rate is similar to the dye-in-ethanol solution while the photofatigue resistance is strongly dependent on the matrix composition and the starting compounds. In the present work, we present results on the effect of matrix composition and starting compounds as well as additives on the photofatigue resistance of SO- OIC photochromic coatings. Sol-gel coatings synthesized from methyltrimethoxysilane (MTMS) and glycidyloxypropyltrimethoxysilane (GPTMS) as starting compounds, and using 1H,1H,2H,2H-perfluoroalkyltrimethoxysilane (FAS) and 1-methylimidazole (MI) as additives provide the SO dye with a favorable matrix environment in terms of photofatigue, so that the overall photochromic performance of the dye can be optimized. The photofatigue resistance reaches the same level as, while both the photochromic response and fading rate are much better than the SO-PMMA coatings.

  5. Dialkylenecarbonate-Bridged Polysilsesquioxanes. Hybrid Organic-Inorganic Sol-Gels with a Thermally Labile Bridging Group

    Assink, Roger A.; Baugher, Brigitta M.; Beach, James V.; Loy, Douglas A.; Shea, Kenneth J.; Small, James H.; Tran, Joseph


    In this paper, we introduce a new approach for altering the properties of bridged polysilsesquioxane xerogels using post-processing mobilization of the polymeric network. The bridging organic group contains latent functionalities that can be liberated thermally, photochemically, or by chemical means after the gel has been processed to a xerogel. These modifications can produce changes in density, volubility, porosity, and or chemical properties of the material. Since every monomer possesses two latent functional groups, the technique allows for the introduction of high levels of functionality in hybrid organic-inorganic materials. Dialkylenecarbonate-bridged polysilsesquioxane gels were prepared by the sol-gel polymerization of bis(triethoxysilylpropyl)carbonate (1) and bis(triethoxysilylisobutyl)-carbonate (2). Thermal treatment of the resulting non-porous xerogels and aerogels at 300-350 C resulted in quantitative decarboxylation of the dialkylenecarbonate bridging groups to give new hydroxyalkyl and olefinic substituted polysilsesquioxane monolithic xerogels and aerogels that can not be directly prepared through direct sol-gel polymerization of organotrialkoxysilanes.

  6. Ferrocene Derivative Mediator Bonded Sol-gel Membrane Glucose Biosensor

    XUAN, Guang-Shan; KIM, Moon-Chang; HER, Dae-Sung; LEE, Heung-Lark


    The sol-gel derived glucose biosensor was developed, and the sol-gel membrane was organically modified by N-(3-triethoxysilylpropyl)-ferrocenylmethylamine (FcSi) as sol-gel precursor to make electrochemical biosensor.The structure of biosensor was sol-gel/FcSi+Gox/GC type (glucose oxidase, Gox). The ferrocene mediator was chemically immobilized to the silane network, and Gox was entrapped to the sol-gel glass network. Therefore,these structures prevented mediator leakage and retained the enzyme activity. Additionally, pH of electrolyte, temperature effects, and interference of positive substances with biosensor were investigated. And the electrochemical performance of biosensor was studied by amperometry. The results indicated that the linear range, detection limit,and response slope of biosensor was 2.00× 10-4-1.57× 10-3 mol·L-1, 2.0× 10-4 mol·L-1 and 5.06× 105 nA·mol-1 · L, respectively.

  7. Fabrication of 2×2 Thermo-Optic Switches with Organic-Inorganic Hybrid Materials Prepared by Sol-Gel Technique


    2×2 Mach-Zehnder interferometric thermo-optic switch was fabricated with organic/inorganic hybrid materials by sol-gel technique and direct UV patterning. The switching time of device was measured to be 4.2 ms and switching power 9.3 mW.

  8. Review on Sol-Gel Derived Coatings:Process, Techniques and Optical Applications


    Sol-gel process is one of the simplest techniques to manufacture thin films. The quality of the prepared films depends on the parameters of the sol-gel process and the used technique for deposition. A great variety of the sol-gel derived films have been prepared for different applications. We present a review on the sol-gel derived coatings. The description of the process is introduced in details. Different sol-gel deposition techniques are mentioned. The optical applications of the sol-gel derived coatings are reviewed.

  9. Safe and Environmentally Acceptable Sol-gel Derived Pyrophoric Pyrotechnics

    Simspon, R L; Satcher, J H; Gash, A


    It was demonstrated that highly porous sol-gel derived iron (III) oxide materials could be reduced to sub-micron-sized metallic iron by heating the materials to intermediate temperatures in a hydrogen atmosphere. Through a large number of experiments complete reduction of the sol-gel based materials was realized with a variety of hydrogen-based atmospheres (25-100% H{sub 2} in Ar, N{sub 2}, CO{sub 2}, or CO) at intermediate temperatures (350 C to 700 C). All of the resulting sol-gel-derived metallic iron powders were ignitable by thermal methods, however none were pyrophoric. For comparison several types of commercial micron sized iron oxides Fe2O3, and NANOCAT were also reduced under identical conditions. All resulting materials were characterized by thermal gravimetric analysis (TGA), differential thermal analysis (DTA), powder X-ray diffraction (PXRD), as well as scanning and transmission electron microscopies (SEM and TEM). In addition, the reduction of the iron oxide materials was monitored by TGA. In general the sol-gel materials were more rapidly reduced to metallic iron and the resulting iron powders had smaller particle sizes and were more easily oxidized than the metallic powders derived from the micron sized materials. The lack of pyrophoricity of the smaller fine metallic powders was unexpected and may in part be due to impurities in the materials that create a passivation layer on the iron. Several recommendations for future study directions on this project are detailed.

  10. Protein interactions with nanoporous sol-gel derived bioactive glasses.

    Lin, Sen; Van den Bergh, Wouter; Baker, Simon; Jones, Julian R


    Sol-gel derived bioactive glasses are excellent candidates for bone regenerative implant materials as they bond with bone, stimulate bone growth and degrade in the body. Their interactions with proteins are critical to understanding their performance after implantation. This study focuses on the interactions between fibrinogen and sol-gel glass particles of the 70S30C (70 mol.% SiO(2), 30 mol.% CaO composition). Sol-gel silica and melt-derived Bioglass® were also used for comparison. Fibrinogen penetration into the nanoporous glasses was observed by live tracking the fluorescent-labelled fibrinogen with confocal microscopy. The effect of pore size on protein penetration was investigated. Nanoporous networks with modal pore diameters larger than 6 nm were accessible to fibrinogen. When the modal nanopore diameter was decreased to 2 nm or less, the penetration of fibrinogen was inhibited. The surface properties of the glasses, which can be modulated by media pH, glass composition and final stabilisation temperature in the sol-gel process, have effects on fibrinogen adsorption via long-range Coulombic forces before the adsorption and via short-range interactions such as hydrogen bonding after the adsorption.

  11. Nonhydrolytic sol-gel approach to facile creation of surface-bonded zirconia organic-inorganic hybrid coatings for sample preparation. Ι. Capillary microextraction of catecholamine neurotransmitters.

    Alhendal, Abdullah; Mengis, Stephanie; Matthews, Jacob; Malik, Abdul


    Nonhydrolytic sol-gel (NHSG) route was used for the creation of novel zirconia-polypropylene oxide (ZrO2-PPO) sol-gel hybrid sorbents in the form of surface coatings for the extraction and preconcentration of catecholamine neurotransmitters and molecules structurally related to their deaminated metabolites. In comparison to other sorbents made of inorganic transition metal oxides, the presented hybrid organic-inorganic sorbents facilitated reversible sorption properties that allowed for efficient desorption of the extracted analytes by LC-MS compatible mobile phases. The presented sol-gel hybrid sorbents effectively overcame the major drawbacks of traditional silica- or polymer-based sorbents by providing superior pH stability (pH range: 0-14), and a variety of intermolecular interactions. Nonaqueous sol-gel treatment of PPO with ZrCl4 was employed for the derivatization of the terminal hydroxyl groups on PPO, providing zirconium trichloride-containing end groups characterized by enhanced sol-gel reactivity. NHSG ZrO2-PPO sorbent provided excellent microextraction performance for catecholamines, low detection limits (5.6-9.6pM), high run-to-run reproducibility (RSD 0.6-5.1%), high desorption efficiency (95.0-99.5%) and high enrichment factors (∼1480-2650) for dopamine and epinephrine, respectively, extracted from synthetic urine samples. The presented sol-gel sorbents provided effective alternative to conventional extraction media providing unique physicochemical characteristics and excellent extraction capability.

  12. Development of durable self-cleaning coatings using organic-inorganic hybrid sol-gel method

    Kumar, Divya; Wu, Xinghua; Fu, Qitao; Ho, Jeffrey Weng Chye; Kanhere, Pushkar D.; Li, Lin; Chen, Zhong


    Self-cleaning coatings with excellent water-repellence and good mechanical properties are in high demand. However, producing such coatings with resistance to mechanical abrasion and environmental weathering remains a key challenge. Mechanically robust coatings based on tetraethylorthosilicate (TEOS) and glycidoxypropyltriethoxysilane (Glymo) have been prepared using a sol-gel method. Emphasis is given to the addition of Glymo, an epoxy silane which creates an organic matrix that blends with the inorganic Sisbnd Osbnd Si matrix formed from the TEOS. The combination of the blended matrix produced coatings with good adhesion to substrates and improved mechanical properties. Fluoroalkylsilane (FAS) and silica fillers were introduced to increase the hydrophobicity of the coating. It was found that the water contact angle (CA) of these coatings increases from 115° to 164° upon decreasing filler size from 1-5 μm to 10-20 nm. The sliding angle (SA) for coatings with 15 wt.% loading of 10-20 nm silica is around 2°. UV weathering does not show significant effect on the properties of the coatings. Mechanical properties and performances including hardness, Young's modulus, coating adhesion and abrasion resistance were systematically analyzed. In the current work, a simple self-cleaning test, which measures the extent of dirt accumulation and subsequent removal by water spray, was performed. The coatings with 15 wt.% loading of 10-20 nm silica particles show the best self-cleaning performance both before and after mechanical abrasion. The developed coating process is simple and can be easily scaled-up for large surfaces that require self-cleaning function.

  13. Fullerenol-containing Materials Derived by Sol-gel Processing

    Haiping XIA; Zhaoyang JIANG; Jianli ZHANG; Jinhao WANG; Yuepin ZHANG; Qiuhua NIE


    Water soluble fullerenols were synthesized and incorporated in SiO2, SiO2-TiO2, GPTMS-SiO2, GPTMS-ATPS inorganic and organic-inorganic materials by sol-gel processes. The maximum concentrations of C60(OH)n and C7o(OH)n in the obtained SiO2 gels were estimated to be about 0.6% and 1.5% in weight, respectively. The characteristics of the UV/visible spectra of fullerenols in H2O and various gels were measured and compared. The thermal stability of fullerenols in gels was investigated with differential thermal analysis (DTA). The results indicate that the absorption features of fullerenols in solid gels are similar to those in H2O and the fullerenols in SiO2 are stable at 400℃. The optical limiting effect of the fullerenols was investigated preliminarily.

  14. Preparation and characteristics of high pH-resistant sol-gel alumina-based hybrid organic-inorganic coating for solid-phase microextraction of polar compounds.

    Liu, Mingming; Liu, Ying; Zeng, Zhaorui; Peng, Tianyou


    A novel alumina-based hybrid organic-inorganic sol-gel coating was first developed for solid-phase microextraction (SPME) from a highly reactive alkoxide precursor, aluminum sec-butoxide, and a sol-gel-active organic polymer hydroxyl-terminated polydimethylsiloxane (OH-TSO). The underlying mechanism was discussed and confirmed by IR spectra. The porous surface structure of the sol-gel coating was revealed by scanning electron microscopy. A detailed investigation was conducted to evaluate the remarked performance of the newly developed sol-gel alumina-OH-TSO hybrid materials. In stark contrast to the sol-gel silica-based coating, the alumina-based coating demonstrated excellent pH stability. In addition, good thermal resistance and coating preparation reproducibility are also its outstanding performance. As compared to silica-based hybrids material, the ligand exchange ability of alumina makes it structurally superior extraction sorbents for polar compounds, such as fatty acids, phenols, alcohols, aldehydes and amines. Practical applicability of the prepared alumina-OH-TSO fiber was demonstrated through the analysis of volatile alcohols and fatty acids in beer. The recoveries obtained ranged from 85.7 to 104% and the relative standard deviation values for all analytes were below 9%.

  15. Sol-gel hosts doped with porphyrin derivatives. Part I. Spectroscopy, hole-burning and spectral diffusion

    Kulikov, S. G.; Veret-Lemarinier, A. V.; Galaup, J. P.; Chaput, F.; Boilot, J. P.


    Pure inorganic sol-gel matrices as well as hybrid organic/inorganic xerogels have been doped with porphyrins derivatives and studied using line narrowing techniques. The role of residual hydroxyl groups is investigated. Free-base porphyrins are protonated in pure inorganic hosts, but the matrix acidity is reduced in hybrid matrices or when fluorinated porphyrins derivatives are used. The linear electron-phonon coupling can be controlled with the choice of the organic group in organic/inorganic matrices. Persistent spectral hole widths increase with temperature according a glass-like Tn dependence and evidence of spectral diffusion is shown in one of these systems.

  16. Preparation of organic/inorganic composite membranes using two types of polymer matrix via a sol-gel process

    Park, Seung-Hee [School of Chemical Engineering, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea); Polymer Electrolyte Fuel Cell Research Center, Hydrogen and Fuel Cell Department, Korea Institute of Energy Research (KIER), 71-2 Jang-dong, Yuseong-gu, Daejeon 305-343 (Korea); Park, Jin-Soo; Yim, Sung-Dae; Park, Seok-Hee; Kim, Chang-Soo [Polymer Electrolyte Fuel Cell Research Center, Hydrogen and Fuel Cell Department, Korea Institute of Energy Research (KIER), 71-2 Jang-dong, Yuseong-gu, Daejeon 305-343 (Korea); Lee, Young-Moo [School of Chemical Engineering, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea)


    Organic/inorganic composite membranes were prepared using two different polymers. BPO{sub 4} particles were introduced into polymers via an in situ sol-gel process. Pre-/post-sulfonated polymers were used to prepare composite membranes as matrix. Pre-sulfonated poly(aryl ether ketone) (SPAEK-6F) copolymer was synthesized via nucleophilic aromatic substitution. Degree of sulfonation was adjusted by the percentage of sulfonated monomer. Post-sulfonated poly(ether ether ketone) (SPEEK) was prepared using concentrated sulfuric acid as sulfonation agent. The membranes were characterized in terms of the ion-exchange capacity (IEC), proton conductivity, water uptake, AFM, SEM and their thermal properties. The SPAEK-6F plain membranes showed higher proton conductivity than that of the SPEEK plain membranes at similar water uptake or IEC due to their structural difference. SEM images of the composite membranes showed that the BPO{sub 4} particles were homogenously dispersed in the polymer matrices and BPO{sub 4} particle size was greatly influenced by polymer matrix. The SPAEK-6F/BPO{sub 4} composite membranes had much smaller BPO{sub 4} particle size than the SPEEK/BPO{sub 4} composite membranes due to well dispersion of BPO{sub 4} sol-like particulates in SPAEK-6F polymer solutions forming more hydrophobic/hydrophilic nanophase than SPEEK polymer solutions. The latter containing a few micrometer-scale BPO{sub 4} particles showed higher proton conductivity than the former containing hundreds nanometer-scale BPO{sub 4} particles at similar water uptake due to the increase in freezable water and effect of particle size. (author)

  17. Preparation of organic/inorganic composite membranes using two types of polymer matrix via a sol-gel process

    Park, Seung-Hee; Park, Jin-Soo; Yim, Sung-Dae; Park, Seok-Hee; Lee, Young-Moo; Kim, Chang-Soo

    Organic/inorganic composite membranes were prepared using two different polymers. BPO 4 particles were introduced into polymers via an in situ sol-gel process. Pre-/post-sulfonated polymers were used to prepare composite membranes as matrix. Pre-sulfonated poly(aryl ether ketone) (SPAEK-6F) copolymer was synthesized via nucleophilic aromatic substitution. Degree of sulfonation was adjusted by the percentage of sulfonated monomer. Post-sulfonated poly(ether ether ketone) (SPEEK) was prepared using concentrated sulfuric acid as sulfonation agent. The membranes were characterized in terms of the ion-exchange capacity (IEC), proton conductivity, water uptake, AFM, SEM and their thermal properties. The SPAEK-6F plain membranes showed higher proton conductivity than that of the SPEEK plain membranes at similar water uptake or IEC due to their structural difference. SEM images of the composite membranes showed that the BPO 4 particles were homogenously dispersed in the polymer matrices and BPO 4 particle size was greatly influenced by polymer matrix. The SPAEK-6F/BPO 4 composite membranes had much smaller BPO 4 particle size than the SPEEK/BPO 4 composite membranes due to well dispersion of BPO 4 sol-like particulates in SPAEK-6F polymer solutions forming more hydrophobic/hydrophilic nanophase than SPEEK polymer solutions. The latter containing a few micrometer-scale BPO 4 particles showed higher proton conductivity than the former containing hundreds nanometer-scale BPO 4 particles at similar water uptake due to the increase in freezable water and effect of particle size.

  18. Organic-inorganic hybrid materials obtained by the sol-gel method with potential use as sunscreens; Materiais hibridos organico-inorganicos (ormosil) obtidos por sol-gel com potencial uso como filtro solar

    Machado, Jane K. de F.B.; Marcal, Alex L.; Lima, Omar J. de; Ciuffi, Katia J.; Nassar, Eduardo J.; Calefi, Paulo S. [Universidade de Franca, SP (Brazil)


    This work aimed at the synthesis and characterization of particles of modified silica containing the organic filter dibenzoylmethane (DBM) by the hydrolytic sol-gel method, with modifications to the Stoeber route. The structures of the resulting Xerogels were characterized by diffuse reflectance UV-VIS spectroscopy in the solid state, infrared absorption spectroscopy, Scanning Electron Microscopy (SEM) and {sup 29}Si Nuclear Magnetic Resonance ({sup 29}Si NRM). The results showed favorable formation of hybrid organic-inorganic nanoparticles with efficient absorption/reflectance of radiation in the UV / VIS range, which enables their potential use as sunscreen. (author)

  19. Structural, vibrational, and gasochromic properties of porous WO sub 3 films templated with a sol-gel organic-inorganic hybrid

    Opara-Krasovec, U; Orel, B; Grdadolnik, J; Drazic, G


    The structure and the gasochromic properties of sol-gel-derived WO sub 3 films with a monoclinic structure (m-WO sub 3) were studied by focusing attention on the size of the monoclinic grains. The size of the m-WO sub 3 grains is modified by the addition of an organic-inorganic hybrid to the initial peroxopolytungstic acid (W-PTA) sols which are based on chemically bonded poly-(propylene glycol) to triethoxysilane end-capping groups (ICS-PPG). The results obtained with scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that the heat treatment (500 sup o C) of WO sub 3 /ICS- IPG (0.5, 1, 2, 5, and 10 mol%) composite films results in a change of their morphology, and nanodimensional pores are formed between the grains. High-resolution TEM (HRTEM) analysis revealed the presence of an amorphous phase on the outside of the m-WO sub 3 grains, whereas energy-dispersive x-ray spectra (EDXS) showed that this amorphous phase contained W and Si. Impregnation of the WO sub 3 /ICS-PPG film ...

  20. Sol-gel derived ceramic electrolyte films on porous substrates

    Kueper, Timothy Walter [Univ. of California, Berkeley, CA (United States)


    A process for the deposition of sol-gel derived thin films on porous substrates has been developed; such films should be useful for solid oxide fuel cells and related applications. Yttria-stabilized zirconia films have been formed from metal alkoxide starting solutions. Dense films have been deposited on metal substrates and ceramic substrates, both dense and porous, through dip-coating and spin-coating techniques, followed by a heat treatment in air. X-ray diffraction has been used to determine the crystalline phases formed and the extent of reactions with various substrates which may be encountered in gas/gas devices. Surface coatings have been successfully applied to porous substrates through the control of substrate pore size and deposition parameters. Wetting of the substrate pores by the coating solution is discussed, and conditions are defined for which films can be deposited over the pores without filling the interiors of the pores. Shrinkage cracking was encountered in films thicker than a critical value, which depended on the sol-gel process parameters and on the substrate characteristics. Local discontinuities were also observed in films which were thinner than a critical value which depended on the substrate pore size. A theoretical discussion of cracking mechanisms is presented for both types of cracking, and the conditions necessary for successful thin formation are defined. The applicability of these film gas/gas devices is discussed.

  1. Sol-gel derived ceramic electrolyte films on porous substrates

    Kueper, T.W.


    A process for the deposition of sol-gel derived thin films on porous substrates has been developed; such films should be useful for solid oxide fuel cells and related applications. Yttria-stabilized zirconia films have been formed from metal alkoxide starting solutions. Dense films have been deposited on metal substrates and ceramic substrates, both dense and porous, through dip-coating and spin-coating techniques, followed by a heat treatment in air. X-ray diffraction has been used to determine the crystalline phases formed and the extent of reactions with various substrates which may be encountered in gas/gas devices. Surface coatings have been successfully applied to porous substrates through the control of substrate pore size and deposition parameters. Wetting of the substrate pores by the coating solution is discussed, and conditions are defined for which films can be deposited over the pores without filling the interiors of the pores. Shrinkage cracking was encountered in films thicker than a critical value, which depended on the sol-gel process parameters and on the substrate characteristics. Local discontinuities were also observed in films which were thinner than a critical value which depended on the substrate pore size. A theoretical discussion of cracking mechanisms is presented for both types of cracking, and the conditions necessary for successful thin formation are defined. The applicability of these film gas/gas devices is discussed.

  2. Sol-gel approach to in situ creation of high pH-resistant surface-bonded organic-inorganic hybrid zirconia coating for capillary microextraction (in-tube SPME).

    Alhooshani, Khalid; Kim, Tae-Young; Kabir, Abuzar; Malik, Abdul


    A novel zirconia-based hybrid organic-inorganic sol-gel coating was developed for capillary microextraction (CME) (in-tube SPME). High degree of chemical inertness inherent in zirconia makes it very difficult to covalently bind a suitable organic ligand to its surface. In the present work, this problem was addressed from a sol-gel chemistry point of view. Principles of sol-gel chemistry were employed to chemically bind a hydroxy-terminated silicone polymer (polydimethyldiphenylsiloxane, PDMDPS) to a sol-gel zirconia network in the course of its evolution from a highly reactive alkoxide precursor undergoing controlled hydrolytic polycondensation reactions. A fused silica capillary was filled with a properly designed sol solution to allow for the sol-gel reactions to take place within the capillary for a predetermined period of time (typically 15-30 min). In the course of this process, a layer of the evolving hybrid organic-inorganic sol-gel polymer got chemically anchored to the silanol groups on the capillary inner walls via condensation reaction. At the end of this in-capillary residence time, the unbonded part of the sol solution was expelled from the capillary under helium pressure, leaving behind a chemically bonded sol-gel zirconia-PDMDPS coating on the inner walls. Polycyclic aromatic hydrocarbons, ketones, and aldehydes were efficiently extracted and preconcentrated from dilute aqueous samples using sol-gel zirconia-PDMDPS coated capillaries followed by thermal desorption and GC analysis of the extracted solutes. The newly developed sol-gel hybrid zirconia coatings demonstrated excellent pH stability, and retained the extraction characteristics intact even after continuous rinsing with a 0.1 M NaOH solution for 24 h. To our knowledge, this is the first report on the use of a sol-gel zirconia-based hybrid organic-inorganic coating as an extraction medium in solid phase microextraction (SPME).

  3. A New Method to Study the Sol-gel Transition Process of Organic/Inorganic Hybrid Materials

    GUO Bin; GAO Jian-gang; CHEN Da-zhu; LIU Jian-ping; HE Ping-sheng; ZHANG Qi-jin


    The sol-gel transition process of PMMA/SiO2 hybrid materials was first studied by means of the dynamic torsional vibration method. The different stages of the transition can be described by the change of torque. The temperature-dependent measurement of the gel time(tg) gives the possibility to determine the apparent activation energy(Ea) of this transition according to Flory′s gelation theory. The non-equilibrium thermodynamic fluctuation theory was used to predict the transition behavior. The isothermal transition experiments on hybrid sols with different TEOS(tetraethyl orthosilicate) contents were carried out. The results show that the Ea of a hybrid sol is higher than that of a non- hybrid sol of a TEOS-water-ethanol system. The increasing of TEOS content in a hybrid sol has no obvious effect on the Ea value, but it can enhance the sol-gel reaction rate.

  4. Preparation, characterization, and biological properties of organic-inorganic nanocomposite coatings on titanium substrates prepared by sol-gel.

    Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando


    When surface-reactive (bioactive) coatings are applied to medical implants by means of the sol-gel dip-coating technique, the biological proprieties of the surface of the implant can be locally modified to match the properties of the surrounding tissues to provide a firm fixation of the implant. The aim of this study has been to synthesize, via sol-gel, organoinorganic nanoporous materials and to dip-coat a substrate to use in dental applications. Different systems have been prepared consisting of an inorganic zirconium-based matrix, in which a biodegradable polymer, the poly-ε-caprolactone was incorporated in different percentages. The materials synthesized by the sol-gel process, before gelation, when they were still in sol phase, have been used to coat a titanium grade 4 (Ti-4) substrate to change its surface biological properties. Thin films have been obtained by means of the dip-coating technique. A microstructural analysis of the obtained coatings was performed using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy. The biological proprieties have been investigated by means of tests in vitro. The bone-bonding capability of the nanocomposite films has been evaluated by examining the appearance of apatite on their surface when plunged in a simulated body fluid (SBF) with ion concentrations nearly equal to those of human blood plasma. The examination of apatite formation on the nanocomposites, after immersion in SBF, has been carried out by SEM equipped with energy-dispersive X-ray spectroscopy. To evaluate cells-materials interaction, human osteosarcoma cell line (Saos-2) has been seeded on specimens and cell vitality evaluated by WST-8 assay.

  5. Sol-gel derived contamination resistant antireflective coatings

    Shen, Jun; Liu, Yuan; Wu, Guangming; Zhou, Bin; Zhang, Zhihua; Zhu, Yumei


    Silica-based sol-gel antireflective (AR) optical coatings are critical components for high peak power laser systems. It is well known that water vapor and volatile organic compounds in both the laser bay and target bay environments will reduce the antireflective efficiency and laser-damage resistance of the sol-gel AR coating. In this study, alkylation with organosilanes in the vapor state was investigated. Sol-gel AR coatings were vapor-phase treated with hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) at room temperature, and the resulting post-treated sol-gel AR coatings were tested for their resistance to contamination by a series of volatile organic compounds. Contact angle measurements were taken to discern the degree of silanization. After the vapor treatment of sol-gel AR coatings with organosilanes, the spectral performance of the coatings were analyzed by spectrophotometer, both before and after the exposure to volatile organic compounds. It is found that the coatings treated with ammonia and HMDS show a better contamination resistant capability. After being contaminated 70 hours with hexane, the transmittance of the coatings presents no obvious decrease. And the vapor treatment produces an increase in their damage threshold at 1064 nm (10ns pulse width) as compared to untreated control samples.

  6. Iron Oxide Silica Derived from Sol-Gel Synthesis

    João Carlos Diniz da Costa


    Full Text Available In this work we investigate the effect of iron oxide embedded in silica matrices as a function of Fe/Si molar ratio and sol pH. To achieve homogeneous dispersion of iron oxide particles, iron nitrate nonahydrate was dissolved in hydrogen peroxide and was mixed with tetraethyl orthosilicate and ethanol in a sol-gel synthesis method. Increasing the calcination temperature led to a reduction in surface area, although the average pore radius remained almost constant at about 10 Å, independent of the Fe/Si molar ratio or sol pH. Hence, the densification of the matrix was accompanied by similar reduction in pore volume. However, calcination at 700 °C resulted in samples with similar surface area though the iron oxide content increased from 5% to 50% Fe/Si molar ratio. As metal oxide particles have lower surface area than polymeric silica structures, these results strongly suggest that the iron oxides opposed the silica structure collapse. The effect of sol pH was found to be less significant than the Fe/Si molar ratio in the formation of molecular sieve structures derived from iron oxide silica.

  7. Poly(ε-caprolactone) reinforced with sol-gel synthesized organic-inorganic hybrid fillers as composite substrates for tissue engineering.

    Russo, Teresa; Gloria, Antonio; D-Antò, Vincenzo; D'Amora, Ugo; Ametrano, Gianluca; Bollino, Flavia; De Santis, Roberto; Ausanio, Giovanni; Catauro, Michelina; Rengo, Sandro; Ambrosio, Luigi


    The importance of polymer-based composite materials to make multifunctional substrates for tissue engineering and the strategies to improve their performances have been stressed in the literature. Bioactive features of sol-gel synthesized poly(ε-caprolactone)/TiO₂ or poly(ε-caprolactone)/ZrO₂ organic-inorganic hybrid materials are widely documented. Accordingly, the aim of this preliminary research was to develop advanced composite substrates consisting of a poly(ε-caprolactone) matrix reinforced with sol-gel synthesized PCL/TiO₂ or PCL/ZrO₂ hybrid fillers. Micro-computed tomography and atomic force microscopy analyses allowed to study surface topography and roughness. On the other hand, mechanical and biological performances were evaluated by small punch tests and Alamar Blue™ assay, respectively. Micro-computed tomography and atomic force microscopy analyses highlighted the effect of the preparation technique. Results from small punch tests and Alamar Blue™ assay evidenced that PCL reinforced with Ti2 (PCL=12, TiO₂=88 wt%) and Zr2 (PCL=12, ZrO₂=88 wt%) hybrid fillers provided better mechanical and biological performances. PCL reinforced with Ti2 (PCL=12, TiO₂=88 wt%) and Zr2 (PCL=12, ZrO₂=88 wt%) hybrid fillers could be considered as advanced composite substrates for hard tissue engineering.

  8. Synthesis of organic-inorganic hybrid sols with nano silica particles and organoalkoxysilanes for transparent and high-thermal-resistance coating films using sol-gel reaction.

    Na, Moonkyong; Park, Hoyyul; Ahn, Myeongsang; Lee, Hyeonhwa; Chung, Ildoo


    Organic-inorganic hybrid sols were synthesized from nano silica particles dispersed in water and from organoalkoxysilanes, using the sol-gel reaction. This work focuses on the effects of the three multifunctional organoalkoxysilanes dimethyldimethoxysilane (DMDMS), methyltrimethoxysilane (MTMS), and tetramethoxysilane (TMOS) to form a transparent and high-thermal-resistance coating film. The stability of the hybrid sol was evaluated as a function of the reaction time for 10 d through the variation of the viscosity. The viscosity of the silica/DMDMS and silica/MTMS sol was slightly increased for 10 d. The multifunctional organoalkoxysilanes formed dense silica networks through hydrolysis and condensation reaction, which enhanced the thermal resistance of the coating films. No thermal degradation of the silica/DMDMS sample occurred up to 600 degrees C, and none of the silica/MTMS and silica/TMOS samples occurred either up to 700 degrees C. The organic-inorganic hybrid sols were coated on the glass substrate using a spin-coating procedure. The organic-inorganic hybrid sols formed flat coating films without cracks. The transmittance of the hybrid sol coating films using MTMS and DMDMS was shown to be over 90%. The transmittance of the silica/TMOS sol coating film reacted for 10 d abruptly decreased due to faster gelation. The silica/DMDMS and silica/MTMS hybrid sols formed smooth coating films while the surface roughness of the silica/TMOS coating film markedly increased when the hybrid sol reacted for 10 d. The increase of the surface roughness of the silica/TMOS coating film can be attributed to the degradation of the stability of the hybrid sol and to the loss of transmittance of the coating film. It was confirmed in this study that the use of organic-inorganic hybrid sol can yield transparent and high-thermal-resistance coating films.

  9. High abrasion resistance coating materials from organic/inorganic hybrid materials produced by the sol-gel method


    A series of new high abrasion resistance coating materials have been prepared utilizing organic/inorganic hybrid materials formed by cohydrolyzing a metal alkoxide sol (e.g. silicon, aluminum, titanium, or zirconium metal alkoxide sol) with one or more bis(trialkoxysilane-containing) organic components or related functionalized species. These hybrid materials show optical clarity and improve the abrasion resistance of polymer substrates when applied as coatings and cured on such substrates.

  10. Application of polyaniline/sol-gel derived tetraethylorthosilicate films to an amperometric lactate biosensor.

    Chaubey, Asha; Pande, K K; Malhotra, B D


    The electrochemical entrapment of polyaniline (PANI) onto sol-gel derived tetraethylorthosilicate (TEOS) films deposited onto indium-tin-oxide (ITO) coated glass has been utilized for immobilization of lactate dehydrogenase (LDH). The performance of these sol-gel/PANI/LDH electrodes has been investigated as a function of the lactate concentration, applied potential, pH of the medium and interferents. The amperometric response of the electrodes under optimum conditions exhibited a linear relationship from 1 mM to 4 mM. An attempt has been made to extend the linearity up to 10 mM for lactate by coating an external layer of polyvinyl chloride (PVC) over the sol-gel/PANI/LDH electrodes with a correlation coefficient of 0.89. These sol-gel/PANI/LDH electrodes have a response time of about 60 s, a shelf life of about 8 weeks at 0-4 degrees C and have implications in a lactate biosensor.

  11. Bioactive behaviour of sol-gel derived antibacterial bioactive glass

    Bellantone, M.; Hench, L.L. [Imperial Coll. of Science, Technology and Medicine, London (United Kingdom). Dept. of Materials


    A new four-component bioactive glass containing Ag{sub 2}O was produced via the sol-gel process. This system releases Ag{sup +} which is a powerful antibacterial agent. The work reported herein is a comparative study of the bioactivity levels of conventional bioactive glass and of the new antibacterial glass. On the basis of XRD patterns, FTIR spectra, and ICP data, the bioactive behaviour of the two biomaterials is nearly equivalent. (orig.)

  12. Nanostructured energetic materials derived from sol-gel chemistry

    Simpson, R L; Tillotson, T M; Hrubesh, L W; Gash, A E


    Initiation and detonation properties are dramatically affected by an energetic material's microstructural properties. Sol-gel chemistry allows intimacy of mixing to be controlled and dramatically improved over existing methodologies. One material goal is to create very high power energetic materials which also have high energy densities. Using sol-gel chemistry we have made a nanostructured composite energetic material. Here a solid skeleton of fuel, based on resorcinol-formaldehyde, has nanocrystalline ammonium perchlorate, the oxidizer, trapped within its pores. At optimum stoichiometry it has approximately the energy density of HMX. Transmission electron microscopy indicated no ammonium perchlorate crystallites larger than 20 nm while near-edge soft x-ray absorption microscopy showed that nitrogen was uniformly distributed, at least on the scale of less than 80 nm. Small-angle neutron scattering studies were conducted on the material. Those results were consistent with historical ones for this class of nanostructured materials. The average skeletal primary particle size was on the order of 2.7 nm, while the nanocomposite showed the growth of small 1 nm size crystals of ammonium perchlorate with some clustering to form particles greater than 10 nm.

  13. Novel Synthesis of Sol-gel Derived Nanosized Mullite Powder

    LIANG Long; LI Jian-bao; LIN Hong; GUO Gang-feng; HE Ming-sheng


    Using hydrous aluminum chloride (AlCl3 6H2O) and silicon ethoxide (Si (OC2H5)4) as raw materials, a kind of nano-sized mullite powder was synthesized with the sol-gel process at the medium calcination temperature. The microstructures of the alumina-silica binary aerogel and calcined nano-sized materials were investigated by means of thermogravimetry-differential thermal analysis (TG-DTA), scanning electron microscopy (SEM) and X-ray diffractometer (XRD). The results show that the mullitization of Al2O3-SiO2 in gel starts from about 1 000 ℃ and its formation of mullite takes place in the range of 1 100 ℃-1 250 ℃. The size of the nano-sized mullite powder calcined at 1 250 ℃ is measured to be about 30 nm.

  14. Sol-gel derived coatings for the conservation of steel

    Erika Kiele


    Full Text Available In this paper, sol-gel processing route has been applied and investigated for the conservation of steel. Nanosilica coatings on steel surface have been prepared using tetraethylorthosilicate (TEOS as a starting material. The methyl-modified silica sols were obtained by mixing of 3 mas.% SiO2 sol solution with hexamethyldisilozane (HMDS. The surface of steel was coated by dip-coating technique. In order to compare the characteristics of coatings, the steel substrates were also coated with commercial polymers Paraloid B67, Cosmolloid H80 and Antik Patina. The surface morphology changes of the uncoated and coated specimens before and after photochemical ageing were investigated by scanning electron microscopy and atomic force microscopy. The structure of the prepared coatings was also investigated by FTIR spectroscopy. The hydrophobicity of surfaces was evaluated by contact angle measurements. Potentiodynamic measurements were obtained in order to compare corrosion parameters of the coatings.

  15. Formation and prevention of fractures in sol-gel-derived thin films.

    Kappert, Emiel J; Pavlenko, Denys; Malzbender, Jürgen; Nijmeijer, Arian; Benes, Nieck E; Tsai, Peichun Amy


    Sol-gel-derived thin films play an important role as the functional coatings for various applications that require crack-free films to fully function. However, the fast drying process of a standard sol-gel coating often induces mechanical stresses, which may fracture the thin films. An experimental study on the crack formation in sol-gel-derived silica and organosilica ultrathin (submicron) films is presented. The relationships among the crack density, inter-crack spacing, and film thickness were investigated by combining direct micrograph analysis with spectroscopic ellipsometry. It is found that silica thin films are more prone to fracturing than organosilica films and have a critical film thickness of 300 nm, above which the film fractures. In contrast, the organosilica films can be formed without cracks in the experimentally explored regime of film thickness up to at least 1250 nm. These results confirm that ultrathin organosilica coatings are a robust silica substitute for a wide range of applications.

  16. Triethylphosphite as a network forming agent enhances in-vitro biocompatibility and corrosion protection of hybrid organic-inorganic sol-gel coatings for Ti6Al4V alloys

    El Hadad, AAG; Barranco, V.; Jiménez-Morales, A; Hickman, G; Galván, J.; Perry, CC


    In Press, Accepted Manuscript The biocompatibility and life of metallic implants can be enhanced through improving the biocompatibility and corrosion protection characteristics of the coatings used with these materials. In this study, triethylphosphite (TEP) was used to introduce phosphorus into organic-inorganic hybrid silica based sol-gel coatings prepared using gamma-methacryloxypropyltrimethoxysilane and tetramethylorthosilicate. Addition of TEP dramatically increased the rate of inter...

  17. Sol-gel derived electrode materials for supercapacitor applications

    Lin, Chuan


    Electrochemical capacitors have been receiving increasing interest in recent years for use in energy storage systems because of their high energy and power density and long cycle lifes. Possible applications of electrochemical capacitors include high power pulsed lasers, hybrid power system for electric vehicles, etc. In this dissertation, the preparation of electrode materials for use as electrochemical capacitors has been studied using the sol-gel process. The high surface area electrode materials explored in this work include a synthetic carbon xerogel for use in a double-layer capacitor, a cobalt oxide xerogel for use in a pseudocapacitor, and a carbon-ruthenium xerogel composite, which utilizes both double-layer and faradaic capacitances. The preparation conditions of these materials were investigated in detail to maximize the surface area and optimize the pore size so that more energy could be stored while minimizing mass transfer limitations. The microstructures of the materials were also correlated with their performance as electrochemical capacitors to improve their energy and power densities. Finally, an idealistic mathematical model, including both double-layer and faradaic processes, was developed and solved numerically. This model can be used to perform the parametric studies of an electrochemical capacitor so as to gain a better understanding of how the capacitor works and also how to improve cell operations and electrode materials design.

  18. Effect of calcium source on structure and properties of sol-gel derived bioactive glasses.

    Yu, Bobo; Turdean-Ionescu, Claudia A; Martin, Richard A; Newport, Robert J; Hanna, John V; Smith, Mark E; Jones, Julian R


    The aim was to determine the most effective calcium precursor for synthesis of sol-gel hybrids and for improving homogeneity of sol-gel bioactive glasses. Sol-gel derived bioactive calcium silicate glasses are one of the most promising materials for bone regeneration. Inorganic/organic hybrid materials, which are synthesized by incorporating a polymer into the sol-gel process, have also recently been produced to improve toughness. Calcium nitrate is conventionally used as the calcium source, but it has several disadvantages. Calcium nitrate causes inhomogeneity by forming calcium-rich regions, and it requires high temperature treatment (>400 °C) for calcium to be incorporated into the silicate network. Nitrates are also toxic and need to be burnt off. Calcium nitrate therefore cannot be used in the synthesis of hybrids as the highest temperature used in the process is typically 40-60 °C. Therefore, a different precursor is needed that can incorporate calcium into the silica network and enhance the homogeneity of the glasses at low (room) temperature. In this work, calcium methoxyethoxide (CME) was used to synthesize sol-gel bioactive glasses with a range of final processing temperatures from 60 to 800 °C. Comparison is made between the use of CME and calcium chloride and calcium nitrate. Using advanced probe techniques, the temperature at which Ca is incorporated into the network was identified for 70S30C (70 mol % SiO(2), 30 mol % CaO) for each of the calcium precursors. When CaCl(2) was used, the Ca did not seem to enter the network at any of the temperatures used. In contrast, Ca from CME entered the silica network at room temperature, as confirmed by X-ray diffraction, (29)Si magic angle spinning nuclear magnetic resonance spectroscopy, and dissolution studies. CME should be used in preference to calcium salts for hybrid synthesis and may improve homogeneity of sol-gel glasses.

  19. Residual stress fields in sol-gel-derived thin TiO2 layers

    Teeuw, D.H.J.; Haas, M. de; Hosson, J.Th.M. De


    This paper discusses the induction of residual stresses during the curing process of thin titania layers, which are derived using a sol-gel process. During this process, stresses may build up in the spinning stage, the drying stage, and the consolidation stage. The magnitude and character of these s

  20. Sulfur dioxide removal by sol-gel sorbent derived CuO/Alumina sorbents in fixed bed adsorber

    Zhong-Min Wang


    Full Text Available Nanostructured alumina supported copper oxide granular sorbents were prepared by the sol-gel method. The properties of the sol-gel derived sorbents were compared with a similar commercial sorbent which has been used in the pilot scale moving-bed copper oxide process for flue gas treatment. The crushing strength of the sol-gel derived sorbents is about 6–7 times that of the commercial samples, while the attrition rate of the former is at least 3 times smaller. At temperatures below 400 °C, SO2 sorption capacity of the sol-gel derived sorbent is about 3 times that of the commercial sorbent with a similar amount of CuO loading (7–9 wt%. The better mechanical properties and higher sulfation capacity of the sol-gel derived alumina supported copper oxide sorbents are due to their unique microstructure and the coating method for CuO.

  1. In vitro Mineralization Behavior of the Sol-gel Derived Bioglass/Collegen Composite Porous Scaffold


    The porous scaffold of the sol-gel derived bioactive glass (BG) in the system CaO-P2 O5- SiO2 was treated with the type I collagen solution. The pore walls of the scaffold were covered by the collagenous network. The in vitro mineralization behavior of the sol-gel derived bioglass/ collegen composite porous scaffold was investigated by immersion in supersaturated calcification solution (SCS) at 37 ℃ for different times. XRD , FTIR, SEM/ EDAX techniques were applied to analyze the crystalline phases, morphology and composition of the minerals formed on the pore walls of the scaffold. It was found that with increasing of immersion time, the morphology of reaction products on the pore walls changed from the spherical particles of calcium phosphate to the flake-like HCA crystals.

  2. Sol-gel derived bioactive coating on zirconia: Effect on flexural strength and cell proliferation.

    Shahramian, Khalil; Leminen, Heidi; Meretoja, Ville; Linderbäck, Paula; Kangasniemi, Ilkka; Lassila, Lippo; Abdulmajeed, Aous; Närhi, Timo


    The purpose of this study was to evaluate the effect of sol-gel derived bioactive coatings on the biaxial flexural strength and fibroblast proliferation of zirconia, aimed to be used as an implant abutment material. Yttrium stabilized zirconia disc-shaped specimens were cut, ground, sintered, and finally cleansed ultrasonically in each of acetone and ethanol for 5 minutes. Three experimental groups (n = 15) were fabricated, zirconia with sol-gel derived titania (TiO2 ) coating, zirconia with sol-gel derived zirconia (ZrO2 ) coating, and non-coated zirconia as a control. The surfaces of the specimens were analyzed through images taken using a scanning electron microscope (SEM), and a non-contact tapping mode atomic force microscope (AFM) was used to record the surface topography and roughness of the coated specimens. Biaxial flexural strength values were determined using the piston-on-three ball technique. Human gingival fibroblast proliferation on the surface of the specimens was evaluated using AlamarBlue assay™. Data were analyzed using a one-way analysis of variance (ANOVA) followed by Tukey's post-hoc test. Additionally, the biaxial flexural strength data was also statistically analyzed with the Weibull distribution. The biaxial flexural strength of zirconia specimens was unaffected (p > 0.05). Weibull modulus of TiO2 coated and ZrO2 coated groups (5.7 and 5.4, respectively) were lower than the control (8.0). Specimens coated with ZrO2 showed significantly lower fibroblast proliferation compared to other groups (p sol-gel derived coatings have no influence on the flexural strength of zirconia. ZrO2 coated specimens showed significantly lower cell proliferation after 12 days than TiO2 coated or non-coated control. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2016.

  3. pH-resistant titania hybrid organic-inorganic sol-gel coating for solid-phase microextraction of polar compounds.

    Li, Xiujuan; Gao, Jie; Zeng, Zhaorui


    A novel titania-hydroxy-terminated silicone oil (titania-OH-TSO) sol-gel coating was developed for solid-phase microextraction of polar compounds. In general, titania-based sol-gel reaction is very fast and need to be decelerated by the use of suitable chelating agents. But in the present work, a judiciously designed sol solution ingredients was used to create the titania-OH-TSO coating without the addition of any chelating agent, which simplified the sol-gel procedure. Thanks to the variety of titania's adsorption sites and their acid-base characteristics, aromatic amines, phenols and polycyclic aromatic hydrocarbons were efficiently extracted and preconcentrated from aqueous samples followed by thermal desorption and GC analysis. The newly developed sol-gel hybrid titania coating demonstrated excellent pH stability, and retained its extraction characteristics intact even after continuous rinsing with a 3 M HCl or NaOH solution for 12 h. Furthermore, it could withstand temperatures as high as 320 degrees C. Practical application was demonstrated through the analysis of six aromatic amines in dye process wastewater. A linearity of four orders of magnitude was obtained with correlation coefficient better than 0.9982. The detection limits ranged from 0.22 to 0.84 microg L(-1) and the repeatability of the measurements was <7.0%. The recoveries of these compounds studied in the wastewater were in the ranges 83.6-101.4%, indicating the method accuracy.

  4. Encapsulation of Polymer Colloids in a Sol-Gel Matrix. Direct-Writing of Coassembling Organic-Inorganic Hybrid Photonic Crystals.

    Mikosch, Annabel; Kuehne, Alexander J C


    The spontaneous self-assembly of polymer colloids into ordered arrangements provides a facile strategy for the creation of photonic crystals. However, these structures often suffer from defects and insufficient cohesion, which result in flaking and delamination from the substrate. A coassembly process has been developed for convective assembly, resulting in large-area encapsulated colloidal crystals. However, to generate patterns or discrete deposits in designated places, convective assembly is not suitable. Here we experimentally develop conditions for direct-writing of coassembling monodisperse dye-doped polystyrene particles with a sol-gel precursor to form solid encapsulated photonic crystals. In a simple procedure the colloids are formulated in a sol-gel precursor solution, drop-cast on a flat substrate, and dried. We here establish the optimal parameters to form reproducible highly ordered photonic crystals with good optical performance. The obtained photonic crystals interact with light in the visible spectrum with a narrow optical stop-gap.

  5. Sol-gel-derived hybrid materials multi-doped with rare-earth metal ions

    Zelazowska, E.; Rysiakiewicz-Pasek, E.; Borczuch-Laczka, M.; Cholewa-Kowalska, K.


    Four different hybrid organic-inorganic materials based on TiO2-SiO2 matrices with organic additives and doped with rare-earth metal ions (III) from the group of europium, cerium, terbium, neodymium, dysprosium and samarium, were synthesized by sol-gel method. Tetraethyl orthosilicate, titanium (IV) isopropoxide and organic compounds, such as butyl acrylate, butyl methacrylate, ethyl acetoacetate, ethylene glycol dimethacrylate, ethyl acetate, propylene carbonate, organic solvents and certain inorganic salts were used in the synthesis. The inorganic part of the sols, which were used in the synthesis of all the hybrid materials, was prepared separately and then the organic parts were added. The materials obtained were aged for three weeks at room temperature and then heated in an electric oven for three hours at temperatures of 80 °C-150 °C. Scanning electron microscopy equipped with energy dispersive X-ray spectroscopy (SEM/EDX); X-ray diffraction (XRD); Fourier transform infrared spectroscopy (KBr technique); 29Si magic-angle spinning nuclear magnetic resonance; and fluorescence spectroscopy were used for the examination of morphology, microstructure and luminescence properties, respectively. Photoluminescence properties with relatively intense narrow emission lines of Tb, Eu, Dy, Nd, Sm respectively to the RE-ions doping, were observed for all the hybrid materials.

  6. Sol-Gel Derived Hydroxyapatite Coating on Mg-3Zn Alloy for Orthopedic Application

    Singh, Sanjay; Manoj Kumar, R.; Kuntal, Kishor Kumar; Gupta, Pallavi; Das, Snehashish; Jayaganthan, R.; Roy, Partha; Lahiri, Debrupa


    In recent years, magnesium and its alloys have gained a lot of interest as orthopedic implant constituents because their biodegradability and mechanical properties are closer to that of human bone. However, one major concern with Mg in orthopedics is its high corrosion rate that results in the reduction of mechanical integrity before healing the bone tissue. The current study evaluates the sol-gel-derived hydroxyapatite (HA) coating on a selected Mg alloy (Mg-3Zn) for decreasing the corrosion rate and increasing the bioactivity of the Mg surface. The mechanical integrity of the coating is established as a function of the surface roughness of the substrate and the sintering temperature of the coating. Coating on a substrate roughness of 15-20 nm and sintering at 400°C shows the mechanical properties in similar range of bone, thus making it suitable to avoid the stress-shielding effect. The hydroxyapatite coating on the Mg alloy surface also increases corrosion resistance very significantly by 40 times. Bone cells are also found proliferating better in the HA-coated surface. All these benefits together establish the candidature of sol-gel HA-coated Mg-3Zn alloy in orthopedic application.

  7. Sol-Gel Derived Eu3+-Doped Gd2Ti2O7 Pyrochlore Nanopowders

    Sanja Ćulubrk


    Full Text Available Herein we presented hydrolytic sol-gel synthesis and photoluminescent properties of Eu3+-doped Gd2Ti2O7 pyrochlore nanopowders. According to Gd2Ti2O7 precursor gel thermal analysis a temperature of 840°C is identified for the formation of the crystalline pyrochlore phase. Obtained samples were systematically characterized by powder X-ray diffraction, scanning and transmission electron microscopy, and photoluminescence spectroscopy. The powders consist of well-crystalline cubic nanocrystallites of approximately 20 nm in size as evidenced from X-ray diffraction. The scanning and transmission electron microscopy shows that investigated Eu3+-doped Gd2Ti2O7 nanopowders consist of compact, dense aggregates composed entirely of nanoparticles with variable both shape and dimension. The influence of Eu3+ ions concentration on the optical properties, namely, photoluminescence emission and decay time, is measured and discussed. Emission intensity as a function of Eu3+ ions concentration shows that Gd2Ti2O7 host can accept Eu3+ ions in concentrations up to 10 at.%. On the other hand, lifetime values are similar up to 3 at.% (~2.7 ms and experience decrease at higher concentrations (2.4 ms for 10 at.% Eu3+. Moreover, photoluminescent spectra and lifetime values clearly revealed presence of structural defects in sol-gel derived materials proposing photoluminescent spectroscopy as a sensitive tool for monitoring structural changes in both steady state and lifetime domains.

  8. Sol-gel derived zinc oxide films alloyed with cobalt and aluminium

    Sharma, Mamta [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India); Mehra, R.M., E-mail: [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India)


    ZnO films codoped with 5 at.% Co and 1 at.% Al were prepared by sol-gel technique on corning glass and silicon substrates with precursor sols of different pH values. The pH was varied from 5.4 to 11 by adding varying amounts of monoethanolamine to the sol. Since pH plays an important role in controlling the properties of films, we discuss in detail the effect of pH value on the structural, morphological and optical properties of the grown films. X-ray diffraction and atomic force microscopy images reveal that the size of crystallites increases with pH of the sol. The variation of pH in the reaction system influences the density of homogeneous nucleation and the crystal growth along the c-axis. High quality Co and Al codoped ZnO films annealed at 600 {sup o}C have been obtained using a sol with pH = 9. These sol-gel derived films find their suitability to be used as dilute magnetic semiconductors.

  9. Synthesis, Consolidation and Characterization of Sol-gel Derived Tantalum-Tungsten Oxide Thermite Composites

    Cervantes, O [Univ. of California, Davis, CA (United States)


    Energetic composite powders consisting of sol-gel (SG) derived nanostructured tungsten oxide were produced with various amounts of micrometer-scale tantalum fuel metal. Such energetic composite powders were ignition-tested and results show that the powders are not sensitive to friction, spark and/or impact ignition. Initial consolidation experiments, using the High Pressure Spark Plasma Sintering (HPSPS) technique, on the SG derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The SG derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta - WO3) energetic composite was consolidated to a density of 9.17 g·cm-3 or 93% relative density. In addition, those samples were consolidated without significant pre-reaction of the constituents, thus retaining their stored chemical energy.

  10. 溶胶-凝胶法制备有机/无机纳米杂化涂料的现状及展望%Current Status and Prospect of Sol-Gel Method in Preparing Organic - Inorganic Hybrid Nano- Paints

    张浩; 王笛


    溶胶-凝胶法制备的有机/无机纳米杂化涂料具有许多优点.介绍了溶胶-凝胶法制备有机/无机纳米杂化涂料的研究现状,并对此作出了展望.%A review was provided of the current status of research on fabricating organic - inorganic hybrid nano - paints by sol - gel method. It was pointed out that sol-gel method as a new method for preparing organic - inorganic hybrid materials had a variety of advantages. Furthermore, suggestions were also given about the development trend of sol-gel method.

  11. The evaluation of physical properties and in vitro cell behavior of PHB/PCL/sol-gel derived silica hybrid scaffolds and PHB/PCL/fumed silica composite scaffolds.

    Ding, Yaping; Yao, Qingqing; Li, Wei; Schubert, Dirk W; Boccaccini, Aldo R; Roether, Judith A


    PHB/PCL/sol-gel derived silica hybrid scaffolds (P5S1S) and PHB/PCL/fumed silica composite scaffolds (P5S1N) with a 5:1 organic/inorganic ratio were fabricated through a combination of electrospinning and sol-gel methods and dispersion electrospinning, respectively. In contrast to the silica nanoparticle aggregates appearing on the fiber surface of P5S1N, smooth and uniform fibers were obtained for P5S1S. The fiber diameter distribution, tensile strength, thermal gravimetric analysis (TGA), and cellular behavior of both types of scaffolds were characterized and studied. The tensile strength results and TGA indicated that the interfacial interaction between the organic and the inorganic phase was enhanced in P5S1S over the nanocomposite scaffolds, and cells exhibited significantly higher alkaline phosphate activity (ALP) for P5S1S, which makes P5S1S hybrid scaffolds candidate materials for bone tissue engineering applications.

  12. The Influence of Type and Thickness of Sol-gel Derived Coatings on the in vitro Osteoblasts Behavior


    To evaluate the cellular response to the most commonly studied coatings fabricated by the sol- gel route, the influence of the coating thickness on the cellular response was studied. 1, 3, 5 layers of hydroxyapatite( HA ), fluorohydroxyapatite (FHA) and titania (TiO2) were coated on the surface of commercially pure titanium (cpTi) discs respectively by the sol-gel route. CpTi discs were taken as control. XRD and SEM were employed to characterize the type and thickness of these coatings. In vitro osteoblasts behavior on the coatings was studied by the culture of MG63 cell line. The experimental results show all groups have good biocompatibility to osteoblasts.However, the type and thickness of the coatings influence the osteoblast response. The optimal type and thickness of sol-gel derived biocoatings were concluded.

  13. Radiation hardening in sol-gel derived Er{sup 3+}-doped silica glasses

    Hari Babu, B., E-mail:, E-mail:; León Pichel, Mónica [Laboratoire des Solides Irradiés, UMR CEA-CNRS 7642, Ecole Polytechnique, Université Paris Saclay, 91128 Palaiseau (France); Institut de Chimie Moléculaire et des Matériaux d' Orsay, UMR CNRS-UPSud 8182, Université Paris Sud, 91405 Orsay (France); Ollier, Nadège [Laboratoire des Solides Irradiés, UMR CEA-CNRS 7642, Ecole Polytechnique, Université Paris Saclay, 91128 Palaiseau (France); El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed [Laboratoire PhLAM (UMR CNRS 8523), IRCICA (USR CNRS 3380), CERLA - FR CNRS 2416, Université Lille 1, Villeneuve d' Ascq Cedex F-59655 (France); Poumellec, Bertrand; Lancry, Matthieu, E-mail:, E-mail: [Institut de Chimie Moléculaire et des Matériaux d' Orsay, UMR CNRS-UPSud 8182, Université Paris Sud, 91405 Orsay (France); Ibarra, Angel [National Fusion Laboratory, CIEMAT, Avda Complutense 40, 28040 Madrid (Spain)


    The aim of the present paper is to report the effect of radiation on the Er{sup 3+}-doped sol-gel silica glasses. A possible application of these sol-gel glasses could be their use in harsh radiation environments. The sol-gel glasses are fabricated by densification of erbium salt-soaked nanoporous silica xerogels through polymeric sol-gel technique. The radiation-induced attenuation of Er{sup 3+}-doped sol-gel silica is found to increase with erbium content. Electron paramagnetic resonance studies reveal the presence of E′{sub δ} point defects. This happens in the sol-gel aluminum-silica glass after an exposure to γ-rays (kGy) and in sol-gel silica glass after an exposure to electrons (MGy). The concentration levels of these point defects are much lower in γ-ray irradiated sol-gel silica glasses. When the samples are co-doped with Al, the exposure to γ-ray radiation causes a possible reduction of the erbium valence from Er{sup 3+} to Er{sup 2+} ions. This process occurs in association with the formation of aluminum oxygen hole centers and different intrinsic point defects.

  14. Sol-gel derived antireflective structures for applications in silicon solar cells

    Karasiński, Paweł; Skolik, Marcin


    This work presents theoretical and experimental results of antireflective coatings (ARCs) obtained for applications in silicon solar cells. ARCs were derived from sol-gel process and dip-coated using silica (SiO2) and titania (TiO2). Theoretical results were obtained using 2×2 transfer matrix calculation method. Technological process of SiO2 and TiO2 thin film fabrication as well as measurement techniques are described in this paper. Strong correlation between theoretical and experimental data is demonstrated. It is shown, that weighted average reflection from a substrate can be reduced ten times with the use of SiO2/TiO2/Si double layer ARCs, when compared to a bare silica substrate.

  15. Sintering behavior of ZnO:Al ceramics fabricated by sol-gel derived nanocrystalline powders

    Bahsi, Z.B. [Dept. of Materials Science and Engineering, Gebze Institute of Technology, Kocaeli (Turkey); Aslan, M.H. [Dept. of Physics, Gebze Institute of Technology, Kocaeli (Turkey); Ozer, M. [Dept. of Physics, Istanbul Kultur University, Istanbul (Turkey); Oral, A.Y.


    ZnO:Al ceramics (Zn:Al, 0.95:0.05) were prepared by using sol-gel derived nanocrystalline powders. XRD patterns of the doped ceramics revealed the existence of both zincite (JCPDS 36-1451) and gahnite (JCPDS 5-0669) phases. Gahnite phase (ZnAl{sub 2}O{sub 4}) was segregated along the ZnO grain boundaries. At the sintering temperature of 1200 C, relative density of the undoped and Al doped ceramics were measured as 0.695 and 0.628, respectively. Both grain size and relative density of the ceramics decreased with Al doping. (copyright 2009 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  16. Nanoporous characteristics of sol-gel-derived ZnO thin film

    Anees A. Ansari; M. A. M. Khan; M. Alhoshan; S. A. Alrokayan; M. S. Alsalhi


    Sol-gel-derived nanoporous ZnO film has been successfully deposited on glass substrate at 200 ℃ and subsequently annealed at different temperatures of 300,400 and 600 ℃.Atomic force micrographs demonstrated that the film was crack-free,and that granular nanoparticles were homogenously distributed on the film surface.The average grain size of the nanoparticles and RMS roughness of the scanned surface area was 10 nm and 13.6nm,respectively,which is due to the high porosity of the film.Photoluminescence (PL) spectra of the nanoporous ZnO film at room temperature show a diffused band,which might be due to an increased amount of oxygen vacancies on the lattice surface.The observed results of the nanoporous ZnO film indicates a promising applicationin the development of electrochemical biosensors due to the porosity of film enhancing the higher loading of biomacromolecules (enzyme and proteins).

  17. A novel sol-gel derived bioactive glass featuring antibacterial properties

    Bellantone, M.; Coleman, N.J.; Hench, L.L. [Imperial Coll. of Science, Technology and Medicine, London (United Kingdom). Dept. of Materials


    Antibacterial effects are highly desirable in biomaterials for dental, orthopaedic, and tissue engineering applications. The study herein reports on the bacteriostatic properties of a new composition of bioactive glass derived by the sol-gel process. Ag{sub 2}O was incorporated into the SiO{sub 2}-CaO-P{sub 2}O{sub 5} system. Leaching of the Ag{sup +} ion from the glass conferred strong bacteriostatic properties to the system. In vitro antibacterial tests on gram (+) and gram (-) bacteria showed that in the presence of bioactive glass no significant alteration of the cell concentration occurs. Conversely, the novel silver-doped bioactive glass causes a dramatic decrease of cell population for each of the bacteria under investigation. Unlike antibiotics the silver ion does not cause bacterial resistance. This property, together with its broad spectrum of action, makes silver an exceptionally versatile in situ antibacterial agent. (orig.)

  18. Sol-gel derived titania coating with immobilized bisphosphonate enhances screw fixation in rat tibia.

    Linderbäck, Paula; Areva, Sami; Aspenberg, Per; Tengvall, Pentti


    A variety of surface modifications have been tested for the enhancement of screw fixation in bone, and locally delivered anti-osteoporosis drugs such as bisphosphonates (BP) are then of interest. In this in vivo study, the impact of surface immobilized BP was compared with systemic BP delivery and screws with no BP. After due in vitro characterization, differently treated stainless steel (SS) screws were divided into four groups with 10 rats each. Three of the groups received screws coated with sol-gel derived TiO(2) and calcium phosphate (SS+TiO(2)+CaP). One of these had no further treatment, one had alendronate (BP) adsorbed to calcium phosphate mineral, and one received systemic BP treatment. The fourth group received uncoated SS screws and no BP (control). The screw pullout force was measured after 4 weeks of implantation in rat tibiae. The immobilized amount and release rate of alendronate could be controlled by different immersion times. The SS+TiO(2)+CaP coating did not increase the pullout force compared to SS alone. Surface delivered alendronate enhanced the pullout force by 93% [p = 0.000; 95% Confidence Interval (CI): 67-118%] compared to SS, and by 39% (p = 0.044; 95% CI: 7-71%) compared to systemic alendronate delivery. Both surface immobilized and systemically delivered alendronate improved implant fixation. Also, locally delivered, that is, surface immobilized alendronate showed a better fixation than systemically delivered. Using sol-gel derived TiO(2) as a platform, it is possible to administer controllable amounts of a variety of BPs.

  19. Evaluating sol-gel ceramic thin films for metal implant applications: III. In vitro aging of sol-gel-derived zirconia films on Ti-6Al-4V.

    Kirk, P B; Filiaggi, M J; Sodhi, R N; Pilliar, R M


    Sol-gel-derived zirconia films were deposited onto polished Ti-6Al-4V substrates by dip-coating from an alkoxide precursor solution. No change in morphology of the zirconia film was observed after aging at 37 degrees C for 4-12 weeks in pH 4.0 buffer solution or Hanks' balanced salt solution (HBSS), although a precipitate predominantly composed of calcium phosphate was formed on those films aged in HBSS. X-ray diffraction identified the phase of the zirconia film as either cubic or tetragonal, and revealed no degradation to the monoclinic phase after aging. By a substrate straining test, the fracture strain of the coating was revealed to be 1.5%, above the yield strain of the titanium alloy substrate. At this strain level, through-thickness cracks formed in the coating where slip bands emerged from the substrate. Qualitatively, the adhesion of the film was sufficient to prevent gross delamination of the film at high strain levels, although small regions of delamination were caused by compressive buckling of the film. This behavior indicates generally good adhesion. No change in this behavior was observed after aging.

  20. A Comparative Study of Solvothermal and Sol-Gel-Derived Nanocrystalline Alumina Catalysts for Ethanol Dehydration

    Mingkwan Wannaborworn


    Full Text Available The ethanol dehydration to ethylene over alumina catalysts prepared by solvothermal and sol-gel methods was investigated. Also, a commercial alumina was used for comparison purposes. The results showed that the catalytic activity depends on the properties of catalyst derived from different preparation methods and reaction temperature. The alumina synthesized by solvothermal method exhibited the highest activity. This can be attributed to the higher surface area and larger amount of acid site, especially the ratio of weak/strong acid strength as determined by N2 physisorption and NH3-TPD studies. The solvothermal-derived catalyst exhibited an excellent performance with complete ethanol conversion and 100% selectivity to ethylene at 350°C in comparison with other ones. In addition, we further studied the catalytic dehydration of alumina catalyst modified with Fe. The presence of 10 wt.% Fe decreased both conversion and ethylene selectivity. However, the acetaldehyde selectivity apparently increased. It was related to the dehydrogenation pathway that takes place on Fe species.

  1. Radiation hardening of sol gel-derived silica fiber preforms through fictive temperature reduction.

    Hari Babu, B; Lancry, Matthieu; Ollier, Nadege; El Hamzaoui, Hicham; Bouazaoui, Mohamed; Poumellec, Bertrand


    The impact of fictive temperature (Tf) on the evolution of point defects and optical attenuation in non-doped and Er3+-doped sol-gel silica glasses was studied and compared to Suprasil F300 and Infrasil 301 glasses before and after γ-irradiation. To this aim, sol-gel optical fiber preforms have been fabricated by the densification of erbium salt-soaked nanoporous silica xerogels through the polymeric sol-gel technique. These γ-irradiated fiber preforms have been characterized by FTIR, UV-vis-NIR absorption spectroscopy, electron paramagnetic resonance, and photoluminescence measurements. We showed that a decrease in the glass fictive temperature leads to a decrease in the glass disorder and strained bonds. This mainly results in a lower defect generation rate and thus less radiation-induced attenuation in the UV-vis range. Furthermore, it was found that γ-radiation "hardness" is higher in Er3+-doped sol-gel silica compared to un-doped sol-gel silica and standard synthetic silica glasses. The present work demonstrates an effective strategy to improve the radiation resistance of optical fiber preforms and glasses through glass fictive temperature reduction.

  2. Morphology of sol-gel derived nano-coated coralline hydroxyapatite.

    Ben-Nissan, B; Milev, A; Vago, R


    Current bone graft materials are mainly produced from coralline hydroxyapatite (HAp). Due to the nature of the conversion process, commercial coralline HAp has retained coral or CaCO(3,) and the structure possesses nanopores within the inter-pore trabeculae, resulting in high dissolution rates. Under certain conditions these features reduce durability and strength and are not utilised where high structural strength is required. To overcome these limitations, a new coral double-conversion technique has been developed. The technique involves a two-stage application route where, in the first stage, complete conversion of coral to pure HAp is achieved. In the second, a new sol-gel-derived HAp nano-coating is directly applied to cover the micro- and nano-pores within the intra-pore material, whilst maintaining the large pores. Biaxial strength was improved two-fold due to this unique double treatment. This application is expected to result in enhanced durability and longevity due to the monophasic hydroxyapatite structure and strength in the physiological environment. It is anticipated that this new material can be applied to load-bearing bone graft applications where high strength requirements are pertinent.

  3. Sol-gel-derived AgCl photochromic coating on glass for holographic application

    Mennig, Martin; Krug, Herbert; Fink-Straube, Claudia; Oliveira, Peter W.; Schmidt, Helmut K.


    A sol-gel derived photochromic glass coating of about 1.5 micrometers in thickness is synthesized by infiltration of Ag+ into a predried Na-Al-B-Si gel layer. The formation of small Ag colloids is initiated by a soft heat treatment and the colloids are converted by a HCl vapor treatment into AgCl crystallites of about 40 nm in diameter. The coating darkens by UV irradiation, forming Ag crystallites of about 5 nm in size. This process is completely reversible at 400 degree(s)C and no decay is observed in numerous cycles. An amplitude hologram which acts as a diffraction grating with a grating period of about 10 micrometers can be produced within this layer by a two-wave mixing experiment with laser light of 351 nm wavelength. The diffraction efficiency of this grating is determined to 0.11%. After thermal erasing the diffraction pattern can be rewritten and erased repeatedly without any loss of efficiency.

  4. The influence of sol-gel-derived silica coatings functionalized with betamethasone on adipose-derived stem cells (ASCs).

    Donesz-Sikorska, Anna; Grzesiak, Jakub; Smieszeka, Agnieszk; Krzak, Justyna; Marycz, Krzysztof


    Silica-based sol-gel coatings have gained attention in bone therapies and orthopedic applications, due to the biocompatibility and bioactivity, including a high potential for the controlled release both in vitro and in vivo. Bioactive materials are created to facilitate the biocompatibility of orthopedic implants. One of the promising alternatives is biomaterials with immobilized drugs. In this study we demonstrated for the first time novel sol-gel-derived silica coatings with active amino groups (SiO2(NH2)) functionalized with a steroid drug-betamethasone, applied to a substrate 316 L using dip coating technique. The presence of betamethasone in functionalized coatings was directly confirmed by Raman spectroscopy and energy-dispersive X-ray spectroscopic analysis. The wettability was evaluated by the sessile drop method, while the surface free energy was estimated based on the contact angles measured. Our results showed a shift in surface properties from hydrophobic to hydrophilic after application of the coatings. We have investigated the morphology, proliferation factor, and the population doubling time of adipose-derived stem cells for biological purposes. Moreover, the analysis of the distribution and localization of cellular microvesicles was performed to evaluate the influence of functionalized surfaces on cellular cytophysiological activity. Increased proliferation and activation of cells, determined by the observations of microvesicles shedding processes, provided evidence of the availability of the drug. Therefore, we conclude that the sol-gel synthesis proposed here allows to improve the metal substrates and can be successfully used for immobilization of betamethasone. This in turn enables the direct delivery of the drug with implanted material into the wound site, and to stimulate the activity of cells to enhance tissue regeneration.

  5. A Hydrogen Peroxide Biosensor Combined HRP Doped Polypyrrole with Ferrocene Modified Sol-gel Derived Composite Carbon Electrode


    A novel amperometric biosensor for the detection of hydrogen peroxide is described.The biosensor was constructed by electrodepositing HRP/PPy membrane on the surface of ferrocenecarboxylic acid mediated sol-gel derived composite carbon electrode. The biosensor gives response to hydrogen peroxide in a few seconds with detection limit of 5×l0-7 mol · L-1(based on signal: noise=3). Linear range is up to 0.2 mmol · L-1.

  6. Surface aspects of sol-gel derived hematite films for the photoelectrochemical oxidation of water.

    Herrmann-Geppert, Iris; Bogdanoff, Peter; Radnik, Jörg; Fengler, Steffen; Dittrich, Thomas; Fiechter, Sebastian


    α-Fe(2)O(3) (hematite) photoanodes for the oxygen evolution reaction (OER) were prepared by a cost-efficient sol-gel procedure. Due to low active photoelectrochemical properties observed, it is assumed that the sol-gel procedure leads to hematite films with defects and surface states on which generated charge carriers are recombined or immobilized in trap processes. Electrochemical activation was proven to diminish unfavourable surface groups to some extent. More efficiently, a plasma treatment improves significantly the photoelectrochemical properties of the OER. X-ray photoelectron spectroscopy (XPS) analysis reveals an oxygen enriched surface layer with new oxygen species which may be responsible for the improved electrochemical activity. Due to surface photovoltage an increased fraction of transferred charge carriers from these newly produced surface defects are identified.

  7. Low-temperature sol-gel-derived nanosilver-embedded silane coating as biofilm inhibitor.

    Babapour, A; Yang, B; Bahang, S; Cao, W


    Silver nanocomposite coatings are prepared by the sol-gel method for the prevention of biofilm formation on the surface of medical implanted devices. High-temperature processing of such coatings can lead to diffusion of nanosilver and reduce the amount of available silver particles for long-term effects. Using a low-temperature sol-gel method, we have successfully prepared silane-based matrices, phenyltriethoxysilane (PhTEOS), containing different amounts of Ag nanoparticles. The incorporation of a silver salt into the sol-gel matrix resulted in a desired silver release rate, i.e. high initial release rate followed by a lower sustained release for more than 15 days, as determined by inductively coupled plasma mass spectrometry (ICP-MS). Scanning electron microscopy (SEM) has been employed to investigate the morphology of the film surfaces before and after immersion in a nutrient-rich bacterial suspension of approximately 10⁸ CFU ml⁻¹, which was incubated for up to 30 days at 37 °C. It was found that thin films containing 35 nm particles could prevent the formation of biofilm for over 30 days. The presence of surface silver before and after 3, 9 and 15 days immersion was confirmed by x-ray photoelectron spectroscopy (XPS).

  8. Sol-gel derived precursors to Group 14 semiconductor nanocrystals - Convenient materials for enabling nanocrystal-based applications

    Veinot, Jonathan G C; Henderson, Eric J; Hessel, Colin M, E-mail: [Department of Chemistry, University of Alberta, Edmonton, Alberta (Canada)


    Semiconductor nanocrystals are intriguing because of their electronic, optical, and chemical characteristics. Silicon nanocrystals (Si-NCs) of sub-5 nm dimension are of particular interest due to their intense photoluminescent response and the promise of linking silicon photonics and electronics. Other related nanomaterials of technological importance include SiC and Ge. The following contribution describes key experimental findings pertaining to synthetic methodology, investigation of nanodomain formation and growth, as determined by X-ray powder diffraction (XRD) and photoluminescence (PL) spectroscopy for a series of sol-gel derived prepolymers suitable for preparing Group 14 based nanocrystal containing composites.

  9. Sol-gel derived precursors to Group 14 semiconductor nanocrystals - Convenient materials for enabling nanocrystal-based applications

    Veinot, Jonathan G. C.; Henderson, Eric J.; Hessel, Colin M.


    Semiconductor nanocrystals are intriguing because of their electronic, optical, and chemical characteristics. Silicon nanocrystals (Si-NCs) of sub-5 nm dimension are of particular interest due to their intense photoluminescent response and the promise of linking silicon photonics and electronics. Other related nanomaterials of technological importance include SiC and Ge. The following contribution describes key experimental findings pertaining to synthetic methodology, investigation of nanodomain formation and growth, as determined by X-ray powder diffraction (XRD) and photoluminescence (PL) spectroscopy for a series of sol-gel derived prepolymers suitable for preparing Group 14 based nanocrystal containing composites.

  10. Optical Absorption of Sol-Gel Derived ZnO/TiO2 Nanocomposite Films

    袁志好; 唐成春; 范守善


    ZnO/TiO2 nanocomposite films on quartz substrates were prepared by the sol-gel method, and the corresponding optical absorption properties were investigated. In the ultraviolet region, it was found that the position of fundamental absorption edge partially depends on the composition of the ZnO/TiO2 films, and shifts toward a shorter wavelength with the increasing content of ZnO in the films. Moreover, a blueshift of the absorption edge resulted from a quantum size effect and the quantum confinement effect was observed in the ZnO/TiO2 system.

  11. Magneto-optical investigations of rare earth doped sol-gel derived silicate xerogels

    Secu, C.E.; Polosan, S. [National Institute of Materials Physics, Optical Processes in Nanostructured Materials Department, P.O. Box MG-7, Bucharest-Magurele, 077125 (Romania); Secu, M., E-mail: [National Institute of Materials Physics, Optical Processes in Nanostructured Materials Department, P.O. Box MG-7, Bucharest-Magurele, 077125 (Romania)


    Rare-earth doped xerogels (Eu{sup 3+}, Sm{sup 3+}, Ho{sup 3+}, Pr{sup 3+}) were prepared by using the sol-gel method and their magneto-optical and optical properties have been studied. The Magnetic Circular Dichroism (MCD) spectra are quite similar to those recorded in the RE-doped fluorozirconate glasses; the fine structures shown by the MCD spectra are better resolved compared to the optical absorption spectra. The MCD technique has been correlated with optical measurements in order to investigate the site symmetry in the particular case of Eu{sup 3+}-doped xerogel and oxyfluoride glasses. In the xerogel, coordination symmetry around the Eu{sup 3+} ions is close to D{sub 3h} and is lower in the oxyfluoride glass. - Highlights: > Rare-earth doped xerogels (Eu{sup 3+}, Sm{sup 3+}, Ho{sup 3+}, Pr{sup 3+}) were prepared by the sol-gel method. > MCD and luminescence methods were applied to probe the site symmetry in europium doped xerogel and oxyfluoride glasses. > Rare-earth site symmetry is close to D{sub 3h} in xerogel and is lower in oxyfluoride glass.

  12. Thickness dependency of sol-gel derived ZnO thin films on gas sensing behaviors

    Kakati, Nitul; Jee, Seung Hyun; Kim, Su Hyun; Oh, Jun Young; Yoon, Young Soo, E-mail:


    ZnO thin films were fabricated by a sol-gel method using Zn(CH{sub 3}COO){sub 2}.2H{sub 2}O as starting material in order to prepare an acetone gas sensor. A homogeneous and stable solution was prepared by dissolving the zinc acetate in a solution of ethanol and monoethanolamine. The sol-gel solution is coated on alumina substrates with various thicknesses by spin coating technique and heat treated to grow crystalline ZnO thin films. The effect of thickness on physical and electrical properties of as deposited ZnO thin films has been studied. The as deposited ZnO thin films were characterized by X-ray diffraction spectroscopy, field emission scanning electron microscopy and atomic force microscopy. The root mean square surface roughness factors increase with thickness of the films and found 3.9, 6.6, 9.0, and 11.28 nm for 80-, 220-, 450- and 620-nm-thin films respectively. The activation energies of the films are calculated from the resistance temperature characteristics. The sensitivities of the ZnO films towards the acetone gas were determined at an operating temperature of 200 {sup o}C. The sensitivity towards acetone vapor is strongly depending on surface morphology of the ZnO thin films.

  13. UV-Irradiation Cured Organic-inorganic Hybrid Nanocomposite Initiated by Ethoxysilane-modified Multifunctional Polymeric Photoinitiator through Sol-gel Process%UV-Irradiation Cured Organic-inorganic Hybrid Nanocomposite Initiated by Ethoxysilane-modified Multifunctional Polymeric Photoinitiator through Sol-gel Process

    Hu, Lihua; Shi, Wenfang


    The UV-cured organic-inorganic hybrid nanocomposite (nano-Si-m-PI) was prepared through the photopolymeri- zation of acrylic resin initiated by ethoxysilane-modified multifunctional oligomeric photoinitiator (Si-m-PI). The es- terification reaction of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone (Irgacure 2959) with thioglycolic acid, and the following addition reactions with dipentaerythritol hexaacrylate and then 3-aminopropyltriethoxysilane were carried out for preparing the Si-m-PI. The Si-m-PI exhibits the similar UV absorption and molar extinction coefficient with Irgacure 2959. The photoinitiating activity study by photo-DSC analysis showed that the Si-m-PI possesses high photopolymerization rate at the peak maximum (Rpax) and final unsaturation conversion (Pf) in the cured hybrid films. From the scanning electron microscope (SEM) observation, the SiO2 nanoparticles dispersed uniformly in the formed nano-Si-m-PI, whereas the aggregation of nanoparticals occurred in nano-Irg, which was prepared through the photopolymerization of acrylic resin initiated by Irgacure 2959. Moreover, compared with the UV-cured pure polymer and nano-Irg, the nano-Si-m-PI showed remarkably enhanced thermal stability and mechanical properties.

  14. Growth and Magnetic Properties of Sol-Gel Derived Co-Doped ZnO Thin Film


    Zn1-xCoxO films were grown on glass by sol-gel spin coating process. A homogeneous and stable Zn1-xCoxO sol was prepared by dissolving zinc acetate dihydrate, cobalt acetate tetrahydrate and aluminium chloride hexahydrate as solutes in solution of isopropanol and monoethanolamine. The films were postheated and vacuum annealed, and investigated for c-axis preferred orientation and electromagnetic properties. Zn1-xCoxO films with different Co concentrations were oriented well along the c-axis, especially the Zn1-xCoxO film with 10% Co(atom fraction) was highly c-axis oriented. The transmittance spectra show that Zn1-xCoxO films occur d-d transition and sp-d exchange interaction between Co2+ ions. The electrical resistivity of the films at 10% Co had the lowest value because the crystallite size became largest and the crystallinity of the c-axis was improved. X-ray photoelectron spectroscopy and alternating gradient magnetometer analyses indicated that no Co metal cluster was formed, and the ferromagnetism at room temperature appeared. The characteristics of the electrical resistivity and room temperature ferromagnetism of sol-gel derived Zn1-xCoxO films suggest a potential application of dilute magnetic semiconductor devices.

  15. Crystallinity and stoichiometry of nano-structured sol-gel-derived BaTiO{sub 3} monolithic gels

    Shimooka, Hirokazu [Kyushu Inst. of Tech., Kitakyushu, Fukuoka (Japan). Dept. of Applied Chemistry; Kuwabara, Makoto [Univ. of Tokyo (Japan). Dept. of Materials Science


    The crystallization behavior and stoichiometric changes of barium titanium alkoxide-derived monolithic gels prepared by the sol-gel process using a high-concentration Ba,Ti precursor solution (0.8 mol/L) were investigated during aging at room temperature. Crystallization of the gels (which were amorphous, per X-ray diffraction analysis immediately after gelation) into the BaTiO{sub 3} perovskite phase increased during aging and was associated with significant shrinkage of the gels. Crystallization reached a value of {approximately}82% by the final stage of shrinkage, assuming the degree of crystallization of a gel treated at 600 C to be 100%. The stoichiometry of the gels (Ba/Ti molar ratio) also changed considerably during aging, as estimated by the concentrations of Ba and Ti that remained in the expelled liquid resulting from syneresis at any time during the aging process. Deviation in the Ba/Ti ratio of the precursor solution ranged from 0.015 at the initial stage of shrinkage to 0.003 at the final stage, a value determined by inductively coupled plasma atomic emission spectroscopy. The present study demonstrates the great advantage of using high-concentration precursor solutions of barium titanium alkoxides, rather than low-concentration solutions, to obtain BaTiO{sub 3} gel monoliths with high density and crystallinity and little stoichiometric deviation, by sol-gel processing at room temperature.

  16. Synthesis of sol-gel derived glass powder and in vitro bioactivity property tested in simulated body fluid

    Fadzli, S. A. Syed Nuzul; Roslinda, S.; Zainuddin, Firuz; Ismail, Hamisah


    The objective of this study is to determine the apatite forming ability of sol-gel derived glass based on chemical composition 50%(SiO2)-40%(CaO)-10%(PO4) by examine the reacted sample surface after soaking in simulated body fluid (SBF). The glass was synthesized via an acid catalyzed low temperature sol-gel route, dried, crushed and uniaxial pressed into pellets before finally heated at 600°C to maintain the amorphous nature and to obtain stabilized glass pellets. The bioactivity test of the glass was carried out in vitro by soaking the pellets into simulated body fluid (SBF) for various times up to 14 days. It was revealed that apatite-like structures were rapidly formed on the surface of the glass showed by the glass surface was totally covered with these crystallized apatite within the first 24 hours of immersion. The formation of crystallized carbonated apatite (HCA) was proved within the first 24 hours of immersion via XRD, FTIR and FE-SEM analysis method. Increased in immersion time period to 14 days was significantly effects in enlargement of the apatite particle sizes and transformation these apatite into a typical coral-like apatite structures.

  17. Preparation and Characterization of LiTaO3 Films Derived by an Improved Sol-Gel Process

    Jun GOU; Jun WANG; Ming YANG; Zehua HUANG; Weizhi LI; Yadong JIANG


    In this paper,an improved sol-gel method was suggested to obtain high-concentration LiTaO3 precursor solution for simplified experimental conditions and thicker films,by mixing lithium acetate and tantalum ethoxide in a 1,2-Propylene glycol solution.Compared to traditional methods,the process was done without weak acidic solution and absolute dry experimental condition.Results of a comparative study of LiTaO3 thin films derived by the improved sol-gel process and a traditional process using 2-methoxy ethanol as solvent were presented.Nano-crystalline LiTaO3 films with rhombohedral structures were formed in both methods after annealing at 650 ° for 5 min.The thickness of each LiTaO3 layer coated onto the substrate increased from 25 nm to 110 nm when 2-methoxy ethanol was replaced by 1,2-Propylene glycol.LiTaO3 films with a stronger preferential orientation were obtained in 1,2-Propylene glycol due to its higher boiling point and slower volatilization rate.On the other hand,the diffraction peak intensity of LiTaO3 thin films prepared using 1,2-Propylene glycol was weaker than that of the films prepared using 2-methoxy ethanol due to decreased times of annealing.

  18. Evaluation of the photocatalytic ability of a sol-gel-derived MgO-ZrO2 oxide material

    Ciesielczyk Filip


    Full Text Available This paper deals with the synthesis and characterization of a novel group of potential photocatalysts, based on sol-gel-derived MgO-ZrO2 oxide material. The material was synthesized in a typical sol-gel system using organic precursors of magnesia and zirconia, ammonia as a promoter of hydrolysis and methanol as a solvent. All materials were thoroughly analyzed, including morphology and particle sizes, chemical composition, identification of characteristic functional groups, porous structure parameters and crystalline structure. The proposed methodology of synthesis resulted in obtaining pure MgO-ZrO2 oxide material with micrometric-sized particles and a relatively high surface area. The samples underwent an additional calcination process which led to the crystalline phase of zirconia being formed. The key element of the study was the evaluation of the effectiveness of decomposition of C.I. Basic Blue 9 dye. It was shown that the calcined materials exhibit both satisfactory adsorption and photocatalytic activity with respect to the decomposition of a selected model organic impurity. Total dye removal varied in the range of 50-70%, and was strongly dependent on process parameters such as quantity of photocatalyst, time of irradiation, and the addition of promoters.

  19. Optical Fiber Chemical Sensor with Sol-Gel Derived Refractive Material as Transducer for High Temperature Gas Sensing in Clean Coal Technology

    Shiquan Tao


    The chemistry of sol-gel derived silica and refractive metal oxide has been systematically studied. Sol-gel processes have been developed for preparing porous silica and semiconductor metal oxide materials. Micelle/reversed micelle techniques have been developed for preparing nanometer sized semiconductor metal oxides and noble metal particles. Techniques for doping metal ions, metal oxides and nanosized metal particles into porous sol-gel material have also been developed. Optical properties of sol-gel derived materials in ambient and high temperature gases have been studied by using fiber optic spectroscopic techniques, such as fiber optic ultraviolet/visible absorption spectrometry, fiber optic near infrared absorption spectrometry and fiber optic fluorescence spectrometry. Fiber optic spectrometric techniques have been developed for investigating the optical properties of these sol-gel derived materials prepared as porous optical fibers or as coatings on the surface of silica optical fibers. Optical and electron microscopic techniques have been used to observe the microstructure, such as pore size, pore shape, sensing agent distribution, of sol-gel derived material, as well as the size and morphology of nanometer metal particle doped in sol-gel derived porous silica, the nature of coating of sol-gel derived materials on silica optical fiber surface. In addition, the chemical reactions of metal ion, nanostructured semiconductor metal oxides and nanometer sized metal particles with gas components at room temperature and high temperatures have also been investigated with fiber optic spectrometric methods. Three classes of fiber optic sensors have been developed based on the thorough investigation of sol-gel chemistry and sol-gel derived materials. The first group of fiber optic sensors uses porous silica optical fibers doped with metal ions or metal oxide as transducers for sensing trace NH{sub 3} and H{sub 2}S in high temperature gas samples. The second group of

  20. Thermal stability of a modified sol-gel derived hydroxyapatite nanopowders

    Herradi, S.; El Bali, B.; Khaldi, M.; Lachkar, M.


    Hydroxyapatite Ca10(PO4)6(OH)2 (HA) powder was successfully synthesized by a modified sol-gel method using a solution of calcium nitrate in ethanol, along with a solution of diammonium hydrogen phosphate in water and NH4OH as starting materials. The Ca/P molar ratio was maintained at 1.67. The powder was subjected to furnace and microwave heating to compare the decomposition of HA and study the crystallite sizes. It was found that microwave heated powders were pure HAP up to 230°C with absence of secondary phases. However, XRD patterns show that furnace heated powders convert completely to β-TCP when treated at 750°C and 1000°C. This result was confirmed by the absence of hydroxyl bands in the FT-IR spectra for these temperatures.

  1. Structure and Waveguide Properties of Sol-Gel Derived Gd2O3 Films

    Guo Hai(郭海); Xiao Teng(肖腾); Yang Xudong(杨旭东); Zhang Weiping(张慰萍); Lou Liren(楼立人); Yin Min(尹民); Jacques Mugnier


    Pure and rare earth doped gadolinium oxide (Gd2O3) waveguide films were prepared by a simple sol-gel process and dip-coating method. Structure of Gd2O3 films annealed at different temperature was investigated by X-ray diffraction and transmission electron microscopy. Oriented growth of (400) face of Gd2O3 has been observed when the films were deposited on amorphous substrate. The refractive index and thickness of films were determined by m-lines spectroscopy. The laser beam (λ=632.8 nm) was coupled into the film by a prism coupler and the propagation length is about 3.5 cm. Luminescence properties of europium ions doped films were measured by waveguide fluorescence spectroscopy, which shows disordered environment for Eu3+ at 400 ℃.

  2. Surface Microstructure Characterization of Sol-gel Derived Porous TiO2 Thin Films


    Porous TiO2 thin films were prepared from alkoxide solutions with and without polyethylene glycol (PEG) by sol-gel route on soda lime glass, and were characterized by atomic force microscopy (AFM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The results show that TiO2 film prepared from precursor solution without PEG is composed of spherical particles of about 100 nm and several nanometer mesoporous pores. With the increase of the amount of PEG added to the precursor solution, the diameter and the depth of the pores in the resultant films increas on the decomposition of PEG during heat-treatment, which lead to the increase of the surface roughness of the films. XRD and TEM results show that the single anatase phase is precipitated and there are some orientation effects in (101) direction.

  3. Study of optical properties of Macrophomina phaseolina impregnated sol-gel derived silica matrices.

    Sharma, Sunita; Vandana; Ghoshal, S K; Arora, Pooja; Dilbaghi, Neeraj; Chaudhury, Ashok


    In the present frame of work, Macrophomina phaseolina is encapsulated in silica matrices at various concentrations by low temperature sol-gel technique using tetraethylorthosilicate (TEOS) as precursor. The optical and photophysical properties of these samples have been studied by second harmonics of Nd:YAG laser at 532 nm. UV-visible absorption spectra of samples have been recorded and it is found that the absorption increases with increase in concentration of fungus. Further, a decrease in output transmission intensity of the laser has been observed with increase in fungus concentration. The temporal response of these samples has also been examined. The results show that the fungus concentration can be measured within approximately 15-20 min. This method of optical sensing of fungus in test sample is faster than other techniques, such as the conventional colorimetric method which takes about 1 h.

  4. Optical and morphological properties of sol gel derived titanium dioxide films

    Sharma, A. B. [Department of Physics, Nabira Mahavidyalaya, Katol-441302 (India); Sharma, S. K. [Centre for Nano Science and Engineering, Indian Institute of Science, Bangalore-560012 (India); M, Vishwas [Department of Physics, Govt. Science College, Bangalore-560067 (India); Rao, K. Narasimha [Department of Instrumentation, Indian Institute of Science, Bangalore-560012 (India)


    Titanium oxide (Titania) thin films were synthesized on different substrates via the sol-gel dip-coating method using alkoxide solution. Some selected samples were also prepared with different percentage of Lead (Pb). The influence of Pb addition in precursor sol on the optical properties of titanium dioxide thin films was studied. The optical transmittance in the visible region has increased with increase in weight percentage of lead. The refractive index was slightly decreased with Pb addition. Crystallization of these coatings was achieved through thermal annealing at temperatures above 400 °C. The structural properties and surface morphology of the crystallized coatings were studied by Scanning Electron Microscopy. Increase in average grain size from 250 nm to 350 nm with increase in Pb concentration is observed. Films were appeared to more coarse with increase in Pb addition. An increase in Pb addition resulted increase in average roughness from 12 nm to 25 nm.

  5. Sol-gel derived oxides and mixed oxides catalysts with narrow mesoporous distribution


    A novel sol-gel process for preparing oxides and mixed oxides sols from precipitation and peptization process is reported in this article. Inorganic salts are used as raw materials in this study. It is found that the amount of acid has great influence on the stability and particle diameter distribution of the precursor sols. Ultrasonic treatment is used to prepare alumina sol at room temperature. The result of 27Al NMR shows that there exist Al137+ species in the sol. By controlling the sol particles with narrow particle diameter distribution, alumina, titania and silica-alumina (SA) materials with narrow mesoporous distribution are formed by regular packing of sol particles during gelation without using any templates. The results also show that the structure and particle diameter distribution of precursor sol determine the final materials' texture.

  6. Sol-gel-derived Hybrid Conductive Films for Electro magnetic Interference (EMI) Shielding

    XIE Jiyuan; GUO Wenfeng; WANG Jianzhong


    The conductive nano-sized zinc particles were embedded in an insulating amorphous silica matrix, and the hybrid films were obtained by a sol-gel method. The stable hybrid sol solution was prepared by hydrolysis and condensation of Methyltrimethoxysilane (MTMS) with a one-step acidic catalyst process. Hybrid films were dip-coated on silicon wafer and cured at 120 ℃ for 60minutes. The structural characterization of hybrid films were investigated by means of attenuated total reflection infrared (ATR-IR) spectroscopy and X-ray diffraetion (XRD). The electrical properties of the films were examined with four-point probe. Hybrid films showed to be relatively dense, uniform and defect free. The conductivity of hybrid films was varied with the different contents of zinc nanoparticles and the thickness of the film. It was observed that there was the percolation threshold for the film's electrical properties.

  7. On the structural, magnetic and electrical properties of sol-gel derived nanosized cobalt ferrite

    Gopalan, E. Veena [Department of Physics, Cochin University of Science and Technology, Cochin 682022, Kerala (India); Joy, P.A. [Physical Chemistry Division, National Chemical Laboratory, Pune 411008 (India); Al-Omari, I.A. [Department of Physics, College of Sciences, P O Box 36, Sultan Qaboos University, PC 123 Muscat (Oman); Kumar, D. Sakthi; Yoshida, Yasuhiko [Bio-Nano Electronics Research Centre, Department of Applied Chemistry, Toyo University, Kawagoe, Saitama 350-8585 (Japan); Anantharaman, M.R., E-mail: [Department of Physics, Cochin University of Science and Technology, Cochin 682022, Kerala (India)


    Nanoparticles of cobalt ferrite were synthesized by sol gel method. These particles were structurally characterized by using X-Ray Diffraction and Transmission Electron Microscopy, High Resolution Transmission Electron Microscopy, Energy Dispersive Spectrum and Inductively Coupled Plasma Analysis and the results confirmed the formation of spherically shaped nanoparticles of cobalt ferrite having a size lying in the range of 13-14 nm. The as prepared sample was sintered at 800 deg. C and the structural, magnetic and dielectric properties were measured. The dielectric properties were studied and analyzed as a function of temperature and frequency. The ac and dc conductivity studies were carried out to delve into the conduction mechanism. The existing models based on quantum mechanical tunneling were effectively employed to explain the frequency dependent conductivity.

  8. Magnetization and Magnetocaloric Effect in Sol-Gel Derived Nanocrystalline Copper-Zinc Ferrite.

    Anwar, M S; Ahmed, Faheem; Koo, Bon Heun


    We report the sol-gel synthesis and magnetocaloric effect in nanocrystalline copper-zinc ferrite (Cu0.5Zn0.5Fe2O4). The synthesized powder was characterized by using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and magnetization measurements. The XRD results confirm the formation of single phase spinel structure. The average particle size was found to be ~58 nm. FE-SEM results suggested that the nanoparticles are agglomerated and spherical in shape. Magnetization measurement reveals that Cu0.5Zn0.5Fe2O4 nanoparticles exhibit transition temperature (Tc) above room temperature. The maximum magnetic entropy change (ΔSM)max shows interesting behaviour and was found to vary with the applied magnetic field. This nanopowder can be considered as potential material for magnetic refrigeration above room temperature.

  9. Sol-gel derived porous bioactive nanocomposites: Synthesis and in vitro bioactivity

    Shankhwar, Nisha; Kothiyal, G. P.; Srinivasan, A.


    Porous bioactive composites consisting of SiO2-CaO-Na2O-P2O5 bioactive glass-ceramic and synthetic water soluble polymer Polyvinylpyrrolidone [PVP (C6H9NO)n, MW˜40000 g/mol] have been synthesized by sol-gel route. As-prepared polymeric composites were characterized by X-ray diffraction (XRD) technique. Two major bone mineral phases, viz., hydroxyapatite [Ca10(PO4)6(OH)2] and wollastonite [calcium silicate (CaSiO3)] have been identified in the XRD patterns of the composites. Presence of these bone minerals indicates the bioactive nature of the composites. In vitro bioactivity tests confirm bioactivity in the porous composites. The flexibility offered by these bioactive polymer composites is advantageous for its application as implant material.

  10. Comparison between sol-gel derived and classic methods for the elaboration process of DSA Ta/IrO{sub 2} electrodes

    Massot, L.; Palau, P.; Savall, A.; Taxil, P. [Paul-Sabatier Univ., Toulouse (France). Chemical Engineering Lab.


    This paper investigated the oxygen evolution of inert anodes in acidic media. The electrodes were composed of a tantalum (Ta) substrate with a catalyst coating of iridium oxide (IrO{sub 2}). Two methods were used to obtain the catalyst coating: (1) a Sol-Gel derived method using iridium acetylacetonate ([CH{sub 3}COCH=COCH{sub 3}]{sub 3}Ir) dissolved in an isopropanol-acetic acid mixture, and (2) iridium chloride (IrCl{sub 4}) dissolved in an ethanol-isopropanol mixture as an iridium oxide precursor. The electrodes were then characterized and compared using thermogravimetric measurements of the precursors. Results of the study showed that the new precursor derived from the Sol-Gel method was more reactive as the IrO{sub 2}3 formation temperature was lower. A higher amount of heat generated by cracking and combustion of the organic compounds was released during the decomposition of the Sol-Gel precursor salts. The enthalpy of conversion into the oxide measured by differential sweeping calorimetry was -15580 J/g in the case of the Sol-Gel derived method and -74.7 J/g in the case of the traditional method. However, the electrodes prepared by the Sol-Gel method were not stable, and the service lives of the electrodes were 4 times less significant than those of the electrodes prepared using the other method due to the low stability of metal iridium under polarization. It was also noted that the fine catalyst particles were less stable during a gaseous evolution. Results indicated that a rise in the thermal processing temperatures may facilitate the formation of iridium oxide, but would involve a more significant oxidation of the substrate. It was concluded that the Sol-Gel method is not suitable for the preparation of Ta/IrO{sub 2} electrodes when the oxidation number of the iridium oxide precursor is 3. 3 refs., 1 tab., 1 fig.

  11. Probing the microenvironment of an oligo-(p-phenylene vinylene) derivative encapsulated in polymer-impregnated sol-gel silica matrix

    TANG Jun; DU Chuang; YU Xiaoqiang; ZHANG Guo; WANG Ce


    Polymer-impregnated silica sol-gel composite materials are hosts for organics in advanced optics application. An oligo-phenylene vinylene derivative 4,4'-(1,4-phenylene dithenylene)-bis-(N-methyl pyridinium iodide)(OPVD) was introduced to poly(hydroxyethyl methacrylate)(PHEMA)-impregnated silica composite film by the sol-gel process. By comparing the X-ray diffraction, UV-visible spectra, steady-state and time-resolved fluorescence spectra of OPVD in three solid matrices (PHEMA/silica composite film, pure PHEMA film, and pure silica film), the similar results of PHEMA/silica composite film and pure PHEMA film demonstrate that the OPVD is primarily surrounded by a PHEMA-like environment in the composite matrix. The model of such structure is presented, which is useful for further understanding and optimizing of properties of doped sol-gel materials.

  12. On the healing mechanism of sol-gel derived hybrid materials containing dynamic di-sulfide bonds

    AbdolahZadeh, M.; Esteves, A.C.C.; Van der Zwaag, S.; Garcia Espallargas, S.J.


    Sol-gel technology is increasingly being used in coatings for corrosion protection and adhesion improvement. So far, the self-healing concept in sol-gel coatings has only been approached from extrinsic healing perspective (i.e. use of nano and micro carriers of corrosion inhibitors) [1]. Despite the

  13. Sol-gel derived silica/chitosan/Fe3O4 nanocomposite for direct electrochemistry and hydrogen peroxide biosensing

    Satvekar, R. K.; Rohiwal, S. S.; Tiwari, A. P.; Raut, A. V.; Tiwale, B. M.; Pawar, S. H.


    A novel strategy to fabricate hydrogen peroxide third generation biosensor has been developed from sol-gel of silica/chitosan (SC) organic-inorganic hybrid material assimilated with iron oxide magnetic nanoparticles (Fe3O4). The large surface area of Fe3O4 and porous morphology of the SC composite facilitates a high loading of horseradish peroxidase (HRP). Moreover, the entrapped enzyme preserves its conformation and biofunctionality. The fabrication of hydrogen peroxide biosensor has been carried out by drop casting of the SC/F/HRP nanocomposite on glassy carbon electrode (GCE) for study of direct electrochemistry. The x-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) confirms the phase purity and particle size of as-synthesized Fe3O4 nanoparticles, respectively. The nanocomposite was characterized by UV-vis spectroscopy, fluorescence spectroscopy and Fourier transform infrared (FTIR) for the characteristic structure and conformation of enzyme. The surface topographies of the nanocomposite thin films were investigated by scanning electron microscopy (SEM). Dynamic light scattering (DLS) was used to determine the particle size distribution. The electrostatic interactions of the SC composite with Fe3O4 nanoparticles were studied by the zeta potential measurement. Electrochemical impedance spectroscopy (EIS) of the SC/F/HRP/GCE electrode displays Fe3O4 nanoparticles as an excellent candidate for electron transfer. The SC/F/HRP/GCE exhibited a pair of well-defined quasi reversible cyclic voltammetry peaks due to the redox couple of HRP-heme Fe (III)/Fe (II) in pH 7.0 potassium phosphate buffer. The biosensor was employed to detect H2O2 with linear range of 5 μM to 40 μM and detection limit of 5 μM. The sensor displays excellent selectivity, sensitivity, good reproducibility and long term stability.

  14. Method of making ionic liquid mediated sol-gel sorbents

    Malik, Abdul; Shearrow, Anne M.


    Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.

  15. Characterization in vitro studies and antibacterial properties on a sol-gel derived silver incorporated bioglass

    Bouhazma, S.; Chajri, S.; Khaldi, M.; Sadiki, M.; Barkai, H.; Elabed, S.; Ibnsouda Koraichi, S.; El Bali, B.; Lachkar, M.


    The SiO2-CaO, SiO2-CaO-P2O5 and SiO2-CaO-P2O5-Ag2O glass systems were synthesized by the sol-gel technique and characterized with different techniques such as X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), and Environmental Scanning Electron Microscopy (ESEM). In vitro bioactivity tests were performed in Simulated Body Fluid (SBF). The antibacterial action of 65S5Ag (65%SiO2 + 24%CaO + 6%P2O5 + 5% Ag2O) is attributed exclusively to the leaching of Ag+ ions from the glass matrix. The activity of SiO2-CaO-P2O5-Ag2O was compared with that of its binary and ternary counterpart glass system. The concentrations of Ag-bioglass, in the range of 0.05 mg/mL of culture medium, were found to inhibit the growth of these bacteria.

  16. Sol-gel derived fluor-hydroxyapatite biocoatings on zirconia substrate.

    Kim, Hae-Won; Kong, Young-Min; Bae, Chang-Jun; Noh, Yoon-Jung; Kim, Hyoun-Ee


    Fluor-hydroxyapatite (FHA) film was coated on a zirconia (ZrO(2)) substrate by a sol-gel method. An appropriate amount of F ions was incorporated into the hydroxyapatite (HA) during the preparation of the sols. The apatite phase began to crystallize after heat treatment at 400 degrees C, and increased in intensity above 500 degrees C. No decomposition was detected by X-ray diffraction analyses up to 800 degrees C, which illustrates the high thermal stability of the FHA films. The films showed a uniform and dense morphology with a thickness of approximately 1 microm after a precisely controlled heat treatment process. These FHA films adhered firmly to the zirconia substrate, representing notable adhesion strengths of approximately 70 MPa after heat treatment above 500 degrees C. The dissolution rate of the FHA coating layer varied according to the heat treatment temperature, which was closely related to the film crystallinity. The dissolution rate of the FHA film was lower than that of the HA film, suggesting the possibility of a functional gradient coating of HA and FHA. The MG63 cells seeded onto the FHA films proliferated in a similar manner to those seeded onto pure HA ceramic and a plastic control.

  17. Effect of aging temperature on formation of sol-gel derived fluor-hydroxyapatite nanoparticles.

    Joughehdoust, S; Behnamghader, A; Jahandideh, R; Manafi, S


    Synthetic hydroxyapatite (HA) has been recognized as one of the most important bone substitute materials in orthopaedics and dentistry over past few decades because of its chemical and biological similarity to the mineral phase of human bone. One solution for reduction the solubility of HA in biological environments is replacing F- by OH in HA structure and forming fluor-hydroxyapatite (FHA) solid solution. In this paper, FHA nanoparticles were successfully synthesized by a sol-gel method. Also, the influence of aging temperature on formation of FHA powder was studied. Equimolar solutions of calcium nitrate tetrahydrate, triethyl phosphite and ammonium fluoride in ethanol were used as Ca, P and F precursors. After aging at different temperatures, the synthesized powders were heat treated at 550 degrees C. The powders were investigated with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), selected area electron diffraction pattern (SAED), energy dispersive analysis of X-ray (EDAX) and zetasizer measurement. The results of XRD proved the presence of fluorapatite (FA) and HA in all samples. In addition, the formation of FHA was confirmed by FT-IR results. XRD studies also showed that the crystallites were in nanometric scale. At the same time, this result was in good agreement with the result of zetasizer analysis.

  18. Sol-gel-derived Poly(dimethylsiloxane) Enzymatic Reactor for Microfluidic Peptide Mapping

    WU, Hui-Ling; YANG, Peng-Yuan; FAN, Guo-Rong; TIAN, Yu-Ping; LU, Hao-Jie; JIN, Hong


    The silica-based poly(dimethylsiloxane) (PDMS) microfluidic enzymatic reactor was reported along with its analytical features in coupling with MALDI TOF and ESI MS. Microfluidic chip was fabricated using PDMS casting and O2-plasma techniques, and used for the preparation of enzymatic reactor. Plasma oxidation for PDMS enabled the channel wall of microfluidics to present a layer of silanol (SiOH) groups. These SiOH groups as anchors onto the microchannel wall were linked covalently with the hydroxy groups of trypsin-encapsulated sol matrix. As a result, the leakage of sol-gel matrix from the microchannel was effectively prevented. On-line protein analysis was performed with the microfluidic enzymatic reactor by attachment of stainless steel tubing electrode and replaceable tip. The success of trypsin encapsulation was investigated by capillary electrophoresis (CE) detection, and MALDI TOF and ESI MS analysis. The lab-made device provided excellent extent of digestion even at the fast flow rate of 7.0 μL/min with very short residence time of ca. 2 s. In addition, the encapsulated trypsin exhibits increased stability even after continuous use. These features are the most requisite for high-throughput protein identification.

  19. Sol-gel derived bioactive hydroxyapatite/titania composite films on Ti6Al4V

    Bing Su; Guoqing Zhang; Xudong Yu; Chengtao Wang


    The composite films consisting of the titania gel impregnated with hydroxyapatite (HAP) submicron particles were prepared on commercial Ti6Al4V plates processed by a sol-gel route. HAP powders were synthesized based on wet chemical precipitation method with Ca(NO3)2.4H2O and (NH4)2HPO4 as starting reagents. After being calcined at 900℃, HAP powders were ultrasonically scattered in ethanol to produce HAP sol. The titania sol was prepared using titanium (Ⅳ) isopropoxide {Ti[OCH(CH3)2]4} as precursor. Both the titania sol and the HAP/titania mixture were sequentially spin-coated on the substrates and calcined at various temperatures.The characteristics and mechanical adhesion of the composite films were investigated. The results show that the as-prepared films are dense, homogeneous, well-crystallized, and there is a good interfacial adhesion between the film and the substrate. The in vitro bioactivities of these films were discussed based on the analysis of the variations of Ca and P concentrations in the simulated body fluid and their surface morphologies against immersion time.

  20. Antibacterial effects of sol-gel-derived bioactive glass nanoparticle on aerobic bacteria.

    Mortazavi, V; Nahrkhalaji, M Mehdikhani; Fathi, M H; Mousavi, S B; Esfahani, B Nasr


    The aim of this work was to evaluate the antibacterial effect of bioactive glass nanopowders. The 58S, 63S, and 72S compositions were prepared via the sol-gel technique. Characterization techniques such as X-ray diffraction, transmission electron microscopy (TEM), Zetasizer, and X-ray fluorescent were used. The antibacterial activity was studied using Escherichia coli, Pseudomonas aeruginosa, Salmonella typhi, and Staphylococcus aureus. Cytotoxicity of the samples was evaluated using mouse fibroblast L929 cell line. The chemical compositions of the prepared samples were as predicted, and the particle size of the samples with an amorphous structure mainly ranged over 20-90 nm. At broth concentrations below 50 mg/mL, they showed no antibacterial activity. The 58S showed the highest antibacterial activity with the minimum bactericidal concentrations of 50 and 100 mg/mL for E. coli plus S. aureus and for P. aeruginosa, respectively. The 63S exhibited bactericidal and bacteriostatic effects on E. coli and S. aureus at concentrations of 100 and 50 mg/mL, respectively, at an minimum bactericidal concentrations of 100 mg/mL. However, 72S bioactive glass nanopowder showed no antibacterial effect. They showed no cytotoxicity. It was concluded that bioactive glass nanopowders could be considered as good candidates for the treatment of oral bone defects and root canal disinfection. (c) 2010 Wiley Periodicals, Inc. J Biomed Mater Res, 2010.

  1. Microstructural evolution of sol-gel derived ZnO thin films

    Miller, James B., E-mail: jbmiller@andrew.cmu.ed [Carnegie Mellon University, Pittsburgh, PA 15213 (United States); National Energy Technology Laboratory, US Department of Energy, Pittsburgh, PA 15236 (United States); Hsieh, Hsin-Jung [Carnegie Mellon University, Pittsburgh, PA 15213 (United States); Howard, Bret H. [National Energy Technology Laboratory, US Department of Energy, Pittsburgh, PA 15236 (United States); Broitman, Esteban [Carnegie Mellon University, Pittsburgh, PA 15213 (United States)


    Zinc oxide thin films, with thicknesses between {approx} 20 and 450 nm, were prepared by spin-coating a sol-gel precursor solution (zinc acetate dihydrate and monoethanolamine in an isopropanol solvent) onto glass substrates, followed by heat treatment at temperatures through 773 K. At 298 and 373 K, the films exhibited the structure of a lamellar ZnO precursor, Layered Basic Zinc Acetate (LBZA). At higher temperatures, LBZA released intercalated water and acetate groups and dehydroxylated to form zinc oxide nanograins with wurtzite structure, which were preferentially oriented in the c-axis direction. Both the degree of the films' c-axis orientation and the topography of their surfaces varied with heat treatment and precursor concentration. For films calcined at 773 K, a minimum of micron-scale surface wrinkles coincided with a maximum in c-axis preference at intermediate concentrations, suggesting that release of mechanical stress during densification of thicker films may have disrupted the ordering process that occurs during heat treatment.

  2. Sliding behavior of water drops on sol-gel derived hydrophobic silica films

    Latthe, Sanjay S.; Dhere, Sunetra L. [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004, Maharashtra (India); Kappenstein, Charles [University of Poitiers, Laboratory of Catalysis in Organic Chemistry, LA CCO, UMR CNRS 6503, Poitiers-86000 (France); Imai, Hiroaki [Faculty of Science and Technology, Keio University, 3-14-1, Hiyoshi, Kohoku-ku, Yokohama 223-8522 (Japan); Ganesan, V. [CSR, Indore Centre, University Campus, Khandwa Road, Indore- 452 017, Madhyapradesh (India); Rao, A. Venkateswara, E-mail: [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004, Maharashtra (India); Wagh, Pratap B.; Gupta, Satish C. [Applied Physics Division, Bhabha Atomic Research Centre (BARC), Trombay, Mumbai 400 085 (India)


    Control on the wettability of solid state materials is a classical and key issue in surface engineering. Optically transparent methyltriethoxysilane (MTES)-based silica films with water sliding angle as low as 9{sup o} were successfully prepared by two-step sol-gel co-precursor method. The emphasis is given to the effect of trimethylethoxysilane (TMES) as a co-precursor on water sliding behavior of silica films. The coating sol was prepared with molar ratio of methyltriethoxysilane (MTES), methanol (MeOH), acidic water (0.01 M, oxalic acid) and basic water (12 M, NH{sub 4}OH) kept constant at 1:12.73:3.58:3.58 respectively, and the molar ratio of TMES/MTES (M) was varied from 0 to 0.22. The static water contact angle as high as 120{sup o} and the water sliding angle as low as 9{sup o} was obtained by keeping the molar ratio (M) of TMES/MTES at 0.22. When the modified films were cured at temperature higher than 280 deg. C, the films became superhydrophilic. Further, the humidity study was carried out at a relative humidity of 90% at 30 deg. C over 60 days. We characterized the water repellent silica films by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), % of optical transmission, humidity tests and static and dynamic water contact angle (CA) measurements.

  3. Sol-gel derived ZnO as an electron transport layer (ETL) for inverted organic solar cells

    Tiwari, D. C.; Dwivedi, Shailendra Kumar; Dipak, Phukhrambam; Chandel, Tarun; Sharma, Rishi


    In this work, we present the study of the fabrication process of the sol-gel derived zinc oxide (ZnO) as an electron transport layer (ETL.). The solution processed inverted bulk heterojunction organic solar cells based on a thin film blend of poly (3-hexylthiophene 2, 5-diyl) and [6,6]-phenyl-C61-butyric acid methyl ester is prepared. ZnO thin films are annealed at different temperature to optimize the solar cell performance and their characterization for their structural and optical properties are carried out. We have observed Voc=70mV, Jsc=1.33 µA/cm2 and FF=26% from the inverted heterojunction solar cell.

  4. Characterization of the bioactive and mechanical behavior of dental ceramic/sol-gel derived bioactive glass mixtures.

    Abbasi, Zahra; Bahrololoum, Mohammad E; Bagheri, Rafat; Shariat, Mohammad H


    Dental ceramics can be modified by bioactive glasses in order to develop apatite layer on their surface. One of the benefits of such modification is to prolong the lifetime of the fixed dental prosthesis by preventing the formation of secondary caries. Dental ceramic/sol-gel derived bioactive glass mixture is one of the options for this modification. In the current study, mixtures of dental ceramic/bioactive glass with different compositions were successfully produced. To evaluate their bioactive behavior, prepared samples were immersed in a simulated body fluid at various time intervals. The prepared and soaked specimens were characterized using Fourier transform infrared spectroscopy, X-ray diffractometry and scanning electron microscopy. Since bioactive glasses have deleterious effects on the mechanical properties of dental ceramics, 3-point bending tests were used to evaluate the flexural strength, flexural strain, tangent modulus of elasticity and Weibull modulus of the specimens in order to find the optimal relationship between mechanical and bioactive properties.

  5. Regulation of cellular behaviors of fibroblasts related to wound healing by sol-gel derived bioactive glass particles.

    Xie, Weihan; Chen, Xiaofeng; Miao, Guohou; Tang, Jieying; Fu, Xiaoling


    Sol-gel derived bioactive glass (BG) holds great potential in the application of skin repair. However, the specific regulation of BG on skin cells is still unclear and demands more investigation. Herein, we synthesized sol-gel derived BGs with different compositions (60S, 70S, 80S, and 90S) and found 90S BGs (90 mol % SiO2 , 6 mol % CaO, 4 mol % P2 O5 ) exhibited the best supportiveness for the proliferation of normal human foreskin fibroblasts. Thus, 90S BG particles were used as a model to systematically study the wound healing related cellular response of fibroblasts to BGs. Time-lapse imaging revealed a promoted fibroblast motility stimulated by 90S BG particles. Results on the expression of extracellular matrix (ECM) related genes illustrated that 90S BG particles modulated the synthesis capacity for critical ECM molecules including type I collagen, type III collagen, fibronectin, and tenascin-C. Moreover, the myofibroblastic differentiation of fibroblasts was greatly inhibited by 90S BG particles. Further analysis on the intracellular signaling pathways demonstrated that 90S BG particles down-regulated the collagen synthesis and fibroblast-to-myofibroblast differentiation via TGF-β1-Smad2 signaling, evidenced by the decreased expression levels of TGF-β receptor I and its downstream effector Smad2. Our study provided a further understanding of the specific regulation of 90S BG particles on fibroblasts, which may guide the future design of BG based wound dressing and benefit the clinical application of BG particles in skin repair. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 2420-2429, 2016.

  6. The effect of heat treatment on the physical properties of sol-gel derived ZnO thin films

    Raoufi, Davood; Raoufi, Taha


    Zinc oxide (ZnO) thin films were deposited on microscope glass substrates by sol-gel spin coating method. Zinc acetate (ZnAc) dehydrate was used as the starting salt material source. A homogeneous and stable solution was prepared by dissolving ZnAc in the solution of monoethanolamine (MEA). ZnO thin films were obtained after preheating the spin coated thin films at 250 °C for 5 min after each coating. The films, after the deposition of the eighth layer, were annealed in air at temperatures of 300 °C, 400 °C and 500 °C for 1 h. The effect of thermal annealing in air on the physical properties of the sol-gel derived ZnO thin films are studied. The powder and its thin film were characterized by X-ray diffractometer (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure (JCPDS 36-1451) and show the c-axis grain orientation. Increasing annealing temperature increased the c-axis orientation and the crystallite size of the film. The annealed films are highly transparent with average transmission exceeding 80% in the visible range (400-700 nm). The measured optical band gap values of the ZnO thin films were between 3.26 eV and 3.28 eV, which were in the range of band gap values of intrinsic ZnO (3.2-3.3 eV). SEM analysis of annealed thin films has shown a completely different surface morphology behavior.

  7. Sol-Gel Derived Adsorbents with Enzymatic and Complexonate Functions for Complex Water Remediation

    Roman P. Pogorilyi


    Full Text Available Sol-gel technology is a versatile tool for preparation of complex silica-based materials with targeting functions for use as adsorbents in water purification. Most efficient removal of organic pollutants is achieved by using enzymatic reagents grafted on nano-carriers. However, enzymes are easily deactivated in the presence of heavy metal cations. In this work, we avoided inactivation of immobilized urease by Cu (II and Cd (II ions using magnetic nanoparticles provided with additional complexonate (diethylene triamine pentaacetic acid or DTPA functions. Obtained nanomaterials were characterized by Fourier transform infrared spectroscopy (FTIR, thermogravimetric analysis (TGA, and scanning electron microscopy (SEM. According to TGA, the obtained Fe3O4/SiO2-NH2-DTPA nanoadsorbents contained up to 0.401 mmol/g of DTPA groups. In the concentration range Ceq = 0–50 mmol/L, maximum adsorption capacities towards Cu (II and Cd (II ions were 1.1 mmol/g and 1.7 mmol/g, respectively. Langmuir adsorption model fits experimental data in concentration range Ceq = 0–10 mmol/L. The adsorption mechanisms have been evaluated for both of cations. Crosslinking of 5 wt % of immobilized urease with glutaraldehyde prevented the loss of the enzyme in repeated use of the adsorbent and improved the stability of the enzymatic function leading to unchanged activity in at least 18 cycles. Crosslinking of 10 wt % urease on the surface of the particles allowed a decrease in urea concentration in 20 mmol/L model solutions to 2 mmol/L in up to 10 consequent decomposition cycles. Due to the presence of DTPA groups, Cu2+ ions in concentration 1 µmol/L did not significantly affect the urease activity. Obtained magnetic Fe3O4/SiO2-NH2-DTPA-Urease nanocomposite sorbents revealed a high potential for urease decomposition, even in presence of heavy metal ions.

  8. The effect of annealing temperature on the structure and optical properties of sol-gel derived nanocrystalline cobalt aluminate spinel

    Kurajica, S., E-mail: [University of Zagreb, Faculty of Chemical Engineering and Technology, 19 Marulic Square, HR-10000 Zagreb (Croatia); Popovic, J. [Division of Materials Physics, Ruder Boskovic Institute, Bijenicka 54, Zagreb (Croatia); Tkalcec, E. [University of Zagreb, Faculty of Chemical Engineering and Technology, 19 Marulic Square, HR-10000 Zagreb (Croatia); Grzeta, B. [Division of Materials Physics, Ruder Boskovic Institute, Bijenicka 54, Zagreb (Croatia); Mandic, V. [University of Zagreb, Faculty of Chemical Engineering and Technology, 19 Marulic Square, HR-10000 Zagreb (Croatia)


    The thermal evolution of a sol-gel derived cobalt aluminate (CoAl{sub 2}O{sub 4}) of a spinel-type structure was studied. The samples were prepared by the sol-gel technique using aluminum-sec-butoxide [Al(O{sup s}Bu){sub 3}] and cobalt nitrate hexahydrate Co(NO{sub 3}){sub 2} Multiplication-Sign 6H{sub 2}O as starting materials and ethyl-acetoacetate (C{sub 6}H{sub 10}O{sub 3}) as a chelating agent. The powder precursors were annealed at various temperatures ranging from 200 to 900 Degree-Sign C. The properties of products were characterized using differential thermal analysis and thermo-gravimetric analysis (DTA/TGA), UV-vis diffuse reflectance spectroscopy (DRS) and X-ray diffraction (XRD). The UV-vis DRS spectra revealed that in samples annealed at temperatures below 700 Degree-Sign C a part of Co existed in a 3 + oxidation state. The accommodation of Co{sup 3+} in octahedral cation sites yields with a green color. Thermal treatment at higher temperatures promote the reduction of Co{sup 3+} ions to Co{sup 2+} and a change of color from green to blue, later being characteristic of Co{sup 2+} ions in tetrahedral coordination. The XRD revealed that annealing of the precursor powder at a lower temperature (500 and 600 Degree-Sign C) resulted in a crystal spinel-type phase Co{sub 2}AlO{sub 4.} Annealing at higher temperatures (700-900 Degree-Sign C) induces a reaction of Co{sub 2}AlO{sub 4} with amorphous alumina producing a phase CoAl{sub 2}O{sub 4} having a partially inverse spinel structure, with {delta} in the range of 0.198-0.260. The spinel powders obtained at all annealing temperatures were in the nanosize range. -- Graphical abstract: UV-vis DRS spectra of cobalt aluminate powders heat treated at various temperatures. Highlights: Black-Right-Pointing-Pointer Sol-gel derived spinel-type CoAl{sub 2}O{sub 4} thermal evolution was monitored. Black-Right-Pointing-Pointer Below 700 Degree-Sign C part of Co exists in 3{sup +} state (octahedral sites), yielding green

  9. Study of hafnium (IV) oxide nanoparticles synthesized by polymerized complex and polymer precursor derived sol-gel methods

    Ramos-González, R.


    This work reports the preparation and characterization of hafnium (IV) oxide (HfO2) nanoparticles grown by derived sol-gel routes that involves the formation of an organic polymeric network. A comparison between polymerized complex (PC) and polymer precursor (PP) methods is presented. For the PC method, citric acid (CA) and ethylene glycol (EG) are used as the chelating and polymerizable reagents, respectively. In the case of PP method, poly(acrylic acid) (PAA) is used as the chelating reagent. In both cases, different precursor gels were prepared and the hafnium (IV) chloride (HfCl4) molar ratio was varied from 0.1 to 1.0 for the PC method and from 0.05 to 0.5 for the PP method. In order to obtain the nanoparticles, the precursors were heat treated at 500 and 800 °C. The thermal characterization of the precursor gels was carried out by thermogravimetric analysis (TGA) and the structural and morphological characterization by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the samples obtained by both methods shows the formation of HfO2 at 500 °C with monoclinic crystalline phase. The PC method exhibited also the cubic phase. Finally, the HfO2 nanoparticles size (4 to 11 nm) was determined by TEM and XRD patterns. © (2010) Trans Tech Publications.


    T. Hlasek


    Full Text Available Although ytterbium aluminum garnets (YbAG belong to a group of promising optical materials, no physical method of thin films deposition has been described so far. In this work we present the comparison of two valuable physical deposition techniques: pulsed laser deposition and electron beam evaporation. Erbium (Er3+ doped ytterbium garnet (Er0.005Yb0.995₃Al₅O12 (Er:YbAG thin films were prepared using own sol-gel derived ceramic targets. The phase composition of the films and crystallite size were determined using X-ray diffraction. Microstructure and surface morphology were studied by scanning electron microscopy and atomic force microscopy. Deposition parameters of used methods were optimized; however, both techniques produced amorphous films with insufficient microstructure. The effect of additional annealing on the crystallinity and luminescent properties of erbium ions was studied. A pure infrared emission of Er3+ ions was observed only in samples prepared by pulsed laser deposition with subsequent annealing.

  11. Characteristic coordination structure around Nd Ions in sol-gel-derived Nd-Al-codoped silica glasses.

    Funabiki, Fuji; Kajihara, Koichi; Kaneko, Ken; Kanamura, Kiyoshi; Hosono, Hideo


    Al codoping can improve the poor solubility of rare-earth ions in silica glasses. However, the mechanism is not well understood. The coordination structure around Nd ions in sol-gel-derived Nd-Al-codoped silica glasses with different Al content was investigated by optical and pulsed electron paramagnetic resonance spectroscopies. Both tetrahedral AlO4 and octahedral AlO6 units were observed around Nd ions as ligands. The average total number of these two types of ligands for each Nd(3+) ion was ∼ 2 irrespective of Al content and was larger by 1-2 orders of magnitude than that calculated for a uniform distribution of codopant ions (∼ 0.08-0.25). With increasing Al content, AlO4 units disappeared and AlO6 units became dominant. The preferential coordination of AlOx (x = 4, 6) units to Nd ions enabled the amount of Al necessary to dissolve Nd ions uniformly in silica glass at a relatively low temperature of 1150-1200 °C to be minimized, and the conversion of AlO4 units to AlO6 units around Nd ions caused the asymmetry of the crystal field at the Nd sites to increase and the site-to-site distribution to decrease.

  12. A Comparative Study of Solvothermal and Sol-Gel-Derived Nanocrystalline Alumina Catalysts for Ethanol Dehydration

    Wannaborworn, Mingkwan; Praserthdam, Piyasan; Jongsomjit, Bunjerd


    .... Also, a commercial alumina was used for comparison purposes. The results showed that the catalytic activity depends on the properties of catalyst derived from different preparation methods and reaction temperature...

  13. Formation and prevention of fractures in sol-gel-derived thin films

    Kappert, E.J.; Pavlenko, D.; Malzbender, J.; Nijmeijer, A.; Benes, N.E.; Tsai, P.A.


    Sol–gel-derived thin films play an important role as the functional coatings for various applications that require crack-free films to fully function. However, the fast drying process of a standard sol–gel coating often induces mechanical stresses, which may fracture the thin films. An experimental

  14. The effect of post annealing treatment on the citrate sol-gel derived nanocrystalline BaFe12O19 powder: structural, morphological, optical and magnetic properties

    Brightlin, B. C.; Balamurugan, S.


    The nanocrystalline BaFe12O19 powders were obtained from citrate sol-gel combustion-derived powder upon annealing at 800-1100 °C, and explored their structural, micro-structural, optical and magnetic properties. The thermal decomposition of citrate sol-gel combustion product was verified by means of thermogravimetric and differential thermal analysis. Structural identification of the citrate sol-gel combustion powder and annealed samples were investigated by powder X-ray diffraction. Though the combustion product exhibits cubic spinel phase material, the annealed powder yields good quality nanocrystalline hexagonal BaFe12O19 phase materials. The thin plate-like flakes morphology with random particle sizes of 100-200 nm with slightly agglomerated particles of BaFe12O19 phase is analyzed by high resolution scanning electron microscopy for the good quality annealed sample. Photoluminescence emission spectrum of BaFe12O19 material reveals broad emission peak at 360 nm under the excitation wavelength of 270 nm. Interestingly, the near infrared relative reflectivity of the nanocrystalline BaFe12O19 materials obtained by citrate sol-gel synthesis method is higher than the nanocrystalline BaFe12O19 materials obtained by mechano-thermal and co-precipitation method. The present dark brown colored BaFe12O19 materials can be applied as a ceramic color pigment which includes several applications. The room temperature magnetic hysteresis loop of the annealed BaFe12O19 sample exhibits a ferromagnetic saturation magnetization, M s of 55.774 emu/g at 15 kOe.

  15. Development of beta-tricalcium phosphate/sol-gel derived bioactive glass composites: physical, mechanical, and in vitro biological evaluations.

    Hesaraki, Saeed; Safari, Mojgan; Shokrgozar, Mohammad Ali


    In this study, composites of beta-tricalcium phosphate (beta-TCP) and sol gel derived bioactive glass (10, 25, and 40 wt %) based on the SiO(2)-CaO-MgO-P(2)O(5) system were prepared and sintered at 1000-1200 degrees C. The mechanical properties were investigated by measuring bending strength, Vickers hardness and fracture toughness. Structural properties were evaluated by XRD and SEM analysis, and the biological properties were studied by soaking the samples in simulated body fluid (SBF) and in contact with osteoblastic cell for viability assay. When the samples were sintered at 1200 degrees C, the mechanical strength increased, up to 34%, by increasing the amount of bioactive glass phase. In contrast, it decreased when the samples were sintered at 1000 and 1100 degrees C. The results showed that the strength could be improved up to 56% when more firing period was used. Incorporation of the bioactive glass phase into beta-TCP increased the microhardness but did not significantly change the fracture toughness. Phase analysis revealed that beta-TCP or magnesium-substituted beta-TCP was the main crystalline phase of the composites beside some calcium silicate crystallized in the bioactive glass phase. Plenty precipitation of calcium phosphate layer onto the surfaces of the beta-TCP/bioactive glass composites soaked in SBF indicated superior bioactivity of these materials compared to pure beta-TCP without any precipitation. The ability of beta-TCP/bioactive glass composites to support the growth of human osteoblastic cells was considerably better than that of pure beta-TCP. These results may be used to indicate which compositions and processing conditions can provide appropriate materials for hard tissue regeneration.

  16. Quartz Crystal Microbalance Coated with Sol-gel-derived Thin Films as Gas Sensor for NO Detection

    S. J. O’Shea


    Full Text Available This paper presents the possibilities and properties of Indium tin oxide (ITO-covered quartz crystal as a NOx toxic gas-sensor. The starting sol-gel solution was prepared by mixing indium chloride dissolved in acetylacetone and tin chloride dissolved in ethanol (0-20% by weight. The ITO thin films were deposited on the gold electrodes of quartz crystal by spin-coating technique and subsequently followed a standard photolithography to pattern the derived films to ensure all sensors with the same sensing areas. All heat treatment processes were controlled below 500°C in order to avoid the piezoelectric characteristics degradation of quartz crystal (Quartz will lose its piezoelectricity at ~573°C due to the phase change from α to β. The electrical and structural properties of ITO thin films were characterized with Hall analysis system, TG/DTA, XRD, XPS, SEM and etc. The gas sensor had featured with ITO thin films of ~100nm as the receptor to sense the toxic gas NO and quartz crystal with frequency of 10MHz as the transducer to transfer the surface reactions (mass loading, etc into the frequency shift. A homemade setup had been employed to measure the sensor response under the static mode. The experimental results had indicated that the ITO-coated QCM had a good sensitivity for NO gas, ~12Hz/100ppm within 5mins. These results prove that the ITO-covered quartz crystals are usable as a gas sensor and as an analytical device.

  17. Controlling the degradation rate of AZ91 magnesium alloy via sol-gel derived nanostructured hydroxyapatite coating.

    Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan


    Magnesium (Mg) alloys have been introduced as new generation of biodegradable orthopedic materials in recent years since it has been proved that Mg is one of the main minerals required for osseous tissue revival. The main goal of the present study was to establish a desired harmony between the necessities of orthopedic patient body to Mg(2+) ions and degradation rate of the Mg based implants as a new class of biodegradable/bioresorbable materials. This prospect was followed by providing a sol-gel derived nanostructured hydroxyapatite (n-HAp) coating on AZ91 alloy using dip coating technique. Phase structural analysis, morphology study, microstructure characterization, and functional group identification were performed using X-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. The prepared samples were immersed in simulated body fluid in order to study the formation of apatite-like precipitations, barricade properties of the n-HAp coating, and to estimate the dosage of released Mg(2+) ions within a specified and limited time of implantation. Electrochemical polarization tests were carried out to evaluate and compare the corrosion behavior of the n-HAp coated and uncoated samples. The changes of the in vitro pH values were also evaluated. Results posed the noticeable capability of n-HAp coating on stabilizing alkalization behavior and improving the corrosion resistance of AZ91 alloy. It was concluded that n-HAp coated AZ91 alloy could be a good candidate as a type of biodegradable implant material for biomedical applications.

  18. In vitro toxicity assessment of extracts derived from sol-gel coatings on polycarbonate intended to be used in food contact applications.

    Séverin, Isabelle; Lionti, Krystelle; Dahbi, Laurence; Loriot, Catherine; Toury, Bérangère; Chagnon, Marie-Christine


    Polycarbonate is a widely used polymer in food contact applications all around the world. However, due to the potential release of Bisphenol A (BPA) during repeated washing cycles, its use becomes compromised as BPA is known for being an endocrine disruptor for rodents. In order to tackle this issue, sol-gel coatings based on organoalkoxysiloxane were developed on PC, to act as a physical barrier. To this end, two sol-gel systems based on tetraethylorthosilicate (TEOS), methyltriethoxysilane (MTES) and 3-glycidyloxypropyltriethoxysilane (GPTES), three common sol-gel precursors, were prepared. The coatings derived from the latter two systems were then studied with regards to their potential toxicity in vitro. Migration tests were performed in food simulants, and the maximal migration was obtained in ethanol 10% (v/v) for one system and in isooctane for the other one. In vitro genotoxicity was assessed with the Ames test (OECD 471) and the micronucleus assay (OECD 487), and no genotoxic effect was observed. Moreover, the estrogenic activity of the extracts was studied with a transcriptional activation assay using transient transfection in human cells; none of the extracts was found estrogenic. These negative in vitro results are highly promising for the future use of these new barrier coating formulations onto food contact materials.

  19. Hybrid Sol-Gel-Derived Films That Spontaneously Form Complex Surface Topographies.

    Destino, Joel F; Jones, Zachary R; Gatley, Caitlyn M; Zhang, Yi; Craft, Andrew K; Detty, Michael R; Bright, Frank V


    Surface patterns over multiple length scales are known to influence various biological processes. Here we report the synthesis and characterization of new, two-component xerogel thin films derived from carboxyethylsilanetriol (COE) and tetraethoxysilane (TEOS). Atomic force microscopy (AFM) reveals films surface with branched and hyper branched architectures that are ∼2 to 30 μm in diameter, that extend ∼3 to 1300 nm above the film base plane with surface densities that range from 2 to 77% surface area coverage. Colocalized AFM and Raman spectroscopy show that these branched structures are COE-rich domains, which are slightly stiffer (as shown from phase AFM imaging) and exhibit lower capacitive force in comparison with film base plane. Raman mapping reveals there are also discrete domains (≤300 nm in diameter) that are rich in COE dimers and densified TEOS, which do not appear to correspond with any surface structure seen by AFM.

  20. Effect of sol size on nanofiltration performance of a sol-gel derived microporous zirconia membrane

    Guizhi Zhu; Qian Jiang; Hong Qi; Nanping Xu


    This paper reports the effect of sol size on nanofiltration performances of sol–gel derived microporous zirconia membranes. Microstructure, pure water flux, molecular weight cut-off (MWCO) and salt retention of zirconia membranes derived from zirconia sols with different sizes were characterized. Thermal evolution, phase compo-sition, microstructure and chemical stability of unsupported zirconia membranes (powder) were determined by thermogravimetric and differential thermal analysis, X-ray diffraction, nitrogen adsorption–desorption and static solubility measurements. Results show that nanofiltration performance of zirconia membranes is highly depen-dent on sol size. The sol with an average size of 3.8 nm, which is smaller than the pore size of theγ-Al2O3 support (pore size:5–6 nm), forms a discontinuous zirconia separation layer because of excessive penetration of sol into the support. This zirconia membrane displays a MWCO value towards polyethylene glycol higher than 4000 Da. A smooth and defect-free zirconia membrane with a MWCO value of 1195 Da (pore size:1.75 nm) and relative high retention rates towards MgCl2 (76%) and CaCl2 (64%) was successfully fabricated by dip-coating the sol with an appropriate size of 8.6 nm. Zirconia sol with an average size of 12 nm exhibits colloidal nature and forms a zirconia membrane with a MWCO value of 2332 Da (pore size:2.47 nm). This promising microporous zirconia membrane presents sufficiently high chemical stability in a wide pH range of 1–12.

  1. Gas separation using sol-gel derived microporous zirconia membranes with high hydrothermal stability☆

    Li Li; Hong Qi


    A microporous zirconia membrane with hydrogen permeance about 5 × 10−8 mol·m−2·s−1·Pa−1, H2/CO2 permselectivity of ca. 14, and excellent hydrothermal stability under steam pressure of 100 kPa was fabricated via polymeric sol–gel process. The effect of calcination temperature on single gas permeance of sol–gel derived zirconia membranes was investigated. Zirconia membranes calcined at 350 °C and 400 °C showed similar single gas permeance, with permselectivities of hydrogen towards other gases, such as oxygen, nitrogen, methane, and sulfur hexafluoride, around Knudsen values. A much lower CO2 permeance (3.7 × 10−9 mol·m−2·s−1·Pa−1) was observed due to the interaction between CO2 molecules and pore wall of membrane. Higher calcination tem-perature, 500 °C, led to the formation of mesoporous structure and, hence, the membrane lost its molecular siev-ing property towards hydrogen and carbon dioxide. The stability of zirconia membrane in the presence of hot steam was also investigated. Exposed to 100 kPa steam for 400 h, the membrane performance kept unchanged in comparison with freshly prepared one, with hydrogen and carbon dioxide permeances of 4.7 × 10−8 and~3 × 10−9 mol·m−2·s−1·Pa−1, respectively. Both H2 and CO2 permeances of the zirconia membrane de-creased with exposure time to 100 kPa steam. With a total exposure time of 1250 h, the membrane presented hydrogen permeance of 2.4 × 10−8 mol·m−2·s−1·Pa−1 and H2/CO2 permselectivity of 28, indicating that the membrane retains its microporous structure.

  2. On the thermal and photochemical stabilities of photochromic spirooxazine dyes encapsulated in Ormocer matrices derived by sol-gel processing

    Hou, Lisong; Hoffmann, Bernd; Mennig, Martin; Schmidt, Helmut K.


    Spiroindolinonaphthoxazine (abbreviated as SO), a most promising class of photochromic dyes due to their better photochromic response to UV irradiation (e.g. sunlight), higher fading rate of the coloured form and higher photofatigue resistance, is incorporated into Ormocer matrices synthesized by the sol-gel route aiming to achieve some application prospects. As for all technical applications the stability of the martials as a function of time and /or under certain harsh circumstances must be...

  3. Stimuli-Triggered Sol-Gel Transitions of Polypeptides Derived from α-Amino Acid N-Carboxyanhydride (NCA) Polymerizations.

    He, Xun; Fan, Jingwei; Wooley, Karen L


    The past decade has witnessed significantly increased interest in the development of smart polypeptide-based organo- and hydrogel systems with stimuli responsiveness, especially those that exhibit sol-gel phase-transition properties, with an anticipation of their utility in the construction of adaptive materials, sensor designs, and controlled release systems, among other applications. Such developments have been facilitated by dramatic progress in controlled polymerizations of α-amino acid N-carboxyanhydrides (NCAs), together with advanced orthogonal functionalization techniques, which have enabled economical and practical syntheses of well-defined polypeptides and peptide hybrid polymeric materials. One-dimensional stacking of polypeptides or peptide aggregations in the forms of certain ordered conformations, such as α helices and β sheets, in combination with further physical or chemical cross-linking, result in the construction of three-dimensional matrices of polypeptide gel systems. The macroscopic sol-gel transitions, resulting from the construction or deconstruction of gel networks and the conformational changes between secondary structures, can be triggered by external stimuli, including environmental factors, electromagnetic fields, and (bio)chemical species. Herein, the most recent advances in polypeptide gel systems are described, covering synthetic strategies, gelation mechanisms, and stimuli-triggered sol-gel transitions, with the aim of demonstrating the relationships between chemical compositions, supramolecular structures, and responsive properties of polypeptide-based organo- and hydrogels.

  4. A new precursor for the immobilization of enzymes inside sol-gel-derived hybrid silica nanocomposites containing polysaccharides.

    Shchipunov, Yurii A; Karpenko, Tat'yana Yu; Bakunina, Irina Yu; Burtseva, Yuliya V; Zvyagintseva, Tat'yana N


    Tetrakis(2-hydroxyethyl) orthosilicate (THEOS) introduced by Hoffmann et al. (J. Phys. Chem. B., 106 (2002) 1528) was first used to prepare hybrid nanocomposites containing various polysaccharides and immobilize enzymes in these materials. Two different types of O-glycoside hydrolyses (EC3.2.1), 1-->3-beta-D-glucanase LIV from marine mollusk Spisula sacchalinensis and alpha-D-galactosidase from marine bacterium Pseudoalteromonas sp. KMM 701, were taken for the immobilization. To reveal whether the polysaccharide inside the hybrid material influences the enzyme entrapment and functioning, negatively charged xanthan, cationic derivative of hydroxyethylcellulose and uncharged locust bean gum were examined. The mechanical properties of these nanocomposites were characterized by a dynamic rheology and their structure by a scanning electron microscopy. It was found that 1-->3-beta-D-glucanase was usually immobilized without the loss of its activity, while the alpha-D-galactosidase activity in the immobilized state depended on the polysaccharide type of material. An important point is that the amount of immobilized enzymes was small, comparable to their content in the living cells. It was shown by the scanning electron microscopy that the hybrid nanocomposites are sufficiently porous that allows the enzymatic substrates and products to diffuse from an external aqueous solution to the enzymes, whereas protein molecules were immobilized firmly and not easily washed out of the silica matrix. A sharp increase of the enzyme lifetime (more than a hundred times) was observed after the immobilization. As established, the efficient entrapment of enzymes is caused by few advantages of new precursor over the currently used TEOS and TMOS: (i) organic solvents and catalysts are not needed owing to the complete solubility of THEOS in water and the catalytic effect of polysaccharides on the sol-gel processes; (ii) the entrapment of enzymes can be performed at any pH which is suitable

  5. Mapping Nanoscale Domains in a Sol-Gel-Derived (Pb, La) (Zr, Ti)O3 Thin Film Using Atomic Force Microscopy

    巴龙; 舒剑; 孙平; 陆祖宏


    Local polarization of a sol-gel-derived (Pb,La)(Zr, Ti)O3 thin film is studied from its piezoelectric response measured by using atomic force microscopy. Topographic and piezoelectric images show that the domain sizes of spontaneous polarization and grain sizes are both within the range of tens to hundreds of nanometres. Nanosized domain arrays have been written in an unpoled region to realize data storage by applying pulse voltage. The results show that the domain sizes grow exponentially when the pulse duration increases.

  6. Effect of heat treatment and additives on the photochromic and mechanical properties of sol-gel derived photochromic coatings containing spirooxazine

    Hou, Lisong; Hoffmann, Bernd; Schmidt, Helmut K.; Mennig, Martin


    The experimental results on the photochromic and mechanical properties of coatings containing 1,3-dihydro-1,3,3-trimethylspiro[2H-indole-2,3''(3H)-naphth(2,1-b)(1,4) oxazine] (SO) derived from 3-glycidyl-oxypropyltrimethoxysilane (GPTMS), bisphenol A (BPA) and 1-methylimidazole (MI) by sol-gel processing are presented. It is shown that heat treatment temperature is a conflicting factor to the photochromic intensity (ΔA0), photostability and abrasion resistance of the photochromic coatin...

  7. Viscoelastic Properties and Bioactivity of Sol-Gel Derived Gelatin-Silicate Composites: Effects of the Incorporated Ca2+ Ions


    Several gelatin-silicate composites, with or without incorporation of Ca2+ ions, were synthesized through sol-gel processing starting from gelatin and 3-(glycidoxypropyl) trimethoxysilane. The structure around the Si atoms was similar for all the samples. The measurement of viscoelastic properties indicated that the glass transition temperature and activation energy decreased with the incorporation of Ca2+ ions. The Ca2+ ion-containing composites were bioactive as they spontaneously deposited apatite when soaked in a simulated body fluid of the Kokubo recipe.

  8. Fabrication of regular TiO2 nanoporous films derived by combining nanoimprint technique with sol-gel method.

    Zhong, Peng; Que, Wenxiu; Zhang, Jin


    In this paper, honeycomb-like regular TiO2 nanoporous films deposited on different substrates including ITO glass and silicon wafer are fabricated by combining a nanoimprint technique with a sol-gel method. A novel soft polymer mold containing a thin layer of polymethylmethacrylate and a thicker layer of polydimethylsiloxane, which is obtained from an anodic aluminum oxide template, is carried out for the nanoimprint process. TiO2 precursor solution prepared by the sol-gel processing is used as the nanoimprinted material. After imprinting, the polydimethylsiloxane back layer is easily peeled off before the polymethylmethacrylate mold is chemically removed to avoid any demolding problem. The SEM images show that the honeycomb-like regular nanostructure of the initial anodic aluminum oxide template can be preserved completely on TiO2 via this method, and the XRD results indicate that there is a crystalline transition from amorphous to anatase of TiO2 after 450 degrees C heat treatment.

  9. Preparation of a sol-gel-derived carbon nanotube ceramic electrode by microwave irradiation and its application for the determination of adenine and guanine

    Abbaspour, Abdolkarim, E-mail: [Department of Chemistry, College of Sciences, Shiraz University, Shiraz, Fars 71456-85464 (Iran, Islamic Republic of); Ghaffarinejad, Ali [Department of Chemistry, College of Sciences, Shiraz University, Shiraz, Fars 71456-85464 (Iran, Islamic Republic of)


    In this study, microwave irradiation was used for the fast preparation (min) of a sol-gel-derived carbon nanotube ceramic electrode (MW-CNCE). For confirmation of the preparation of the ceramic by MW irradiation, Fourier transform infrared, X-ray diffraction spectra and scanning electron microscopy images of the produced ceramic were compared with those of conventional ceramic (which is produced by drying the ceramic in air for 48 h). The electrochemical behavior of MW-CNCE in nicotinamide adenine dinucleotide, L-cysteine, adenine and guanine was compared with that of a conventional sol-gel-derived carbon nanotube ceramic electrode (CNCE). In all systems, similar peak potentials and lower background currents were obtained with respect to CNCE. Finally, the MW-CNCE was used for the simultaneous determination of adenine and guanine using differential pulse voltammetry. The linear ranges of 0.1-10 and 0.1-20 muM were obtained for adenine and guanine, respectively. These results are comparable with some modified electrodes that have recently been reported for the determination of adenine and guanine, with the advantage that the proposed electrode did not contain modifier. In addition, the proposed electrode was successfully used for the oxidation of adenine and guanine in DNA, and the detection limit for this measurement was 0.05 mug mL{sup -1} DNA.

  10. Nanocrystal/sol-gel nanocomposites

    Petruska, Melissa A.; Klimov, Victor L.


    The present invention is directed to solid composites including colloidal nanocrystals within a sol-gel host or matrix and to processes of forming such solid composites. The present invention is further directed to alcohol soluble colloidal nanocrystals useful in formation of sol-gel based solid composites.

  11. Microstructural changes in NiFe{sub 2}O{sub 4} ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

    Chauhan, Lalita, E-mail:; Sreenivas, K. [Department of Physics & Astrophysics, University of Delhi, Delhi-110007 (India); Bokolia, Renuka


    Structural properties of Nickel ferrite (NiFe{sub 2}O{sub 4}) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe{sub 2}O{sub 4} powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe{sub 2}O{sub 4} ceramics with a uniform microstructure and a large grain size.

  12. Spectroscopic studies of triethoxysilane sol-gel and coating process.

    Li, Ying-Sing; Ba, Abdul


    Silica sol-gels have been prepared under different conditions using triethoxysilane (TES) as precursor. The prepared sol-gels have been used to coat aluminum for corrosion protection. Vibrational assignments have been made for most vibration bands of TES, TES sol-gel, TES sol-gel-coated aluminum and xerogel. It has been noticed that air moisture may have helped the hydrolysis of the thin coating films. Xerogels have been obtained from the sol-gel under different temperature conditions and the resulting samples have been characterized by using infrared and Raman spectroscopic methods. IR data indicate that the sol-gel process is incomplete under the ambient conditions although an aqueous condition can have slightly improved the process. Two nonequivalent silicon atoms have been identified from the collected 29Si NMR spectra for the sol-gel, supporting the result derived from the IR data. The frequency of Si-H bending vibration has been found to be more sensitive to the skeletal structure than that of the Si-H stretching vibration. A higher temperature condition could favor the progression of hydrolysis and condensation. A temperature higher than 300 degrees C would cause sample decomposition without seriously damaging the silica network. From infrared intensity measurements and thermo-gravimetric analyses, the fractions of incomplete hydrolysis and condensation species have been estimated to be 4% and 3%, respectively. Electrochemical data have shown that the sol-gel coating significantly improves the corrosion protection properties of aluminum.

  13. Influence of Eu(3+) doping content on antioxidant properties of Lu2O3 sol-gel derived nanoparticles.

    Olvera Salazar, Arturo; García Hernández, Margarita; López Camacho, Perla Yolanda; López Marure, Arturo; Reyes de la Torre, Adriana Isabel; Morales Ramírez, Ángel de Jesús; Hernández Santiago, Felipe; Aguilera Vázquez, Luciano


    This paper presents the synthesis of pure and europium-doped lutetium oxide (Lu2O3) powders prepared by sol-gel method. The influence of europium ion concentration into Lu2O3 nanocrystallites was investigated for first time in an in vitro system using a modified ABTS radical cation decolorization assay to determine the antioxidant activity. The crystalline structure of Lu2O3 and Eu:Lu2O3 powders was elucidated by XRD obtaining cubic phase in all system without secondary products in accordance with FT-IR results. By TEM and Scherrer equation, it was determined that Lu2O3 and Eu:Lu2O3 powders presented nearly spherical particle morphology with crystallites sizes in the range of 8 to 13nm. The antioxidant assays results revealed that europium ion enhance Lu2O3 powders antioxidant properties, showing that 12.5mol% of europium is sufficient to reach its maximum capacity.

  14. Sol-gel-derived lead-magnesium-niobium titanate thin films for ultrahigh-value capacitor applications

    Copuroglu, M; O' Brien, S; Winfield, R [Tyndall National Institute, Advanced Materials and Surfaces Group, Lee Maltings, Prospect Row, Cork (Ireland); Malic, B; Kuznik, B; Kosec, M [Jozef Stefan Institute, Electronic Ceramics Department, Jamova 39, 1000 Ljubljana (Slovenia); Zhu, X; Defay, E, E-mail: mehmet.copuroglu@tyndall.i [CEA, LETI, MINATEC, 17 Rue des Martyrs, F38054 Grenoble Cedex 9 (France)


    A Pb(Mg{sub 0.33}Nb{sub 0.67}){sub 0.65}Ti{sub 0.35}O{sub 3} material system was synthesized by the sol-gel method; thin films were deposited via the spin-coating technique, and processed using the rapid thermal annealing. Effects of preparation parameters, such as annealing temperature and atmosphere, on the phase composition, microstructure and electrical properties were identified. Morphologically uniform and crack-free films were obtained. Among the obtained films, the highest k value was found to be 1425 for the 380 nm thick film that was annealed at 750 deg. C in O{sub 2} indicating the suitability of this material system for ultrahigh-value capacitor applications.

  15. Effect of Annealing Conditions on Properties of Sol-Gel Derived Al-Doped ZnO Thin Films

    GAO Mei-Zhen; ZHANG Feng; LIU Jing; SUN Hui-Na


    Transparent conductive Al-doped ZnO (AZO) thin films are prepared on normal glass substrates by the sol-gel spin coating method.The effects of drying conditions,annealing temperature and cooling rate on the structural,electrical and optical properties of AZO films are investigated by x-ray diffraction,scanning electron microscopy,the four-point probe method and UV- VIS spectrophotometry,respectively.The deposited films show a hexagonal wurtzite structure and high preferential c-axis orientation.As the drying temperature increases from 100℃ to 300℃ the resistivity of AZO films decreases dramatically.In contrast to the annealed films cooled in a furnace and in air,the resistivity of the annealed film which is cooled at -15℃ is greatly reduced.Increasing the cooling rate dramatically increases the electrical conductivity of AZO films.

  16. Effect of sol-age on the surface and optical properties of sol-gel derived mesoporous zirconia thin films

    Manish Kumar


    Full Text Available Mesoporous ZrO2 thin films have been deposited by a modified sol-gel dip coating technique using HCl as catalyst. Effects of sol-age on the surface and on the optical properties are studied. Transmission electron micrographs of the films reveal the pore dimensions in mesoporous regime. A strong correlation in surface topography with sol-age has been observed where increase in sol-age induces a systematic enhancement in the value of root mean square roughness of the films. Optical study shows that deposited films have high transmittance and an enhancement of 5.6 times in porosity in films prepared with sol-age of 10 days with respect to that of 1 day. Band gap estimation by Tauc's plots of films is observed to 5.74 eV, which shows invariance with the sol-age.

  17. Effects of lithium doping on microstructure, electrical properties, and chemical bonds of sol-gel derived NKN thin films

    Lin, Chun-Cheng; Chen, Chan-Ching; Weng, Chung-Ming; Chu, Sheng-Yuan; Hong, Cheng-Shong; Tsai, Cheng-Che


    Highly (100/110) oriented lead-free Lix(Na0.5K0.5)1-xNbO3 (LNKN, x = 0, 0.02, 0.04, and 0.06) thin films are fabricated on Pt/Ti/SiO2/Si substrates via a sol-gel processing method. The lithium (Li) dopants modify the microstructure and chemical bonds of the LNKN films, and therefore improve their electrical properties. The optimal values of the remnant polarization (Pr = 14.3 μC/cm2), piezoelectric coefficient (d33 = 48.1 pm/V), and leakage current (Poole-Frenkel emission effect under high electric fields.

  18. Structural characterization and magnetic properties of sol-gel derived ZnxFe3-xO4 nanoparticles

    Petrova, E.; Kotsikau, D.; Pankov, V.


    Nanocrystalline ZnxFe3-xO4 solid solutions (with x=0, 0.18, 0.45, 1) with crystallite sizes of 5-10 nm, specific surface of about 180 m2/g were synthesized via an inorganic variant of the sol-gel approach. The composition and structure of the formed nanoparticles were examined with the help of powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma atomic emission spectrometry and Fourier transform infrared spectroscopy. Hysteresis loops recorded for the samples indicate their ferromagnetic behavior at 5 K and superparamagnetic behavior at 300 K. The highest maximum magnetization of 59 emu/g at room temperature corresponds to Zn0.18Fe2.82O4 composition, and at 5 K to Zn0.45Fe2.55O4 (86 emu/g). The saturation magnetization of the pure magnetite was measured to be respectively 62 and 49 emu/g.

  19. Dependence Properties of Sol-Gel Derived CuO@SiO2 Nanostructure to Diverse Concentrations of Copper Oxide

    V. Homaunmir


    Full Text Available Various concentrations of copper oxide were embedded into silica matrix of xerogel forms using copper source Cu(NO32·3H2O. The xerogel samples were prepared by hydrolysis and condensation of tetraethyl orthosilicate (TEOS with determination of new molar ratios of the components by the sol-gel method. In this paper, three samples of copper oxide were doped into silica matrices using different concentrations. We obtained 10, 20, and 30 wt.% of copper oxide in silica matrices labeled as A, B, and C, respectively. The absorption and transmittance spectra of the gel matrices were treated at different concentrations by Uv-vis spectrophotometer. Quantities of water and transparency in the silica network change the spectral characteristics of Cu2+ ions in the host silica. Absorption spectra of the samples heated to higher concentration complete the conversion of Cu2+ ions to Cu+ ions. The effects of concentration of copper oxide were characterized by X-ray diffraction (XRD patterns, and the transmission electron microscope (TEM micrographs. Also, textural properties of samples were studied by surface area analysis (BET method at different concentrations.

  20. Biocompatibility and Corrosion Protection Behaviour of Hydroxyapatite Sol-Gel-Derived Coatings on Ti6Al4V Alloy

    Amir A. El Hadad


    Full Text Available The aim of this work was to prepare hydroxyapatite coatings (HAp by a sol-gel method on Ti6Al4V alloy and to study the bioactivity, biocompatibility and corrosion protection behaviour of these coatings in presence of simulated body fluids (SBFs. Thermogravimetric/Differential Thermal Analyses (TG/DTA and X-ray Diffraction (XRD have been applied to obtain information about the phase transformations, mass loss, identification of the phases developed, crystallite size and degree of crystallinity of the obtained HAp powders. Fourier Transformer Infrared Spectroscopy (FTIR has been utilized for studying the functional groups of the prepared structures. The surface morphology of the resulting HAp coatings was studied by Scanning Electron Microscopy (SEM. The bioactivity was evaluated by soaking the HAp-coatings/Ti6Al4V system in Kokubo’s Simulated Body Fluid (SBF applying Inductively Coupled Plasma (ICP spectrometry. 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide (MTT and Alamar blue cell viability assays were used to study the biocompatibility. Finally, the corrosion behaviour of HAp-coatings/Ti6Al4V system was researched by means of Electrochemical Impedance Spectroscopy (EIS. The obtained results showed that the prepared powders were nanocrystalline HAp with little deviations from that present in the human bone. All the prepared HAp coatings deposited on Ti6Al4V showed well-behaved biocompatibility, good bioactivity and corrosion protection properties.

  1. Electrical and Pyroelectric Properties of Sol-Gel Derived (Pb, Ca)TiO3 Thin Films with Various Orientations

    唐新桂; 丁爱丽; 王丽华


    (Pb0.76Ca0.24)TiO3(PCT)thin films with various orientations were grown on Pt/Ti/SiO2/Si substrates by using a sol-gel process and by controlling the temperature of heat-treatment.The PCT thin films with(100)and random orientation showed well-saturated hysteresis loops at an applied field of 800kV/cm,with remanent polarization and coercive electric field of 23.6 μC/cm2 and 225 k V/cm,17.8 μC/cm2 and 195 k V/cm,respectively.For highly(100)-and random-oriented PCT films,the dielectric constant and dielectric loss values of these films are 121 and 0.016,121 and 0.024 at 1 kHz,respectively.The pyroelectric coefficients p of the PCT thin films are measured by a dynamic technique.At room temperature,the p values and figures of merits of the highly(100)-and random-oriented PCT films are 185μC/m2K and 1.79 × 10-5Pa-0.5,176μC/m2K and 1.39 × 10-5Pa-0.5,respectively.


    Seyed Mohsen Latifi


    Full Text Available Ca ion release from bioactive biomaterials could play an important role in their bioactivity and osteoconductivity properties. In order to improve hydroxyapatite (HA dissolution rate, in situ apatite-silica nanocomposite powders with various silica contents were synthesized via sol-gel method and mechanisms controlling the Ca ion release from them were investigated. Obtained powders were characterized by X-ray diffraction (XRD and transmission electron spectroscopy (TEM techniques, acid dissolution test, and spectroscopy by atomic absorption spectrometer (AAS. Results indicated the possible incorporation of (SiO44- into the HA structure and tendency of amorphous silica to cover the surface of HA particles. However, 20 wt. % silica was the lowest amount that fully covered HA particles. All of the nanocomposite powders showed more Ca ion release compared with pure HA, and HA - 10 wt. % silica had the highest Ca ion release. The crystallinity, the crystallite size, and the content of HA, along with the integrity, thickness, and ion diffusion possibility through the amorphous silica layer on the surface of HA, were factors that varied due to changes in the silica content and were affected the Ca ion release from nanocomposite powders.

  3. Ferroelectric properties of sol-gel derived Nd-doped SrBi4Ti4O15 thin films

    FAN Suhua; ZHANG Fengqing; WANG Peiji; REN Yanxia


    Neodymium-doped strontium bismuth titanate (SrBi4-xNdxTi4O15) ferroelectric thin films were fabricated using the sol-gel method on Pt/Ti/SiO2/Si substrates. The influence of Nd content on the microstructure and ferroelectric properties of SrBi4-xNdxTi4O15 thin films were systematically studied. The results indicated that the SrBi3.88Nd0.12Ti4O15 (SBNT0.12) thin films had better ferroelectric properties, with a remanent polarization of (2Pr) of 34.3 μC/cm2 and a coercive field (2Ec) of 220 kV/cm. This could be attributed to the fact that SBNT0.12 ferroelectric thin films consisted of more and larger ball-like grains, approximately 150-200 nm, with structure distortion, which greatly contributed to the improvement of the ferroelectric properties of the films. Furthermore, the film exhibited a good fatigue resistant property. The value of 2Pr after 1010 switching cycles did not change significantly. The SrBi3.88Nd0.12Ti4O15 films were promising candidates for the application of FeRAMs.

  4. Structural, Morphological and Antibacterial Investigation of Ag-Impregnated Sol-Gel-Derived 45S5 NanoBioglass Systems.

    Durgalakshmi, D; Balakumar, S; Raja, C Ashok; George, Rani P; Mudali, U Kamachi


    An increasing percentage of ageing population requires 30-year survivability of orthopedic devices that is not possible with the current bioinert materials, having a maximum of 15-year survivability. To satisfy this growing need, a shift is needed from replacement of tissues to regeneration of tissues. This is highly possible through the use of silica-bioactive glasses. However, a failure of implant can occur due to infections even by using such materials. Advances in using silver for antibacterial applications have been commercialized. However, higher concentrations of silver also lead to toxic effects. In this study, nanoBioglass 45S5 (NBG) and Ag-NBG were synthesized by using sol-gel method followed by solution-phase method, respectively. The bioactive crystals such as Na2Ca2Si3O9, CaCO3, and AgPO3, very much needed in the field of bone tissue engineering and in antibacterial strategies, were obtained in the NBG Matrix. The morphological investigation of NBG with 1 mM Ag+ concentrations shows the nanospikes arrangement of size 30-40 nm with spherical porous structure of size 10-20 nm, which supports the formation of collagen molecular fibrils on the surface of NBG matrices and enhances osseointegration. Both gram-positive and gram-negative strains show higher antibacterial activity for nanoBioglass with 1 mM Ag+ concentration.

  5. Sol-gel derived Al-Ga co-doped transparent conducting oxide ZnO thin films

    Serrao, Felcy Jyothi, E-mail: [Department of studies in Physics, Mangalore University, Mangalagangothri 574199 (India); Department of Physics, Karnataka Government Research centre SCEM, Mangalore, 575007 (India); Sandeep, K. M.; Bhat, Shreesha; Dharmaprakash, S. M. [Department of studies in Physics, Mangalore University, Mangalagangothri 574199 (India)


    Transparent conducting ZnO doped with Al, Ga and co-doped Al and Ga (1:1) (AGZO) thin films were grown on glass substrates by cost effective sol-gel spin coating method. The XRD results showed that all the films are polycrystalline in nature and highly textured along the (002) plane. Enhanced grain size was observed in the case of AGZO thin films. The transmittance of all the films was more than 83% in the visible region of light. The electrical properties such as carrier concentration and mobility values are increased in case of AGZO compared to that of Al and Ga doped ZnO thin films. The minimum resistivity of 2.54 × 10{sup −3} Ω cm was observed in AGZO thin film. The co-doped AGZO thin films exhibited minimum resistivity and high optical transmittance, indicate that co-doped ZnO thin films could be used in transparent electronics mainly in display applications.

  6. Preparation and Characterization of Sol-Gel Derived Au Nanoparticle Dispersed Y2O3:Eu Films

    Guo Hai; Zhang Weiping; Dong Ning; Lou Liren; Yin Min; Tillement O; Mugnier J; Bernstein E; Brevet P F


    Gold nanoparticles dispersed Y2O3 films were prepared through a sol-gel method by using yttrium acetate and Au nanoparticles colloid as precursors. The films were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV-VIS absorption spectra. XRD patterns and TEM images of Y2O3+Au films give the same results on structure and particle size as that of pure Y2O3 films. The surface plasma resonance (SPR) of Au nanoparticles in Y2O3+Au film was observed around 550 nm in the absorption spectrum and its position shifts to red with increasing annealing temperature is caused by the increase of dielectric constant of Y2O3 matrix and the size of Au nanoparticles. The second and third order nonlinear optical effects of Y2O3+Au films were also observed. The photoluminescent properties of Y2O3:Eu+Au films were investigated and results indicate that there exist an energy transfer from Eu3+ to Au nanoparticles and this energy transfer decreases the emission of Eu3+ in Y2O3:Eu+Au film.

  7. Effects of lithium doping on microstructure, electrical properties, and chemical bonds of sol-gel derived NKN thin films

    Lin, Chun-Cheng [Department of Electrical Engineering, National Cheng Kung University, Tainan 701, Taiwan (China); Department of Mathematic and Physical Sciences, R.O.C. Air Force Academy, Kaohsiung 820, Taiwan (China); Chen, Chan-Ching; Weng, Chung-Ming [Department of Electrical Engineering, National Cheng Kung University, Tainan 701, Taiwan (China); Chu, Sheng-Yuan, E-mail: [Department of Electrical Engineering, National Cheng Kung University, Tainan 701, Taiwan (China); Center for Micro/Nano Science and Technology, National Cheng Kung University, Tainan 701, Taiwan (China); Hong, Cheng-Shong [Department of Electronic Engineering, National Kaohsiung Normal University, Kaohsiung 802, Taiwan (China); Tsai, Cheng-Che [Department of Digital Game and Animation Design, Tung-Fang Design University, Kaohsiung 829, Taiwan (China)


    Highly (100/110) oriented lead-free Li{sub x}(Na{sub 0.5}K{sub 0.5}){sub 1−x}NbO{sub 3} (LNKN, x = 0, 0.02, 0.04, and 0.06) thin films are fabricated on Pt/Ti/SiO{sub 2}/Si substrates via a sol-gel processing method. The lithium (Li) dopants modify the microstructure and chemical bonds of the LNKN films, and therefore improve their electrical properties. The optimal values of the remnant polarization (P{sub r} = 14.3 μC/cm{sup 2}), piezoelectric coefficient (d{sub 33} = 48.1 pm/V), and leakage current (<10{sup −5} A/cm{sup 2}) are obtained for a lithium addition of x = 0.04 (i.e., 4 at. %). The observation results suggest that the superior electrical properties are the result of an improved crystallization, a larger grain size, and a smoother surface morphology. It is shown that the ion transport mechanism is dominated by an Ohmic behavior under low electric fields and the Poole-Frenkel emission effect under high electric fields.

  8. Structural studies of the NaCaPO 4-SiO 2 sol-gel derived materials

    Sitarz, M.; Rokita, M.; Handke, M.; Galuskin, E.


    Structural studies of the NaCaPO 4-SiO 2 materials have been carried out. Amorphous materials from this system, after controlled crystallization process, can be used as potential nanomaterials. Structural studies of nanomaterials are of fundamental importance in view their future applications. Materials of different [PO 4] 3-/[SiO 4] 4- tetrahedra proportion have been prepared. Na + and Ca 2+ cations have compensated the negative charge of the lattice. Amorphous and crystalline materials have been obtained by sol-gel as well as conventional melting methods. The XRD phase identification has enabled amorphous and crystalline materials identification and suggests the separation of phosphorus and silicate crystalline phases. The obtained materials were examined using the electron scanning microscope and EDX spectrometer. Analysis of electron scanning microscope maps shows considerable inhomogeneity of crystalline samples. Fluctuations in ions distribution, in case of amorphous materials, have been noted too. DTA investigations have enabled to find the probable characteristic temperatures of glass crystallization. Detailed infrared spectroscopy measurements have been carried out. The spectra of obtained materials have been compared with the spectra of cristobalite. Spectroscopic studies confirm the inhomogeneity of materials.

  9. sol-gel

    Humberto A. Monreal


    Full Text Available En este trabajo sintetizamos nanocilindros de dióxido de titanio de 30 a 400 nm por medio de ADN del plásmido pBR322 de 4,362 pares de bases y el uso de isopropóxido de titanio como precursor por medio del proceso sol-gel. Los geles resultantes fueron calcinados y los polvos caracterizados por medio de Microscopio Electrónico de Barrido (MEB, Espectroscopía de Energía Dispersiva, Microscopio Electrónico de Transmisión (MET y Difracción de Rayos X. Los resultados muestran que la síntesis in vitro de nanorods en presencia de ADN, puede ser activada. Muchas otras moléculas sintéticas pueden producirse por medio del uso de sistemas orgánicos, es así como reportamos la síntesis de híbridos hechos de ácidos nucleicos en materiales inorgánicos que pueden tener diversas aplicaciones en sistemas catalíticos, biomateriales y materiales nanoestructurados.

  10. Organic/inorganic hybrid coatings for anticorrosion

    He, Zhouying

    Compared to organic coatings, organic-inorganic hybrid coatings can potentially improve the anticorrosion performance. The organic phase provides the excellent mechaincal and barrier properties while the inorganic phase acts as an adhesion promoter and corrosion inhibitor. Despite that many studies on alkoxylsilane-based hybrid coatings have been developed and studied, their weatherability and anticorrosion performance has been rarely evaluated. On the other hand, organic-inorganic hybrid coatings based on mixed sol-gel precursors have received much less attention compared to alkoxylsilane-based hybrid coatings. In the first part, polyurethane hybrid coatings with a unique hybrid crosslinked structure as an improved unicoat were successfully prepared. The effect of polyesters on physical properties of the hybrid coatings was studied. Polyurethane coatings derived from cycloaliphatic polyester show comparable properties than those derived from the commercially viable aromatic polyester. Introducing the polysiloxane part into the polyurethane coatings enhanced the crosslinking density, Tg, mechanical properties, and general coating properties. The increased adhesion between the hybrid coating and the substrate make the hybrid coating a good candidate for anticorrosion application, which is shown by electrochemical impedance spectroscopy (EIS). The degradation mechanism of the polyurethane/polysiloxane hybrid coatings under various weathering conditions was shown to be the scission of the urethane and ester groups in the organic phase along with reorganizing and rearranging of the inorganic phase. The anticorrosion performance of the cycloaliphatic hybrid was much better than that of aromatic based hybrid under outdoor weathering based on visual observation and EIS analysis. Acid undercutting is an issue for TEOS based hybrid coating. In the second part, design of experiments (DOEs) was used to statistically investigate on the effect of sol-gel precursors. The

  11. Sol-gel derived HA/TiO2 double coatings on Ti scaffolds for orthopaedic applications



    Hydroxyapatite/titania (HA/TiO2) double layers were coated onto Ti scaffolds throughout for orthopaedic applications by sol-gel method. Differential scanning calorimetry (DSC),thermogravimetric analysis (TG) and X-ray diffractometry (XRD) were used for the characterisation of the phase transformations of the dried gels and coated surface structures. Scanning electron microscope (SEM) equipped with energy dispersive spectrometry (EDS) was used for the observation and evaluation of the morphology and phases of the surface layers and for the assessment of the in vitro tests. The in vitro assessments were performed by soaking the HA/TiO2 double coated samples into the simulated body fluid (SBF) for various periods. The TiO2 layer was coated by a dipping-coating method at a speed of 12 cm/min,followed by a heat treatment at 600 ℃ for 20 min. The HA layer was subsequently dipping-coated on the outer surface at the same speed and then heat-treated at difference temperatures. The results indicat that the HA phase begins to crystallize after a heat treatment at 560 ℃. The crystallinity increases obviously at 760 ℃. SEM observations find no delamination or crack at the interfaces of HA/TiO2 and TiO2/Ti. The HA/TiO2 coated Ti scaffolds displays excellent bone-like apatite forming ability when it is soaked into SBF. Ti scaffolds after HA/TiO2 double coatings can be anticipated as promising implant materials for orthopaedic applications

  12. Low-temperature perovskite-type cadmium titanate thin films derived from a simple particulate sol-gel process

    Mohammadi, M.R. [Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge CB2 3QZ (United Kingdom); Department of Materials Science and Engineering, Sharif University of Technology, Azadi Street, Tehran (Iran, Islamic Republic of)], E-mail:; Fray, D.J. [Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge CB2 3QZ (United Kingdom)


    Low-temperature perovskite-type cadmium titanate (CdTiO{sub 3}) with a nanocrystalline and mesoporous structure was prepared at various Ti:Cd molar ratios by a straightforward particulate sol-gel route. The prepared sols had a narrow particle size distribution, in the range 23-26 nm. X-ray diffraction and Fourier transform infrared spectroscopy revealed that the powders contained a mixture of ilmenite-CdTiO{sub 3}, perovskite-CdTiO{sub 3}, anatase and rutile phases, depending on the annealing temperature and the Ti:Cd molar ratio. Perovskite-CdTiO{sub 3} was the major type obtained from cadmium-prominent powders at low temperature, whereas ilmenite-CdTiO{sub 3} was the major type obtained from titanium-prominent powders at high temperature. It was observed that the anatase-to-rutile phase transformation accelerated with decreasing Ti:Cd molar ratio. Furthermore, the ilmenite-to-perovskite phase transformation accelerated with a decrease in both the Ti:Cd molar ratio and the annealing temperature. The crystallite sizes of the ilmenite- and perovskite-CdTiO{sub 3} phases reduced with increasing the Ti:Cd molar ratio. Field emission scanning electron microscopic analysis revealed that the average grain size of the thin films decreased with an increase in the Ti:Cd molar ratio. Moreover, atomic force microscope images showed that CdTiO{sub 3} thin films had a columnar-like morphology. Based on Brunauer-Emmett-Taylor analysis, cadmium titanate powder containing Ti:Cd = 75:25 showed the greatest surface area and roughness and the smallest pore size among all the powders annealed at 500 deg. C. This is one of the smallest crystallite sizes and largest surface areas reported in the literature, and can be used in many applications in areas from optical electronics to gas sensors.

  13. Effect of Mn doping on structural and optical properties of sol gel derived ZnO nanoparticles

    Husain, Shahid, E-mail: [Department of Physics, Aligarh Muslim University, Aligarh 202002 (India); Alkhtaby, Lila A. [Department of Physics, Aligarh Muslim University, Aligarh 202002 (India); Giorgetti, Emilia [Istituto dei Sistemi Complessi ISC-CNR Sezione di Firenze, Sesto Fiorentino 50019, Firenze (Italy); Zoppi, Angela; Muniz Miranda, Maurizio [Department of Chemistry, University of Firenze, Sesto Fiorentino 50019, Firenze (Italy)


    We have synthesized the Zn{sub 1−x} Mn{sub x} O (x=0.01, 0.02, 0.03 and 0.05) nanoparticles by the sol–gel method. These samples are characterized using x-ray diffraction (XRD), Scanning Electron Microscope (SEM), Ultraviolet/Visible (UV/Vis) spectroscopy, Fluorescence spectroscopy, Raman spectroscopy and Fourier transform infra red (FTIR) spectroscopy. The x-ray diffraction patterns show that all the samples are formed in single phase with a complete solubility of Mn ions in the ZnO matrix. SEM micrographs show that the Mn doped ZnO nanoparticles are hexagonal with wurtzite structure.The particle sizes range between 18 and 35 nm. We have observed a decrease in fluorescence intensity on Mn doping and all the Mn doped samples show lower value of intensity as compared to pure ZnO in the visible range of spectrum. Raman spectroscopy reveals that the characteristic intense band of ZnO at 435 cm{sup −1} exhibits a decrease in intensity and slightly red shifts for 5% Mn doping. FTIR spectra exhibit additional bands on Mn doping as compared to pure ZnO. -- Highlights: • Mn doped ZnO nanoparticels are synthesized through sol gel process. • All the samples show wurtzite crystal symmetry with particle sizes which are found to be in the range from 18 to 35 nm. • The energy band-gap estimated using UV/Vis spectra is found to increase with the Mn doping. • Raman spectra reveal that characteristic intense band of ZnO at 436 cm{sup −1} exhibit a decrease in intensity but peak position does not shift with Mn doping.

  14. Sol-gel microextraction phases for sample preconcentration in chromatographic analysis.

    Segro, Scott S; Tran, Minh Phuong; Kesani, Sheshanka; Alhendal, Abdullah; Turner, Erica B


    Sol-gel technology provides a simple and reliable method for solid-phase microextraction (SPME) fiber preparation through in situ creation of surface-bonded organic-inorganic hybrid coatings characterized by enhanced thermal stability and solvent-resistance properties that are important for the coupling of SPME with GC and HPLC, respectively. The sol-gel coating technology has led to the development of an extensive array of sol-gel sorbent coatings for SPME. In this article, sol-gel microextraction coatings are reviewed, with particular attention on their synthesis, characterization, and applications in conjunction with GC and HPLC analyses. In addition, the development of sol-gel-coated stir bars, their inherent advantages, and applications are discussed. Next, the development and applications of sol-gel capillary microextraction (CME) in hyphenation with GC and HPLC is extensively reviewed. The newly emerging germania- and titania-based sol-gel microextraction phases look promising, especially in terms of pH and hot solvent stability. Finally, sol-gel monolithic beds for CME are reviewed. Such monolithic beds are in a position to greatly improve the extracting capabilities and enhanced sensitivity in CME.

  15. Thin Films Derived by a Particulate Sol-Gel Route with Various Cr:Ti Molar Ratios

    Mohammadi, M. R.; Fray, D. J.


    Nanocrystalline and nanostructured TiO2-Cr2O3 thin films and powders were prepared by a facile and straightforward aqueous particulate sol-gel route at low temperature of 400°C. The prepared sols showed a narrow particle size distribution with hydrodynamic diameter in the range of 17.7 nm to 19.0 nm. Moreover, the sols were stable over 4 months, with constant zeta potential measured during this period. The effect of the Cr:Ti molar ratio on the crystallization behavior of the products was studied. X-ray diffraction (XRD) analysis revealed that the powders crystallized at low temperature of 400°C, containing anatase-TiO2, rutile-TiO2, and Cr2O3 phases, depending on the annealing temperature and Cr:Ti molar ratio. Furthermore, it was found that Cr2O3 retarded the anatase to rutile transformation up to 800°C. The activation energy of crystallite growth was calculated to be in the range of 1.3 kJ/mol to 2.9 kJ/mol. Transmission electron microscopy (TEM) imaging showed that one of the smallest crystallite sizes was obtained for TiO2-Cr2O3 binary mixed oxide, being 5 nm at 500°C. Field-emission scanning electron microscopy (FESEM) analysis revealed that the deposited thin films had nanostructured morphology with average grain size in the range of 20 nm to 40 nm at 500°C. Thin films produced under optimized conditions showed excellent microstructural properties for gas sensing applications. They exhibited a remarkable response towards low concentrations of NO2 gas at low operating temperature of 200°C, resulting in increased thermal stability of sensing films as well as a decrease in their power consumption. Furthermore, calibration curves revealed that TiO2-Cr2O3 sensors followed the power law (where S is the sensor response, the coefficients A and B are constants, and [gas] is the gas concentration) for two types of gas, exhibiting excellent capability for detection of low gas concentrations.

  16. Optical Waveguides from Organic/Inorganic Hybrid Materials


    Organic/inorganic material has attracted great attentions because its importance as photonic materials. We report on our recent results on organic/inorganic hybrid sol-gel materials and optical waveguides like splitter, thermo-optic switch and micro-cavity laser.

  17. Optical Waveguides from Organic/Inorganic Hybrid Materials

    Liying Liu; Lei Xu; Wencheng Wang


    Organic/inorganic material has attracted great attentions because its importance as photonic materials. We report on our recent results on organic/inorganic hybrid sol-gel materials and optical waveguides like splitter,thermo-optic switch and micro-cavity laser.

  18. Sol-gel-based biosensing applied to medicinal science.

    Moreira, Felismina T C; Moreira-Tavares, Ana P; Sales, M Goreti F


    Biosensors have opened new horizons in biomedical analysis, by ensuring increased assay speed and flexibility, and allowing point-of-care applications, multi-target analyses, automation and reduced costs of testing. This has been a result of many studies merging nanotechnology with biochemistry over the years, thereby enabling the creation of more suitable environments to biological receptors and their substitution by synthetic analogue materials. Sol-gel chemistry, among other materials, is deeply involved in this process. Sol-gel processing allows the immobilization of organic molecules, biomacromolecules and cells maintaining their properties and activities, permitting their integration into different transduction devices, of electrochemical or optical nature, for single or multiple analyses. Sol-gel also allows to the production of synthetic materials mimicking the activity of natural receptors, while bringing advantages, mostly in terms of cost and stability. Moreover, the biocompatibility of sol-gel materials structures of biological nature allowed the use of these materials in emerging in vivo applications. In this chapter, biosensors for biomedical applications based on sol-gel derived composites are presented, compared and described, along with current emerging applications in vivo, concerning drug delivery or biomaterials. Sol-gel materials are shown as a promising tool for current, emerging and future medical applications.

  19. Luminescent hybrid porphyrinosilica obtained by sol gel chemistry

    Neri Cláudio Roberto


    Full Text Available The sol-gel process is a methodology used to obtain organic-inorganic hybrid solids, which open new possibilities in the field of material science. The sol-gel technique offers a low temperature attractive approach for introducing organic molecules into amorphous materials. In order to introduce tetrakis (2-hydroxy-5-nitrophenylporphyrin covalently bounded to a silicate matrix, the inorganic precursor 3-isocyanatopropyltriethoxysilane was added (molar ratio 2:1 to the porphyrin solution in anhydrous dimethylformamide and triethylamine. The isolated porphyrin and the hybrid porphyrinosilica have excitation maximum centred at 400 nm and 424 nm, respectively and the emission spectra for both materials has bands centred at 650 nm and 713 nm. The formation of hybrid matrix was investigated by FTIR.

  20. Sol-gel derived multiwalled carbon nanotubes ceramic electrode modified with molecularly imprinted polymer for ultra trace sensing of dopamine in real samples

    Prasad, Bhim Bali, E-mail: [Department of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi 221 005 (India); Kumar, Deepak; Madhuri, Rashmi; Tiwari, Mahavir Prasad [Department of Chemistry, Faculty of Science, Banaras Hindu University, Varanasi 221 005 (India)


    Highlights: > MWCNTs-CE was prepared by silane acrylate which provides a nanometer thin MIP film. > The sensor was modified by iniferter and MIP using 'surface grafting-from approach'. > A comparative study was performed between differentially designed ceramic electrodes. > The sensor can detect dopamine in real samples with LODs (0.143-0.154 ng mL{sup -1}). - Abstract: A new class of composite electrodes made of sol-gel derived ceramic-multiwalled carbon nanotubes is used for the growth of a nanometer thin film adopting 'surface grafting-from approach'. For this the multiwalled carbon nanotubes-ceramic electrode surface is first modified with an iniferter (benzyl N,N-diethyldithiocarbamate) and then dopamine imprinted polymer, under UV irradiation, for differential pulse anodic stripping voltammetric sensing of dopamine in aqueous, blood serum, cerebrospinal fluid, and pharmaceutical samples (detection limit 0.143-0.154 ng mL{sup -1}, 3{sigma}), without any cross reactivity, interferences and false-positive contributions. Such composite electrodes offer higher stability, electron kinetics, and renewable porous surface of larger electroactive area (with insignificant capacitance) than carbon ceramic electrodes. Additional cyclic voltammetry (stripping mode) and chronocoulometry experiments were performed to explore electrodics and kinetics of electro-oxidation of dopamine.

  1. Identification of TiO2 clusters present during synthesis of sol-gel derived TiO2 nano-particles

    Simonsen, Morten Enggrob; Søgaard, Erik Gydesen

    can be varied in order to obtain TiO2 particles with specific properties (Tailored materials). The TiO2 particles are formed by hydrolysis and condensation of titanium alkoxides. The properties of the final TiO2 particles are strongly affected by the kinetics of these reactions.1 Experimental...... nano-particles is lacking but is highly important for full control of the synthesis and production of nano-particles. In this study titanium dioxide clusters present during nucleation and growth of sol-gel derived TiO2 nanoparticles was investigated by help of electro spray mass spectrometry (ESI......-MS) and dynamic light scattering (DLS). Depending on the involved precursor TiO2 clusters of different sizes were identified (TTIP ~ 11-12 Ti atoms, TTB ~ 10-11 Ti atoms, and TTE ~ 5-7 Ti atoms).4 The Ti-O-Ti backbone/core of the titanium clusters were found to be quite stable after formation and do not easily...

  2. Carbon nanotubes incorporated with sol-gel derived La(OH)3 nanorods as platform to simultaneously determine ascorbic acid, dopamine, uric acid and nitrite.

    Zhang, Yu; Yuan, Ruo; Chai, Yaqin; Zhong, Xia; Zhong, Huaan


    A novel material, sol-gel derived La(OH)(3) nanorods (La(OH)(3)NRs) with excellent film forming ability was prepared, and it was first designed to incorporate with carbon nanotubes (CNTs) to modify glassy carbon electrode (GCE) to simultaneously voltammetric determine ascorbic acid (AA), dopamine (DA), uric acid (UA), and nitrite (NO(2)(-)). Cyclic voltammetry (CV), transmission electron microscopy (TEM), and X-ray diffraction (XRD) were employed to characterize the sensor. Under optimal conditions, the linear response range for AA, DA, UA, and NO(2)(-) were 0.5 μmol L(-1) to 1.46 mmol L(-1), 50 nmol L(-1) to 35.36 μmol L(-1), 50 nmol L(-1) to 0.79 mmol L(-1), and 0.55 μmol L(-1) to 0.72 mmol L(-1), respectively and the detection limits were 1.67 μmol L(-1), 1.67 nmol L(-1), 1.67 nmol L(-1), and 0.18 μmol L(-1). The sensor demonstrated well stability, high selectivity and sensitivity. More importance, this material can be extended to construct other electrochemical sensors by the immobilization of enzymes and antibodies.

  3. Study of the surface modification with oleic acid of nanosized HfO{sub 2} synthesized by the polymerized complex derived sol-gel method

    Ramos-Gonzalez, R., E-mail: [Centro de Investigacion en Quimica Aplicada, Blvd. Enrique Reyna Hermosillo No. 140, Saltillo, Coahuila 25250 (Mexico); Garcia-Cerda, L.A. [Centro de Investigacion en Quimica Aplicada, Blvd. Enrique Reyna Hermosillo No. 140, Saltillo, Coahuila 25250 (Mexico); Quevedo-Lopez, M.A. [University of Texas at Dallas, 800 West Campbell Road, Richardson, TX 75080-3021 (United States)


    The synthesis of nanosized hafnium oxide by the polymerized complex derived sol-gel method is reported. The structural and morphological characterization of the HfO{sub 2} was carried out by X-ray diffraction and scanning electron microscopy. The surface of hafnium oxide nanoparticles was modified by capping with oleic acid. The nanoparticle surface area was measured by the gas adsorption technique in order to determine the minimal amount of oleic acid needed to obtain a uniform coverage of the hafnium oxide. The existence of organic layer can be confirmed by Fourier transform spectroscopy, solid state nuclear magnetic resonance spectroscopy, thermal gravimetric analysis and transmission electron microscopy. The FTIR and solid state NMR results reveal that oleic acid is chemisorbed as a carboxylate onto the HfO{sub 2} nanoparticle surface and confirm the formation of a monomolecular layer of oleic acid surrounding the HfO{sub 2}. The cover density of oleic acid on the HfO{sub 2} increases with the amount of oleic acid used to modify the nanoparticles and the surface properties of HfO{sub 2} nanoparticles modified with oleic acid change from hydrophilic to hydrophobic.

  4. Absorbability of bulk sol-gel bioactive glasses

    Hamadouche, M.; Meunier, A.; Blanchat, C.; Sedel, L. [Paris-7 Univ. (France). Lab. de Recherches Orthopediques; Greenspan, D.C.; Zhong, J.P.; Torre, G.P. la [US Biomaterials Corp., Alachua, FL (United States)


    Melt-derived bioactive glasses have been used with success in various clinical applications for over 10 years. Recently, particles of sol-gel derived bioactive glasses with an initial high specific area have exhibited high osteoconductive properties, but also a significant degradability. In this work, we explored the in-vivo bioactivity and degradability of bulk sol-gel derived glasses. Two sol-gel compositions (58S and 77S Bioglass) were used. Bulk 45S5 were used as a control. Both sol-gel derived demonstrated similar osteoconductive properties to 45S% Bioglass. In addition, absorbability was observed for sol-gel derived glasses after 12 weeks of implantation. Total absorption reached 40% after 52 weeks. No degradation could be measured in the case of 45S5 melt derived Bioglass. The degradation process was highly time dependent as demonstrated by regression analysis. New bone formation was found to fill in areas that had been resorbed similar to bone remodeling. New bone was found to fill in areas that had been absorbed, similar to natural bone remodeling. This absorbability can be assumed to be at least partially related to an osteoclastic resorption, as viable osteoclasts-like cells were found directly in contact with the glass surfaces. (orig.)

  5. Development and Characterization of 316 L Stainless Steel Coated by Melt-derived and Sol-gel derived 45S5 Bioglass for orthopedic applications

    Seyed Morteza Naghib


    Full Text Available The 316L austenitic stainless steel (SS was coated by 45S5 bioactive glass produced by melting and sol-gel techniques to increase the bioactivity and to provide a high mechanical strength for orthopedic and dental applications. The morphologies of coated specimens were investigated by scanning electron microscopy (SEM. Then, the coated specimens were immersed in simulated body fluid (SBF at 37°C for 14 days, and their microstructures after withdrawal were also investigated by SEM. All the specimens were analyzed by FTIR and XRD in order to survey the formation of hydroxyapatite layer.

  6. The Sol-Gel Process

    Khalid Suliman Aboodh


    Abstract An increasingly important application of liquid jets is the disintegration of the jet to form droplets of liquid containing nuclear fuel. These droplets are then dried and sintered to form ceramic micro spheres for use in fuel elements in nuclear reactors. The total operations required to form the droplets convert them to solids and fire them to ceramic bodies comprise what are known as Sol-Gel processes Reference 13.

  7. Selective catalytic reduction of NO with NH{sub 3} over sol-gel-derived CuO-CeO{sub 2}-MnOx/y-Al{sub 2}O{sub 3} catalysts

    Zhao, Q.S.; Sun, L.S.; Xiang, J.; Su, S.; Hu, S. [Huazhong Univ. of Science and Technology, Wuhan, Hubei (China). State Key Laboratory of Coal Combustion


    Sulfur dioxide (SO{sub 2}) and nitrogen oxides (NO{sub X}) are major air pollutants. Before emitting flue gas into the atmosphere, these pollutants must be removed using various processes. A sol-gel process has been developed to prepare alumina granular support and catalyst. The sol-gel-derived alumina granules have a large surface area, large pore volume, uniform pore size distribution, and excellent mechanical properties such as attrition resistance and crush strength. This paper discussed an experiment that synthesized two catalysts using the sol-gel oil-drop method. The paper described the experimental procedure and presented the results of the experiment. This included the effect of temperature on the catalytic activity of CuO-CeO{sub 2}-MnOx/y-Al{sub 2}O{sub 3} catalysts; desorption of ammonia (NH{sub 3}) and nitric oxide (NO) on the CuO-CeO{sub 2}-MnOx/y-Al{sub 2}O{sub 3} catalysts; transient response of NH{sub 3} and NO on CuO-CeO{sub 2}-MnOx/y-Al{sub 2}O{sub 3} catalysts; and the reaction kinetics and characterization of CuO-CeO{sub 2}-MnOx/y-Al{sub 2}O{sub 3} catalysts. It was concluded that the CuO-CeO{sub 2}-MnOx/y-Al{sub 2}O{sub 3} catalysts made by the sol-gel method have higher activity and a wider operating temperature range. 17 refs., 1 tab., 9 figs.

  8. Evolution of structural and optical properties in the course of thermal evolution of sol-gel derived cobalt-doped gahnite

    Kurajica, S., E-mail: [University of Zagreb, Faculty of Chemical Engineering and Technology, Marulicev trg 19, HR-10000 Zagreb (Croatia); Tkalcec, E. [University of Zagreb, Faculty of Chemical Engineering and Technology, Marulicev trg 19, HR-10000 Zagreb (Croatia); Grzeta, B. [Division of Materials Physics, Ruder Boskovic Institute, Bijenicka 54, HR-10000 Zagreb (Croatia); Ivekovic, D. [University of Zagreb, Faculty of Food Technology and Biotechnology, Pierottijeva 6, HR-10000 Zagreb (Croatia); Mandic, V. [University of Zagreb, Faculty of Chemical Engineering and Technology, Marulicev trg 19, HR-10000 Zagreb (Croatia); Popovic, J. [Division of Materials Physics, Ruder Boskovic Institute, Bijenicka 54, HR-10000 Zagreb (Croatia); Kranzelic, D. [University of Zagreb, Faculty of Chemical Engineering and Technology, Marulicev trg 19, HR-10000 Zagreb (Croatia)


    Research highlights: > Distribution of Co{sup 2+} ions in zinc cobalt aluminate lattice seats depend on Co loading. The green color of samples at lower temperatures is a consequence of partial oxidation of Co{sup 2+} ions and their accommodation in octahedral sites. Thermal treatment at higher temperatures promotes gradual change of color to blue, characteristic for tetrahedrally coordinated Co{sup 2+} ions. The spectra evolution could be interpreted as a progressive reduction of Co{sup 3+} to Co{sup 2+} ions at higher temperatures. - Abstract: Thermal evolution of sol-gel derived gahnite (ZnAl{sub 2}O{sub 4}) with 4, 8 and 12 at.% of Zn replaced with Co was studied by thermal analysis techniques (DTA/TGA), X-ray diffraction (XRD) and UV-vis diffuse reflectance spectroscopy (DRS). Zinc-cobalt spinel powders were produced by gel heat treatment at temperatures as low as 400 {sup o}C. Crystal structure was characterized using Rietveld refinement of X-ray diffraction patterns for the samples annealed at 800 {sup o}C, simultaneously with the analysis of diffraction line broadening. It was found out that the distribution of Co{sup 2+} ions in tetrahedral and octahedral sites of zinc cobalt aluminate crystal lattice, crystallite size and lattice strain depend on Co loading. The green color of samples thermally treated at T < 800 deg. C has been explained as a consequence of partial oxidation of Co{sup 2+} ions at lower temperatures and accommodation of Co{sup 3+} ions in octahedral sites. Thermal treatment at higher temperatures promote gradual change of color from green to blue, characteristic for tetrahedrally coordinated Co{sup 2+} ions. The spectra evolution could be interpreted as a progressive reduction of Co{sup 3+} to Co{sup 2+} ions at higher temperatures.

  9. Surface enhanced Raman scattering activity of TiN thin film prepared via nitridation of sol-gel derived TiO2 film

    Dong, Zhanliang; Wei, Hengyong; Chen, Ying; Wang, Ruisheng; Zhao, Junhong; Lin, Jian; Bu, Jinglong; Wei, Yingna; Cui, Yi; Yu, Yun


    Surface-enhanced Raman scattering (SERS) is a powerful and non-destructive analytical technique tool for chemical and biological sensing applications. Metal-free SERS substrates have recently been developed by using semiconductor nanostructures. The optical property of TiN film is similar to that of gold. Besides that, its good chemical inertness and thermodynamic stability make TiN thin film an excellent candidate for SERS. In order to investigate its SERS activity, the TiN thin film was successfully prepared via direct nitridation of the sol-gel derived TiO2 thin film on the quartz substrate using ammonia gas as reducing agent. The crystallite structures and morphology of TiN thin film were determined by XRD, RAMAN and FE-SEM. The results show that the thin film obtained is cubic titanium nitride with a lattice parameter of 4.2349 Å. The surface of TiN thin film is rough and with the particles of 50 nm in average sizes. The thickness of TiN thin film is about 130 nm. The TiN thin film displays a surface Plasmon resonance absorption peak at around 476 nm, which can lead to a strong enhancement of the EM field on the interface. The Raman signal of the probe molecule R6G was greatly enhanced through TiN thin film substrates. The enhancement factor is about 4.1×103 and the detection limit achieves 10-6 M for R6G. The TiN thin film substrate also shows a good reproducibility of SERS performance. The results indicate that TiN thin film is an attractive material with potential application in SERS substrates.

  10. In Vitro and In Vivo Evaluation of Sol-Gel Derived TiO2 Coatings Based on a Variety of Precursors and Synthesis Conditions

    Krzysztof Marycz


    Full Text Available The effect of synthesis way of TiO2 coatings on biocompatibility of transplanted materials using an in vitro and in vivo rat model was investigated. TiO2 layers were synthesized by a nonaqueous sol-gel dip-coating method on stainless steel 316L substrates applying two different precursors and their combination. Morphology and topography of newly formed biomaterials were determined as well as chemical composition and elemental distribution of a surface samples. In vitro tests were conducted by adipose-derived mesenchymal stem cells cultured on TiO2 coatings and stainless steel without coatings to assess the bioreactivity of obtained materials. A positive biological effect of TiO2/316L/1 coatings—based on titanium(IV ethoxide—was found in both in vitro and in vivo models. The TiO2/316L/1 exhibited the highest roughness and the lowest titanium concentration in TiO2 than TiO2/316L/2—based on titanium(IV propoxide and TiO2/316L/3—based on both above-mentioned precursors. The proper fibroblast-like morphology and higher proliferation rate of cells cultured on TiO2/316L/1 were observed when compared to the other biomaterials. No inflammatory response in the bone surrounding implant covered by each of the obtained TiO2 was present. Our results showed that improvement of routinely used stainless steel 316L with TiO2/316L/1 layer can stimulate beneficial biological response.

  11. Transferability and Adhesion of Sol-Gel-Derived Crystalline TiO2 Thin Films to Different Types of Plastic Substrates.

    Amano, Natsumi; Takahashi, Mitsuru; Uchiyama, Hiroaki; Kozuka, Hiromitsu


    Anatase thin films were prepared on various plastic substrates by our recently developed sol-gel transfer technique. Polycarbonate (PC), poly(methyl methacrylate) (PMMA), polyethylene terephthalate (PET), polyethylene (PE), polypropylene (PP), polyether ether ketone (PEEK), and polyvinylidene chloride (PVDC) were employed as plastic substrates. A Si(100) substrate was first coated with a polyimide (PI)/polyvinylpyrrolidone (PVP) mixture layer, and an alkoxide-derived titania gel film was deposited on it by spin-coating. The resulting titania gel film was heated to 600 °C, during which the PI/PVP layer decomposed and the gel film was converted into a 60 nm thick anatase film. The anatase film was then transferred from the Si(100) substrate to the plastic substrate. This was achieved by heating the plastic/anatase/Si(100) stack in a near-infrared image furnace to 120-350 °C, depending on the type of plastic substrate, under unidirectional pressure. The anatase film cracked during transfer to PE, PP, PEEK, and PVDC substrates but did not crack during transfer to PC, PMMA, and PET substrates. The fraction of the total film area that was successfully transferred was assessed with the aid of image analysis. This fraction tended to be large for plastics with C═O and C-O groups and small for those without these groups. The film/substrate adhesion assessed by cross-cut tape tests also tended to be high for plastics with C═O and C-O groups and low for those without these groups. The adhesion to plastics without C═O or C-O groups could be enhanced and their transfer area fraction increased by oxidizing the native plastic surface by ultraviolet-ozone treatment prior to transfer.

  12. Luminescent features of sol-gel derived rare-earth multi-doped oxyfluoride nano-structured phosphors for white LED application

    Gouveia-Neto, A.S., E-mail: [Departamento de Fisica, Universidade Federal Rural de Pernambuco, Recife, PE (Brazil); Silva, A.F. da; Bueno, L.A.; Costa, E.B. da [Departamento de Fisica, Universidade Federal Rural de Pernambuco, Recife, PE (Brazil)


    Rare-earth doped oxyfluoride 75SiO{sub 2}:25PbF{sub 2} nano-structured phosphors for white-light-emitting diodes were synthesized by thermal treatment of precursor sol-gel derived glasses. Room temperature luminescence features of Eu{sup 3+}, Sm{sup 3+}, Tb{sup 3+}, Eu{sup 3+}/Tb{sup 3+}, and Sm{sup 3+}/Tb{sup 3+} ions incorporated into low-phonon-energy PbF{sub 2} nanocrystals dispersed in the aluminosilicate glass matrix and excited with UV light emitting diode were investigated. The luminescence spectra exhibited strong emission signals in the red (600, 610, 625, and 646 nm), green (548 and 560 nm), and blue (485 nm) wavelength regions. White-light emission was observed in Sm/Tb and Eu/Tb double-doped activated phosphors employing UV-LED excitation at 395 nm. The dependence of the luminescence emission intensities upon annealing temperature and rare-earth concentration was also examined. The results indicated that there exist optimum annealing temperature and activator ion concentration in order to obtain intense visible emission light with high color rendering index. The study suggests that the nanocomposite phosphor based upon 75SiO{sub 2}:25PbF{sub 2} host herein reported is a promising contender for white-light LED applications. - Highlights: Black-Right-Pointing-Pointer White-light emission in double-doped activated phosphors employing UV-LED excitation. Black-Right-Pointing-Pointer Luminescent features of europium, samarium, and terbium in nanocrystals dispersed in aluminosilicate glass. Black-Right-Pointing-Pointer New nanocomposite phosphor host for white-light LED applications.

  13. Near-infrared to visible up-conversion emissions of Er3+ doped Al2O3 powders derived from the sol-gel method


    The Er3+ doped Al2O3 powders were prepared by the sol-gel method using the aluminium isopropoxide [Al(OC3H7)3]-derived Al2O3 sols with addition of the erbium nitrate [Er(NO3)3.5H2O]. The different phase structure, including three crystalline types of (Al,Er)2O3 phases, γ, θ, α, and two Er-Al-O phases, ErAlO3 and Al10Er6O24, was obtained with the 1 mol% Er3+ doped Al2O3 powders at the different sintering temperatures of 600―1200℃. The green and red up-conversion emissions centered at about 523, 545 and 660 nm, corresponding respectively to the 2H11/2, 4S3/2→4I15/2 and 4F9/2→4I15/2 transitions of Er3+, were detected by a 978 nm semiconductor laser diodes excitation. The phase structure and OH content had evident influence on the up-conversion emissions intensity. The maximum intensities of both the green and red emissions were obtained respectively for the Er3+ doped Al2O3 powders sintered at 1200 ℃, which was composed mainly of α-(Al,Er)2O3, less of ErAlO3 and Al10Er6O24 phases, and with the least OH content. The two-photon absorption up-conversion process was involved in the green and red up-conversion emissions of the Er3+ doped Al2O3 powders.

  14. Role of a waste-derived polymeric biosurfactant in the sol-gel synthesis of nanocrystalline titanium dioxide

    Boffa, Vittorio; Perrone, Daniele G.; MAGNACCA, Giuliana; Montoneri, Enzo


    An inexpensive polymeric biosurfactant isolated from urban bio-wastes is shown to be a useful chemical aid in the synthesis of nanostructured materials with tunable pore size and surface hydrophilicity. Photocatalytic active TiO2 powders were prepared by sol–gel reaction in the presence of variable amounts of a waste-derived polymeric biosurfactant. The products were characterized for morphology, crystal structures and surface hydrophilicity. The porosity data indicate that an increase of the...

  15. Sol-Gel Glasses

    Mukherjee, S. P.


    Multicomponent homogeneous, ultrapure noncrystalline gels/gel derived glasses are promising batch materials for the containerless glass melting experiments in microgravity. Hence, ultrapure, homogeneous gel precursors could be used to: (1) investigate the effect of the container induced nucleation on the glass forming ability of marginally glass forming compositions; and (2) investigate the influence of gravity on the phase separation and coarsening behavior of gel derived glasses in the liquid-liquid immiscibility zone of the nonsilicate systems having a high density phase. The structure and crystallization behavior of gels in the SiO2-GeO2 as a function of gel chemistry and thermal treatment were investigated. As are the chemical principles involved in the distribution of a second network former in silica gel matrix being investigated. The procedures for synthesizing noncrystalline gels/gel-monoliths in the SiO2-GeO2, GeO2-PbO systems were developed. Preliminary investigations on the levitation and thermal treatment of germania silicate gel-monoliths in the Pressure Facility Acoustic Levitator were done.

  16. Metal-silica sol-gel materials

    Stiegman, Albert E. (Inventor)


    The present invention relates to a single phase metal-silica sol-gel glass formed by the co-condensation of a transition metal with silicon atoms where the metal atoms are uniformly distributed within the sol-gel glass as individual metal centers. Any transition metal may be used in the sol-gel glasses. The present invention also relates to sensor materials where the sensor material is formed using the single phase metal-silica sol-gel glasses. The sensor materials may be in the form of a thin film or may be attached to an optical fiber. The present invention also relates to a method of sensing chemicals using the chemical sensors by monitoring the chromatic change of the metal-silica sol-gel glass when the chemical binds to the sensor. The present invention also relates to oxidation catalysts where a metal-silica sol-gel glass catalyzes the reaction. The present invention also relates to a method of performing oxidation reactions using the metal-silica sol-gel glasses. The present invention also relates to organopolymer metal-silica sol-gel composites where the pores of the metal-silica sol-gel glasses are filled with an organic polymer polymerized by the sol-gel glass.

  17. Sol-Gel Derived Nanocomposites


    Phase distribution in nanocomposite hybrid materials can be analyzed by Force modulation Atomic Force Microscopy (AFM). The combination of this method with conventional analytical methods, e.g. IR spectroscopy and Scanning Electron Microscopy (SEM), leads to a new insight in the formation of these new materials and contributes to tailor their properties. Thin films of such materials were investigated, in order to understand the interactions between the components and their application as natu...

  18. One-step sol-gel imprint lithography for guided-mode resonance structures.

    Huang, Yin; Liu, Longju; Johnson, Michael; C Hillier, Andrew; Lu, Meng


    Guided-mode resonance (GMR) structures consisting of sub-wavelength periodic gratings are capable of producing narrow-linewidth optical resonances. This paper describes a sol-gel-based imprint lithography method for the fabrication of submicron 1D and 2D GMR structures. This method utilizes a patterned polydimethylsiloxane (PDMS) mold to fabricate the grating coupler and waveguide for a GMR device using a sol-gel thin film in a single step. An organic-inorganic hybrid sol-gel film was selected as the imprint material because of its relatively high refractive index. The optical responses of several sol-gel GMR devices were characterized, and the experimental results were in good agreement with the results of electromagnetic simulations. The influence of processing parameters was investigated in order to determine how finely the spectral response and resonant wavelength of the GMR devices could be tuned. As an example potential application, refractometric sensing experiments were performed using a 1D sol-gel device. The results demonstrated a refractive index sensitivity of 50 nm/refractive index unit. This one-step fabrication process offers a simple, rapid, and low-cost means of fabricating GMR structures. We anticipate that this method can be valuable in the development of various GMR-based devices as it can readily enable the fabrication of complex shapes and allow the doping of optically active materials into sol-gel thin film.

  19. Electrochemical and In Vitro Behavior of Nanostructure Sol-Gel Coated 316L Stainless Steel Incorporated with Rosemary Extract

    Motalebi, Abolfazl; Nasr-Esfahani, Mojtaba


    The corrosion resistance of AISI 316L stainless steel for biomedical applications, was significantly enhanced by means of hybrid organic-inorganic sol-gel thin films deposited by spin-coating. Thin films of less than 100 nm with different hybrid characters were obtained by incorporating rosemary extract as green corrosion inhibitor. The morphology, composition, and adhesion of hybrid sol-gel coatings have been examined by SEM, EDX, and pull-off test, respectively. Addition of high additive concentrations (0.1%) did not disorganize the sol-gel network. Direct pull-off test recorded a mean coating-substrate bonding strength larger than 21.2 MPa for the hybrid sol-gel coating. The effect of rosemary extract, with various added concentrations from 0.012 to 0.1%, on the anticorrosion properties of sol-gel films have been characterized by electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization tests in simulated body fluid (SBF) solution and has been compared to the bare metal. Rosemary extract additions (0.05%) have significantly increased the corrosion protection of the sol-gel thin film to higher than 90%. The in vitro bioactivity of prepared films indicates that hydroxyapatite nuclei can form and grow on the surface of the doped sol-gel thin films. The present study shows that due to their excellent anticorrosion properties, bioactivity and bonding strength to substrate, doped sol-gel thin films are practical hybrid films in biomedical applications.

  20. Sol-gel electrochromic device


    All solid state electrochromic devices have potential applications in architectural and automotive fields to regulate the transmission and reflection of radiant energy. We present the optical and electrochemical characteristics of two solid state windows having the configuration glass/ITO/TiO2-CeO2/TiO2/TiO2-CeO2/ITO/glass and glass/ITO/WOa/TiO2/TiO2-CeO2/ITO/glass where the three internal layers have been prepared by sol gel methods. The preparation of the individual sols and some physical p...

  1. Sol-gel precursors and products thereof

    Warren, Scott C.; DiSalvo, Jr., Francis J.; Weisner, Ulrich B.


    The present invention provides a generalizable single-source sol-gel precursor capable of introducing a wide range of functionalities to metal oxides such as silica. The sol-gel precursor facilitates a one-molecule, one-step approach to the synthesis of metal-silica hybrids with combinations of biological, catalytic, magnetic, and optical functionalities. The single-source precursor also provides a flexible route for simultaneously incorporating functional species of many different types. The ligands employed for functionalizing the metal oxides are derived from a library of amino acids, hydroxy acids, or peptides and a silicon alkoxide, allowing many biological functionalities to be built into silica hybrids. The ligands can coordinate with a wide range of metals via a carboxylic acid, thereby allowing direct incorporation of inorganic functionalities from across the periodic table. Using the single-source precursor a wide range of functionalized nanostructures such as monolith structures, mesostructures, multiple metal gradient mesostructures and Stober-type nanoparticles can be synthesized. ##STR00001##

  2. Sol-gel precursors and products thereof

    Warren, Scott C.; DiSalvo, Jr., Francis J.; Weisner, Ulrich B.


    The present invention provides a generalizable single-source sol-gel precursor capable of introducing a wide range of functionalities to metal oxides such as silica. The sol-gel precursor facilitates a one-molecule, one-step approach to the synthesis of metal-silica hybrids with combinations of biological, catalytic, magnetic, and optical functionalities. The single-source precursor also provides a flexible route for simultaneously incorporating functional species of many different types. The ligands employed for functionalizing the metal oxides are derived from a library of amino acids, hydroxy acids, or peptides and a silicon alkoxide, allowing many biological functionalities to be built into silica hybrids. The ligands can coordinate with a wide range of metals via a carboxylic acid, thereby allowing direct incorporation of inorganic functionalities from across the periodic table. Using the single-source precursor a wide range of functionalized nanostructures such as monolith structures, mesostructures, multiple metal gradient mesostructures and Stober-type nanoparticles can be synthesized. ##STR00001##

  3. Fabrication of advanced electrochemical energy materials using sol-gel processing techniques

    Chu, C. T.; Chu, Jay; Zheng, Haixing


    Advanced materials play an important role in electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. They are being used as both electrodes and electrolytes. Sol-gel processing is a versatile solution technique used in fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. The application of sol-gel processing in the fabrication of advanced electrochemical energy materials will be presented. The potentials of sol-gel derived materials for electrochemical energy applications will be discussed along with some examples of successful applications. Sol-gel derived metal oxide electrode materials such as V2O5 cathodes have been demonstrated in solid-slate thin film batteries; solid electrolytes materials such as beta-alumina for advanced secondary batteries had been prepared by the sol-gel technique long time ago; and high surface area transition metal compounds for capacitive energy storage applications can also be synthesized with this method.

  4. Humidity sensing properties of La~(3+)/Ce~(3+)-doped TiO_2-20 wt.% SnO_2 thin films derived from sol-gel method

    李红霞; 史志铭; 刘红伟


    The humidity sensing properties of La3+/Ce3+-doped TiO2-20 wt.%SnO2 thin films were studied.Sol-gel method was employed to prepare the films on alumina substrates.By constructing a humidity-impedance measuring system,the sensing behaviors were inspected for the films sintered at different temperatures.Experimental results showed that,0.5 wt.% of La2O3 or Ce2O3 doped films sintered at 500 °C for 2 h had the best humidity sensing properties,the impedance decreasing from 109 ? to below 104 ? in the humidity ra...

  5. Concentration and annealing effect on PL properties of sol-gel derived SiO_2-Y_2O_3:Eu~(3+) nanocomposites

    王忆; 曾庆光; 胡社军; 吴坤彬; 蒋俊宏; 陈根廷


    An improved sol-gel method was employed to prepare Eu3+ ions doped SiO2-Y2O3 nanocomposites.Systematic study was carried out on the effect of post-annealing treatment on photoluminescence(PL) properties of the samples under various europium ions doping concentrations.X-ray diffraction(XRD) patterns indicated that the samples showed an amorphous matrix structure,and the scanning electron microscopy(SEM) pictures showed that the samples presented a nano size(from 21 to 42 nm) granular-stack structure after hi...

  6. Nanostructure of sol-gel derived TiO{sub 2} for thin films on glass substrates measured by small angle scattering of synchrotron light

    Lucic-Lavcevic, Magdy [Department of Physics, Faculty of Technology, University of Split, Teslina 10/V, 21000 Split (Croatia); Dubcek, Pavo; Etlinger, Bozidar; Turkovic, Aleksandra; Sokcevic, Damir [Institute Ruder Boskovic, P.O. Box 1016, 10000 Zagreb (Croatia); Milat, Ognjen [Institute of Physics, University of Zagreb, P.O. Box 162, 10000 Zagreb (Croatia); Amenitsch, Heinz [Sincrotrone Trieste S.c.p.A., ss. 14, km 163, 5 Basovizza, 34012 Trieste (Italy)


    Nanosized TiO{sub 2} thin films on glass substrate of thicknesses ranging from 3 to 12.5 {mu}m were prepared using sol-gel procedure. The TiO{sub 2} crystallite size increased in `average particle radii` values from 2.5 nm to 3.7 nm with increase of film thickness up to 12.5 {mu}m. A new SAXS (small angle X-ray scattering) beamline at synchrotron ELLETRA was used to determine grain sizes and specific surface area of these films

  7. Ionic liquid-mediated bis[(3-methyldimethoxysilyl)propyl] polypropylene oxide-based polar sol-gel coatings for capillary microextraction.

    Shearrow, Anne M; Bhansali, Shekhar; Malik, Abdul


    Two ionic liquids (IL), namely, 1-methyl-3-octylimidazolium chloride (MOIC) and trihexyltetradecylphosphonium tetrafluoroborate (TTPT) were used to prepare polar and nonpolar sol-gel coatings for capillary microextraction (CME). Bis[(3-methyldimethoxysilyl)propyl] polypropylene oxide (BMPO), containing sol-gel active terminal methoxysilyl groups and polar propylene oxide repeating units, was used to prepare polar sol-gel hybrid organic-inorganic coatings. Hydroxy-terminated poly(dimethyl-co-diphenylsiloxane) was used as the sol-gel active organic component for nonpolar sol-gel hybrid coatings. Compared to a sol-gel BMPO coating prepared without IL, the sol-gel BMPO coatings prepared with the use of both of these ILs provided more efficient extraction as is evidenced by more pronounced GC peak areas. The MOIC-mediated sol-gel BMPO coating provided larger GC peak areas compared to the TTPT-mediated sol-gel BMPO coating. Scanning electron microscopy results suggested that MOIC provided a more porous morphology of the sol-gel BMPO extraction media compared to that prepared with TTPT. Thus, individual ILs can affect the porosity of sol-gel materials to different degrees. Overall, the sol-gel BMPO coating prepared with the ILs could extract nonpolar to polar analytes directly from aqueous samples. Detection limits were on the order of nanograms per liter (1.9-330.5 ng/L) depending on the analyte class. Furthermore, the MOIC-mediated sol-gel BMPO coating demonstrated high thermal stability (330 degrees C), solvent resistance, and fast extraction equilibrium (10-15 min) for polar and moderately polar analytes.

  8. Sol-gel composite material characteristics caused by different dielectric constant sol-gel phases

    Kimoto, Keisuke; Matsumoto, Makoto; Kaneko, Tsukasa; Kobayashi, Makiko


    Ultrasonic transducers prepared by a sol-gel composite method have been investigated in the field of nondestructive testing (NDT). Sol-gel composite materials could be ideal piezoelectric materials for ultrasonic transducer applications in the NDT field, and a new sol-gel composite with desirable characteristics has been developed. Three kinds of sol-gel composite materials composed of different dielectric constant sol-gel phases, Pb(Zr,Ti)O3 (PZT), Bi4Ti3O12 (BiT), and BaTiO3 (BT), and the same piezoelectric powder phase, PbTiO3 (PT), were fabricated and their properties were compared quantitatively. As a result, the PT/BT, sol-gel composite with the highest dielectric constant sol-gel phase showed the highest d 33 and signal strength. In addition, only PT/BT was successfully poled by room-temperature corona poling with reasonable signal strength.

  9. Anticorrosive organic/inorganic hybrid coatings

    Gao, Tongzhai

    Organic/inorganic hybrid coating system was developed for anticorrosion applications using polyurea, polyurethane or epoxide as the organic phase and polysiloxane, formed by sol-gel process, as the inorganic phase. Polyurea/polysiloxane hybrid coatings were formulated and moisture cured using HDI isocyanurate, alkoxysilane-functionalized HDI isocyanurate, and tetraethyl orthosilicate (TEOS) oligomers. Two urethanes were prepared using the same components as abovementioned in addition to the oligoesters derived from either cyclohexane diacids (CHDA) and 2-butyl-2-ethyl-1,3-propanediol (BEPD) or adipic acid (AA), isophthalic acid (IPA), 1,6-hexanediol (HD), and trimethylol propane (TMP). Accelerated weathering and outdoor exposure were performed to study the weatherability of the polyurethane/polysiloxane hybrid coating system. FTIR and solid-state 13C NMR revealed that the degradation of the hybrid coatings occurred at the urethane and ester functionalities of the organic phase. DMA and DSC analyses showed the glass transition temperature increased and broadened after weathering. SEM was employed to observe the change of morphology of the hybrid coatings and correlated with the gloss variation after weathering. Rutile TiO2 was formulated into polyurethane/polysiloxane hybrid coatings in order to investigate the effect of pigmentation on the coating properties and the sol-gel precursor. Chemical interaction between the TiO2 and the sol-gel precursor was investigated using solid-state 29Si NMR and XPS. The morphology, mechanical, viscoelastic, thermal properties of the pigmented coatings were evaluated as a function of pigmentation volume concentration (PVC). Using AFM and SEM, the pigment were observed to be well dispersed in the polymer matrix. The thermal stability, the tensile modulus and strength of the coatings were enhanced with increasing PVC, whereas the pull-off adhesion and flexibility were reduced with increasing PVC. Finally, the pigmented coatings were

  10. A sol-gel derived pH-responsive bovine serum albumin molecularly imprinted poly(ionic liquids) on the surface of multiwall carbon nanotubes

    Liu, Mingming, E-mail: [Key Laboratory of Arable Land Conservation (Middle and Lower Reaches of Yangtse River), Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Pi, Jiangyan; Wang, Xiaojie; Huang, Rong; Du, Yamei; Yu, Xiaoyang; Tan, Wenfeng; Liu, Fan [Key Laboratory of Arable Land Conservation (Middle and Lower Reaches of Yangtse River), Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Shea, Kenneth J., E-mail: [Department of Chemistry, University of California-Irvine, Irvine, CA 92697 (United States)


    A pH-responsive surface molecularly imprinted poly(ionic liquids) (MIPILs) was prepared on the surface of multiwall carbon nanotubes (MWCNTs) by a sol-gel technique. The material was synthesized using a 3-aminopropyl triethoxysilane modified multiwall carbon nanotube (MWCNT-APTES) as the substrate, bovine serum albumin (BSA) as the template molecule, an alkoxy-functionalized IL 1-(3-trimethoxysilyl propyl)-3-methyl imidazolium chloride ([TMSPMIM]Cl) as both the functional monomer and the sol-gel catalyst, and tetraethoxysilane (TEOS) as the crosslinking agent. The molecular interaction between BSA and [TMSPMIM]Cl was quantitatively evaluated by UV–vis spectroscopy prior to polymerization so as to identify an optimal template/monomer ratio and the most suitable pH value for the preparation of the MWCNTs@BSA-MIPILs. This strategy was found to be effective to overcome the problems of trial-and-error protocol in molecular imprinting. The optimum synthesis conditions were as follows: template/monomer ratio 7:20, crosslinking agent content 2.0–2.5 mL, temperature 4 °C and pH 8.9 Tris–HCl buffer. The influence of incubation pH on adsorption was also studied. The result showed that the imprinting effect and selectivity improved significantly with increasing incubation pH from 7.7 to 9.9. This is mainly because the non-specific binding from electrostatic and hydrogen bonding interactions decreased greatly with the increase of pH value, which made the specific binding affinity from shape selectivity strengthened instead. The polymers synthesized under the optimal conditions were then characterized by BET surface area measurement, FTIR, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The adsorption capacity, imprinting effect, selective recognition and reusability were also evaluated. The as-prepared MWCNTs@BSA-MIPILs were also found to have a number of advantages including high surface area (134.2 m{sup 2} g{sup −1}), high adsorption

  11. Sol-gel based alumina powders with catalytic applications

    Crişan, Maria; Zaharescu, Maria; Kumari, Valluri Durga; Subrahmanyam, Machiraju; Crişan, Dorel; Drăgan, Nicolae; Răileanu, Mălina; Jitianu, Mihaela; Rusu, Adriana; Sadanandam, Gullapelli; Krishna Reddy, Jakkidi


    The sol-gel process provides a new approach to the preparation of oxide materials and offers many advantages for making catalysts. Since homogeneous mixing can be achieved at the molecular scale, the chemical reactivity of the oxide surface can be greatly enhanced; thus powders with high surface area and optimized pore size distribution can be obtained at low temperatures. In the present work NiO/Al 2O 3 sol-gel catalysts were obtained by simultaneous gelation of aluminium isopropoxide and nickel nitrate. A comparative study with pure sol-gel alumina was also realized. By physical-structural studies the changes induced by the introduction of the Ni precursor, before and after aluminium alkoxide hydrolysis were highlighted. The introduction of Ni at the beginning of the reaction favors γ-Al 2O 3 crystallization. When Ni is added at the end of reaction, it delays the alumina crystallization and induces the disorder of the lattice. The obtained Ni doped sol-gel derived alumina has been used as catalyst in the finished form for glycerol reforming to generate H 2 for fuel cell applications. Some evaluation results of Ni-doped alumina combined with TiO 2 in photocatalytic glycerol reforming reaction have been included.

  12. Applications of sol gel ceramic coatings

    Barrow, D. [Datec Coating Corp., Kingston, Ont. (Canada)


    The sol gel method is a chemical technique in which polycrystalline ceramic films are fabricated from a solution of organometallic precursors. The technique is attractive for many industrial applications because it is a simple (films are processed in air), flexible (can be used to coat complex geometries) and cost effective (does not require expensive equipment) process. In addition, dense, high quality coatings can be achieved at much lower temperatures than is generally required for sintering bulk ceramics. In this paper the conventional sol gel method and the new datec process are reviewed and potential applications of sol gel coatings in automotive, aerospace, petrochemical, nuclear and electronic industries are discussed. (orig.)

  13. Optical and electrical properties study of sol-gel derived Cu2ZnSnS4 thin films for solar cells

    B. L. Guo


    Full Text Available The fabrication of environmental-friendly Cu2ZnSnS4 (CZTS thin films with pure kesterite phase is always a challenge to researchers in the field of solar cells. We introduce a simple non-vacuum sol-gel method to fabricate kesterite CZTS films. Ethylenediamine is used as the chelating agent and stabilizer and plays an important role in preparing stable precursor. X-ray diffraction, Raman and scanning electron microscopy studies suggest that the microstructure and optical properties of CZTS films depend strongly on annealing temperatures. The temperature dependence of conductivity of 500 °C annealed CZTS film shows that the Mott law dominates in the low temperature region and thermionic emission is predominant at high temperatures.

  14. High luminescent Eu{sup 3+} and Tb{sup 3+} doped SnO{sub 2} sol-gel derived films deposited on porous silicon

    Elhouichet, H.; Moadhen, A.; Oueslati, M. [Laboratoire de Physique de la Matiere Condensee, Departement de Physique, Faculte des Sciences de Tunis, 1060 Le Belvedere, Tunis (Tunisia); Ferid, M. [Institut National de Recherche Scientifique et Technique, B.P. 95, Hammam-Lif 2050 (Tunisia); Canut, B.; Roger, J.A. [Departement de Physique de la Matiere Condensee et Nanostructures, UMR CNRS 5586, Universite Claude Bernard, Lyon 1, 69622 Villeurbanne Cedex (France)


    Tin oxide doped with europium (SnO{sub 2}:Eu{sup 3+}) or doped with europium and terbium (SnO{sub 2}:(Eu{sup 3+}+Tb{sup 3+})), prepared from the sol-gel technique, is incorporated into luminescent porous silicon (PS) layers. Rutherford Backscattering (RBS) measurements reveal a complete and uniform penetration of tin, oxygen, and rare earth into the PS layer. Photoluminescence (PL) studies show that the PL peaks of rare earth are superposed to the PL band of the PS. It has been found that the recovered PL signal of the PS band is improved by adding Eu{sup 3+} to the SnO{sub 2} sol and is further improved by adding Eu{sup 3+} and Tb{sup 3+}. We show that a process of excitation transfer occurs from Eu{sup 3+} and Tb{sup 3+} to Si nanocrystallites. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

  15. Eu3+ probe ion for rare-earth dopant site structure in sol-gel derived LiYF4 oxyfluoride glass-ceramic

    Secu, C. E.; Negrea, R. F.; Secu, M.


    Sol-gel route using metal alkoxides and trifluoroacetic acid as precursors has been used to prepare oxyfluoride glass-ceramic containing Eu3+-doped LiYF4 nanocrystals of about tens of nm size embedded in a silica matrix through controlled crystallization at higher temperatures of the xerogel. Photoluminescence spectra and decay curves recorded in the Eu3+-doped LiYF4 polycrystalline pellet and glass ceramic have been discussed using group-theoretical arguments. In the glass-ceramic Eu3+ ions are embedded dominantly inside the LiYF4 nanocrystals most probably as Eu-O center and/or dimer centers in low symmetry (C2v) sites; oxygen ions were incorporated in their neighborhood during the glass ceramization.

  16. Enhanced self-repairing capability of sol-gel derived SrTiO3/nano Al2O3 composite films

    Yao, Manwen; Peng, Yong; Xiao, Ruihua; Li, Qiuxia; Yao, Xi


    SrTiO3/nano Al2O3 inorganic nanocomposites were prepared by using a conventional sol-gel spin coating process. For comparison, SrTiO3 films doped by equivalent amount of sol-Al2O3 have also been investigated. Aluminum deposited by using vacuum evaporation was used as the top electrode. The nanocomposites exhibited a significantly enhanced dielectric strength of 506.9 MV/m, which was increased by 97.4% as compared with the SrTiO3 films doped with sol-Al2O3. The leakage current maintained of the same order of microampere until the ultimate breakdown of the nanocomposites. The excellent electrical performances are ascribed to the anodic oxidation reaction in origin, which can repair the internal and/or surface defects of the films.

  17. Preparation of Scratch-Resistant Nano-Porous Silica Films Derived by Sol-Gel Process and Their Anti-reflective Properties

    Guangming WU; Jun SHEN; Tianhe YANG; Bin ZHOU; Jue WANG


    Structural strengthening of the nano porous silica films has been reported. The films were prepared with a base/acid two-step catalyzed TEOS-based sol-gel processing and dip-coating, and then baked in the mixed gas of ammonia and water vapor. The silica films were characterized with TEM, AFM, FTIR, spectrophotometer, ellipsometer, and abrasion test, respectively. The experimental results have shown that the films have a nanostructure with a low refractive index and can form an excellent scratch-resistant broadband anti-reflectance. The two-step catalysis noticeably strengthens the films, and the mixed gas treatment further improves mechanical strength of the silica network. Finally the strengthening mechanism has been discussed.

  18. Site-selective spectroscopy in Sm{sup 3+}-doped sol-gel-derived nano-glass-ceramics containing SnO{sub 2} quantum dots

    Yanes, A C; Castillo, J del [Departamento de Fisica Basica, Universidad de La Laguna, E-38206 La Laguna, Tenerife (Spain); Velazquez, J J; Mendez-Ramos, J; RodrIguez, V D [Departamento de Fisica Fund. y Experimental, Universidade La Laguna, E-38206 La Laguna, Tenerife (Spain)], E-mail:, E-mail:


    Nano-glass-ceramics of composition 95SiO{sub 2}-5SnO{sub 2} doped with 0.4 Sm{sup 3+} (mol%) were synthesized by the thermal treatment of precursor sol-gel glasses. Structural and luminescence measurements were carried out. The precipitated SnO{sub 2} nanocrystals in the glass matrix constitute a wide bandgap quantum-dot system with size comparable to the bulk exciton Bohr radius. A site-selective excitation, by energy transfer from the semiconductor host, reveals that a fraction of the Sm{sup 3+} ions are incorporated in the SnO{sub 2} nanocrystals, whereas the rest remains in the silica glassy phase. An evolution in the Sm{sup 3+} emission spectra has been observed when the SnO{sub 2} nanocrystals are excited with different UV wavelengths, which has been ascribed to selective excitation of nanocrystal sets with predetermined size.

  19. Sol-gel synthesis of Y xGd 2- xSiO 5:Eu 3+ phosphors derived from the in situ assembly of multicomponent hybrid precursors

    Huang, Honghua; Yan, Bing


    Using rare earth coordination polymers with salicylic acid as precursors for the luminescence species Y xGd 2- xSiO 5:Eu 3+, composing the polyvinyl alcohol (PVA) as dispersing media, nanophosphors of Y xGd 2- xSiO 5:Eu 3+ ( x = 0.10, 0.25, 0.50, 0.75, 0.90) with different molar ratio of Y and Gd were synthesized by the sol-gel process. Both X-ray diffraction and scanning electronic microscope show that these materials have the nanometer size of 100-200 nm. These nanometer materials exhibit red emission at 612 nm. When x = 0.5, Y 0.5Gd 1.5SiO 5:Eu 3+ shows the strongest emission intensity comparing with other molar ratio of Y to Gd.

  20. Sol-gel deposited electrochromic coatings

    Ozer, N.; Lampert, C.M.


    Electrochromic devices have increasing application in display devices, switchable mirrors and smart windows. A variety of vacuum deposition technologies have been used to make electrochromic devices. The sol- gel process offers an alternative approach to the synthesis of optical quality and low cost electrochromic device layers. This study summarizes the developments in sol-gel deposited electrochromic films. The sol-gel process involves the formation of oxide networks upon hydrolysis-condensation of alkoxide precursors. In this study we cover the sol-gel deposited oxides of WO[sub 3], V[sub 2]O[sub 5], TiO[sub 2], Nb[sub 2]O[sub 5], and NiO[sub x].

  1. Sol-gel antireflective coating on plastics

    Ashley, Carol S.; Reed, Scott T.


    An antireflection film made from a reliquified sol-gel hydrolyzation, condensation polymeric reaction product of a silicon, alkoxides and/or metal alkoxides, or mixtures thereof. The film is particularly useful for coating plastics.

  2. A silica sol-gel design strategy for nanostructured metallic materials.

    Warren, Scott C; Perkins, Matthew R; Adams, Ashley M; Kamperman, Marleen; Burns, Andrew A; Arora, Hitesh; Herz, Erik; Suteewong, Teeraporn; Sai, Hiroaki; Li, Zihui; Werner, Jörg; Song, Juho; Werner-Zwanziger, Ulrike; Zwanziger, Josef W; Grätzel, Michael; DiSalvo, Francis J; Wiesner, Ulrich


    Batteries, fuel cells and solar cells, among many other high-current-density devices, could benefit from the precise meso- to macroscopic structure control afforded by the silica sol-gel process. The porous materials made by silica sol-gel chemistry are typically insulators, however, which has restricted their application. Here we present a simple, yet highly versatile silica sol-gel process built around a multifunctional sol-gel precursor that is derived from the following: amino acids, hydroxy acids or peptides; a silicon alkoxide; and a metal acetate. This approach allows a wide range of biological functionalities and metals--including noble metals--to be combined into a library of sol-gel materials with a high degree of control over composition and structure. We demonstrate that the sol-gel process based on these precursors is compatible with block-copolymer self-assembly, colloidal crystal templating and the Stöber process. As a result of the exceptionally high metal content, these materials can be thermally processed to make porous nanocomposites with metallic percolation networks that have an electrical conductivity of over 1,000 S cm(-1). This improves the electrical conductivity of porous silica sol-gel nanocomposites by three orders of magnitude over existing approaches, opening applications to high-current-density devices.

  3. Preparation and application of the sol-gel-derived acrylate/silicone co-polymer coatings for headspace solid-phase microextraction of 2-chloroethyl ethyl sulfide in soil.

    Liu, Mingming; Zeng, Zhaorui; Fang, Huaifang


    Three types of novel acrylate/silicone co-polymer coatings, including co-poly(methyl acrylate/hydroxy-terminated silicone oil) (MA/OH-TSO), co-poly(methyl methacrylate/OH-TSO) (MMA/OH-TSO) and co-poly(butyl methacrylate/OH-TSO) (BMA/OH-TSO), were prepared for the first time by sol-gel method and cross-linking technology and subsequently applied to headspace solid-phase microextraction (HS-SPME) of 2-chloroethyl ethyl sulfide (CEES), a surrogate of mustard, in soil. The underlying mechanisms of the coating process were discussed and confirmed by IR spectra. The selectivity of the three types of sol-gel-derived acrylate/silicone coated fibers was studied, and the BMA/OH-TSO coated fibers exhibited the highest extraction ability to CEES. The concentration of BMA and OH-TSO in sol solution was optimized, and the BMA/OH-TSO (3:1)-coated fibers possessed the highest extraction efficiency. Compared with commercially available polyacrylate (PA) fiber, the sol-gel-derived BMA/OH-TSO (3:1) fibers showed much higher extraction efficiency to CEES. Therefore, the BMA/OH-TSO (3:1)-coated fibers were chosen for the analysis of CEES in soil matrix. The reproducibility of coating preparation was satisfactory, with the RSD 2.39% within batch and 3.52% between batches, respectively. The coatings proved to be quite stable at high temperature (to 350 degrees C) and in different solvents (organic or inorganic), thus their lifetimes (to 150 times) are longer than conventional fibers. Extraction parameters, such as the volume of water added to the soil, extraction temperature and time, and the ionic strength were optimized. The linearity was from 0.1 to 10 microg/g, the limit of detection (LOD) was 2.7 ng/g, and the RSD was 2.19%. The recovery of CEES was 88.06% in agriculture soil, 92.61% in red clay, and 101.95% in sandy soil, respectively.

  4. Luminescence characterization of sol-gel derived Pr{sup 3+} doped NaGd(WO{sub 4}){sub 2} phosphors for solid state lighting applications

    Durairajan, A., E-mail: [Crystal Growth Centre, Anna University, Chennai, 600025 (India); I3N-Aveiro, Department of Physics, University of Aveiro, Aveiro, 3810 193 (Portugal); Thangaraju, D. [Research Institute of Electronics, Shizuoka University, 3-5-1 Johoku, Hamamatsu, Shizuoka, 432-8011 (Japan); Moorthy Babu, S. [Crystal Growth Centre, Anna University, Chennai, 600025 (India); Valente, M.A. [I3N-Aveiro, Department of Physics, University of Aveiro, Aveiro, 3810 193 (Portugal)


    In the present work, xPr{sup 3+}:NaGd(WO{sub 4}){sub 2} (0.5 ≤ x ≤ 5.0 mol%) sub-micron phosphors were synthesised by sol-gel method. Low cost precursors of metal nitrates and low temperature thermal treatment was used compared to conventional solid state reaction. The formation of highly crystalline phosphors with tetragonal structure was confirmed by XRD and increase of Pr{sup 3+} ions content in host matrix leads to expansion of the unit cell volume. The surface morphology, size and particle distribution of the phosphors were observed by field emission scanning electron microscopy (FE-SEM). A rectangular shape particle with a size distribution ranging from 400 to 600 nm and tightly packed surface was seen in FE-SEM micrographs. The various internal and external phonon modes vibration corresponding to double tungstate structure was observed in Raman spectra. The optical properties of the synthesised phosphors were explored by ultraviolet visible (UV–Vis) absorption in diffuse reflectance and photoluminescence (PL) measurements. UV–Vis measurements distinguished the host and Pr{sup 3+} absorption and also reveal an increase in optical band gap values with an increase of Pr{sup 3+}. The PL measurements show various emissions from green and red regions under 450 nm. The maximum intensity emission at 489 nm is due to {sup 3}P{sub 0} → {sup 3}H{sub 4} transition of Pr{sup 3+}. From the maximum emission the critical doping concentration was calculated to be at 3.5 mol% and critical distance between two adjacent Pr{sup 3+} ions as 20.43 Å. - Highlights: • A sol-gel method was used to prepare Pr{sup 3+} doped NaGd(WO{sub 4}){sub 2} at low temperature. • Structural, spectroscopic, morphological, and optical and luminescence properties were studied. • The praseodymium ions are in trivalent state, the site symmetry is distorted and S{sub 4} local symmetry with Na{sup +} ions. • Strong green emission was observed under UV and visible excitation.

  5. A sol-gel derived pH-responsive bovine serum albumin molecularly imprinted poly(ionic liquids) on the surface of multiwall carbon nanotubes.

    Liu, Mingming; Pi, Jiangyan; Wang, Xiaojie; Huang, Rong; Du, Yamei; Yu, Xiaoyang; Tan, Wenfeng; Liu, Fan; Shea, Kenneth J


    A pH-responsive surface molecularly imprinted poly(ionic liquids) (MIPILs) was prepared on the surface of multiwall carbon nanotubes (MWCNTs) by a sol-gel technique. The material was synthesized using a 3-aminopropyl triethoxysilane modified multiwall carbon nanotube (MWCNT-APTES) as the substrate, bovine serum albumin (BSA) as the template molecule, an alkoxy-functionalized IL 1-(3-trimethoxysilyl propyl)-3-methyl imidazolium chloride ([TMSPMIM]Cl) as both the functional monomer and the sol-gel catalyst, and tetraethoxysilane (TEOS) as the crosslinking agent. The molecular interaction between BSA and [TMSPMIM]Cl was quantitatively evaluated by UV-vis spectroscopy prior to polymerization so as to identify an optimal template/monomer ratio and the most suitable pH value for the preparation of the MWCNTs@BSA-MIPILs. This strategy was found to be effective to overcome the problems of trial-and-error protocol in molecular imprinting. The optimum synthesis conditions were as follows: template/monomer ratio 7:20, crosslinking agent content 2.0-2.5 mL, temperature 4 °C and pH 8.9 Tris-HCl buffer. The influence of incubation pH on adsorption was also studied. The result showed that the imprinting effect and selectivity improved significantly with increasing incubation pH from 7.7 to 9.9. This is mainly because the non-specific binding from electrostatic and hydrogen bonding interactions decreased greatly with the increase of pH value, which made the specific binding affinity from shape selectivity strengthened instead. The polymers synthesized under the optimal conditions were then characterized by BET surface area measurement, FTIR, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The adsorption capacity, imprinting effect, selective recognition and reusability were also evaluated. The as-prepared MWCNTs@BSA-MIPILs were also found to have a number of advantages including high surface area (134.2 m(2) g(-1)), high adsorption capacity (55.52

  6. Structural and Electrical Properties of TiO2 Thin Film Derived from Sol-gel Method using Titanium (IV Butoxide

    Isrihetty Senain


    Full Text Available Fabrication of titanium dioxide (TiO2 thin film on microscope glass using sol-gel method has been studied intensively. The starting materials were titanium (IV butoxide, ethanol, acetic acid, triton x-100, hydrochloric acid and deionized water. The materials were mixed together to form the sols. Then, the heat and ageing treatment was applied to form stable sols. The sols were then spin coated on the glass substrate to form the homogenous and transparent TiO2 thin film. The TiO2 thin film was coated at several layers using specific conditions. To evaluate the performance of thin film, the crystallinity of the thin film was determined by using the x-ray diffractometer  (XRD. The change on the surface morphology was observed using atomic force microscope (AFM. The electrical property of the thin film was determined by doing the current-voltage (I-V analysis on the thin film. It has been successfully shown that the anatase crystalline phase was observed when the TiO2 thin film was heated at 500°C. The roughness and the crystalline phase of TiO2 thin film changed drastically with the growth conditions. Finally, the effect of film preparation to the film resistivity also showed a critical aspect where we should take into account during the preparation of TiO2 thin film.

  7. Microstructure evolution of zinc oxide films derived from dip-coating sol-gel technique: formation of nanorods through orientation attachment.

    Huang, Nan; Sun, Chao; Zhu, Mingwei; Zhang, Bin; Gong, Jun; Jiang, Xin


    ZnO:Al thin films with Al incorporation of 0-20 at.% were deposited through the sol-gel technique. Such a film undergoes a significant microstructure development, from columnar to granular structures and then nanorod arrays with increasing Al content. The important role of Al incorporation level in the microstructure evolution was determined using scanning electron microscopy, x-ray photoelectron spectroscopy and transmission electron microscopy. At low Al level, the transition from columnar to granular grains can be attributed to the coarsening barrier resulting from the introduction of Al into the matrix. However, oriented structures of ZnO nanorod arrays are formed at a high Al level. TEM investigation reveals that a nanorod with smooth morphology at the top and rough morphology at the bottom has a single-crystalline wurtzite structure, which is the aggregation of nanoparticles of a few nanometers in size formed through the orientation attachment mechanism followed by epitaxial growth on the aggregated particles. Finally, the physical properties of the ZnO films with different degrees of Al concentration are discussed. Such detailed microstructure studies may aid the understanding of the doping effect process on the growth of a film, which is essential to altering its physical or chemical properties.

  8. Sr and Mn co-doped sol-gel derived BiFeO3 ceramics with enhanced magnetism and reduced leakage current

    Sharma, Nandni; Kumar, Sanjeev; Mall, Ashish Kumar; Gupta, Rajeev; Garg, Ashish


    In this manuscript, we report the effect of Sr and Mn doping on the electrical and magnetic characteristics of BiFeO3 nanoparticles, synthesized by sol-gel technique. While powder diffraction analysis of the samples suggested absence of any structural distortion in both Sr-doped and Sr and Mn co-doped BiFeO3 nanoparticles, Rietveld refinement of the data suggested that the unit cell volume decreases with doping. Room temperature Raman studies of the samples confirmed the incorporation of Sr and Mn in BiFeO3. It was seen that Sr doping of BiFeO3 showed substantial reduction in the leakage current whilst co-doping with Sr and Mn led to lower reduction in the leakage current through offering better performance over undoped BiFeO3, due to changes brought in the defect chemistry upon doping. Additionally, Sr and Mn co-doped BiFeO3 samples exhibit enhanced magnetization in comparison to undoped and Sr doped BiFeO3, possibly due to interruptions in the spin cycloid of BiFeO3.

  9. Characterization of Sol-gel-derived TiO2 and TiO2-SiO2 Films for Biomedical Applications

    Jingxiao LIU; Fei SHI; Dazhi YANG


    In order to improve the corrosion resistance and biocompatibility of NiTi surgical alloy, TiO2 and TiO2-SiO2 thin films were prepared by sol-gel method. The surface characteristics of the film, which include surface composition, microstructure and surface morphology, were studied by X-ray diffraction (XRD), atomic force microscopy (AFM) and X-ray photoelectron spectra (XPS), respectively. A scratching test was used to assess the interface adhesive strength between the film and substrate. The corrosion resistance of NiTi alloy coated with oxide films were studied by anodic polarization curves measurement in biological solution. Additionally, a preliminary study of the in vitro bioactivity of the films was conducted. The results indicated that TiO2 and TiO2-SiO2 (Ti/Si=4:1) films have higher electrochemical corrosion resistance and can be used as protective layers on NiTi alloy. In addition, TiO2-SiO2 composite films have better bioactivity than TiO2 film.

  10. Influence of surfactant and annealing temperature on optical properties of sol-gel derived nano-crystalline TiO2 thin films.

    Vishwas, M; Sharma, Sudhir Kumar; Rao, K Narasimha; Mohan, S; Gowda, K V Arjuna; Chakradhar, R P S


    Titanium dioxide thin films have been synthesized by sol-gel spin coating technique on glass and silicon substrates with and without surfactant polyethylene glycol (PEG). XRD and SEM results confirm the presence of nano-crystalline (anatase) phase at an annealing temperature of 300 degrees C. The influence of surfactant and annealing temperature on optical properties of TiO(2) thin films has been studied. Optical constants and film thickness were estimated by Swanepoel's (envelope) method and by ellipsometric measurements in the visible spectral range. The optical transmittance and reflectance were found to decrease with an increase in PEG percentage. Refractive index of the films decreased and film thickness increased with the increase in percentage of surfactant. The refractive index of the un-doped TiO(2) films was estimated at different annealing temperatures and it has increased with the increasing annealing temperature. The optical band gap of pure TiO(2) films was estimated by Tauc's method at different annealing temperature.

  11. Investigation of the surface reactivity of a sol-gel derived glass in the ternary system SiO 2-CaO-P 2O 5

    Mami, Mohamed; Lucas-Girot, Anita; Oudadesse, Hassane; Dorbez-Sridi, Rachida; Mezahi, Fatima; Dietrich, Elodie


    A new glass formulation, with the molar composition 60% SiO 2-35% CaO-5% P 2O 5, was synthesized using the sol-gel process, for applications as biomaterial in orthopaedic or maxillo facial surgery. Pellets, made of glass powder, were uniaxially compacted and soaked in simulated body fluid (SBF) for up to 7 days at 37 °C to evaluate glass bioactivity. Ionic exchanges at the interface glass-SBF were evaluated by studying evolutions of calcium, phosphorus and silicon concentrations in SBF using ICP-OES. Changes in glass surface, and the formation of crystalline phases were analyzed using XRD, SEM, EDS and FTIR methods. Results form ICP-OES showed a high reactivity of the glass surface with a very high and continuous release of calcium, a limited glass dissolution and an uptake of phosphorous from SBF. Results from both FTIR and XRD analysis indicated that the glass surface was progressively covered by two different phases: CaCO 3 as calcite and a carbonated apatite layer. The formation of these phases, following two different schemas, was observed after 2 h of immersion and confirmed after 7 days. SEM micrographs and EDS analysis demonstrated that the main phase, a carbonated apatite, was present as micro-spheroids and the secondary phase, calcite, was materialized by agglomerates which have diameters up to 10-15 μm. These results are in accordance with a bioactive feature of the glass studied.

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

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


    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.

  13. The influence of silver nanostructures formed in situ in silica sol-gel derived films on the rate of Förster resonance energy transfer.

    Holmes-Smith, A Sheila; McDowell, Gary R; Toury, Marion; McLoskey, David; Hungerford, Graham


    The efficiency of Förster resonance energy transfer (FRET) can be enhanced in the presence of a metal. Herein, we demonstrate the increased efficiency for a novel model sensor system where FRET is shown to occur between Rhodamine 6G in the bulk sol-gel matrix and Texas Red, which is held a fixed distance away by covalent attachment onto a silane spacer. Silver colloids are formed using light to initiate the reduction of a silver salt, which can be achieved at controlled locations within the film. Both the fluorescence intensity and lifetime maps and analysis indicate that an enhanced FRET efficiency has been achieved in the presence of silver nanoparticles. An increase in efficiency of 1.2-1.5 times is demonstrated depending on the spacer used. The novelty of our approach lies in the method of silver-nanoparticle formation, which allows for the accurate positioning of the silver nanoparticles and hence selective fluorescence enhancement within a biocompatible host material. Our work gives a practical demonstration of metal-enhanced FRET and demonstrates the ability of such systems to be developed for molecular-recognition applications that could find use in lab-on-a-chip technologies. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Highly (1 1 1)-oriented and pyrochlore-free PMN-PT thin films derived from a modified sol-gel process

    Feng, M. [Institute for Advanced Ceramics, Department of Materials Science and Engineering, Harbin Institute of Technology, No. 92, West Da-Zhi Street, Heilongjiang, Harbin 150001 (China); Wang, W., E-mail: [Institute for Advanced Ceramics, Department of Materials Science and Engineering, Harbin Institute of Technology, No. 92, West Da-Zhi Street, Heilongjiang, Harbin 150001 (China); Ke, H.; Rao, J.C.; Zhou, Y. [Institute for Advanced Ceramics, Department of Materials Science and Engineering, Harbin Institute of Technology, No. 92, West Da-Zhi Street, Heilongjiang, Harbin 150001 (China)


    Ferroelectric PMN-PT (68/32) thin films, about 250 nm in thickness, have been successfully grown on Pt/Ti/SiO{sub 2}/Si substrate by a modified sol-gel process. Pure perovskite phase with highly (1 1 1)-preferred orientation, determined by X-ray diffraction, was formed in the PMN-PT thin films when annealed at 650 {sup o}C. The pyrochlore phase has been effectively avoided through a variation of the processing parameters such as Mg content, Mg precursor and annealing temperature during thin film deposition. FE-SEM investigation showed that the films have a smooth and crack-free surface with densely packed grains after annealed at 650 {sup o}C. The annealed films exhibited well-defined hysteresis loops, with a respective remanent polarization P{sub r} of 16.1 {mu}C/cm{sup 2} and coercive field E{sub c} of 71.2 kV/cm at an applied electric field of 400 kV/cm at room temperature.

  15. Microwave sol-gel derived NaCaGd(MoO4)3:Er3+/Yb3+ phosphors and their upconversion photoluminescence properties

    Lim, Chang Sung


    Ternary molybdate NaCaGd1-x(MoO4)3:Er3+/Yb3+ phosphors with the proper doping concentrations of Er3+ and Yb3+ (x = Er3+ + Yb3+, Er3+ = 0, 0.05, 0.1, 0.2 and Yb3+ = 0, 0.2, 0.45) were successfully synthesized by microwave sol-gel method for the first time. Well-crystallized particles formed after heat-treatment at 900 °C for 16 h showed a fine and homogeneous morphology with particle sizes of 3-5 μm. The optical properties were examined comparatively using photoluminescence emission and Raman spectroscopy. Under excitation at 980 nm, the doped particles exhibited a strong 525-nm emission band, a weak 550-nm emission band in the green region, which correspond to the 2H11/2 → 4I15/2 and 4S3/2 → 4I15/2 transitions, and a very weak 655-nm emission band in the red region, which corresponds to the 4F9/2 → 4I15/2 transition. The optimal Yb3+:Er3+ ratio was obtained to be 9:1, as indicated by the composition-dependent quenching effect of Er3+ ions. The pump power dependence of upconversion emission intensity and Commission Internationale de L'Eclairage chromaticity coordinates of the phosphors were evaluated in detail.

  16. In vitro antibacterial evaluation of sol-gel-derived Zn-, Ag-, and (Zn + Ag)-doped hydroxyapatite coatings against methicillin-resistant Staphylococcus aureus.

    Samani, S; Hossainalipour, S M; Tamizifar, M; Rezaie, H R


    Hydroxyapatite (HAp) coatings were applied using sol-gel method. Phosphor pentoxide and calcium nitrate were used as phosphorous and calcium precursors, respectively. Zinc nitrate and silver nitrate were used as substitute of calcium in HAp structure. As a base concentration, 1.5 wt %Ag and 2.5 wt %Zn were used. The weight percent of Ag was increased at 0.3 wt% and Zn content was scaled down at 0.5 wt%. Phase analysis and chemical bonds of synthesized materials were studied by XRD and FTIR. Antibacterial activity of Ag- and Zn-doped samples against methicilin-resistant Staphylococcus aureus (MRSA) were assessed by the plate-counting method. The XRD and FTIR results proved formation of HAp compound. Colony counting showed that silver and zinc ions prevent proliferation and growth of MRSA. Interestingly, co-presence of metal ions improves the antibacterial effectiveness of the coatings and the combined effect was greater than sum of the individual effects when each was administered alone. Overall, synergism between antibacterial activities of Zn(2+) and Ag(+) ions against MRSA can be suggested. Thus, cell toxicity decreases and biocompatibility increases without any decrement in antibacterial activity.

  17. Sol-gel-derived bioactive glass containing SiO2-MgO-CaO-P2O5 as an antibacterial scaffold.

    Fooladi, Abbas Ali Imani; Hosseini, Hamideh Mahmoodzadeh; Hafezi, Forough; Hosseinnejad, Fatemeh; Nourani, Mohammad Reza


    Bioactive glass (BG) composites with a base of SiO2-Na2O-CaO-P2O5 are biocompatible biomaterials. The assessment of their abilities for medical applications has interested researchers. We produced a BG-containing SiO2-MgO-CaO-P2O5 by the sol-gel method. To determine the antibacterial effects, we analyzed the minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) properties of this product on three microorganisms, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa, known causative agents for biofilm formation on implant surfaces. In addition, we performed the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay to study the cytotoxic effects of our composite on animal cells. Our results demonstrated that our BG product inhibited the growth of bacteria in a concentration-dependent manner without any cytotoxic effects. Therefore, our BG product can be utilized as an appropriate implant for treating bone and tooth defects.

  18. Evaluation of sol-gel derived Eu{sup 2+} activated SrMgAl{sub 2}SiO{sub 7} as a novel nanostructure luminescent pigment

    Sameie, H.; Salimi, R. [Faculty of Polymer and Color Engineering, Amirkabir University of Technology, P.O. Box 15875-4413, Tehran (Iran, Islamic Republic of); Sabbagh Alvani, A.A., E-mail: [Color and Polymer Research Center (CPRC), Amirkabir University of Technology, P.O. Box 15875-4413, Tehran (Iran, Islamic Republic of); Sarabi, A.A. [Faculty of Polymer and Color Engineering, Amirkabir University of Technology, P.O. Box 15875-4413, Tehran (Iran, Islamic Republic of); Moztarzadeh, F.; Tahriri, M. [Biomaterials Group, Faculty of Biomedical Engineering, Amirkabir University of Technology, P.O. Box 15875-4413, Tehran (Iran, Islamic Republic of)


    A novel nanostructure pigment of Eu{sup 2+} doped SrMgAl{sub 2}SiO{sub 7} was prepared via the sol-gel route. The phase composition and condition of crystallites during heating were characterized by X-ray diffraction (XRD) analysis. Investigation of optical properties by spectrophotometer illustrated that under short ultraviolet excitation wavelength, the main emission peak occurred at about 415-420 nm. Also, relatively pure purplish blue color was observed that can be ascribed to the 4f{sup 6}5d{sup 1}({sup 2}D){yields}4f{sup 7}({sup 8}S{sub 7/2}) transition of Eu{sup 2+}. The effect of calcination temperature on the luminescence properties of the phosphors was evaluated and, also in this case, scanning electron microscope (SEM) was employed. From colorimetry results, color coordinations of phosphor shift towards the deep blue region as calcination temperature increases. Finally, grain size of products at optimum calcination temperature was estimated to be about 20-30 nm using Scherrer's equation, which was consistent with transmission electron microscopy (TEM) observations.

  19. First observation of sol-gel derived Al:CsZnO/CsZnO bilayer thin film for solar cells application

    Ahmadi, Mehdi; Rashidi Dafeh, Sajjad; Alinazmabadi, Saeid


    In this research, we fabricated CsZnO and Al:CsZnO/CsZnO bilayer thin films grown by the spin-coating-assisted sol-gel method on ITO substrate. The influence of diverse velocity of spin-coating (500, 1000, 1500, 2000, 2500 and 3000RPM) and also annealing times (30, 60, 90, 120, 150 and 180min) on the characteristics of the ZnO thin film was examined. The samples were examined by X-ray diffraction, scanning electron microscopy, Uv-Vis spectrometer and conductivity measurement. With the optimization of the velocity of spin-coating (2500RPM) and annealing times (60min), we fabricated Al:CsZnO/CsZnO bilayer thin films with diverse dopant concentration. By comparing the effect of dopant concentration with different dopant ratio (0, 0.5, 1.0 and 2%), 0.5% of CsZnO and Al:CsZnO/CsZnO bilayer was found as the most effective doping level with the best conductivity properties among the selected doping concentrations.

  20. Influence of heat treatment on bond strength and corrosion resistance of sol-gel derived bioglass-ceramic coatings on magnesium alloy.

    Shen, Sibo; Cai, Shu; Xu, Guohua; Zhao, Huan; Niu, Shuxin; Zhang, Ruiyue


    In this study, bioglass-ceramic coatings were prepared on magnesium alloy substrates through sol-gel dip-coating route followed by heat treatment at the temperature range of 350-500°C. Structure evolution, bond strength and corrosion resistance of samples were studied. It was shown that increasing heat treatment temperature resulted in denser coating structure as well as increased interfacial residual stress. A failure mode transition from cohesive to adhesive combined with a maximum on the measured bond strength together suggested that heat treatment enhanced the cohesion strength of coating on the one hand, while deteriorated the adhesion strength of coating/substrate on the other, thus leading to the highest bond strength of 27.0MPa for the sample heat-treated at 450°C. This sample also exhibited the best corrosion resistance. Electrochemical tests revealed that relative dense coating matrix and good interfacial adhesion can effectively retard the penetration of simulated body fluid through the coating, thus providing excellent protection for the underlying magnesium alloy.

  1. Effect of polyvinyl alcohol content and after synthesis neutralization on structure, mechanical properties and cytotoxicity of sol-gel derived hybrid foams

    Agda Aline Rocha de Oliveira


    Full Text Available Bioactive glass/polymer hybrids are promising materials for biomedical applications because they combine the bioactivity of these glasses with the flexibility of polymers. In this work it was evaluated the effect of increasing the PVA content of the on structural characteristics and mechanical properties of hybrid. The hybrids were prepared with 70 wt. (% SiO2-30 wt. (% CaO and PVA fractions of 20 to 60 wt. (% by the sol-gel method. The structural and mechanical characterization was done by FTIR, SEM and compression tests. To reduce the acidic character of the hybrids due to the catalysts added, different neutralization solutions were tested. The calcium acetate alcoholic solution was the best neutralizing method, resulting in foams with final pH of about 7.0 and small sample contraction. The foams presented porosity of 60-85 wt. (% and pore diameters of 100-500 μm with interconnected structure. An increase of PVA fraction in the hybrids improved their mechanical properties. The scaffolds produced provided a good environment for the adhesion and proliferation of osteoblasts.

  2. Solvent-resistant sol-gel polydimethyldiphenylsiloxane coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

    Segro, Scott S; Malik, Abdul


    A sol-gel polydimethyldiphenylsiloxane (PDMDPS) coating was developed for capillary microextraction on-line hyphenated with high-performance liquid chromatography (HPLC). This coating was created using methyltrimethoxysilane (MTMS) as the sol-gel precursor and di-hydroxy-terminated PDMDPS as the sol-gel active polymer. The methyl and phenyl groups on the sol-gel active polymer and the methyl groups on the sol-gel precursor ultimately turned into pendant groups providing the ability to extract non-polar analytes. A 40-cm segment of 0.25 mm I.D. fused silica capillary containing the sol-gel PDMDPS coating was installed as an external sampling loop in an HPLC injection port. Aqueous samples containing polycyclic aromatic hydrocarbons (PAHs), aromatic compounds, ketones, and aldehydes were passed through this capillary wherein the analytes were extracted by the sol-gel coating. The extracted analytes were then transferred to the HPLC column using isocratic or gradient elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for non-polar (e.g., polycyclic aromatic hydrocarbons and aromatic compounds) as well as moderately polar compounds, such as aromatic amines, ketones, and aldehydes. The test results indicate that PDMDPS can be successfully immobilized into a sol-gel network and that the resulting solvent-resistant sol-gel organic-inorganic hybrid coating can be effectively used for on-line hyphenation of capillary microextraction with high-performance liquid chromatography. The test results also indicate that the sol-gel PDMDPS coated capillary is resistant to high-temperature solvents, making it suitable for applications in high-temperature HPLC. To the best of our knowledge, this is the first report on the creation of a silica-based sol-gel PDMDPS coating used in capillary microextraction on-line hyphenated to HPLC.

  3. Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

    Chu, Chung-tse; Zheng, Haixing


    Advanced materials play an important role in the development of electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. The sol-gel process is a versatile solution for use in the fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. This processing technique is particularly useful in producing porous materials with high surface area and low density, two of the most desirable characteristics for electrode materials. In addition,the porous surface of gels can be modified chemically to create tailored surface properties, and inorganic/organic micro-composites can be prepared for improved material performance device fabrication. Applications of several sol-gel derived electrode materials in different energy storage devices are illustrated in this paper. V2O5 gels are shown to be a promising cathode material for solid state lithium batteries. Carbon aerogels, amorphous RuO2 gels and sol-gel derived hafnium compounds have been studied as electrode materials for high energy density and high power density electrochemical capacitors.

  4. A solid-phase microextraction coating of sol-gel-derived perhydroxy cucurbit[6]uril and its application on to the determination of polycyclic aromatic hydrocarbon.

    Dong, Nan; Li, Tao; Luo, Yujie; Shao, Lin; Tao, Zhu; Zhu, Chun


    A novel solid-phase microextraction coating that contains perhydroxy cucurbit[6]uril((OH)12Q[6]) was prepared by a sol-gel method. (OH)12Q[6] was used as a starting coating material with hydroxy-terminated poly(dimethylsiloxane) (OH-PDMS) to bond chemically to a fused-silica substrate using 3-(2-cyclooxypropoxyl)propyltrimethoxysilane as cross-linking agent; hydrolysis and polycondensation reactions then led to the formation of a (OH)12Q[6]/PDMS-coating. The coating has a high thermal stability (360°C), long lifetime and can withstand organic and inorganic solvent rinsing because of the chemical binding between the coating and silica substrate. Its performance was tested by headspace (HS) solid-phase microextraction fiber coupled with gas chromatography to determine polycyclic aromatic hydrocarbon (PAHs) compounds in water samples. The (OH)12Q[6]/PDMS-coated fiber exhibited higher enrichment factors from fourfold for naphthalene to tenfold for pyrene compared with commercial PDMS fiber, and the enrichment factors increased with the number of condensed PAH rings. The strong adsorption affinity is believed to be attributed to hydrogen bonding and CH⋯π interactions between PAHs and (OH)12Q[6], according to the results of quantum chemical calculations. In the PAH analysis, the (OH)12Q[6]-coated fiber showed a good repeatability (<4.7%) and reproducibility between fibers (<9.4%), low detection limits (0.03-0.15μgL(-1)), and a wide linearity (0.1-1000μgL(-1)) under optimized conditions. This method was used for the simultaneous determination of seven PAHs with satisfactory recoveries of 90.56%-107.4% for Huaxi river water samples and 90.23%-109.5% for local wastewater samples, respectively.

  5. Synthesis and Characterization of Sol-Gel-Derived (Pb1-xLax)Ti1-x/4O3 Thin Films

    Chopra, Sonalee; Sharma, Seema; Goel, Tara Chand; Mendiratta, Raj Gopal


    Ferroelectric lead lanthanum titanate (Pb1-xLaxTi1-x/4O3) (PLTx) thin films (x=0.04, 0.08 and 0.12) have been prepared by sol-gel spin-coating process on ITO- coated 7059 Corning glass substrates. Investigations have been made on the crystal structure, surface morphology, dielectric and ferroelectric properties of the thin films. Characterization of these films by X-ray diffraction shows that the films annealed at 650°C exhibit tetragonal structure with perovskite phase. Replacement of lanthanum in lead titanate results in reduction of the tetragonal ratio (c/a), thereby resulting in better mechanical stability. Microstructural analyses of the films are carried out by obtaining atomic force microscope (AFM) images. AFM images are characterized by slight surface roughness with a uniform crack-free, densely packed structure. Dielectric, pyroelectric and ferroelectric studies carried out on these films have been reported. The dielectric constant increases with La concentration. The Curie temperature is found to decrease with the addition of lanthanum. The pyroelectric coefficient increases from 17 nC/cm2K to 31 nC/cm2K as La content increases from 4 to 12%. The pyroelectric figures of merit of the films have been calculated from these studies. These studies indicate that 8% lanthanum is the material best suited for infrared detectors owing to its high pyroelectric coefficient (˜29 nC/cm2K), high voltage responsivity (˜420 Vcm2/J), high detectivity (˜1.04× 10-5 Pa-1/2) and low variation of pyrocoefficient with temperature.

  6. Effect of annealing temperature on the structural, photoluminescence and magnetic properties of sol-gel derived Magnetoplumbite-type (M-type) hexagonal strontium ferrite

    Teh, Geok Bee, E-mail: [Division of Bioscience and Chemistry, School of Arts and Science, Tunku Abdul Rahman College, Jalan Genting Kelang, 53300 Kuala Lumpur (Malaysia); Wong, Yat Choy [Faculty of Engineering and Industrial Sciences, Swinburne University of Technology, PO Box 218, Hawthorn, Victoria 3122 (Australia); Tilley, Richard D. [School of Chemical and Physical Sciences, MacDiarmid Institute of Advanced Materials and Nanotechnology, Victoria University of Wellington, PO Box 600, Wellington (New Zealand)


    Magnetoplumbite-type (M-type) hexagonal strontium ferrite particles were synthesized via sol-gel technique employing ethylene glycol as the gel precursor at two different calcination temperatures (800 and 1000 deg. C). Structural properties were systematically investigated via X-ray diffraction (XRD), field emission scanning electron microscopy, high resolution transmission electron microscopy (HRTEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), photoluminescence spectrophotometry and superconducting quantum interference device magnetometer. XRD results showed that the sample synthesized at 1000 deg. C was of single-phase with a space group of P6{sub 3}/mmc and lattice cell parameter values of a=5.882 A and c=23.048 A. EDS confirmed the composition of strontium ferrite calcined at 1000 deg. C being mainly of M-type SrFe{sub 12}O{sub 19} with HRTEM micrographs confirming the ferrites exhibiting M-type long range ordering along the c-axis of the crystal structure. The photoluminescence (PL) property of strontium ferrite was examined at excitation wavelengths of 260 and 270 nm with significant PL emission peaks centered at 350 nm being detected. Strontium ferrite annealed at higher temperature (1000 deg. C) was found to have grown into larger particle size, having higher content of oxygen vacancies and exhibited 83-85% more intense PL. Both the as-prepared strontium ferrites exhibited significant oxygen vacancies defect structures, which were verified via TGA. Higher calcination temperature turned strontium ferrite into a softer ferrite. - Highlights: > High annealing temperature produced M-type ferrite with higher oxygen vacancies. > Photoluminescence intensity is proportional to the existence of oxygen vacancies. > XRD data showed cell contraction well suited to the change of oxygen vacancies. > Shift in hysteresis loop due to defect-induced exchange bias was observed.

  7. Preparation and bioactivity of sol-gel macroporous bioactive glass

    Zhihua Zhou; Jianming Ruan; Jianpeng Zou; Zhongcheng Zhou


    Bioactive glass is well known for its ability of bone regeneration, and sol-gel bioactive glass has many advantages com-pared with melt-derived bioactive glass. 3-D scaffold prepared by the sol-gel method is a promising substrate material for bone tissue engineering and large-scale bone repair. Porous sol-gel glass in the CaO-SiO2-P2O5 system with macropores larger than 100 μm was prepared by the addition of stearic acid as a pore former. The diameter of the pore created by the pore former varied from 100 to 300μm. The formation of a hydroxyapatite layer on the glass was analyzed by studying the surface of the porous glass by scanning elec-tron microscopy, energy dispersive spectroscopy, X-ray diffraction, and Raman spectra after they had been immersed in simulated body fluid (SBF) for some time, and the porous glass shows good bioactivity.

  8. Hybrid sol-gel optical materials

    Zeigler, John M.


    Hybrid sol-gel materials comprise silicate sols cross-linked with linear polysilane, polygermane, or poly(silane-germane). The sol-gel materials are useful as optical identifiers in tagging and verification applications and, in a different aspect, as stable, visible light transparent non-linear optical materials. Methyl or phenyl silicones, polyaryl sulfides, polyaryl ethers, and rubbery polysilanes may be used in addition to the linear polysilane. The linear polymers cross-link with the sol to form a matrix having high optical transparency, resistance to thermooxidative aging, adherence to a variety of substrates, brittleness, and a resistance to cracking during thermal cycling.

  9. Sol-gel synthesis of lithium aluminate

    Valenzuela, M.A. [Inst. Politecnico Nacional, Mexico City (Mexico); Jimenez-Becerril, J. [Inst. Nacional de Investigaciones Nucleares, Mexico City (Mexico). Dept. de Quimica]|[Univ. Autonoma Metropolitana, Iztapalapa (Mexico). Dept. de Quimica; Bulbulian, S. [Inst. Nacional de Investigaciones Nucleares, Mexico City (Mexico). Dept. de Quimica; Lara, V.H. [Univ. Autonoma Metropolitana, Iztapalapa (Mexico). Dept. de Quimica


    LiAlO{sub 2} was prepared by two sol-gel methods using simultaneous hydrolysis of the reagents: aluminum sec-butoxide/lithium methoxide and aluminum sec-butoxide/LiOH. The resulting ceramic powders were compared with those prepared by two conventional methods (i.e., solid-state fusion and peroxide). The sol-gel method provided powders with a very high {gamma}-LiAlO{sub 2} content after calcining at temperatures as low as 700 C when LiOH was used. The solids were characterized by AAS, DTA, TGA, XRD, and SEM.

  10. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna


    Application of sol-gel process to synthesis of aluminoborosilicate powders shows potential for control of microstructures of materials. Development of materials having enhanced processing characteristics prove advantageous in extending high-temperature endurance of fibrous refractory composite insulation made from ceramic fibers.

  11. Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

    Hou Aiqin, E-mail: [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China); Chen Huawei [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China)


    The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

  12. Semiconductor TiO{sub 2}-Ga{sub 2}O{sub 3} thin film gas sensors derived from particulate sol-gel route

    Mohammadi, M.R. [Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge CB2 3QZ (United Kingdom) and Department of Materials Science and Engineering, Sharif University of Technology, Azadi Street, Tehran (Iran, Islamic Republic of)]. E-mail:; Fray, D.J. [Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge CB2 3QZ (United Kingdom)


    Nanostructured and mesoporous TiO{sub 2}-Ga{sub 2}O{sub 3} thin films with various Ti:Ga atomic ratios were prepared by a new straightforward particulate sol-gel route. Titanium isopropoxide and gallium (III) nitrate hydrate were used as precursors, and hydroxypropyl cellulose (HPC) was used as a polymeric fugitive agent (PFA) in order to increase the specific surface area (SSA). XRD and TEM analysis of the powders revealed that the Ga{sub 2}O{sub 3} formed from the nitrate precursor retarded anatase-to-rutile transformation, crystallization and crystal growth. The average crystallite size of pure TiO{sub 2} powder annealed at 600-1000 deg. C were in the range 4-10 nm; the values that could be decreased to 2-6 nm for TiO{sub 2}-Ga{sub 2}O{sub 3} powders. Furthermore, one of the highest SSA was obtained by introducing Ga{sub 2}O{sub 3} into TiO{sub 2}, being 305 m{sup 2} g{sup -1} for TG11 (Ti:Ga = 50:50 atomic ratio) binary oxide annealed at 600 deg. C. Thin films produced under optimized conditions showed excellent microstructural properties for gas sensing applications. They exhibited a remarkable response towards low concentrations of CO and NO{sub 2} gases at low operating temperature of 200 deg. C, resulting in increased thermal stability of sensing films as well as a decrease in their power consumption. TG11 sensor showed the highest response towards all CO and NO{sub 2} concentrations operated at 200 deg. C. The response magnitude of 13.7 and 4.3 with response times of 30 s and 108 s were achieved for TG11 sensor towards 400 ppm CO and 10 ppm NO{sub 2}, respectively. Furthermore, calibration curves revealed that TiO{sub 2}-Ga{sub 2}O{sub 3} sensors follow the power law (S = A[gas] {sup B}) (where S is sensor response, coefficients A and B are constants and [gas] is gas concentration) for the two types of gases, and they have excellent capability for the detection of low gas concentrations (25 ppm CO and 0.5 ppm NO{sub 2}). The maximum response of TiO{sub 2

  13. Photochromic organic-inorganic hybrid materials.

    Pardo, Rosario; Zayat, Marcos; Levy, David


    Photochromic organic-inorganic hybrid materials have attracted considerable attention owing to their potential application in photoactive devices, such as optical memories, windows, photochromic decorations, optical switches, filters or non-linear optics materials. The growing interest in this field has largely expanded the use of photochromic materials for the purpose of improving existing materials and exploring new photochromic hybrid systems. This tutorial review summarizes the design and preparation of photochromic hybrid materials, and particularly those based on the incorporation of organic molecules in organic-inorganic matrices by the sol-gel method. This is the most commonly used method for the preparation of these materials as it allows vitreous hybrid materials to be obtained at low temperatures, and controls the interaction between the organic molecule and its embedding matrix, and hence allows tailoring of the performance of the resulting devices.

  14. Organic-Inorganic Hybrid Silica Material Derived from a Monosilylated Grubbs-Hoveyda Ruthenium Carbene as a Recyclable Metathesis Catalyst

    Michel Wong Chi Man


    Full Text Available The synthesis of a monosilylated Grubbs-Hoveyda ruthenium alkylidene complex is described, as well as the preparation and characterization of the corresponding material by sol-gel cogelification with tetraethoxysilane (TEOS and the assay of this recyclable supported catalyst in ring-closing diene and enyne metathesis reactions under thermal and microwave conditions.

  15. Sol-gel immobilized short-chain poly(ethylene glycol) coating for capillary microextraction of underivatized polar analytes.

    Kulkarni, Sameer; Shearrow, Anne M; Malik, Abdul


    Sol-gel coating with covalently bonded low-molecular-weight (MWsol-gel chemistry proved effective in the immobilization of low-molecular-weight PEGs thanks to the formation of chemical bonds between the organic-inorganic hybrid sol-gel PEG coating and the fused silica capillary inner surface. This chemical anchorage provided excellent thermal and solvent stability to the created sol-gel PEG coating as is evidenced by its high upper limit of allowable conditioning temperature (340 degrees C) and its practically identical performance before and after rinsing with various solvents. The prepared sol-gel PEG coating provided simultaneous extraction of moderately polar and highly polar analytes from aqueous samples without requiring derivatization, pH adjustment or salting-out procedures. Detection limits on the order of nanogram per liter (ng/L) were achieved in CME-GC-flame ionization detection experiments designed for the preconcentration and trace analysis of both highly polar and moderately polar compounds extracted directly from aqueous media using sol-gel short-chain PEG coated microextraction capillaries.

  16. Sol-gel layers for ceramic microsystems application

    Czok, Mateusz; Golonka, Leszek


    This paper describes research on sol-gel solutions preparation process. Utilize of a sol-gel layers in the LTCC technology for reduction of surface roughness and influence on the ceramics properties is examined and described. The influence of sol-gel layer on possible sedimentation of dyes or biological substances in channels, mixers or chambers of ceramic microfluidic structures was investigated. Moreover, properties of sol-gel coated surfaces have been precisely examined and described. Finally, positive results of conducted experiments made it possible to design and manufacture a simple microfluidic ceramic structure, with embedded protective layer of sol-gel, for fluorescence measurements.

  17. Study of the thermal degradation of bioactive sol-gel coatings for the optimization of its curing process

    Hernández-Escolano, Miriam; Ramis Juan, Xavier; Jiménez-Morales, A; Juan-Díaz, M.; Suay, Julio


    A set of materials has been prepared by sol-gel process containing different quantities of hydroxyapatite (0, 2.5 and 5% HAp w/w) using as silica precursors glycidyloxypropyltrimethoxysilane (GPTMS) and triethoxyvinylsilane (VTES). In order to optimize the curing process to obtain sintherized systems (inorganic network) or hybrid systems (organic&-inorganic) a TG and FTIR studies have been developed and degradation kinetic triplet parameters were obtained (the activation energy, pre-exponenti...

  18. Synthesis and characterization of four organic-inorganic salts: sulfates of 2-aminopyridinium derivatives.

    Bednarchuk, Tamara J; Kinzhybalo, Vasyl; Pietraszko, Adam


    Hybrid materials, fabricated by the combination of inorganic and organic components, have potential applications in chemistry and are endowed with the advantages of both building elements. There are several types of intermolecular interactions present in these hybrid compounds, including electrostatic forces, π-π stacking and hydrogen-bonding interactions, the latter playing an important role in the construction of three-dimensional architectures and stabilizing supramolecular crystal structures. Analysis of the intermolecular interactions and their influence on packing modes therefore requires focused scientific attention. Four new organic-inorganic salts, namely 2-amino-4-methyl-3-nitropyridinium hydrogen sulfate, C6H8N3O2(+)·HSO4(-), bis(2-amino-4-methyl-3-nitropyridinium) sulfate, 2C6H8N3O2(+)·SO4(2-), 2-amino-3-methylpyridinium hydrogen sulfate, C6H9N2(+)·HSO4(-), and bis(2-amino-3-methylpyridinium) sulfate monohydrate, 2C6H9N2(+)·SO4(2-)·H2O, have been synthesized and characterized by X-ray diffraction. The crystal structures are stabilized by intra- and intermolecular hydrogen bonds, as well as by weak π-π stacking and lp-π (lp is lone pair) interactions. Hirshfeld surface analysis was employed in order to study intermolecular interactions.

  19. Modified sol-gel coatings for biotechnological applications

    Beganskiene, A [Department of General and Inorganic Chemistry, Vilnius University, Vilnius LT-03225 (Lithuania); Raudonis, R [Department of General and Inorganic Chemistry, Vilnius University, Vilnius LT-03225 (Lithuania); Jokhadar, S Zemljic [Faculty of Medicine, Institute of Biophysics, Lipiceva 2, Ljubljana SI-1000 (Slovenia); Batista, U [Faculty of Medicine, Institute of Biophysics, Lipiceva 2, Ljubljana SI-1000 (Slovenia); Kareiva, A [Department of General and Inorganic Chemistry, Vilnius University, Vilnius LT-03225 (Lithuania)


    The modified sol-gel derived silica coatings were prepared and characterized. The amino and methyl groups were introduced onto the colloidal silica. The silica coatings with different wettability properties: coloidal silica (water contact angle 17 deg.), polysiloxane (61 deg.), methyl-modified (158 deg. and 46 deg.) coatings samples were tested for CaCo-2 cells proliferation. Methyl-modified coating (46 deg.) proved to be the best substrate for cell proliferation. CaCo-2 cell proliferation two days post seeding was significantly faster on almost laminine, fibronectin and collagen-1 coated samples compared to corresponding controls.

  20. Up-conversion in nanostructured Yb{sup 3+}-Tm{sup 3+} co-doped sol-gel derived SiO{sub 2}-LaF{sub 3} transparent glass-ceramics

    Mendez-Ramos, J.; Velazquez, J.J. [Departamento de Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Yanes, A.C.; Del-Castillo, J. [Departamento de Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Rodriguez, V.D.


    Nanostructured transparent glass-ceramics with composition of 95SiO{sub 2}-5LaF{sub 3} doped with 0.1 mol% of Tm{sup 3+} or co-doped with 0.1 mol% of Tm{sup 3+} and 0.3 mol% of Yb{sup 3+} were synthesized by thermal treatment of precursor sol-gel derived glasses. A comparative luminescence analysis in terms of different temperatures of thermal treatments has been carried out. Segregation of LaF{sub 3} nanocrystals in the matrix was confirmed by X-ray diffraction. Blue and red efficient up-conversion emissions were observed under 980 nm excitation at room temperature. These results indicate partition of a significant fraction of co-dopants into the precipitated LaF{sub 3} nanocrystals. The mechanisms involved in the up-conversion emissions have been analyzed and can be ascribed to processes with two, three and four photons. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)


    Xiao Huang; Jian Wang; Ling-zhi Zhang; Zhi-gang Cai; Zhao-xi Lianga


    Four phenoxysilicon networks for nonlinear optical (NLO) applications were designed and prepared by an extended sol-gel process without additional H20 and catalyst. All poled polymer network films possess high second-order nonlinear optical coefficients (d33) of 10-?~10-8 esu. The investigation of NLO temporal stability at room temperature and elevated temperature (120°C) indicated that these films exhibit high d33 stability because the orientation of the chromophores are locked in the phenoxysilicon organic/inorganic networks.

  2. Ring-Resonator/Sol-Gel Interferometric Immunosensor

    Bearman, Gregory; Cohen, David


    A proposed biosensing system would be based on a combination of (1) a sensing volume containing antibodies immobilized in a sol-gel matrix and (2) an optical interferometer having a ring resonator configuration. The antibodies would be specific to an antigen species that one seeks to detect. In the ring resonator of the proposed system, light would make multiple passes through the sensing volume, affording greater interaction length and, hence, greater antibody- detection sensitivity.

  3. Epoxy Sol-Gel Hybrid Thermosets

    Angels Serra


    Full Text Available Sol-gel methodologies are advantageous in the preparation of hybrid materials in front of the conventional addition of nanoparticles, because of the fine dispersion of the inorganic phase that can be reached in epoxy matrices. In addition, the use of organoalkoxysilanes as coupling agents allows covalent linkage between organic and inorganic phases, which is the key point in the improvement of mechanical properties. The sol-gel process involves hydrolysis and condensation reactions under mild conditions, starting from hydrolysable metal alkoxides, generally alkoxy silanes. Using the sol-gel procedure, the viscosity of the formulation is maintained, which is an important issue in coating applications, whereas the transparency of the polymer matrix is also maintained. However, only the proper combination of the chemistries and functionalities of both organic and inorganic structures leads to thermosets with the desired characteristics. The adequate preparation of hybrid epoxy thermosets enables their improvement in characteristics such as mechanical properties (modulus, hardness, scratch resistance, thermal and flame resistance, corrosion and antimicrobial protection, and even optical performance among others.

  4. Sol-Gel Manufactured Energetic Materials

    Simpson, Randall L.; Lee, Ronald S.; Tillotson, Thomas M.; Hrubesh, Lawrence W.; Swansiger, Rosalind W.; Fox, Glenn A.


    Sol-gel chemistry is used for the preparation of energetic materials (explosives, propellants and pyrotechnics) with improved homogeneity, and/or which can be cast to near-net shape, and/or made into precision molding powders. The sol-gel method is a synthetic chemical process where reactive monomers are mixed into a solution, polymerization occurs leading to a highly cross-linked three dimensional solid network resulting in a gel. The energetic materials can be incorporated during the formation of the solution or during the gel stage of the process. The composition, pore, and primary particle sizes, gel time, surface areas, and density may be tailored and controlled by the solution chemistry. The gel is then dried using supercritical extraction to produce a highly porous low density aerogel or by controlled slow evaporation to produce a xerogel. Applying stress during the extraction phase can result in high density materials. Thus, the sol-gel method can be used for precision detonator explosive manufacturing as well as producing precision explosives, propellants, and pyrotechnics, along with high power composite energetic materials.

  5. Tantalum-Tungsten Oxide Thermite Composite Prepared by Sol-Gel Synthesis and Spark Plasma Sintering

    Cervantes, O; Kuntz, J; Gash, A; Munir, Z


    Energetic composite powders consisting of sol-gel derived nanostructured tungsten oxide were produced with various amounts of micrometer-scale tantalum fuel metal. Such energetic composite powders were ignition tested and results show that the powders are not sensitive to friction, spark and/or impact ignition. Initial consolidation experiments, using the High Pressure Spark Plasma Sintering (HPSPS) technique, on the sol-gel derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The sol-gel derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta - WO{sub 3}) energetic composite was consolidated to a density of 9.17{sup -3} or 93% relative density. In addition those parts were consolidated without significant pre-reaction of the constituents, thus the sample retained its stored chemical energy.

  6. Ionogel Electrolytes through Sol-Gel Processing

    Horowitz, Ariel I.

    Electrical energy needs have intensified due to the ubiquity of personal electronics, the decarbonization of energy services through electrification, and the use of intermittent renewable energy sources. Despite developments in mechanical and thermal methods, electrochemical technologies are the most convenient and effective means of storing electrical energy. These technologies include both electrochemical cells, commonly called batteries, and electrochemical double-layer capacitors, or "supercapacitors", which store energy electrostatically. Both device types require an ion-conducting electrolyte. Current devices use solutions of complex salts in organic solvents, leading to both toxicity and flammability concerns. These drawbacks can be avoided by replacing conventional electrolytes with room-temperature molten salts, known as ionic liquids (ILs). ILs are non-volatile, non-flammable, and offer high conductivity and good electrochemical stability. Device mass can be reduced by combining ILs with a solid scaffold material to form an "ionogel," further improving performance metrics. In this work, sol-gel chemistry is explored as a means of forming ionogel electrolytes. Sol-gel chemistry is a solution-based, industrially-relevant, well-studied technique by which solids such as silica can be formed in situ. Previous works used a simple acid-catalyzed sol-gel reaction to create brittle, glassy ionogels. Here, both the range of products that can be accomplished through sol-gel processing and the understanding of interactions between ILs and the sol-gel reaction network are greatly expanded. This work introduces novel ionogel materials, including soft and compliant silica-supported ionogels and PDMS-supported ionogels. The impacts of the reactive formulation, IL identity, and casting time are detailed. It is demonstrated that variations in formulation can lead to rapid gelation and open pore structures in the silica scaffold or slow gelation and more dense silica

  7. Processing, properties, and applications of sol-gel silica optics

    Nogues, Jean-Luc R.; LaPaglia, Anthony J.


    For many years the market share maintained by U.S. optics manufacturers has been declining continuously caused in part by intense competition principally from countries in the Far East, and in part by the lack of a highly trained cadre of opticians to replace the current generation. This fact could place in jeopardy the defense system of the United States in case of international war. For example, in 1987, optical glass component imports accounted for approximately 50 percent of the Department of Defense (DOD) consumption. GELTECH's sol-gel technology is a new process for making a high quality optical glass and components for commercial and military uses. This technology offers in addition to being a local source of optics, the possibility to create new materials for high-tech optical applications, and the elimination of the major part of grinding and polishing for which the skill moved off-shore. This paper presents a summary of the solgel technology for the manufacture of high quality optical glass and components. Properties of pure silica glass made by solgel process (Type V and Type VI silicas) are given and include: ultraviolet, visible and near infrared spectrophotometry, optical homogeneity and thermal expansion. Many applications such as near net shape casting or Fresnel lens surface replication are discussed. Several potential new applications offered by the solgel technology such as organic-inorganic composites for non linear optics or scintillation detection are also reported in this paper.

  8. Sol-gel synthesis of hydroxyapatite; Sintese de hidroxiapatita via sol-gel

    Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P., E-mail: [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil)


    Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

  9. Proline and benzylpenicillin derivatives grafted into mesoporous MCM-41: Novel organic-inorganic hybrid catalysts for direct aldol reaction

    Dwairath Dhar; Ian Beadham; Srinivasan Chandrasekaran


    New organic-inorganic hybrid catalysts were synthesized by covalent grafting of proline and benzylpenicillin derivatives into mesoporous MCM-41. These catalysts were extensively characterized using FT-IR, 13C CP MAS solid state NMR, XRD and TEM techniques. These were used as catalysts for direct, asymmetric aldol reaction between acetone and activated aromatic aldehydes. In the reaction of 4-nitro and 4-fluoro benzaldehyde, the aldol products were obtained in 36% and 59% ee respectively. The catalysts were reusable with neither significant drop in enantioselectivity nor loss of mesostructure. An attempt was made to substantiate the proposed `enamine’ mechanism for direct aldol reaction by trapping the intermediate between proline-MCM-41 and acetone.

  10. Sol-gel processing to form doped sol-gel monoliths inside hollow core optical fiber and sol-gel core fiber devices made thereby

    Shaw, Harry C. (Inventor); Ott, Melanie N. (Inventor); Manuel, Michele V. (Inventor)


    A process of fabricating a fiber device includes providing a hollow core fiber, and forming a sol-gel material inside the hollow core fiber. The hollow core fiber is preferably an optical fiber, and the sol-gel material is doped with a dopant. Devices made in this manner includes a wide variety of sensors.

  11. Ultrafast Sol-Gel Synthesis of Graphene Aerogel Materials

    Lim, Mathew; Hu, Matthew; Manandhar, Sandeep; Sakshaug, Avery; Strong, Adam; Riley, Leah; Pauzauskie, Peter J.


    Graphene aerogels derived from graphene-oxide (GO) starting materials recently have been shown to exhibit a combination of high electrical conductivity, chemical stability, and low cost that has enabled a range of electrochemical applications. Standard synthesis protocols for manufacturing graphene aerogels require the use of sol-gel chemical reactions that are maintained at high temperatures for long periods of time ranging from 12 hours to several days. Here we report an ultrafast, acid-catalyzed sol-gel formation process in acetonitrile in which wet GO-loaded gels are realized within 2 hours at temperatures below 45°C. Spectroscopic and electrochemical analysis following supercritical drying and pyrolysis confirms the reduction of the GO in the aerogels to sp2 carbon crystallites with no residual carbon–nitrogen bonds from the acetonitrile or its derivatives. This rapid synthesis enhances the prospects for large-scale manufacturing of graphene aerogels for use in numerous applications including sorbents for environmental toxins, support materials for electrocatalysis, and high-performance electrodes for electrochemical capacitors and solar cells.

  12. Effects of phosphorus-doping on energy band-gap, structural, surface, and photocatalytic characteristics of emulsion-based sol-gel derived TiO2 nano-powder

    Ganesh, Ibram


    Different amounts of phosphorus (P)-doped TiO2 (PDT) nano-powders (P = 0-10 wt.%) were synthesized by following a new emulsion-based sol-gel (EBSG) route and calcined at 400 °C-800 °C for 6 h. These calcined PDT powders were then thoroughly characterized by means of XRD, XPS, SEM, FT-IR, FT-Raman, DRS, BET surface area, zeta-potential, cyclic-voltammetry and photocatalytic evaluation using methylene blue (MB) as a model-pollutant and established the effects of phosphorous doping on structural, surface, band-gap energy, and photocatalytic characteristics of TiO2 nano-powder formed in EBSG route. The characterization results suggest that the EBSG derived TiO2 nano-powder after calcination at 400 °C for 6 h is in the form of anatase phase when it was doped with 8 wt.% P. Furthermore, these EBSG derived PDT powders own high negative zeta-potentials, high specific surface areas (up to >250 m2/g), and suitable band-gap energies (<3.34 eV). Surprisingly, these PDT powders exhibit very high MB adsorption (up to 50%) from its aqueous 0.01 mM, 0.02 mM and 0.03 mM solutions during 30 min stirring in the dark, whereas, the commercial Degussa P-25 TiO2 nano-powder shows no adsorption. Among various photocatalysts investigated in this study, the 1 wt.% P-doped TiO2 nano-powder formed in EBSG route exhibited the highest photocatalytic activity for MB degradation reaction.

  13. Progress on sol-gel sphere-pac development

    Suchomel, R R


    The ORNL sol-gel program is reviewed briefly. Advantages of the sol-gel sphere-pac are listed. Three sizes of microspheres are being used; the two largest sized fractions are blended and then loaded into the fuel rod, followed by packing of the smallest microspheres into void spaces using a low-energy vibrator. Sol-gel sphere-pac also appears attractive for breeder reactor fuel fabrication. (DLC)

  14. Hard X-rays for processing hybrid organic-inorganic thick films.

    Jiang, Yu; Carboni, Davide; Pinna, Alessandra; Marmiroli, Benedetta; Malfatti, Luca; Innocenzi, Plinio


    Hard X-rays, deriving from a synchrotron light source, have been used as an effective tool for processing hybrid organic-inorganic films and thick coatings up to several micrometres. These coatings could be directly modified, in terms of composition and properties, by controlled exposure to X-rays. The physico-chemical properties of the coatings, such as hardness, refractive index and fluorescence, can be properly tuned using the interaction of hard X-rays with the sol-gel hybrid films. The changes in the microstructure have been correlated especially with the modification of the optical and the mechanical properties. A relationship between the degradation rate of the organic groups and the rise of fluorescence from the hybrid material has been observed; nanoindentation analysis of the coatings as a function of the X-ray doses has shown a not linear dependence between thickness and film hardness.

  15. Design of hybrid sol gel films for direct x-ray and electron beam nanopatterning

    Brusatin, Giovanna; Della Giustina, Gioia; Romanato, Filippo; Guglielmi, Massimo


    New epoxy based sol-gel organic inorganic materials, showing lithographic resist-like properties without the addition of any photocatalysts, are presented. To obtain a material sensitive to radiation, specific sol-gel syntheses based on an organically modified alkoxide containing an epoxy ring, 3-glycidoxypropyltrimethoxysilane (GPTMS), have been developed. The synthesis and the patternability of hybrid materials have been obtained controlling the inorganic crosslinking degree and with an almost total absence of organic polymerization. Two examples of directly patternable hybrid films, called GB and GGe, have been synthesized using acidic (GGe) and basic (GB) conditions and obtaining different compositions. After electron beam lithography (EBL) or x-ray synchrotron radiation lithography (XRL) the polymerization of the organic component of the sol-gel film occurs, generating a hardening of the structure after post-exposure baking. The exposed polymerized material becomes insoluble, determining a negative resist-like behaviour of the film: the lithographic process of nanopatterning results from the dissolution of the unexposed areas in proper solvents (developers). Spatial resolution of the order of 200 nm is reported and a contrast of 2.2 is achieved. The novelty of this work is that epoxy based materials, which have enhanced thermomechanical stability with respect to the more usual acrylic based resins, are directly nanopatterned for the first time by electron beam (EB) and/or x-ray beam radiation exposure without the aid of catalysts for polymerization. In contrast to common resists that are sacrificial layers of the fabrication process, direct patternable sol-gel hybrids constitute the final material of the devices. In fact, an example of doping with a light emitting dye is reported together with the achievement of directly patterned structures by EBL and XRL.

  16. Sol-gel overganger for microsilica


    Oppgaven er en grunnleggende undersøkelse av sol-gel overganger i vandige dispersjoner av Microsilica. Den er delt i tre deler: 1) undersøkelse av Microsilica kolloid- og overflateegenskaper 2) identifisering av parametere som er av størst betydning for gelingsforløpet i Microsilica slurryer og 3) en nærmere undersøkelse av mulige mekanismer for gelingen. Prøven av Microsilica som ble benyttet i forsøkene var en relativt ren kvalitet med et SiO2 -innhold på 97,3 vekt%. P...

  17. Sol-gel processing of ceramics

    Schmidt, Helmut K.


    The sol-gel process can be considered as an interesting method for the synthesis of tailor-made ceramic raw materials. Two points of view are of special interest: powder synthesis and the processing of ultrafine raw materials. In the case of powder synthesis, high quality and multicomponent powders can be synthesized by control of surface chemistry and agglomerate-free subµm powder can be obtained. The preparation of tailor-made sols offers the possibility of powder-free processing of coating...

  18. Spontaneous Pattern Formation Induced by Bénard-Marangoni Convection for Sol-Gel-Derived Titania Dip-Coating Films: Effect of Co-solvents with a High Surface Tension and Low Volatility.

    Uchiyama, Hiroaki; Matsui, Tadayuki; Kozuka, Hiromitsu


    Evaporation-driven surface tension gradient in the liquid layer often causes the convective flow, i.e., Bénard-Marangoni convection, resulting in the formation of cell-like patterns on the surface. Here, we prepared sol-gel-derived titania films from Ti(OC3H7(i))4 solutions by dip coating and discussed the effect of the addition of co-solvents with a high surface tension and low volatility on the spontaneous pattern formation induced by Bénard-Marangoni convection. Propylene glycol (PG, with a surface tension of 38.6 mN m(-1)) and dipropylene glycol (DPG, with a surface tension of 33.9 mN m(-1)) were added to the coating solutions containing 2-propanol (2-Pr, with a surface tension of 22.9 mN m(-1)) for controlling the evaporation-driven surface tension gradient in the coating layer on a substrate. During dip coating at a substrate withdrawal speed of 50 cm min(-1) in a thermostatic oven at 60 °C, linearly arranged cell-like patterns on a micrometer scale were spontaneously formed on the titania gel films, irrespective of the composition of coating solutions. Such surface patterns remained even after the heat treatment at 200 and 600 °C, where the densification and crystallization of the titania films progressed. The width and height of the cell-like patterns increased with increasing PG and DPG contents in the coating solutions, where the addition of PG resulted in the formation of cells with a larger height than DPG.

  19. Alkali cold gelation of whey proteins. Part I: sol-gel-sol(-gel) transitions.

    Mercadé-Prieto, Ruben; Gunasekaran, Sundaram


    The cold gelation of preheated whey protein isolate (WPI) solutions at alkaline conditions (pH>10) has been studied to better understand the effect of NaOH in the formation and destruction of whey protein aggregates and gels. Oscillatory rheology has been used to follow the gelation process, resulting in novel and different gelation profiles with the gelation pH. At low alkaline pH, typical sol-gel transitions are observed, as in many other biopolymers. At pH>11.5, the system gels quickly, after approximately 300 s, followed by a slow degelation step that transforms the gel to a viscous solution. Finally, there is a second gelation step. This results in a surprising sol-gel-sol-gel transition in time at constant gelation conditions. At very high pH (>12.5), the degelation step is very severe, and the second gelation step is not observed, resulting in a sol-gel-sol transition. The first quick gelation step is related to the quick swelling of the WPI aggregates in alkali, as observed from light scattering, which enables the formation of new noncovalent interactions to form a gel network. These interactions are argued to be destroyed in the subsequent degelation step. Disulfide cross-linking is observed only in the second gelation step, not in the first step.

  20. High-temperature solvent stability of sol-gel germania triblock polymer coatings in capillary microextraction on-line coupled to high-performance liquid chromatography.

    Segro, Scott S; Malik, Abdul


    Germania-based sol-gel organic-inorganic hybrid coatings were prepared for on-line coupling of capillary microextraction with high-performance liquid chromatography. For this, a germania-based sol-gel precursor, tetra-n-butoxygermane and a hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide) were used. These sol-gel germania triblock polymer coatings were chemically anchored to the inner walls of a fused silica capillary (0.25 mm I.D.) in course of its evolution from the sol solution. Scanning electron microscopy images of the sol-gel germania triblock polymer coating were obtained to estimate the coating thickness. For the first time, the analyte distribution constants between a sol-gel germania organic-inorganic hybrid coating and the samples (K(cs)) were determined. For a variety of analytes from different chemical classes, including polycyclic aromatic hydrocarbons (PAHs), ketones, alcohols, phenols and amines, the K(cs) values ranged from 8.1 x 10(1) to 5.6 x 10(4). Also, for the first time, the stability of the sol-gel germania-based coating in high-temperature reversed-phase solvent environment was evaluated. The sol-gel germania triblock polymer coatings were capable of surviving exposure to high-temperature solvent conditions (200 degrees C) with little change in extraction capabilities. This demonstrates that sol-gel germania triblock polymer hybrid materials might be suitable for further applications in high-temperature HPLC. The reproducibility of the method for preparation of the sol-gel germania triblock polymer coatings was also evaluated, and the capillary-to-capillary RSD values ranged from 5.3 to 6.5%. The use of higher flow rates in extraction was found to significantly reduce the time required (from 30-40 to 10-15 min) to reach equilibrium between the sol-gel germania triblock polymer coating and the analytes in the sample solution.

  1. Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method. Optimisation, characterisation and rheology.

    Tredwin, Christopher J; Young, Anne M; Georgiou, George; Shin, Song-Hee; Kim, Hae-Won; Knowles, Jonathan C


    Currently, most titanium implant coatings are made using hydroxyapatite and a plasma spraying technique. There are however limitations associated with plasma spraying processes including poor adherence, high porosity and cost. An alternative method utilising the sol-gel technique offers many potential advantages but is currently lacking research data for this application. It was the objective of this study to characterise and optimise the production of Hydroxyapatite (HA), fluorhydroxyapatite (FHA) and fluorapatite (FA) using a sol-gel technique and assess the rheological properties of these materials. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethylphosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the sol-gel derived FHA and FA. Optimisation of the chemistry and subsequent characterisation of the sol-gel derived materials was carried out using X-ray Diffraction (XRD) and Differential Thermal Analysis (DTA). Rheology of the sol-gels was investigated using a viscometer and contact angle measurement. A protocol was established that allowed synthesis of HA, FHA and FA that were at least 99% phase pure. The more fluoride incorporated into the apatite structure; the lower the crystallisation temperature, the smaller the unit cell size (changes in the a-axis), the higher the viscosity and contact angle of the sol-gel derived apatite. A technique has been developed for the production of HA, FHA and FA by the sol-gel technique. Increasing fluoride substitution in the apatite structure alters the potential coating properties. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

  2. Sol-gel method for encapsulating molecules

    Brinker, C. Jeffrey; Ashley, Carol S.; Bhatia, Rimple; Singh, Anup K.


    A method for encapsulating organic molecules, and in particular, biomolecules using sol-gel chemistry. A silica sol is prepared from an aqueous alkali metal silicate solution, such as a mixture of silicon dioxide and sodium or potassium oxide in water. The pH is adjusted to a suitably low value to stabilize the sol by minimizing the rate of siloxane condensation, thereby allowing storage stability of the sol prior to gelation. The organic molecules, generally in solution, is then added with the organic molecules being encapsulated in the sol matrix. After aging, either a thin film can be prepared or a gel can be formed with the encapsulated molecules. Depending upon the acid used, pH, and other processing conditions, the gelation time can be from one minute up to several days. In the method of the present invention, no alcohols are generated as by-products during the sol-gel and encapsulation steps. The organic molecules can be added at any desired pH value, where the pH value is generally chosen to achieve the desired reactivity of the organic molecules. The method of the present invention thereby presents a sufficiently mild encapsulation method to retain a significant portion of the activity of the biomolecules, compared with the activity of the biomolecules in free solution.

  3. Photocurable bioactive bone cement based on hydroxyethyl methacrylate-poly(acrylic/maleic) acid resin and mesoporous sol gel-derived bioactive glass.

    Hesaraki, S


    This paper reports on strong and bioactive bone cement based on ternary bioactive SiO2-CaO-P2O5 glass particles and a photocurable resin comprising hydroxyethyl methacrylate (HEMA) and poly(acrylic/maleic) acid. The as-cured composite represented a compressive strength of about 95 MPa but it weakened during soaking in simulated body fluid, SBF, qua its compressive strength reached to about 20 MPa after immersing for 30 days. Biodegradability of the composite was confirmed by reducing its initial weight (~32%) as well as decreasing the molecular weight of early cured resin during the soaking procedure. The composite exhibited in vitro calcium phosphate precipitation in the form of nanosized carbonated hydroxyapatite, which indicates its bone bonding ability. Proliferation of calvarium-derived newborn rat osteoblasts seeded on top of the composite was observed during incubation at 37 °C, meanwhile, an adequate cell supporting ability was found. Consequently, it seems that the produced composite is an appropriate alternative for bone defect injuries, because of its good cell responses, high compressive strength and ongoing biodegradability, though more in vivo experiments are essential to confirm this assumption.

  4. Dye Sensitized Solar Cell with Conventionally Annealed and Post-Hydrothermally Treated Nanocrystalline Semiconductor Oxide TiO2 Derived from Sol-Gel Process

    Akhmad Yuwono


    Full Text Available Dye-sensitized solar cell (DSSC is one of the very promising alternative renewable energy sources to anticipate the declination in the fossil fuel reserves in the next few decades and to make use of the abundance of intensive sunlight energy in tropical countries like Indonesia. In the present study, TiO2 nanoparticles of different nanocrystallinity was synthesized via sol−gel process with various water to inorganic precursor ratio (Rw of 0.85, 2.00 and 3.50 upon sol preparation, followed with subsequent drying, conventional annealing and post-hydrothermal treatments. The resulting nanoparticles were integrated into the DSSC prototype and sensitized with an organic dye made of the extract of red onion. The basic performance of the fabricated DSSC has been examined and correlated to the crystallite size and band gap energy of TiO2 nanoparticles. It was found that post-hydrothermally treated TiO2 nanoparticles derived from sol of 2.00 Rw, with the most enhanced nanocrystalline size of 12.46 nm and the lowest band gap energy of 3.48 eV, showed the highest open circuit voltage (Voc of 69.33 mV.

  5. Photocurable bioactive bone cement based on hydroxyethyl methacrylate-poly(acrylic/maleic) acid resin and mesoporous sol gel-derived bioactive glass

    Hesaraki, S., E-mail:


    This paper reports on strong and bioactive bone cement based on ternary bioactive SiO{sub 2}-CaO-P{sub 2}O{sub 5} glass particles and a photocurable resin comprising hydroxyethyl methacrylate (HEMA) and poly(acrylic/maleic) acid. The as-cured composite represented a compressive strength of about 95 MPa but it weakened during soaking in simulated body fluid, SBF, qua its compressive strength reached to about 20 MPa after immersing for 30 days. Biodegradability of the composite was confirmed by reducing its initial weight (~ 32%) as well as decreasing the molecular weight of early cured resin during the soaking procedure. The composite exhibited in vitro calcium phosphate precipitation in the form of nanosized carbonated hydroxyapatite, which indicates its bone bonding ability. Proliferation of calvarium-derived newborn rat osteoblasts seeded on top of the composite was observed during incubation at 37 °C, meanwhile, an adequate cell supporting ability was found. Consequently, it seems that the produced composite is an appropriate alternative for bone defect injuries, because of its good cell responses, high compressive strength and ongoing biodegradability, though more in vivo experiments are essential to confirm this assumption. - Highlights: • Light cure cement based on SiO{sub 2}-CaO-P{sub 2}O{sub 5} glass and polymer-like matrix was formed. • The matrix includes poly(acrylic/maleic acid) and poly(hydroxyethyl methacrylate). • The cement is as strong as polymethylmethacrylate bone cement. • The cement exhibits apatite formation ability in simulated body fluid. • The cement is biodegradable and supports proliferation of osteoblastic cells.

  6. Chitosan bio-based organic-inorganic hybrid aerogel microspheres.

    El Kadib, Abdelkrim; Bousmina, Mosto


    Recently, organic-inorganic hybrid materials have attracted tremendous attention thanks to their outstanding properties, their efficiency, versatility and their promising applications in a broad range of areas at the interface of chemistry and biology. This article deals with a new family of surface-reactive organic-inorganic hybrid materials built from chitosan microspheres. The gelation of chitosan (a renewable amino carbohydrate obtained by deacetylation of chitin) by pH inversion affords highly dispersed fibrillar networks shaped as self-standing microspheres. Nanocasting of sol-gel processable monomeric alkoxides inside these natural hydrocolloids and their subsequent CO(2) supercritical drying provide high-surface-area organic-inorganic hybrid materials. Examples including chitosan-SiO(2), chitosan-TiO(2), chitosan-redox-clusters and chitosan-clay-aerogel microspheres are described and discussed on the basis of their textural and structural properties, thermal and chemical stability and their performance in catalysis and adsorption.

  7. Self-Healing Corrosion Protective Sol-Gel Coatings

    Abdolah Zadeh, M.


    Inspired by the state of the art and the recent advances in the field of self-healing corrosion protective coatings, the thesis entitled “Self-healing corrosion protective sol-gel coatings” addresses novel routes to self-healing corrosion protective sol-gel coatings via extrinsic and intrinsic

  8. Self-Healing Corrosion Protective Sol-Gel Coatings

    Abdolah Zadeh, M.


    Inspired by the state of the art and the recent advances in the field of self-healing corrosion protective coatings, the thesis entitled “Self-healing corrosion protective sol-gel coatings” addresses novel routes to self-healing corrosion protective sol-gel coatings via extrinsic and intrinsic heali

  9. Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

    Kulkarni, Suhasini; Tran, Vu; Ho, Maggie K.-M.; Phan, Chieu; Chin, Elizabeth; Wemmer, Zeke; Sommerhalter, Monika


    This experiment was performed in an upper-level undergraduate biochemistry laboratory course. Students learned how to immobilize an enzyme in a sol-gel matrix and how to perform and evaluate enzyme-activity measurements. The enzyme acid phosphatase (APase) from wheat germ was encapsulated in sol-gel beads that were prepared from the precursor…

  10. Synthesis of organic-inorganic hybrid sols using trifunctional organoalkoxysilanes for dispersion agents.

    Park, Hoyyul; Kang, Dongjun; Ahn, Myeongsang; Lee, Hyeonhwa


    We investigated the properties of synthetically produced organic-inorganic hybrid coatings by a sol-gel process. The properties of organic-inorganic hybrid materials arise from the synergism between the properties of the individual components. One of the typical way to synthesize the organic-inorganic hybrid materials is to use silica and silanes. A colloidal silica sol was used as an inorganic material. Methyltrimethoxysilane and phenyltrimethoxysilane were used as the trifunctional organoalkoxysilanes. Hybrid sols of colloidal silica and silanes were synthesized as a function of reaction time and methyltrimethoxysilane/phenyltrimethoxysilane ratio by a sol-gel process. Physical properties of sol solutions such as stability, viscosity, and transmittance were investigated. The surface roughness and surface free energy of the coatings were also measured.

  11. Optical and electrochemical sol-gel sensors for inorganic species



    The use of sol-gels as a sensing matrix for the development of unique sensing strategies is discussed.Sol-gels offer almost limitless possibilities for sensing substrates due to the variety of physical properties that can be obtained by altering a number of discussed fabrication conditions and techniques.By careful consideration of the sensing requirements,novel detection methods have been developed for a variety of analytes and applications.Here,sol-gels have been used to monitor pH at the extreme ends of the scale([H+] = 1―11 M and [OH-] = 1―10 M) and in mixed solvent/solute systems using dual sensing approaches.The use of ligand-grafted sol-gel monoliths for optical determination of metal ion species is also discussed.The electrochemical determination of Cr(Ⅵ) by electrodeposited sol-gel modified electrodes is also presented.

  12. Optical and electrochemical sol-gel sensors for inorganic species



    The use of sol-gels as a sensing matrix for the development of unique sensing strategies is discussed.Sol-gels offer almost limitless possibilities for sensing substrates due to the variety of physical properties that can be obtained by altering a number of discussed fabrication conditions and techniques.By careful consideration of the sensing requirements,novel detection methods have been developed for a variety of analytes and applications.Here,sol-gels have been used to monitor pH at the extreme ends of the scale ([H~+]=1-11 M and[OH~-]=1-10 M) and in mixed solvent/solute systems using dual sensing approaches.The use of ligand-grafted sol-gel monoliths for optical determination of metal ion species is also discussed.The electrochemical determination of Cr(Ⅵ) by electrodeposited sol-gel modified electrodes is also presented.

  13. Isomerization and optical bistability of DR1 doped organic-inorganic sol-gel thin film

    Gao, Tianxi; Que, Wenxiu; Shao, Jinyou


    To investigate the isomerization process of the disperse red 1 (DR1) doped TiO2/ormosil thin film, both the photo-isomerization and the thermal isomerization of the thin films were observed as a change of the absorption spectrum. Under a real-time heat treatment, the change of the linear refractive index shows a thermal stable working temperature range below Tg. The optical bistability (OB) effect of the DR1 doped thin films based on different matrices was studied and measured at a wavelength of 532 nm. Results indicate that the TiO2/ormosils based thin film presents a better OB-gain than that of the poly (methyl methacrylate) (PMMA) based thin film due to its more rigid network structure. Moreover, it is also noted that higher titanium content is helpful for enhancing the OB-gain of the as-prepared hybrid thin films.

  14. Organic-inorganic Polymer Nano-hybrids Based on Sol-gel Reaction

    Yoshiki; Chujo


    1 Results Nano-ordered composite materials consisting of organic polymers and inorganic materials have been attracting attention for the purpose of the creation of high-performance or high-functional polymeric materials. Especially,the word of "polymer hybrid" claims the blends of organic and inorganic components at nano-level dispersion. By using this idea,an enhancement of mechanical strength of organic polymers with silica particles is possible.High transparency of this material is another important ...

  15. Sol-Gel Synthesis of Phosphate-Based Glasses for Hydrophilic Enamel Applications

    Kim, Dae-Sung; Ryu, Bong-ki [Pusan National University, Busan (Korea, Republic of)


    In this study, quaternary phosphate-based sol-gel derived glasses were synthesized from a P{sub 2}O{sub 5}-CaO-Na{sub 2}O-TiO{sub 2} system with a high TiO{sub 2} content of up to 50 mol%. The sol-gel method was chosen because incorporating a high percentage of titanium into a phosphate network via traditional melt-quench methods is non-trivial. The structure and thermal properties of the obtained stabilized sol-gel glasses were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and differential scanning calorimetry (DSC). The XRD results confirmed the amorphous nature of all of the stabilized sol–gel derived glasses. The FTIR results revealed that added TiO{sub 2} enters the network as (TiO{sub 6}), which likely acts as a modifier oxide. Consequently, the number of terminal oxygen atoms increases, leading to an increase in the number of P-OH bonds. In addition, DSC results confirmed a decrease in glass transition and crystallization temperatures with increasing TiO{sub 2} content. This is the first report of a sol-gel synthesis strategy combined with enameling to prepare glass at low processing temperatures and the first use of such a system for both hydrophilic and chemical resistance purposes.

  16. One step antiglare sol-gel coating for screens by sol-gel techniques

    Schelle, Christian; Mennig, Martin; Krug, Herbert; Jonschker, Gerhard; Schmidt, Helmut K.


    Anti-reflection coatings on glass substrates were prepared by the application of sol-gel coatings of silica containing crystalline tin oxide particles. The sol was coated on commercially available float glass by dip-coating and spin-coating techniques. Increasing the surface roughness of the float glass (factor of 50) by a particulate coating material resulted in anti-reflection effects comparable to frosted glass. Haze and clarity, which are a measure for the contrast and definition of an op...

  17. Environmentally benign sol-gel antifouling and foul-releasing coatings.

    Detty, Michael R; Ciriminna, Rosaria; Bright, Frank V; Pagliaro, Mario


    application, and the waterborne nature of sol-gel coatings all support the diffusion of these paints to efficiently reduce the accumulation of fouling layers on valued surfaces immersed in marine or fluvial waters. Furthermore, sol-gel glassy coatings are transparent and can be effectively applied to optical devices, windows, and solar panels used in lake, fluvial, or marine environments. Sol-gel technology is eminently versatile, and the first generation sol-gel paints have already shown good performance. Even so, vast opportunities still exist for chemists to develop novel sol-gel derived coatings to both prevent biofouling and enhance the hydrodynamic properties of boat and ship hulls. Moreover, researchers have prepared and applied multifunctional sol-gel coatings providing protection against both biofouling and corrosion. They have tested these in the marine environment with good preliminary results. In this Account, we discuss some of our new strategies for the controlled functionalization of surfaces for the development of efficient antifouling and foul-releasing systems and summarize the main achievements with biocidal and nonbiocidal sol-gel coatings. We conclude by giving insight into the marine coatings and sol-gel products markets, providing arguments to justify our conclusion that the sol-gel coatings technology is now a mature platform for the development of economically viable and environmentally friendly antifouling and foul-release formulations of enhanced performance.

  18. Bioorganically doped sol-gel materials containing amyloglucosidase activity

    Vlad-Oros Beatrice


    Full Text Available Amyloglucosidase (AMG from Aspergillus niger was encapsulated in various matrices derived from tetraethoxysilane, methyltriethoxysilane, phenyltriethoxysilane and vinyltriacetoxysilane by different methods of immobilization. The immobilized enzyme was prepared by entrapment in two steps, in one-step and entrapment/deposition, respectively. The activities of the immobilized AMG were assayed and compared with that of the native enzyme. The effects of the organosilaneprecursors and their molar ratios, the immobilization method, the inorganic support (white ceramic, red ceramic, purolite, alumina, TiO2, celite, zeolite and enzyme loading upon the immobilized enzyme activity were tested. The efficiency of the sol-gel biocomposites can be improved through combination of the fundamental immobilization techniques and selection of the precursors.

  19. Renewable-surface sol-gel derived carbon ceramic electrode fabricated by [Ru(bpy)(tpy)Cl]PF6 and its application as an amperometric sensor for sulfide and sulfur oxoanions.

    Salimi, Abdollah; Pourbeyram, Sima; Amini, Mohamad Kazem


    A highly sensitive and fast responding sensor for the determination of thiosulfate, sulfite, sulfide and dithionite is described. It consists of a chemically modified carbon ceramic composite electrode (CCE) containing [Ru(bpy)(tpy)Cl]PF6 complex that was constructed by the sol-gel technique. A reversible redox couple of Ru(II)/Ru(III) was observed as a solute in acetonitrile solution and as a component of carbon based conducting composite electrode. Electrochemical behavior and stability of modified CCE were investigated by cyclic voltametry, the apparent electron transfer rate constant (kappa(S)) and transfer coefficient (a) were determined by cyclic voltametry which were about 28 s(-1) and 0.43 respectively. Electrocatalytic oxidation of S(2-), SO3(2-), S2O4(2-) and S2O3(2-) were effective at the modified electrode at significantly reduced overpotentials and in the pH range 1-11. Optimum pH values for amperometric detection of thiosulfate, dithionite, sulfide and sulfite are 7, 9, 2 and 2. Under the optimized conditions the calibration curves are linear in the concentration ranges 1-500, 3-80, 2-90 and 1-100 microM for S2O3(2-), SO3(2-), S2- and S2O4(2-) determination. The detection limit (signal to noise is 3) and sensitivity are 0.5 and 12, 2.8 and 6, 1.6 and 8, and 0.65 microM and 80 nA microM(-1) for thiosulfate, sulfite, sulfide and dithionite detection. The modified carbon ceramic electrode doped with Ru-complex shows good reproducibility, a short response time (t 6 month) and especially good surface renewability by simple mechanical polishing (RSD for eight successive polishing is 2%). The advantages of this sulfur compound amperometric detector based on ruthenium doped CCE are high sensitivity, inherent stability at a broader pH range, excellent catalytic activity, less expense and simplicity of preparation in comparison with recently published papers. This sensor can be used as a chromatographic detector for analysis of sulfur derivatives.

  20. Non-cytotoxic organic-inorganic hybrid bioscaffolds: An efficient bedding for rapid growth of bone-like apatite and cell proliferation

    John, Lukasz, E-mail: [Faculty of Chemistry, University of Wroclaw, 14 F. Joliot-Curie, 50-383 Wroclaw (Poland); Baltrukiewicz, Marta; Sobota, Piotr [Faculty of Chemistry, University of Wroclaw, 14 F. Joliot-Curie, 50-383 Wroclaw (Poland); Brykner, Renata; Cwynar-Zajac, Lucja [Department of Histology and Embryology, Wroclaw Medical University, 6a Chalubinskiego, 50-368 Wroclaw (Poland); Dziegiel, Piotr [Department of Histology and Embryology, Wroclaw Medical University, 6a Chalubinskiego, 50-368 Wroclaw (Poland); Department of Histology and Embryology, Poznan University of Medical Sciences, 6 Swiecickiego, 61-781 Poznan (Poland)


    Synthesis and characterization of organic-inorganic macroporous hybrid scaffolds were investigated. The materials were prepared by combining 2-hydroxyethylmethacrylate (HEMA) and triethoxyvinylsilane (TEVS) chemically modified by Ca{sup 2+} and PO{sub 4}{sup 3-} ions via sol-gel route. In this study we have constructed a sugar-based cracks-free three-dimensional (3D) network with interconnected porous architecture within the range of 150-300 {mu}m and rough topography. The obtained results revealed that both topography and composition of prepared materials allow rapid growth of the bone-like apatite (HAp) layer on their surface after soaking in biological medium. Preliminary studies have shown that hybrids covered by HAp are non-cytotoxic and allow cell proliferation that make them a promising scaffolds in the field of bone regenerative medicine. The materials were mainly characterized by powder X-ray diffraction analysis (PXRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy-energy-dispersive spectroscopy (SEM-EDS) and transmission electron microscopy-energy-dispersive spectroscopy (TEM-EDS). Highlights: Black-Right-Pointing-Pointer Sol-gel derived biomaterials. Black-Right-Pointing-Pointer 3D organic-inorganic hybrid composites for bone tissue engineering. Black-Right-Pointing-Pointer Sugar-templated cracks-free macroporous scaffolds. Black-Right-Pointing-Pointer 2-hydroxyethylmethacrylate/triethoxyvinylsilane blend doped with calcium and phosphate ions. Black-Right-Pointing-Pointer Non-cytotoxic bedding for fibroblasts proliferation.

  1. Influence of Experimental Parameters Using the Dip-Coating Method on the Barrier Performance of Hybrid Sol-Gel Coatings in Strong Alkaline Environments

    Rita B. Figueira


    Full Text Available Previous studies have shown that the barrier effect and the performance of organic-inorganic hybrid (OIH sol-gel coatings are highly dependent on the coating deposition method as well as on the processing conditions. However, studies on how the coating deposition method influences the barrier properties in alkaline environments are scarce. The aim of this experimental research was to study the influence of experimental parameters using the dip-coating method on the barrier performance of an OIH sol-gel coating in contact with simulated concrete pore solutions (SCPS. The influence of residence time (Rt, a curing step between each dip step and the number of layers of sol-gel OIH films deposited on hot-dip galvanized steel to prevent corrosion in highly alkaline environments was studied. The barrier performance of these OIH sol-gel coatings, named U(400, was assessed in the first instants of contact with SCPS, using electrochemical impedance spectroscopy and potentiodynamic methods. The durability and stability of the OIH coatings in SCPS was monitored during eight days by macrocell current density. The morphological characterization of the surface was performed by Scanning Electronic Microscopy before and after exposure to SCPS. Glow Discharge Optical Emission Spectroscopy was used to investigate the thickness of the U(400 sol-gel coatings as a function of the number of layers deposited with and without Rt in the coatings thickness.

  2. Soluble polymers in sol-gel silica

    Beaudry, Christopher Laurent

    In the last few years, the inherent versatility of sol-gel processing has led to a significant research effort on inorganic/organic materials. One method of incorporating an organic phase into sol-gel silica is dissolving an organic polymer in a tetraethylorthosilicate (TEOS) solution, followed by in situ polymerization of silica in the presence of organic polymer. The first part of the study involved the development of a two-step (acid-base) synthesis procedure to allow systematic control of acidity in TEOS solutions. With this procedure, it was possible to increase the pH of the TEOS solution while correlating the acidity and properties. The properties were the gelation time, syneresis rate, drying behavior, and xerogel pore structure, as determined by nitrogen sorption. Furthermore, controlling the acidity was shown to control the silica xerogel pore structure. In the second part of the study, the two-step procedure was used to synthesize silica/poly(ethylene glycol) (PEG), and silica/poly(vinyl acetate) (PVAc) composite materials. The content of organic polymer and the molecular weight were varied. The gelation time, the syneresis rate, the drying behavior, and the pore structure were determined for compositions with 10% PEG (M.W. 2,000), 5, 10, and 15% PEG (M.W. 3,400), and 10 and 25% PVAc (M.W. 83,000). Other compositions and molecular weights of PEG lead to sedimentation. In the PEG compositions, the tendency to phase separate was correlated with the effects of the processing variables on the segregation strength and polymerization rate. The PVAc compositions did not show any visible phase separation during processing, giving the composite xerogels an appearance similar to pure silica. The property differences between gels with PEG and gels with PVAc show the relative strength of the interactions with silica. Both polymers exhibit hydrogen bonding between the phases. In the case of PEG, hydrogen bonding between the ether oxygens of the polymer and silanol

  3. Synthesis, characterization and electrical properties of sol-gel derived 0.63Bi(Mg{sub 1/2}Ti{sub 1/2})O{sub 3}-0.37PbTiO{sub 3} high-T{sub c} piezoelectric ceramics

    Ji Xun [Institute of Electro Ceramics and Devices, School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); Zuo Ruzhong, E-mail: [Institute of Electro Ceramics and Devices, School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); Qi Shishun; Liu Longdong [Institute of Electro Ceramics and Devices, School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China)


    The nano-scaled powders of a high Curie temperature piezoelectric system with a composition of 0.63Bi(Mg{sub 1/2}Ti{sub 1/2})O{sub 3}-0.37PbTiO{sub 3} (0.63BMT-0.37PT) have been synthesized via a citrate sol-gel method. The thermal decomposition process of the as-prepared xerogel was investigated through the thermo-gravitometry and differential scanning calorimetry. The lattice structure of the powders as the function of heat-treatment temperatures was explored by using X-ray diffraction, Fourier-transform infra-red and Raman spectra. The results indicated that the transparent gel could be obtained via the chelate reaction of citric acid with ethylene glycol and ethanolamine assist. Gels can be transformed into crystallite powders with a single-phase perovskite structure when heat-treated at 600 Degree-Sign C for 3 h, much lower than that of traditional solid-state reaction method. The sol-gel derived 0.63BMT-0.37PT ceramics sintered at 1020 Degree-Sign C exhibit excellent dielectric, ferroelectric and piezoelectric properties of T{sub c} = 463 Degree-Sign C, {epsilon}{sub 33}{sup T}=1208, tan {delta} = 0.063, P{sub r} = 22.1 {mu}C cm{sup -2} and d{sub 33} = 230 pC N{sup -1}. Moreover, a small amount of Mn{sup 2+} doping could cause the reduced leakage current and slightly increased T{sub c} values. - Highlights: Black-Right-Pointing-Pointer We synthesize BMT-PT superfine powders of a high Curie temperature piezoelectric system of via citrate sol-gel method. Black-Right-Pointing-Pointer We characterize the powders by means of DSC, XRD, FT-IR, Raman and TEM. Black-Right-Pointing-Pointer Sol-gel derived BMT-PT ceramics sintered at 1020 Degree-Sign C exhibit optimum electrical properties.

  4. Dialkylenecarbonate-Bridged Polysilsesquioxanes. Hybrid Organic Sol-Gels with a Thermally Labile Bridging Group

    Loy, D.A.; Beach, J.V.; Baugher, B.M.; Assink, R.A.; Shea, K.J.; Tran, J.; Small, J.H.


    In this paper, we introduce a new approach for altering the properties of bridged polysilsesquioxane xerogels using post-processing modification of the polymeric network. The bridging organic group contains latent functionalities that can be liberated thermally, photochemically, or by chemical means after the gel has been processed to a xerogel. These modifications can produce changes in density, volubility, porosity, and or chemical properties of the material. Since every monomer possesses two latent functional groups, the technique allows for the introduction of high levels of functionality in hybrid organic-inorganic materials. Dialkylenecarbonate-bridged polysilsesquioxane gels were prepared by the sol-gel polymerization of bis(triethoxysilylpropyl)carbonate (1) and bis(triethoxysilylisobutyl)-carbonate (2). Thermal treatment of the resulting non-porous xerogels and aerogels at 300-350 C resulted in quantitative decarboxylation of the dialkylenecarbonate bridging groups to give new hydroxyalkyl and olefinic substituted polysilsesquioxane monolithic xerogels and aerogels that can not be directly prepared through direct sol-gel polymerization of organotrialkoxysilanes.

  5. Entrapment of glucoamylase by sol-gel technique in PhTES/TEOS hybrid matrixes

    B. Vlad-Oros


    Full Text Available Mesoporous silica particles were prepared by the sol-gel method from different alkoxysilane precursors and used as a host matrix for encapsulation of glucoamylase, an enzyme widely used in fermentative industry. The aim was to investigate the physico-chemical properties of the different silica powders and their effect on the enzyme kinetics. The encapsulated enzymes followed Michaelis-Menten kinetics. The Michaelis constant (KM and the maximum rate of starch hydrolysis reaction (Vmax were calculated according to the Michaelis-Menten and Lineweaver-Burke plots. The values of the Michaelis constant (KM of the encapsulated enzymes were higher than those of the free enzyme. The temperature and pH infl uence on the activity of free and immobilized glucoamylase were also compared. The results of this study show that the enzymes immobilized in organic/inorganic hybrid silica matrixes (obtained by the sol-gel method, allowing the entrapped glucoamylase to retain its biological activity, are suitable for many different applications, (medicinal, clinical, analytical.

  6. Biological evaluation of zirconia/PEG hybrid materials synthesized via sol-gel technique.

    Catauro, M; Papale, F; Bollino, F; Gallicchio, M; Pacifico, S


    The objective of the following study has been the synthesis via sol-gel and the characterization of novel organic-inorganic hybrid materials to be used in biomedical field. The prepared materials consist of an inorganic zirconia matrix containing as organic component the polyethylene glycol (PEG), a water-soluble polymer used in medical and pharmaceutical fields. Various hybrids have been synthesized changing the molar ratio between the organic and inorganic parts. Fourier transform spectroscopy suggests that the structure of the interpenetrating network is realized by hydrogen bonds between the Zr-OH group in the sol-gel intermediate species and both the terminal alcoholic group and ethereal oxygen atoms in the repeating units of polymer The amorphous nature of the gels has been ascertained by X-ray diffraction analysis. The morphology observation has been carried out by using the Scanning Electron Microscope and has confirmed that the obtained materials are nanostructurated hybrids. The bioactivity of the synthesized system has been shown by the formation of a hydroxyapatite layer on the surface of samples soaked in a fluid simulating the human blood plasma. The potential biocompatibility of hybrids has been assessed as performing indirect MTT cytotoxicity assay towards 3T3 cell line at 24, 48, and 72 h exposure times. Copyright © 2014. Published by Elsevier B.V.

  7. Micro-ion beam analysis of physico-chemical reactions in vitro induced by nano-structured sol-gel derived bioactive glasses; Caracterisation par micro-faisceau d'ions des reactions physico-chimiques induites in vitro par des verres bioactifs nanostructures elabores par la methode sol-gel

    Lao, J


    The study of bioactive glasses is a multi-field area of research aiming at a major goal: the development of new generation biomaterials that would be able to bond with host tissues through the formation of a strong interfacial bond, together with helping the body heal itself through the stimulation of specific cellular responses. Thus clinical applications of bioactive glasses mainly concern dental surgery and orthopedics, for filling osseous defects. For this purpose, we have elaborated bioactive glasses in the binary SiO{sub 2}-CaO system, ternary SiO{sub 2}-CaO-P{sub 2}O{sub 5} system, and for the first time, to our knowledge, strontium-doped SiO{sub 2}-CaO-SrO and SiO{sub 2}-CaO-P{sub 2}O{sub 5}-SrO glasses. The materials were elaborated using the sol-gel process, which allowed the synthesis of nano-porous materials with great purity and homogeneity. The bio-activity of the glasses was clearly demonstrated in vitro: in contact with biological fluids, the whole lot of mate-rials were able to induce the formation of a Ca-P-Mg layer a few microns thick at their surface. Our work is characterized by the use of PIXE-RBS nuclear microprobes to study the bioactive glass/biological fluids interface. Thanks to these methods we obtained chemical maps that made possible the analysis of major and trace elements concentrations at the interface. Moreover, quantitative information regarding the local reactivity of glasses were acquired. These data are important to evaluate the kinetics and amplitude of the physico-chemical reactions involved in the bio-activity process. Thus, we highlighted that the binary glass is the highest reactive regarding the dissolution of the glassy matrix as well as the first appearance of the Ca-P rich layer. However the Ca/P atomic ratio calculated at the glass/biological fluids interface decreases slowly, indicating that the Ca-P-Mg layer encounters difficulties to be changed into a more stable apatitic phase. For the P-containing glasses, the de

  8. Sol-gel materials for optofluidics - process and applications

    Mikkelsen, Morten Bo Lindholm


    This Ph.D. thesis is concerned with the use of sol-gel materials in optofluidic applications and the physics of DNA molecules in nanoconfinement. The bottom-up formation of solid material, which is provided by the sol-gel process, enables control of the chemical composition and porosity...... of the material. At early stages of gelation, thin gel coatings can be structured by nanoimprint lithography, and purely inorganic silica materials can be obtained by subsequent thermal annealing. The sol-gel process thus constitutes a unique method for nanofabrication of silica materials of special properties....... In this work, sol-gel silica is introduced as a new material class for the fabrication of lab-on-a-chip devices for DNA analysis. An imprint process with a rigid, non-permeable stamp was developed, which enabled fabrication of micro- and nanofluidic silica channels in a single process step without use of any...

  9. Sol-Gel/Hydrothermal Synthesis of Mixed Metal Oxide

    Mixed metal oxides of titanium and zinc nanocomposites were prepared through sol-gel method under hydrothermal ... the production of TiO -ZnO nanoparticles use. 2 either titanium ... involved using titanium sulphate and thioacetamide for ...

  10. Production of continuous mullite fiber via sol-gel processing

    Tucker, Dennis S.; Sparks, J. Scott; Esker, David C.


    The development of a continuous ceramic fiber which could be used in rocket engine and rocket boosters applications was investigated at the Marshall Space Flight Center. Methods of ceramic fiber production such as melt spinning, chemical vapor deposition, and precursor polymeric fiber decomposition are discussed and compared with sol-gel processing. The production of ceramics via the sol-gel method consists of two steps, hydrolysis and polycondensation, to form the preceramic, followed by consolidation into the glass or ceramic structure. The advantages of the sol-gel method include better homogeneity and purity, lower preparation temperature, and the ability to form unique compositions. The disadvantages are the high cost of raw materials, large shrinkage during drying and firing which can lead to cracks, and long processing times. Preparation procedures for aluminosilicate sol-gel and for continuous mullite fibers are described.

  11. Optical and electrochemical properties of sol-gel spin coated CeO{sub 2}-TiO{sub 2} films

    Ozer, N.; DeSouza, S.; Lampert, C.M.


    There are numerous literature reports on the fabrication of CeO{sub 2}-TiO{sub 2} thin films for use in electrochromic applications. As such, CeO{sub 2}-TiO{sub 2} have attracted interest as transparent counter electrodes for smart windows. Here, the optical and electrochemical properties of sol-gel spin coated CeO{sub 2}-TiO{sub 2} (50% CeO{sub 2}) films were investigated for electrochromic applications. The coating solutions were prepared by using mixed organic-inorganic [Ti(OC{sub 2}H{sub 5}){sub 4} and Ce(NH{sub 4}){sub 2} (NO{sub 3}){sub 6}] precursors. X-ray diffraction studies showed the sol-gel spin-coated films were composed of an amorphous matrix of titanium oxide containing nanocrystallites of cerium oxide. The coating solar transmission value was T{sub s} = 0.8 (250 nm thick). The refractive index and the extinction coefficient were derived from transmittance measurements in the UV-VIS-NIR regions. These films had refractive index value of n = 2.18 and extinction coefficient value of k = 8 {times} 10{sup 4} at {lambda} = 550 m. Cyclic voltammetric measurements showed reversible electrochemical insertion of lithium ions in a CeO{sub 2}-TiO{sub 2}/LiClO{sub 4}-propylene carbonate electrochemical cell. During cycling the films maintain high optical transmittance. Spectrophotometric and electrochemical investigations performed on CeO{sub 2}-TiO{sub 2} films revealed that these films are suitable as an optically passive counter-electrode in lithium electrochromic devices.

  12. Chemical tailoring of hybrid sol-gel thick coatings as hosting matrix for functional patterned microstructures.

    Falcaro, Paolo; Costacurta, Stefano; Malfatti, Luca; Buso, Dario; Patelli, Alessandro; Schiavuta, Piero; Piccinini, Massimo; Grenci, Gianluca; Marmiroli, Benedetta; Amenitsch, Heinz; Innocenzi, Plinio


    A phenyl-based hybrid organic - inorganic coating has been synthesized and processed by hard X-ray lithography. The overall lithography process is performed in a two-step process only (X-rays exposure and chemical etching). The patterns present high aspect ratio, sharp edges, and high homogeneity. The coating has been doped with a variety of polycyclic aromatic hydrocarbon functional molecules, such as anthracene, pentacene, and fullerene. For the first time, hard X-rays have been combined with thick hybrid functional coatings, using the sol-gel thick film directly as resist. A new technique based on a new material combined with hard X-rays is now available to fabricate optical devices. The effect due to the high-energy photon exposure has been investigated using FT-IR and Raman spectroscopy, laser scanner, optical profilometer, and confocal and electron microscope. High-quality thick hybrid fullerene-doped microstructures have been fabricated.

  13. Optical Properties of BDK-Doped Highly Photosensitive Sol-Gel Hybrid Film

    XU Ming; SHEN Wei-Dong; ZHANG Yue-Guang; ZHEN Hong-Yu; LIU Xu


    @@ A new organic-inorganic by brid material doped with BDK that exhibits a large photo-induced change in optical properties is prepared by the sol-gel method.The photosensitivity of the film under ultraviolet irradiation is investigated with various exposure times.An increase in refractive index from 1.558 to 1.592 at A=550nm is observed together with a 57.3% expansion in physical thickness.The film's optical thickness exhibits an exponential change with the irradiation time.The photo-decomposition of BDK organic groups confirmed by the infrared absorption spectrum contributes to the photosensitive mechanism.A first example of photo-patterning is finally presented by direct light writing.

  14. Europium incorporated in silica matrix obtained by sol-gel: luminescent materials

    Eduardo José Nassar


    Full Text Available In this work we report some aspects of the chemistry involved in the preparation of modified silicon oxide by the sol-gel process. Europium III compounds were used as luminescent probe. An organic-inorganic hybrid was obtained by hydrolysis of tetraethylorthosilicate (TEOS and 3-aminopropyltriethoxysilane (APTS. The Eu III compounds were added in different ways. In the first, silica was prepared in the presence of Eu III, and in the second, Eu III was added on the silica surface. These materials were studied by luminescence, infrared spectroscopy and termogravimetric analysis. The results obtained for the hybrid material show different behavior for Eu III emission, which could be excited by the antenna effect and the influence of the surrounding in the luminescence quenching. The thermogravimetric data present different mass loss in samples to range temperature 50 - 150 °C. Thermogravimetric and infrared spectra showed that inorganic polymers incorporated the organic part.

  15. Immobilization of Biocatalysts and Cells on Hybrid Membranes Syntheses on Sol-gel Method

    Yotova L.


    Full Text Available The investigations in the area of enzyme action in the living organisms give us the opportunity for applications of these biochemical catalysts in the different purposes of medicine, industry and analytical practice. Using of soluble enzymes is connected with many difficulties, because the enzymes are no regenerative and they are instability. By immobilization of the enzymes on to different carriers the more of these problems are overcome. The application of soluble enzymes caused many difficulties, by the reason that the enzymes can not be regenerated. The immobilization of the enzymes by means of different reagents and carriers overcomes this problem. The aim of this study to develop a sol-gel method of synthesis of new hybrid membrane, with immobilized biocatalysts (microbial cells and enzymes for biosensor construction. This study shows that hybrid organic-inorganic membranes were synthesized.

  16. Self-Healing Corrosion Protective Sol-Gel Coatings

    Abdolah Zadeh, M.


    Inspired by the state of the art and the recent advances in the field of self-healing corrosion protective coatings, the thesis entitled “Self-healing corrosion protective sol-gel coatings” addresses novel routes to self-healing corrosion protective sol-gel coatings via extrinsic and intrinsic healing approaches. The employed approaches aim at extending the service life of the coating and the underlying substrate by multiple damage closure/sealing and metal surface protection through incorpor...

  17. Chemical Sensors Based on Molecularly Imprinted Sol-Gel Materials

    Dickert, Franz L.; Lieberzeit, Peter A.; Adnan Mujahid


    The sol-gel technique is earning the worldwide attention of researchers in the field of material science, due to its versatility in synthesizing inorganic ceramic materials at mild conditions. High purity, homogeneity, controlled porosity, stable temperature and nanoscale structuring are the most remarkable features offered by this method for generating highly sensitive and selective matrices to incorporate analyte molecules. The crafting of sol-gel sensors through molecular imprinting has pu...

  18. Electrochemical and spectroscopic characterization of surface sol-gel processes.

    Chen, Xiaohong; Wilson, George S


    (3-Mercaptopropyl)trimethoxysilane (MTS) forms a unique film on a platinum substrate by self-assembly and sol-gel cross-linking. The gelating and drying states of the self-assembled MTS sol-gel films were probed by use of electrochemical and spectroscopic methods. The thiol moiety was the only active group within the sol-gel network. Gold nanoparticles were employed to detect the availability of the thiol group and their interaction further indicated the physicochemical states of the sol-gel inner structure. It was found that the thiol groups in the open porous MTS aerogel matrix were accessible to the gold nanoparticles while thiol groups in the compact MTS xerogel network were not accessible to the gold nanoparticles. The characteristics of the sol-gel matrix change with time because of its own irreversible gelating and drying process. The present work provides direct evidence of gold nanoparticle binding with thiol groups within the sol-gel structures and explains the different permeability of "aerogel" and "xerogel" films of MTS on the basis of electrochemical and spectroscopic results. Two endogenous species, hydrogen peroxide and ascorbic acid, were used to test the permeability of the self-assembled sol-gel film in different states. The MTS xerogel film on the platinum electrode was extremely selective against ascorbic acid while maintaining high sensitivity to hydrogen peroxide in contrast to the relatively high permeability of ascorbic acid in the MTS aerogel film. This study showed the potential of the MTS sol-gel film as a nanoporous material in biosensor development.

  19. Liquid Density Sensing Using Resonant Flexural Plate Wave Device with Sol-Gel PZT Thin Films

    Yu, Jyh-Cheng


    This paper presents the design, fabrication and preliminary experimental results of a flexure plate wave (FPW) resonator using sol-gel derived lead zirconate titanates (PZT) thin films. The resonator adopts a two-port structure with reflecting grates on the composite membrane of PZT and SiNx. The design of the reflecting grate is derived from a SAW resonator model using COM theory to produce a sharp resonant peak. The comparison between the mass and the viscosity effects from the theoretical expression illustrates the applications and the constraints of the proposed device in liquid sensing. Multiple coatings of sol-gel derived PZT films are adopted because of the cost advantage and the high electromechanical coupling effect over other piezoelectric films. The fabrication issues of the proposed material structure are addressed. Theoretical estimations of the mass and the viscosity effects are compared with the experimental results. The resonant frequency has a good linear correlation with the density of low v...

  20. Nanocrystalline Pentaerythritoltetranitrate using Sol-Gel Process

    Sanjay Vishwasrao Ingale


    Full Text Available The secondary explosives developed with reduced particle size tend to be more insensitive for mechanical stimuli and may release energy with faster rate and gaining more importance nowadays. Therefore, aiming to reduce the particle size of one of the popular explosives, viz., pentaerythritoltetranitrate (PETN to the nanometer range, a method for preparation of nanocrystalline PETN in the silica (SiO2 gel matrix using sol-gel process has been demonstrated. The PETN-SiO2 xerogels were prepared containing PETN content ranging from 50 per cent to 90 per cent (w/w and the xerogels were characterised using different techniques. An exothermic peak at around 185 oC preceded by an endotherm in thermal analysis accompanied with weight loss in the temperature range from 150 oC to 200 oC   for the xerogel confirmed the presence of PETN in xerogel. Infrared spectra of xerogels showed peaks at around 1285 cm-1 and 1700 cm-1 assigned to O-NO2 and C-O bond representing PETN. Small angle x-ray scattering measurements on xerogels indicated that PETN entered in the pores of silica matrix. Transmission electron microscopy revealed that cystalline PETN    with particle size of around 15 nm dispersed in silica xerogel. The specific surface area for the PETN-SiO2 (90:10 xerogels was found to be 75 m2/g.Defence Science Journal, 2011, 61(6, pp.534-539, DOI:

  1. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong


    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column.

  2. Corrosion and Wear Resistance Characterization of Environmentally Friendly Sol-gel Hybrid Nanocomposite Coating on AA5083

    Hamed Rahimi; Reza Mozaffarinia; Akbar Hojjati Najafabadi


    Environmentally friendly organic-inorganic hybrid nanocomposite films have been developed by sol-gel method for corrosion protection of AA5083 alloy.The hybrid nanocomposite coatings have been synthesized from tetraethylorthosilicate (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTMS) precursors.The multilayer coatings were prepared by dip-coating technique.Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy was carried out to show the formation of the Si-O-Si structural backbone of the hybrid coatings.Structure and surface morphology of the coatings were studied by optical microscopy (OM),scanning electron microscopy (SEM) and atomic force microscopy (AFM).Characterization of the coatings with respect to pencil scratch hardness,adhesive and abrasion resistance was performed.The corrosion protection performance of these coatings was examined by using cyclic potentiodynamic polarization technique in Persian Gulf water.The results revealed that crack-free films with smooth surface were obtained.With increasing the number of sol-gel coated layers,corrosion resistance increased from 81 to 419 kΩ cm2,while the abrasion wear resistance did not change significantly.However,the triple sol-gel coated layer offered excellent protection against corrosion.

  3. Perovskite phase transformation in 0.65Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-0.35PbTiO{sub 3} nanoparticles derived by sol-gel

    Singh, Satyendra [Materials Research Centre, Indian Institute of Science, Bangalore - 560012 (India); Applied Sciences Department, PEC University of Technology, Chandigarh - 12 (India); Krupanidhi, S. B. [Materials Research Centre, Indian Institute of Science, Bangalore - 560012 (India)


    Fabrication of 0.65Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-0.35PbTiO{sub 3} (PMN-PT) nanoparticles with an average size of about 40 nm and their phase transformation behavior from pyrochlore to perovskite phase is investigated. A novel sol-gel method was used for the synthesis of air-stable and precipitate-free diol-based sol of PMN-PT which was dried and partially calcined at 450 deg. C for 1 h to decompose organics and bring down the free energy barrier for perovskite crystallization and then finally annealed in the temperature range 600 to 700 deg. C. Annealed at around 700 deg. C for 1 h, PMN-PT gel powder exhibited nanocrystalline morphology with perovskite phase as confirmed by the transmission electron microscopy and X-ray diffraction techniques.

  4. White light up-conversion in transparent sol-gel derived glass-ceramics containing Yb{sup 3+}-Er{sup 3+}-Tm{sup 3+} triply-doped YF{sub 3} nanocrystals

    Santana-Alonso, A. [Departamento Fisica Basica, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Mendez-Ramos, J. [Departamento Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Yanes, A.C., E-mail: [Departamento Fisica Basica, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Castillo, J. del [Departamento Fisica Basica, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain); Rodriguez, V.D. [Departamento Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206, La Laguna, Tenerife (Spain)


    Transparent glass-ceramics containing YF{sub 3} nanocrystals triply-doped with Yb{sup 3+}-Er{sup 3+}-Tm{sup 3+} ions have been successfully obtained under adequate thermal treatment of precursor sol-gel glasses for the first time to our knowledge. X-ray diffraction and high resolution transmission electron microscopy analysis pointed out the precipitation of YF{sub 3} nanocrystals. Up-conversion luminescence features confirm the effective partition of luminescent ions into precipitated nanocrystals. Corresponding energy transfer up-conversion mechanisms and the dependence of the overall emitting colour have been analyzed as a function of doping ions, with varying concentration. In particular, very bright and efficient up-conversion emission, almost matching the standard equal energy white light illumination point of the standard chromaticity diagram, has been achieved showing up as promising candidate material for potential applications in photonic integrated devices and infrared tuneable phosphors.

  5. Low temperature synthesis of magnesium oxide and spinel powders by a sol-gel process

    Li-Zhai Pei; Wan-Yun Yin; Ji-Fen Wang; Jun Chen; Chuan-Gang Fan; Qian-Feng Zhang


    Magnesium oxide and magnesium aluminate (MgAl2O4) spinel (MAS) powders have been synthesized by a simple aqueous sol-gel process using citrate polymeric precursors derived from magnesium chloride, aluminium nitrate and citrate. The thermal decomposition of the precursors and subsequent formation of cubic MgO and MAS were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetry-differential scanning calorimetry (TG-DSC) and Fourier transform infrared spectr...

  6. Slow Release of Plant Volatiles Using Sol-Gel Dispensers.

    Bian, L; Sun, X L; Cai, X M; Chen, Z M


    The black citrus aphid, also known as the tea aphid, (Toxoptera aurantii Boyer) attacks economically important crops, including tea (Camellia sinensis (L.) O. Kuntze). In the current study, silica sol-gel formulations were screened to find one that could carry and release C. sinensis plant volatiles to lure black citrus aphids in a greenhouse. The common plant volatile trans-2-hexen-1-al was used as a model molecule to screen for suitable sol-gel formulations. A zNose (Electronic Sensor Technology, Newbury Park, CA) transportable gas chromatograph was used to continuously monitor the volatile emissions. A sol-gel formulation containing tetramethyl orthosilicate and methyltrimethoxysilane in an 8:2 (vol:vol) ratio was selected to develop a slow-release dispenser. The half-life of trans-2-hexen-1-al in the sol-gel dispenser increased slightly with the volume of this compound in the dispenser. Ten different volatiles were tested in the sol-gel dispenser. Alcohols of 6-10 carbons had the longest half-lives (3.01-3.77 d), while esters of 6-12 carbons had the shortest (1.53-2.28 d). Release of these volatiles from the dispensers could not be detected by the zNose after 16 d (cis-3-hexenyl acetate) to 26 d (3,7-dimethylocta-1,6-dien-3-ol). In greenhouse experiments, trans-2-hexen-1-al and cis-3-hexen-1-ol released from the sol-gel dispensers attracted aphids for ≍17 d, and release of these volatiles could not be detected by the zNose after ≍24 d. The sol-gel dispensers performed adequately for the slow release of plant volatiles to trap aphids in the greenhouse.

  7. Sol-gel germania triblock polymer coatings of exceptional pH stability in capillary microextraction online-coupled to high-performance liquid chromatography.

    Segro, Scott S; Triplett, Judy; Malik, Abdul


    For the first time, a germania-based sol-gel coating was used in capillary microextraction (CME) in combination with high-performance liquid chromatography (HPLC). A hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide), was covalently bonded into a sol-gel germania matrix in the course of its creation from an alkoxide precursor via hydrolytic polycondensation reactions. A thin layer of this in situ-created sol-gel hybrid material was covalently anchored to the inner walls of a 0.25 mm i.d. fused silica capillary to produce a sol-gel germania triblock polymeric sorbent in the form of a highly stable surface coating. Such a coating served as an effective extracting phase for the preconcentration of a wide range of polar and nonpolar analytes (e.g., alcohols, amines, ketones, phenols, and polycyclic aromatic hydrocarbons) with nanomolar and picomolar detection limits. Most significantly, the sol-gel germania triblock polymer coating demonstrated impressive resistance to extreme pH conditions, surviving 5 days of continuous exposure to 1.0 M HCl (pH approximately 0.0) or 1.0 M NaOH (pH approximately 14.0), practically without any changes in performance. This shows the suitability of sol-gel germania hybrid organic-inorganic hybrid materials for use as sorbents or stationary phases under extreme pH conditions, often needed in a variety of separation and sample preparation techniques and applications, including ion chromatography, hydrophobic interaction chromatography, proteomics, HPLC with electrochemical detection, isoelectric focusing, and extraction of acidic and basic analytes.

  8. Formation of macroporous gel morphology by phase separation in the silica sol-gel system containing nonionic surfactant

    Junsheng Wu; Xiaogang Li; Wei Du; Hua Chen


    The phase separation and gel formation behavior in an alkoxy-derived silica sol-gel system containing Ci6EOi5 has been investigated. Various gel morphologies similar to other sol-gel systems containing organic additives were obtained by changing the preparation conditions. Micrometer-range interconnected porous gels were obtained by freezing transitional structures of phase separation in the sol-gel process. The dependence of the resulting gel morphology on several important reaction parameters such as the starting composition, reaction temperature and acid catalyst concentration was studied in detail. The experimental results indicate that the gel morphology is mainly determined by the time relation between the onset of phase separation and gel formation.

  9. Preparation and Characterisation of Hydroxyapatite Coatings on Nanotubular TiO2 Surface Obtained by Sol-Gel Process.

    Shin, Jin-Ho; Kim, Jung-Hwa; Koh, Jeong-Tae; Lim, Hyun-Pil; Oh, Gye-Jeong; Lee, Seok-Woo; Lee, Kwang-Min; Yun, Kwi-Dug; Park, Sang-Won


    Hydroxyapatite (HA) coating on titanium dioxide (TiO2) nanotubular surface has been developed to complement the defects of both TiO2 and HA. A sol-gel processing technique was used to coat HA on TiO2 nanotubular surface. All the titanium discs were blasted with resorbable blast media (RBM). RBM-blasted Ti surface, anodized Ti surface, and sol-gel HA coating on the anodized Ti surface were prepared. The characteristics of samples were observed using scanning electron microscopy and X-ray photoemission spectroscopy. Biologic responses were evaluated with human osteosarcoma MG63 cells in vitro. The top of the TiO2 nanotubes was not completely covered by HA particles when the coating time was less than 60 sec. It was demonstrated the sol-gel derived HA film was well-crystallized and this enhanced biologic responses in early stage cell response.

  10. Synthesis and optical features of an europium organic-inorganic silicate hybrid

    Franville, A.C.; Zambon, D.; Mahiou, R.; Chou, S.; Cousseins, J.C. [Universite Blaise Pascal, Aubiere (France). Lab. des Materiaux Inorganiques; Troin, Y. [Laboratoire de Chimie des Heterocycles et des Glucides, EA 987, Universite Blaise-Pascal and ENSCCF, F-63177 Aubiere Cedex (France)


    A europium organic-inorganic silicate hybrid was synthesized by grafting a coordinative group (dipicolinic acid) to a silicate network precursor (3-aminopropyltriethoxysilane) via a covalent bonding. Sol-gel process and complexation were performed using different experimental conditions. The hybrid materials, in particular the Eu{sup 3+} coordination mode, were characterized by infrared and luminescence spectroscopies. Morphology of the materials and TG analysis showed that grafted silica enhanced thermal and mechanical resistances of the organic part. (orig.) 7 refs.

  11. Scripting approach in hybrid organic-inorganic condensation simulation: the GPTMS proof-of-concept

    Maly, Marek; Posocco, Paola; Fermeglia, Maurizio; Pricl, Sabrina


    Abstract Silica-based hybrid organic-inorganic materials prepared by sol-gel chemistry exhibit unique chemical and physical properties by virtue of their anisotropic organization. (3-glycidoxypropyl)trimethoxysilane (GPTMS)-based networks represent an archetype of this class of substances, with a vast range of applications. In the present study, a new computational recipe has been developed within Materials Studio software platform to generate atomistic models of GPTMS crosslinked ...

  12. Determination of Aromatic Amines Using Solid-Phase Microextraction Based on an Ionic Liquid-Mediated Sol-Gel Technique.

    Abbasi, Vajihe; Sarafraz-Yazdi, Ali; Amiri, Amirhassan; Vatani, Hossein


    A headspace solid-phase microextraction (HS-SPME) method was developed for isolation of monocyclic aromatic amines from water samples followed by gas chromatography-flame ionization detector (GC-FID). In this work, the effect of the presence of ionic liquid (namely, 1-hexyl-3-methyl-imidazolium hexafluorophosphate [C6MIM][PF6]) was investigated in the sol-gel coating solutions on the morphology and extraction behavior of the resulting hybrid organic-inorganic sol-gel sorbents utilized in SPME. Hydroxy-terminated poly(dimethylsiloxane) (PDMS) was used as the sol-gel active organic component for sol-gel hybrid coatings. Two different coated fibers that were prepared are PDMS and PDMS-IL ([C6MIM][PF6]) fibers. Under the optimal conditions, the method detection limits (S/N = 3) with PDMS-IL were in the range of 0.001-0.1 ng/mL and the limits of quantification (S/N = 10) between 0.005 and 0.5 ng/mL. The relative standard deviations for one fiber (n = 5) were obtained from 3.1 up to 8.5% and between fibers or batch to batch (n = 3) in the range of 5.3-10.1%. The developed method was successfully applied to real water and juice fruits samples while the relative recovery percentages obtained for the spiked water samples at 0.1 ng/mL were from 83.3 to 95.0%.

  13. Sol-gel preparation and electrical behaviour of Ln: YAG (Ln = Ce, Nd, Ho, Er



    Full Text Available A sol-gel method has been developed to prepare pure yttrium aluminum garnet, Y3Al5O12 (YAG, and rare-earth substituted (Ce-Y3Al5O12, Nd-Y3Al5O12, Ho-Y3Al5O12, and Er-Y3Al5O12 samples. The XRD patterns of the polycrystalline powders sintered at 1000ºC showed the formation of monophasic garnet materials. The micro-structural features in the polycristalline samples were studied by scanning electron microscopy. A homogeneous distribution of rare-earth dopants in the YAG lattice was achieved in all of the cases. Electrical conductivity measurements were also performed on the compacts of sol-gel derived Ln-YAG samples. In contrast to the expected dielectric behaviour, the conducting properties of the examined specimens indicate metallic behaviour with the resistivity increasing gradually with increasing temperature.

  14. Structural evolution and stability of sol-gel biocatalysts

    Rodgers, L.E. [School of Biotechnology and Biomolecular Sciences, University of New South Wales, NSW 2052 (Australia)]. E-mail:; Knott, R.B. [Australian Nuclear Science and Technology Organisation, PMB 1, Menai, NSW 2234 (Australia); Holden, P.J. [Australian Nuclear Science and Technology Organisation, PMB 1, Menai, NSW 2234 (Australia); Pike, K.J. [Australian Nuclear Science and Technology Organisation, PMB 1, Menai, NSW 2234 (Australia); Hanna, J.V. [Australian Nuclear Science and Technology Organisation, PMB 1, Menai, NSW 2234 (Australia); Foster, L.J.R. [School of Biotechnology and Biomolecular Sciences, University of New South Wales, NSW 2052 (Australia); Bartlett, J.R. [Australian Nuclear Science and Technology Organisation, PMB 1, Menai, NSW 2234 (Australia)


    Immobilisation strategies for catalytic enzymes are important as they allow recovery and reuse of the biocatalysts. In this work, sol-gel matrices have been used to immobilise Candida antarctica lipase B (CALB), a commonly used industrial enzyme. The sol-gel bioencapsulate is produced through fluoride-catalysed hydrolysis of mixtures of tetramethylorthosilicate (TMOS) and methyltrimethoxysilane (MTMS) in the presence of CALB, yielding materials with controlled pore sizes and surface chemistries. Sol-gel matrices prolong the catalytic life and enhance the activity of CALB, although the molecular basis for this effect has yet to be elucidated due to the limitations of analytical techniques applied to date. Small angle neutron scattering (SANS) allows such multi-component systems to be characterised through contrast matching. In the sol-gel bioencapsulate system at the contrast match point for silica, residual scattering intensity is due to the CALB and density fluctuations in the matrix. A SANS contrast variation series found the match point for the silica matrix, both with and without enzyme present, to be around 35%. The model presented here proposes a mechanism for the interaction between CALB and the surrounding sol-gel matrix, and the observed improvement in enzyme activity and matrix strength. Essentially, the inclusion of CALB modulates silicate speciation during evolution of the inorganic network, leading to associated variations in SANS contrast. The SANS protocol developed here may be applied more generally to other encapsulated enzyme sys0010te.

  15. Bioactivity of sol-gel derived apatite/wollastonite porous bioactive glass-ceramic%溶胶-凝胶法制备磷灰石-硅灰石多孔生物活性玻璃陶瓷的生物活性

    杨为中; 周成昕; 肖斌; 尹光福; 周大利


    .MATERIALS: AWGC.METHODS: This experiment was conducted at the laboratory of College of Materials Science and Engineering of Sichuan University between August 2002 and May 2003. AWGC was prepared from sol-gel and followed by heattreating process. Bioactivity was investigated in vitro by immersing in the simulate body fluid (SBF) at 37 ℃ for 7 days . JL-1155 laser particle analyzer, X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscope were used for micro-morphological structure analysis.MAIN OUTCOME MEASURES: ①The crystalline structure and microstructure of sol-gel derived glass-ceramic② The apatite forming process in simulate body fluid③ The diameter of the pore of the sol-gel derived apatite/wollastonite glass-ceramicRESULTS: ①Main crystalline phases of the sol-gel derived glass-ceramic materials were hydroxyapatite/fluoroapatite [Ca10(PO4)6(OH, F)] and β-wollastonite[β-CaSiO3]; Microstructure contained many micro-pores of 2-3μ m;② Sol-gel derived AW glass ceramic had excellent bioactivity: plenty of apatite granules were generated on the surface of the material after soaking for 7 days. ③Porous scaffolds possessed good macro-porous structure with the interconnected macro pores of 300-400 μm in diameter;CONCLUSION: Apatite-wollastonite containing glass-ceramic (AWGC)with excellent bioactivity was developed by sol-gel process. The material is expected to be a good candidate for bone-repairing and bone tissue engineering scaffold materials.

  16. Natamycin based sol-gel antimicrobial coatings on polylactic acid films for food packaging.

    Lantano, Claudia; Alfieri, Ilaria; Cavazza, Antonella; Corradini, Claudio; Lorenzi, Andrea; Zucchetto, Nicola; Montenero, Angelo


    In this work a comprehensive study on a new active packaging obtained by a hybrid organic-inorganic coating with antimicrobial properties was carried out. The packaging system based on polylactic acid was realised by sol-gel processing, employing tetraethoxysilane as a precursor of the inorganic phase and polyvinyl alcohol as the organic component, and incorporating natamycin as the active agent. Films with different organic-inorganic ratios (in a range between 1:19 and 1:4) were prepared, and the amount of antimycotic entrapped was found to be modulated by the sol composition, and was between 0.18 and 0.25mg/dm(2). FTIR microspectroscopic measurements were used to characterise the prepared coatings. The antifungal properties of the films were investigated against mould growth on the surface of commercial semi-soft cheese. The release of natamycin from the films to ethanol 50% (v/v) was studied by means of HPLC UV-DAD. The maximal level released was about 0.105 mg/dm(2), which is far below the value allowed by legislation.

  17. Chemical Sensors Based on Molecularly Imprinted Sol-Gel Materials

    Franz L. Dickert


    Full Text Available The sol-gel technique is earning the worldwide attention of researchers in the field of material science, due to its versatility in synthesizing inorganic ceramic materials at mild conditions. High purity, homogeneity, controlled porosity, stable temperature and nanoscale structuring are the most remarkable features offered by this method for generating highly sensitive and selective matrices to incorporate analyte molecules. The crafting of sol-gel sensors through molecular imprinting has put great influence on the development of innovative chemical sensors, which can be seen from the growing number of publications in this field. The review provides a brief overview of sol-gel sensor applications, and discusses the contribution of molecular imprinting in exploring the new world of sensors.

  18. Optical Sensors for Biomolecules Using Nanoporous Sol-Gel Materials

    Fang, Jonathan; Zhou, Jing C.; Lan, Esther H.; Dunn, Bruce; Gillman, Patricia L.; Smith, Scott M.


    An important consideration for space missions to Mars is the ability to detect biosignatures. Solid-state sensing elements for optical detection of biological entities are possible using sol-gel based biologically active materials. We have used these materials as optical sensing elements in a variety of bioassays, including immunoassays and enzyme assays. By immobilizing an appropriate biomolecule in the sol-gel sensing element, we have successfully detected analytes such as amino acids and hormones. In the case of the amino acid glutamate, the enzyme glutamate dehydrogenase was the immobilized molecule, whereas in the case of the hormone cortisol, an anti-cortisol antibody was immobilized in the sensing element. In this previous work with immobilized enzymes and antibodies, excellent sensitivity and specificity were demonstrated in a variety of formats including bulk materials, thin films and fibers. We believe that the sol-gel approach is an attractive platform for bioastronautics sensing applications because of the ability to detect a wide range of entities such as amino acids, fatty acids, hopanes, porphyrins, etc. The sol-gel approach produces an optically transparent 3D silica matrix that forms around the biomolecule of interest, thus stabilizing its structure and functionality while allowing for optical detection. This encapsulation process protects the biomolecule and leads to a more "rugged" sensor. The nanoporous structure of the sol-gel matrix allows diffusion of small target molecules but keeps larger, biomolecules immobilized in the pores. We are currently developing these biologically active sol-gel materials into small portable devices for on-orbit cortisol detection

  19. Sol-gel processing with inorganic metal salt precursors

    Hu, Zhong-Cheng


    Methods for sol-gel processing that generally involve mixing together an inorganic metal salt, water, and a water miscible alcohol or other organic solvent, at room temperature with a macromolecular dispersant material, such as hydroxypropyl cellulose (HPC) added. The resulting homogenous solution is incubated at a desired temperature and time to result in a desired product. The methods enable production of high quality sols and gels at lower temperatures than standard methods. The methods enable production of nanosize sols from inorganic metal salts. The methods offer sol-gel processing from inorganic metal salts.

  20. Micro-PIXE-RBS methods highlighting the influence of phosphorus on the in vitro bioactivity of sol-gel derived glass particles in the SiO 2-CaO-P 2O 5 system

    Lao, J.; Nedelec, J. M.; Moretto, Ph.; Jallot, E.


    Ion beam analysis methods were used to characterize the interface of bioactive glasses with surrounding biological fluids. Glass particles in the SiO2-CaO and SiO2-CaO-P2O5 compositions were made by sol-gel processing and soaked in biological fluids for periods up to 4 days. The surface changes were characterized using PIXE-RBS, which are efficient methods for multielemental analysis and accurate trace elements quantification. Elemental maps of major and trace elements were obtained at a micrometer scale and revealed the bone bonding ability of the materials. Glass particles are quickly coated with a thin calcium phosphate-rich layer containing traces of magnesium. After a few days, SiO2-CaO-P2O5 glass particles are entirely changed into calcium phosphates, whereas SiO2-CaO particles exhibit a different behavior: the previously Ca-P enriched periphery has been dissolved and glass particles consist of a silicate network. Calculation of the Ca-P atomic ratios at the glass/biological fluids interface provides us with an explanation for this: an enduring apatitic phase seems to be formed at the periphery of SiO2-CaO-P2O5 glass particles. Presence of phosphorus in the glass matrix thus has an influence on the amplitude and the kinetics of reaction of the bioactivity process. It might result in an improved chemical bond with living tissues.

  1. Influence of calcinated and non calcinated nanobioglass particles on hardness and bioactivity of sol-gel-derived TiO2-SiO2 nano composite coatings on stainless steel substrates.

    Dadash, Mohammad Saleh; Karbasi, Saeed; Esfahani, Mojtaba Nasr; Ebrahimi, Mohammad Reza; Vali, Hojatollah


    Thick films of calcinated and non calcinated nanobioglass (NBG)-titania composite coatings were prepared on stainless steel substrates by alkoxide sol-gel process. Dip-coating method was used for the films preparation. The morphology, structure and composition of the nano composite films were evaluated using environmental scanning electron microscope, X-ray diffraction and Fourier transform infrared spectroscope. The SEM investigation results showed that prepared thick NBG-titania films are smooth and free of macrocracking, fracture or flaking. The grain size of these films was uniform and nano scale (50-60 nm) which confirmed with TEM. Also FTIR confirmed the presence of Si-O-Si bands on the calcinated NBG-titania films. The hardness of the prepared films (TiO(2)-calcinated NBG and TiO(2)-Non calcinated NBG) was compared by using micro hardness test method. The results verified that the presence of calcinated NBG particles in NBG-titania composite enhanced gradually the mechanical data of the prepared films. The in vitro bioactivity of these films was discussed based on the analysis of the variations of Ca and P concentrations in the simulated body fluid (SBF) and their surface morphologies against immersion time. Surface morphology and Si-O-Si bands were found to be of great importance with respect to the bioactivity of the studied films. The results showed that calcinated NBG-titania films have better bioactivity than non calcinated NBG-titania films.

  2. Remarkable enhancement of the photoreactivity of a polyfluoroalkyl azobenzene derivative in an organic-inorganic nano-layered microenvironment.

    Ramakrishnan, Vivek; Yamamoto, Daisuke; Sasamoto, Shin; Shimada, Tetsuya; Nabetani, Yu; Tachibana, Hiroshi; Inoue, Haruo


    Organic-inorganic hybrids composed of polyfluoroalkyl azobenzene surfactant (abbreviated as C3F-Azo-C6H) and inorganic layered compounds are able to undergo reversible three-dimensional morphology changes such as interlayer space changes and nanosheet sliding in a giant scale due to reversible trans-cis isomerization of the azobenzene moiety upon photo-irradiation. In this paper, we have systematically studied the relationship between the layered hybrid microstructures of C3F-Azo-C6H-clay and their photoreactivity for understanding the mechanism of the photo-induced morphology change. The photoreactivity was found to be very much affected by the surrounding microenvironments. As compared with it in solution, the cis-trans photo-isomerization in C3F-Azo-C6H-clay nano-layered film was substantially enhanced with the quantum yield exceeding unity (Φ = 1.9), while the trans-cis isomerization was rather retarded. The corresponding hydrocarbon analogue of the azobenzene surfactant (C3H-Azo-C6H) did not show such an enhancement. The enhancement was discussed in terms of a cooperative effect among adjacent azobenzene moieties along with polyfluoroalkyl chains and the inorganic clay nanosheet to prevent a dissipation of the excess energy being liberated during the photo-isomerization within the nano-layered microenvironment.

  3. Sol-gel matrices for direct colorimetric detection of analytes

    Charych, Deborah H.; Sasaki, Darryl; Yamanaka, Stacey


    The present invention relates to methods and compositions for the direct detection of analytes using color changes that occur in immobilized biopolymeric material in response to selective binding of analytes to their surface. In particular, the present invention provides methods and compositions related to the encapsulation of biopolymeric material into metal oxide glass using the sol-gel method.

  4. Analyses of laser and furnace treated sol-gel coatings

    De Hosson, JT; De Haas, M; Sudarshan, TS; Jeandin, M; Khor, KA


    Here we explore a new method that allows thin films to be made with almost any composition and degree of porosity by means of a combination of sol-gel and laser technology. Results are presented for furnace and laser treated TEOTI-(tetraethylorthotitanate as sol precursor) coated silicon samples.

  5. Stoichiometric hydroxyapatite obtained by precipitation and sol gel processes

    C. Guzmán Vázquez; C. Piña Barba; N. Munguía


    Three methods for obtaining hydroxiapatite (HA) are described. HA is a very interesting ceramic because of its many medical applications. The first two precipitation methods start from calcium and phosphorous compounds, whereas the third method is a sol-gel process that uses alcoxides. The products were characterized and compared. The observed differences are important for practical applications.

  6. Analyses of laser and furnace treated sol-gel coatings

    De Hosson, JT; De Haas, M; Sudarshan, TS; Jeandin, M; Khor, KA


    Here we explore a new method that allows thin films to be made with almost any composition and degree of porosity by means of a combination of sol-gel and laser technology. Results are presented for furnace and laser treated TEOTI-(tetraethylorthotitanate as sol precursor) coated silicon samples. Fr


    In this study, the effectiveness of TiO2 nanoparticles in arsenic adsorption was examined. TiO2 particles (LS) were synthesized via sol-gel techniques and characterized for their crystallinity, surface area and pore volume. Batch adsorption studies were perf...

  8. Process of forming a sol-gel/metal hydride composite

    Congdon, James W.


    An external gelation process is described which produces granules of metal hydride particles contained within a sol-gel matrix. The resulting granules are dimensionally stable and are useful for applications such as hydrogen separation and hydrogen purification. An additional coating technique for strengthening the granules is also provided.

  9. Photolithography fabrication of sol-gel ridge waveguides

    Sara, Rahmani; Touam, Tahar; Blanchetiere, Chantal; Saddiki, Z.; Saravanamuttu, Kalaichelvi; Du, Xin M.; Chrostowski, Jacek; Andrews, Mark P.; Najafi, S. Iraj


    We report on fabrication of ridge waveguides in UV-light sensitive glass sol-gel thin films, deposited on silicon substrate, using a simple photolithography process. The single-layer films are prepared at low temperature and deep UV-light (DUV) is employed to make the waveguides. The effect of fabrication parameters on waveguide shape is investigated.

  10. Neutron detector based on lithiated sol-gel glass

    Wallace, S; Miller, L F; Dai, S


    A neutron detector technology is demonstrated based on sup 6 Li/ sup 1 sup 0 B doped sol-gel glass. The detector is a sol-gel glass film coated silicon surface barrier detector (SBD). The ionized charged particles from (n, alpha) reactions in the sol-gel film enter the SBD and are counted. Data showing that gamma-ray pulse amplitudes interfere with identifying charged particles that exit the film layer with energies below the gamma-ray energy is presented. Experiments were performed showing the effect of sup 1 sup 3 sup 7 Cs and sup 6 sup 0 Co gamma rays on the SBD detector. The reaction product energies of the triton and alpha particles from sup 6 Li are significantly greater than the energies of the Compton electrons from high-energy gamma rays, allowing the measurement of neutrons in a high gamma background. The sol-gel radiation detection technology may be applicable to the characterization of transuranic waste, spent nuclear fuel and to the monitoring of stored plutonium.

  11. Application de la technologie des materiaux sol-gel et polymere a l'optique integree

    Saddiki, Zakaria


    With the advancement of optical telecommunication systems, "integrated optics" and "optical interconnect" technology are becoming more and more important. The major components of these two technologies are photonic integrated circuits (PICs), optoelectronic integrated circuits (OEICs), and optoelectronic multichip modules ( OE-MCMs). Optical signals are transmitted through optical waveguides that interconnect such components. The principle of optical transmission in waveguides is the same as that in optical fibres. To implement these technologies, both passive and active optical devices are needed. A wide variety of optical materials has been studied, e.g., glasses, lithium niobate, III-V semiconductors, sol-gel and polymers. In particular, passive optical components have been fabricated using glass optical waveguides by ion-exchange, or by flame hydrolysis deposition and reactive ion etching (FHD and RIE ). When using FHD and RIE, a very high temperatures (up to 1300°C) are needed to consolidate silica. This work reports on the fabrication and characterization of a new photo-patternable hybrid organic-inorganic glass sol-gel and polymer materials for the realisation of integrated optic and opto-electronic devices. They exhibit low losses in the NIR range, especially at the most important wavelengths windows for optical communications (1320 nm and 1550 nm). The sol-gel and polymer process is based on photo polymerization and thermo polymerization effects to create the wave-guide. The single-layer film is at low temperature and deep UV-light is employed to make the wave-guide by means of the well-known photolithography process. Like any photo-imaging process, the UV energy should exceed the threshold energy of chemical bonds in the photoactive component of hybrid glass material to form the expected integrated optic pattern with excellent line width control and vertical sidewalls. To achieve optical wave-guide, a refractive index difference Delta n occurred between

  12. Tribological Performance of Sol-Gel Derived Superhydrophobic Film%溶胶-凝胶法制备超疏水性薄膜摩擦学性能的研究

    万勇; 张泉; 李杨


    A simple two-step process was developed in this study to render aluminum with lower friction and superhydrophobicity. Alumina film was firstly fabricated on aluminum by Sol-Gel technology. Fatty acid was then deposited on alumina film to endow superhydrophobicity. The surface morphology of alumina film after treatment using boiling water or hydrazine solution was evaluated. The effect of molecular structure of fatty acid on the wettability of the composite film was investigated. Friction-reducing behavior of the superhydrophobic films on aluminum was determined in a ball-on-plate configuration. It was found that the stearic acid film on alumina film treated by hydrazine solution showed superhydrophobicity and low friction, leading to significantly extending lifespan of the alumina film.%采用溶胶–凝胶技术在铝表面涂覆氧化铝薄膜,再利用长链脂肪酸对氧化铝薄膜进行疏水改性,在金属铝表面构筑了具有较强减摩性能的超疏水薄膜。研究了沸水及水合肼溶液处理对氧化铝薄膜表面微纳织构的影响;探讨了脂肪酸分子结构对薄膜静态和动态润湿性的影响,利用球盘式微纳米摩擦磨损试验机评价了薄膜的摩擦学性能。结果显示,水合肼溶液处理后的氧化铝薄膜经硬脂酸改性后不仅表现出超疏水性能,而且具有较强的减摩性能。

  13. The effect of dual complexing agents of lactic and citric acids on the formation of sol-gel derived Ag–PbTiO{sub 3} percolative thin film

    Su, Yanbo; Hu, Tao; Tang, Liwen; Weng, Wenjian; Han, Gaorong; Ma, Ning; Du, Piyi, E-mail:


    Controlling the formation of conductive particles to be nano-scale is important for achieving percolation effect in metal dispersed thin film composite to contribute extraordinary dielectric properties required for miniaturization of electronic devices. In this paper, lactic acid (LA) and citric acid (CA) were used as dual complexing agents to prepare a typical Ag nanoparticle dispersed PbTiO{sub 3} (PTO) composite thin film by using a sol-gel method. The phase structure of the thin film and the coordination effect between complexing agent and metallic ions were investigated. It revealed that LA coordinated with Ti{sup 4+} and Pb{sup 2+} and CA coordinated with Ag{sup +}. Lead was fixed inside the gel network by LA and restricted to evaporate during heat treatment thus the pyrochlore phase was prevented from forming in the thin film. Ag{sup +} was coordinated by CA and the diffusion and thus aggregation of silver during gelation and annealing process were weakened. Silver nanoparticles dispersed in the PTO matrix formed with dual complexing agents of LA and CA introduced during the preparation process. The composite thin film of perfect perovskite phase with silver nanoparticles embedded was obtained at the molar ratio of LA/lead = 0.5 and CA/lead = 0.5. The dielectric constant of the thin film with silver nanoparticles is 5 times higher than that without silver nanoparticles. - Highlights: • Ag nanoparticle–PbTiO{sub 3} percolative film with high dielectric property is prepared. • Evaporation of lead was prevented by coordinating Pb with lactic acid agent. • Dual complexing agents contribute block and pinning effects to form Ag nanoparticles.

  14. Reaction of Silane Alkoxide with Acid Anhydride as a Novel Synthetic Method for Organic-Inorganic Hybrid Materials

    Masahiro Fujiwara


    @@ 1Introduction Sol-gel method is a potent method to produce new inorganic and organic-inorganic hybrid materials. The key step of this methodology is the hydrolysis of a metal alkoxide or other metal substrates such as acetylacetonates to form hydroxyl metal species, followed by their condensation to metal-oxygen-metal (M - O - M)bonds. In this process, the utilization of water, generally in excess, is essential and alcoholic solvents such as ethanol are often required to homogenize the solution when organic compounds coexist. As the common sol-gel method using water allows for limited uses of organic substrates due to their low solubility and stability in aqueous solution, modified variations of sol-gel method are required. Recently, some processes were reported for preparing metal oxides from metal alkoxides without the utilization of water.

  15. Evaluation of sol-gel based magnetic 45S5 bioglass and bioglass-ceramics containing iron oxide.

    Shankhwar, Nisha; Srinivasan, A


    Multicomponent oxide powders with nominal compositions of (45-x)·SiO2·24.5CaO·24.5Na2O·6P2O5xFe2O3 (in wt.%) were prepared by a modified sol-gel procedure. X-ray diffraction (XRD) patterns and high resolution transmission electron microscope images of the sol-gel products show fully amorphous structure for Fe2O3 substitutions up to 2 wt.%. Sol-gel derived 43SiO2·24.5CaO·24.5Na2O·6P2O5·2Fe2O3 glass (or bioglass 45S5 with SiO2 substituted with 2 wt.% Fe2O3), exhibited magnetic behavior with a coercive field of 21 Oe, hysteresis loop area of 33.25 erg/g and saturation magnetization of 0.66 emu/g at an applied field of 15 kOe at room temperature. XRD pattern of this glass annealed at 850 °C for 1h revealed the formation of a glass-ceramic containing sodium calcium silicate and magnetite phases in nanocrystalline form. Temperature dependent magnetization and room temperature electron spin resonance data have been used to obtain information on the magnetic phase and distribution of iron ions in the sol-gel glass and glass-ceramic samples. Sol-gel derived glass and glass-ceramic exhibit in-vitro bioactivity by forming a hydroxyapatite surface layer under simulated physiological conditions and their bio-response is superior to their melt quenched bulk counterparts. This new form of magnetic bioglass and bioglass ceramics opens up new and more effective biomedical applications.

  16. Optical detection of parasitic protozoa in sol-gel matrices

    Livage, Jacques; Barreau, J. Y.; Da Costa, J. M.; Desportes, I.


    Whole cell parasitic protozoa have been entrapped within sol-gel porous silica matrices. Stationary phase promastigote cells of Leishmania donovani infantum are mixed with a silica sol before gelation occurs. They remain trapped within the growing oxide network and their cellular organization appears to be well preserved. Moreover protozoa retain their antigenic properties in the porous gel. They are still able to detect parasite specific antibodies in serum samples from infected patients via an enzyme linked immunosorbent assay (ELISA). Antigen- antibody associations occurring in the gel are optically detected via the reactions of a peroxidase conjugate with ortho-phenylenediamine leading to the formation of a yellow coloration. A clear-cut difference in optical density is measured between positive and negative sera. Such an entrapment of antigenic species into porous sol-gel matrices avoids the main problems due to non specific binding and could be advantageously used in diagnostic kits.

  17. Tough ceramic coatings: Carbon nanotube reinforced silica sol-gel

    Lopez, A.J., E-mail: [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain); Rico, A.; Rodriguez, J.; Rams, J. [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain)


    Silica coatings reinforced with carbon nanotubes were produced via sol-gel route using two mixing techniques of the sol-gel precursors, mechanical and ultrasonic mixing, and dip-coating as deposition process on magnesium alloy substrates. Effective incorporation and distribution of 0.1 wt.% of carbon nanotubes in the amorphous silica matrix of the coatings were achieved using both techniques. Fabrication procedure determines the morphological aspects of the coating. Only mechanical mixing process produced coatings dense and free of defects. Nanoindentation technique was used to examine the influence of the fabrication process in the mechanical features of the final coatings, i.e. indentation fracture toughness, Young's modulus and hardness. A maximum toughening effect of about 24% was achieved in silica coatings reinforced with carbon nanotubes produced by the mechanical mixing route. Scanning electron microscopy investigation revealed that the toughening of these reinforced coatings was mainly due to bridging effect of the reinforcement.

  18. Sol-Gel Synthesized Adsorbents for Metal Separation


    A series of organo-ceramic adsorbents have been synthesized by a sol-gel processing technique for metal ion extraction. These adsorbents generally have significantly high metal uptake capacities, good physical-chemical stabilities, and well-designed pore geometries compared to other pre-existing metalchelating ceramic-based adsorbents. This work describes the synthesis and evaluation of pyrazole and calix[4]arene crown adsorbents for selective separation of platinum, palladium, and gold and cesium ions,respectively, from solutions. These materials exhibit mesoporous properties with high surface areas and pore volumes. The sol-gel synthesis starting with precursor silanes and titania results in gel particles of desired pore characteristics and high capacity and stability. Characterization studies, such as adsorption isotherms, breakthrough curves for fixed bed operation, and material stability, show promising results for applications to metal sepation.

  19. Tunable Optical Properties of Metal Nanoparticle Sol-Gel Composites

    Smith, David D.; Snow, Lanee A.; Sibille, Laurent; Ignont, Erica


    We demonstrate that the linear and non-linear optical properties of sol-gels containing metal nanoparticles are highly tunable with porosity. Moreover, we extend the technique of immersion spectroscopy to inhomogeneous hosts, such as aerogels, and determine rigorous bounds for the average fractional composition of each component, i.e., the porosity of the aerogel, or equivalently, for these materials, the catalytic dispersion. Sol-gels containing noble metal nanoparticles were fabricated and a significant blue-shift in the surface plasmon resonance (SPR) was observed upon formation of an aerogel, as a result of the decrease in the dielectric constant of the matrix upon supercritical extraction of the solvent. However, as a result of chemical interface damping and aggregation this blue-shift does not strictly obey standard effective medium theories. Mitigation of these complications is achieved by avoiding the use of alcohol and by annealing the samples in a reducing atmosphere.

  20. Nanostructured energetic materials using sol-gel methodologies

    Tillotson, T M; Simpson, R L; Hrubesh, L W; Gash, A E; Thomas, I M; Poco, J F


    The fundamental differences between energetic composites and energetic materials made from a monomolecular approach are the energy density attainable and the energy release rates. For the past 4 years, we have been exploiting sol-gel chemistry as a route to process energetic materials on a microstructural scale. At the last ISA conference, we described four specific sol-gel approaches to fabricating energetic materials and presented our early work and results on two methods - solution crystallization and powder addition. Here, we detail our work on a third approach, energetic nanocomposites. Synthesis of thermitic types of energetic nanocomposites are presented using transition and main group metal-oxide skeletons. Results on characterization of structure and performance will also be given.

  1. Nanostructured Energetci Matreials with sol-gel Chemistry

    Gash, A; Satcher, J; Simpson, R; Clapsaddle, B


    The utilization of nanomaterials in the synthesis and processing of energetic materials (i.e., pyrotechnics, explosives, and propellants) is a relatively new area of science and technology. Previous energetic nanomaterials have displayed new and potentially beneficial properties, relative to their conventional analogs. Unfortunately some of the energetic nanomaterials are difficult and or expensive to produce. At LLNL we are studying the application of sol-gel chemical methodology to the synthesis of energetic nanomaterials components and their formulation into energetic nanocomposites. Here sol-gel synthesis and formulation techniques are used to prepare Fe{sub 2}O{sub 3}/Al pyrotechnic nanocomposites. The preliminary characterization of their thermal properties and the degree of mixing between fuel and oxidizer phases is contrasted with that of a conventional pyrotechnic mixture.

  2. Sol-gel multicapillary columns for gas-solid chromatography.

    Sidelnikov, Vladimir N; Patrushev, Yuri V; Belov, Yuri P


    In this work, we report the method for the preparation of multicapillary columns (MCCs) for gas-solid chromatography. The porous layer adsorbent is formed on capillary walls by the hydrolysis of aluminum alkoxide in the presence of polypropylene glycol (PPG) and HCl. Porosity and selectivity of the adsorbent depend on reaction conditions and the concentration of PPG. Sol-gel MCCs are well suited for high-speed chromatographic analysis of light hydrocarbons by gas-solid chromatography. Nine-component mixtures of C1-C4 hydrocarbons are separated within 8-12 s. The efficiency of 25-30 cm long alumina sol-gel MCCs consisting of approximately 1400 capillaries of 40 microm diameter is up to 2500-3000 theoretical plates.

  3. Hybrid Organic/Inorganic Coatings Through Dual-Cure Processes: State of the Art and Perspectives

    Giulio Malucelli


    Full Text Available This paper reviews the current state of the art related to the synthesis and characterization of hybrid organic-inorganic (O/I coatings obtained through the exploitation of dual-cure processes, which involve a photo-induced polymerization followed by a thermal treatment: this latter allows the occurrence of sol-gel reactions of suitable alkoxy precursors already embedded in the UV-curable system. After a brief introduction on hybrid organic-inorganic coatings, the first part of the review is focused on the design and feasibility issues provided by the dual-cure method, emphasizing the possibility of tuning the structure of the final hybrid network on the basis of the composition of the starting liquid mixture. Then, some recent examples of hybrid organic-inorganic networks are thoroughly described, showing their potential advances and the application fields to which they can be addressed.

  4. Tribological investigations of sol-gel ceramic films

    张文光; 王成焘; 刘维民


    Tribological properties of the TiO2, doped TiO2, AI2O3 and SiO2 thin films prepared by different sol-gel processes are reported. The results indicate that doping deteriorates the wear resistance of TiO2; organic modifier can improve the tribological property of AI2O3 significantly; and the SiO2 film prepared from inorganic salt sodium silicate registers much better wear resistance than that from ethyl orthosilicate.

  5. Sol-Gel Thin Films for Plasmonic Gas Sensors

    Enrico Della Gaspera


    Full Text Available Plasmonic gas sensors are optical sensors that use localized surface plasmons or extended surface plasmons as transducing platform. Surface plasmons are very sensitive to dielectric variations of the environment or to electron exchange, and these effects have been exploited for the realization of sensitive gas sensors. In this paper, we review our research work of the last few years on the synthesis and the gas sensing properties of sol-gel based nanomaterials for plasmonic sensors.

  6. Tribological investigations of sol-gel ceramic films

    张文光; 刘维民; 王成焘


    Tribological properties of the TiO2, doped TiO2, Al2O3 and SiO2 thin films prepared by different sol-gel processes are reported. The results indicate that doping deteriorates the wear resistance of TiO2; organic modifier can improve the tribological property of Al2O3 significantly; and the SiO2 film prepared from inorganic salt sodium silicate registers much better wear resistance than that from ethyl orthosilicate.



    The objective of the submitted work was to prepare and to characterize two types of silicate coatings prepared by the sol-gel method using the dip-coating technique on a titanium substrate. Efforts have been made to use mechanical properties of bio-inert titanium and bioactive properties of a silicate layer enriched with an admixture of compounds identified below. The first group consisted of silicate coatings containing silver, brushite and monetite. The other group of silicate coatings cont...

  8. Non-hydrolytic sol-gel routes to heterogeneous catalysts

    Debecker, Damien P.; Mutin, P. Hubert


    Oxides and mixed oxides have a tremendous importance in the field of heterogeneous catalysis, serving either as catalysts or as supports for active species. The performance of a catalyst depends directly on its composition, texture, structure and surface properties, which have to be precisely controlled and adapted to each application. In this context, the sol-gel process is a unique tool for the preparation and understanding of catalytic materials, owing to its exceptional versatility. In th...

  9. Composite sol-gel coatings on steel for tribological applications

    Hermange, Kurt


    This thesis focuses on the elaboration and the characterization of composite sol-gel coatings “CSG” on austenitic stainless steelAISI 304. The aim of the thesis is to develop the process and to study the mechanical properties and tribological behavior of thecoatings. The first experimental part presents the optimization of the synthesis conditions of a stable alumina sol and the influence of the thermal treatment of the gel on the physic-chemical and thermostructural properties. The studied p...

  10. Sol-Gel Synthesis of Non-Silica Monolithic Materials

    Bartłomiej Gaweł


    Full Text Available Monolithic materials have become very popular because of various applications, especially within chromatography and catalysis. Large surface areas and multimodal porosities are great advantages for these applications. New sol-gel preparation methods utilizing phase separation or nanocasting have opened the possibility for preparing materials of other oxides than silica. In this review, we present different synthesis methods for inorganic, non-silica monolithic materials. Some examples of application of the materials are also included.

  11. Alumina Coating on Carbon Fibers by Sol-Gel Method


    Alumina precursor film was coated on carbon fibers by a sol-gel method using aluminum alkoxide solution. The optimum coating condition for the concentration of alumina alkoxide and silane coupling agent was determined to uniformly coat alumina precursor on carbon fibers. Alumina precursor converted to alumina ceramics by heating at 750℃. SEM and EPMA showed that alumina ceramics was uniformly coated on carbon fibers. The thickness of alumina layer increased with increasing coating times. The ...

  12. Molecularly imprinted polymer grafted on polysaccharide microsphere surface by the sol-gel process for protein recognition.

    Li, Feng; Li, Jing; Zhang, Shusheng


    An interfacial organic-inorganic hybridization concept was applied to the preparation of a new spherical imprinted material for protein recognition. The functional biopolymer chitosan (CS), shaped as microsphere and high-density cross-linked, constituted of the polysaccharide core for surface imprinting. After the model template protein, bovine serum albumin, was covalently immobilized by forming imine bonds with the functional amine groups of CS, two kinds of organic siloxane (3-aminopropyltrimethoxysiloxane: APTMS, and tetraethoxysiloxane: TEOS) assembled and polymerized on the polysaccharide-protein surface via sol-gel process in aqueous solution at room temperature. After template removal, the protein-imprinted sol-gel surface exhibited a prevalent preference for the template protein in adsorption experiments, as compared with four contrastive proteins. Bioinformatics methods were also employed to investigate the imprinting process and the recognition effect. The influence of siloxane type, pH, siloxane/water ratio on template removal and recognition selectivity was assessed. Under optimized imprinting conditions, a large quantity of well-distributed pores was observed on the immobilized-template imprinted surface. The surface-imprinted adsorbent offered a fast kinetics for template re-adsorption and could be reused. Compared with the imprinted material prepared with free-template, material prepared with immobilized-template possessed higher adsorption capacity towards template protein. Easy preparation of the described imprinted material, high affinity and good reusability make this approach attractive and broadly applicable in biotechnology for down-stream processing and biosensor.

  13. Fully compatible magneto-optical sol-gel material with glass waveguides technologies: application to mode converters

    Royer, François; Jamon, Damien; Broquin, Jean-Emmanuel; Amata, Hadi; Kekesi, Renata; Neveu, Sophie; Blanc-Mignon, Marie-Françoise; Ghibaudo, Elise


    To overcome the difficult problem of the integration of magneto-optical materials with classical technologies, our group has developped a composite magneto-optical material made of a hybrid organic-inorganic silica type matrix doped by magnetic nanoparticles. Thin films of this material are obtained through a soft chemistry sol-gel process which gives a full compatibility with an integration on glass substarte. Due to an interesting magneto optical activity (Faraday rotation of 310°/cm) several magneto-optical functionnalities have been realized. A thin film of such composite material coated on a pyrex™ substrate acts as non-reciprocal TE/TM mode converter. An hybrid stucture made of a composite film coated on an ion-exchanged glass waveguide has been realized with a good propagation of light through a hybrid mode. Finally, the sol gel process has been adapted in order to obtain 3D inverse opals which should behave as magnetophotonic crystals. Transmittance curves reveal the photonic band gap of such opals doped with magnetic nanoparticles.

  14. Preparation and Characterization of Organic/Inorganic Hybrid Nanofibers

    WU Ning; WEI Qu-fu; LI Qi; XU Wen-zheng


    A new class of nanocomposites based on organic and inorganic species integrated at a nanoscale has obtained more attention these years. Organic-inorganic hybrids have both the advantages of organic materials, such as light weight, flexibility and good moldability, and inorganic materials, such as high strength, heat stability and chemical resistance. In this work, PVAc/TiO2 organicinorganic hybrid was prepared by sol-gel process. Electrospinning technique was used to fabricate PVAc/TiO2hybrid nanofibers. The structures and properties of the hybrid nanofibers were characterized by Scanning Electron Microscopy (SEM), Atomic Force Microscope (AFM),Differential Scanning Calorimeter (DSC) and Fouriertransform infrared (FTIR) spectra. SEM and AFM were employed to study the topography of the hybrid nanofibers.The chemical structure of the hybrid nanofibers were examined by FTIR. The DSC scansrevealed the second order transition temperature of the hybrid materials were higher than PVAc.

  15. The Influence of Microgravity on Silica Sol-Gel Formation

    Sibille, L.; Smith, D. D.; Cronise, R.; Hunt, A. J.; Wolfe, D. B.; Snow, L. A.; Oldenberg, S.; Halas, N.; Rose, M. Franklin (Technical Monitor)


    We discuss space-flight experiments involving the growth of silica particles and gels. The effect of microgravity on the growth of silica particles via the sol-gel route is profound. In four different recipes spanning a large range of the parameter space that typically produces silica nanoparticles in unit-gravity, low-density gel structures were instead formed in microgravity. The particles that did form were generally smaller and more polydisperse than those grown on the ground. These observations suggest that microgravity reduces the particle growth rate, allowing unincorporated species to form aggregates and ultimately gel. Hence microgravity favors the formation of more rarefied structures, providing a bias towards diffusion-limited cluster-cluster aggregation. These results further suggest that in unit gravity, fluid flows and sedimentation can significantly perturb sol-gel substructures prior to gelation and these deleterious perturbations may be "frozen" into the resulting microstructure. Hence, sol-gel pores may be expected to be smaller, more uniform, and less rough when formed in microgravity.

  16. Magnetization of microorganism cells by sol-gel method

    CHEN Bo; ZHAN TianZhuo; LIAN ZhiYang; ZHANG DeYuan


    Microorganism cells could be used as templates during fabrication of magnetic or conductive microstructures in different standard shapes.In this paper,feasibility of magnetizing microorganism cells by sol-gel method,which is to coat cells of Spirulina (a type of natural micro-helical microorganism) with the ferrite (a kind of magnetic material),was discussed and investigated.Then the cell form,compo-nents and the phase structure were observed and analyzed using various tools including optical microscopy,scanning electron microscopy (SEM),energy dis-persive X-ray detector (EDX),transmission electron microscopy (TEM),and X-ray diffraction analysis (XRD).Results showed that spirulina cells could be coated with ferrite after the sol-gel process,with the shape of natural helixes well kept,that the components of different sampling points on the surface layer were consistent and the thickness of layer was uniform,and that the type of the surface ferrite layer formed was cubic Fe304.It was also observed that there were nano-parUcles yielded in the cells and certain deposit on the walls between cells.The kinetics of the cell magnetization technology by sol-gel was also discussed.

  17. Magnetization of microorganism cells by sol-gel method


    Microorganism cells could be used as templates during fabrication of magnetic or conductive microstructures in different standard shapes. In this paper, feasibility of magnetizing microorganism cells by sol-gel method, which is to coat cells of Spirulina (a type of natural micro-helical microorganism) with the ferrite (a kind of magnetic material), was discussed and investigated. Then the cell form, components and the phase structure were observed and analyzed using various tools including optical microscopy, scanning electron microscopy (SEM), energy dispersive X-ray detector (EDX), transmission electron microscopy (TEM), and X-ray diffraction analysis (XRD). Results showed that spirulina cells could be coated with ferrite after the sol-gel process, with the shape of natural helixes well kept, that the components of different sampling points on the surface layer were consistent and the thickness of layer was uniform, and that the type of the surface ferrite layer formed was cubic Fe3O4. It was also observed that there were nano-particles yielded in the cells and certain deposit on the walls between cells. The kinetics of the cell magnetization technology by sol-gel was also discussed.

  18. High Refractive Organic–Inorganic Hybrid Films Prepared by Low Water Sol-Gel and UV-Irradiation Processes

    Hsiao-Yuan Ma


    Full Text Available Organic-inorganic hybrid sols (Ti–O–Si precursor were first synthesized by the sol-gel method at low addition of water, and were then employed to prepare a highly refractive hybrid optical film. This film was obtained by blending the Ti–O–Si precursor with 2-phenylphenoxyethyl acrylate (OPPEA to perform photo-polymerization by ultraviolet (UV irradiation. Results show that the film transparency of poly(Ti–O–Si precursor-co-OPPEA film is higher than that of a pure poly(Ti–O–Si precursor film, and that this poly(Ti–O–Si precursor-co-OPPEA hybrid film exhibits a high transparency of ~93.7% coupled with a high refractive index (n of 1.83 corresponding to a thickness of 2.59 μm.

  19. Evolution of microstructure in mixed niobia-hybrid silica thin films from sol-gel precursors.

    Besselink, Rogier; Stawski, Tomasz M; Castricum, Hessel L; ten Elshof, Johan E


    The evolution of structure in sol-gel derived mixed bridged silsesquioxane-niobium alkoxide sols and drying thin films was monitored in situ by small-angle X-ray scattering. Since sol-gel condensation of metal alkoxides proceeds much faster than that of silicon alkoxides, the incorporation of d-block metal dopants into silica typically leads to formation of densely packed nano-sized metal oxide clusters that we refer as metal oxide building blocks in a silica-based matrix. SAXS was used to study the process of niobia building block formation while drying the sol as a thin film at 40-80°C. The SAXS curves of mixed niobia-hybrid silica sols were dominated by the electron density contrast between sol particles and surrounding solvent. As the solvent evaporated and the sol particles approached each other, a correlation peak emerged. Since TEM microscopy revealed the absence of mesopores, the correlation peak was caused by a heterogeneous system of electron-rich regions and electron poor regions. The regions were assigned to small clusters that are rich in niobium and which are dispersed in a matrix that mainly consisted of hybrid silica. The correlation peak was associated with the typical distances between the electron dense clusters and corresponded with distances in real space of 1-3 nm. A relationship between the prehydrolysis time of the silica precursor and the size of the niobia building blocks was observed. When 1,2-bis(triethoxysilyl)ethane was first hydrolyzed for 30 min before adding niobium penta-ethoxide, the niobia building blocks reached a radius of 0.4 nm. Simultaneous hydrolysis of the two precursors resulted in somewhat larger average building block radii of 0.5-0.6 nm. This study shows that acid-catalyzed sol-gel polymerization of mixed hybrid silica niobium alkoxides can be rationalized and optimized by monitoring the structural evolution using time-resolved SAXS.

  20. Biocompatibility improvement of titanium implants by coating with hybrid materials synthesized by sol-gel technique.

    Catauro, M; Bollino, F; Papale, F


    Organic-inorganic hybrid materials based on zirconia and polyethylene glycol (PEG) have been synthesized via sol-gel method in the present study. Those materials, still in the sol phase, have been used to coat a titanium grade 4 (Ti-4) substrate to improve its biological properties. Dip-coating technique has been used to obtain thin films. PEG, a biocompatible polymer, used as the organic phase, has been incorporated with different percentages in an inorganic zirconium-based matrix. Those hybrids have been characterized by Fourier transform infrared spectroscopy (FTIR) to detect interactions between the two phases. The films have been examined using SEM to detect morphological changes with PEG percentages. The potential applications of the hybrid coatings in biomedical field have been evaluated by bioactivity and cytotoxicity tests. The coated titanium was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated, as that feature can be used as an index of bone-bonding capability. SEM equipped with energy dispersive spectrometer (EDS) was used to examine hydroxyapatite formation. NIH 3T3 mouse embryonic fibroblast cells were seeded on specimens to evaluate cells-materials interactions and cell vitality was inspected using WST-8 Assay.

  1. Synthesis of phthalocyanine doped sol-gel materials

    Dunn, Bruce


    The synthesis of sol-gel silica materials doped with three different types of metallophthalocyanines has been studied. Homogeneous materials of good optical quality were prepared and the first optical limiting measurements of dyes in sol-gel hosts were carried out. The properties of these solid state limiters are similar to limiters based on phthalocyanine (Pc) in solution. Sol-gel silica materials containing copper, tin and germanium phthalocyanines were investigated. The initial step in all cases was to prepare silica sols by the sonogel method using tetramethoxy silane (TMOS), HCl and distilled water. Thereafter, the synthesis depended upon the specific Pc and its solubility characteristics. Copper phthalocyanine tetrasulfonic acid tetra sodium salt (CuPc4S) is soluble in water and various doping levels (1 x 10 (exp -4) M to 1 x 10 (exp -5) M) were added to the sol. The group IV Pc's, SnPc(OSi(n-hexyl)3)2 and GePc(OSi(n-hexyl)3)2, are insoluble in water and the process was changed accordingly. In these cases, the compounds were dissolved in THF and then added to the sol. The Pc concentration in the sol was 2 x 10(exp -5)M. The samples were then aged and dried in the standard method of making xerogel monoliths. Comparative nanosecond optical limiting experiments were performed on silica xerogels that were doped with the different metallophthalocyanines. The ratio of the net excited state absorption cross section (sigma(sub e)) to the ground state cross section (sigma(sub g)) is an important figure of merit that is used to characterize these materials. By this standard the SnPc sample exhibits the best limiting for the Pc doped sol-gel materials. Its cross section ratio of 19 compares favorably with the value of 22 that was measured in toluene. The GePc materials appear to not be as useful as those containing SnPc. The GePc doped solids exhibit a higher onset energy (2.5 mj and lower cross section ratio, 7. The CuPc4S sol-gel material has a still lower cross

  2. Phenyl Functionalized Sol-gel Silica Sorbent for Capillary Microextraction and Chromia-Based Sol-gel Ucon Stationary Phase for Capillary Gas Chromatography

    McLean, Michael M.

    The first chapter of this thesis presents an introduction to sol-gel methodology whose usefulness as a synthetic route will be demonstrated with two applications in chromatography. The first application involves the fabrication of a capillary micro-extraction (CME) device by coating a phenyl functionalized extracting phase on the inner surface of a fused silica capillary for analyte pre-concentration. The device was coupled on-line to a RP-HPLC system and practicality was demonstrated using allergens as target analytes. The allergens chosen as model analytes are typically found in fragrance products and food. Most of the 26 fragrance allergens that are monitored by various government authorities have a phenyl organic moiety (a strong chromophore), thus making them appropriate probes for exploring the extraction efficiency of the coating using a UV detector. The CME device showed ppt level limit of detection which makes it suitable for trace analyses of allergens and similar compounds in a variety of matrices. The second application explores the feasibility of using sol-gel derived chromia-based stationary phase in gas chromatographic columns. The organic moiety of the stationary phase was derived from Ucon 75-H-90,000 while the inorganic backbone was prepared using chromium(III) dichloride hydroxide - methacrylic acid - aqua complex, 40% in isopropanol/acetone . Usefulness of prepared chromia-based GC stationary phase was examined for petrochemical application. Promising results were obtained using aliphatic-aromatics, polyaromatic hydrocarbons, BTEX test mixture, cycloalkanes, branched alkanes and akylbenzenes. The column was able to perform without degradation despite being rinsed multiples times sequentially with the following solvents: dichloromethane, methanol, water and finally methanol again. Maximum theoretical plate number calculated is around 2,400 plates/m. The plate number clearly needs improvement but is a promising result for the newly explored

  3. Recubrimientos de hidroxiapatita preparados mediante un proceso sol-gel

    Peón, E.


    Full Text Available Hydroxyapatite coatings (HAp have been obtained starting from precursors of sol-gel type. The coatings previously oxidized were deposited on metal surfaces of a based on iron alloy so-called MA956. The alloys were at high temperatures, in order to improve the adhesion with the hydroxyapatite coatings. The sol-gel coating was obtained applying an aqueous route, using triethyl phosphite and aqueous calcium nitrate, as precursors of phosphorous and calcium, respectively. Different sintering thermal treatments were applied on the resulting gels in order to obtain a homogeneous, adherent and crystalline hydroxyapatite coating. The characterization techniques used for this study were optical microscopy, SEM/EDX, XDR and FTIR. Moreover, the adhesion between the hydroxylapatite coating and the substrate was assessed according to the ASTM D 3359-02 standard test method. The results of this study showed that the best thermal treatment is obtained for a sintering temperature of 550 °C during a time of 72 h.

    Se han preparado nuevos recubrimientos de hidroxiapatita (HAp obtenidos a partir de precursores de tipo sol-gel, depositados sobre sustratos metálicos de una aleación de base hierro denominada MA956, previamente oxidados a elevadas temperaturas, para mejorar la adherencia con los recubrimientos de hidroxiapatita. El recubrimiento sol-gel se obtuvo aplicando una ruta acuosa, utilizando como precursores del fósforo y del calcio trietilfosfito y nitrato cálcico tetrahidratado, respectivamente. Sobre los geles resultantes se aplicaron distintos tratamientos térmicos de sinterización, hasta la obtención de recubrimientos de hidroxiapatita homogéneos, adherentes y cristalinos. Las técnicas de caracterización utilizadas para realizar este estudio han sido microscopía óptica, MBE/EDX, DRX y FTIR. Así mismo, se ha determinado la adherencia entre el substrato y el recubrimiento de hidroxiapatita según la norma ASTM D 3359-02. Los resultados

  4. Synthesis of lithium doped zinc oxide by sol gel



    Li-doped ZnO thin films were prepared by sol-gel method and deposed on glass substrate using spin coating technique. The effects of Li on structural and optical properties were investigated. The X-ray diffraction (XRD) analysis reveals that Li incorporation leads to the great improvement of the crystalline quality of ZnO thin films. Scanning electron microscopy (SEM) images showed that nanowires are aligned nearly perpendicular to the substrate plane and are affected significantly by Li incorporation. The optical transmission of the films was higher than 80% in the visible region. It is found that the optical gap and the refractive index remain practically constant.

  5. The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

    Ales Styskalik


    Full Text Available This review is devoted to non-hydrolytic sol-gel chemistry. During the last 25 years, non-hydrolytic sol-gel (NHSG techniques were found to be attractive and versatile methods for the preparation of oxide materials. Compared to conventional hydrolytic approaches, the NHSG route allows reaction control at the atomic scale resulting in homogeneous and well defined products. Due to these features and the ability to design specific materials, the products of NHSG reactions have been used in many fields of application. The aim of this review is to present an overview of NHSG research in recent years with an emphasis on the syntheses of mixed oxides, silicates and phosphates. The first part of the review highlights well known condensation reactions with some deeper insights into their mechanism and also presents novel condensation reactions established in NHSG chemistry in recent years. In the second section we discuss porosity control and novel compositions of selected materials. In the last part, the applications of NHSG derived materials as heterogeneous catalysts and supports, luminescent materials and electrode materials in Li-ion batteries are described.

  6. Hybrid Sol-Gel Coatings: Smart and Green Materials for Corrosion Mitigation

    Rita B. Figueira


    Full Text Available Corrosion degradation of materials and metallic structures is one of the major issues that give rise to depreciation of assets, causing great financial outlays in their recovery and or prevention. Therefore, the development of active corrosion protection systems for metallic substrates is an issue of prime importance. The promising properties and wide application range of hybrid sol-gel-derived polymers have attracted significant attention over recent decades. The combination of organic polymers and inorganic materials in a single phase provides exceptional possibilities to tailor electrical, optical, anticorrosive, and mechanical properties for diverse applications. This unlimited design concept has led to the development of hybrid coatings for several applications, such as transparent plastics, glasses, and metals to prevent these substrates from permeation, mechanical abrasion, and corrosion, or even for decorative functions. Nevertheless, the development of new hybrid products requires a basic understanding of the fundamental chemistry, as well as of the parameters that influence the processing techniques, which will briefly be discussed. Additionally, this review will also summarize and discuss the most promising sol-gel coatings for corrosion protection of steel, aluminium, and their alloys conducted at an academic level.

  7. Mullite glass-ceramic glazes synthesized through a sol-gel and ceramic mixed process

    Nunez, I.; Hohemberger, J.M.; Carda, J.B. [Universitat Jaume I, Castellon (Spain). Dept. Quimica Inorganica y Organica; Jovani, M.A.; Nebot, A. [Colorobbia Espana S.A. Villafames, Castellon (Spain)


    The main objective of the present work is the development of a glass-ceramic glaze with similar properties to the mullite crystalline phase. We have developed new glass-ceramic materials, which are formed through devitrification of mullite. The synthesis process combines the traditional ceramic method and the more innovative sol-gel methodologies. Amorphous precursors for the glass-ceramic glazes were obtained through precalcination of previously synthesized gels. These amorphous materials served as crystallization nuclei when introduced in the enamel composition. Gels were synthesized by the polymeric sol-gel method using AlCl{sub 3}, t-BuOH and TEOS as precursors. Composition of frit was optimized in such a way that a frit rich in aluminum and silicon would have the adequate physical and chemical characteristics for the desired application. Microstructure and structure of all the obtained materials were characterized. DTA-TG profiles and mechanical, chemical and optical properties were evaluated. On the other hand, the glass-ceramic glazes were compared first to glass-crystalline mullite glazes, which were obtained by addition of mullite crystals to the frit and then, to the glaze derived of just the frit. (orig.)

  8. Fabrication and Crystal Structure of Sol-Gel Deposited BST Thin Films with Compositional Gradient

    Czekaj D.


    Full Text Available In the present research technology of compositionally graded barium strontium titanate Ba1-xSrxTiO3 thin films deposited on stainless steel substrates by sol-gel spin coating followed with thermal annealing at T = 650°C is reported. Results of thermal behavior of the sol-gel derived powders with compositions used for fabrication of graded structure (i.e. with Sr mole fraction x = 0.5, 0.4 and 0.3 are described. X-ray diffraction studies of the phase composition and crystal structure of such complex thin film configuration are given. It was found that gel powders exhibited a large total weight loss of about Δm ≈ 44-47%. Three stages of weight loss took place at temperature ranges: below T ≈ 300°C, at ΔT ≈ 300-500°C and between T = 600°C and T = 800°C. Phase analysis has shown that the dominating phase is Ba0.67Sr0.33TiO3 compound while the second phase is Ba0.7Sr0.3TiO3 or Ba0.5Sr0.5TiO3 for “up-graded” and “down-graded” structure, respectively.

  9. Citrate sol-gel combustion preparation and photoluminescence properties of YAG:Ce phosphors

    ZHANG Le; LU Zhou; ZHU Jinzhen; YANG Hao; HAN Pengde; CHEN Yan; ZHANG Qitu


    Yellow-emitting YAG:Ce3+ nanocrystalline phosphors were prepared by citrate sol-gel combustion method using citric acid as the fuel and chelating agent.The influence of mole ratio of citric acid to metallic ions (MRCM),pH value of the solution,calcination temperature and Ce-doped concentration on the structures and properties of as-prepared powders were investigated in detail.Higher crystallinity and better luminescence performance powders were obtained at MRCM=2,pH=3 and the calcination temperature of 1200 ℃.The phosphors exhibited the characteristic broadband visible luminescence of YAG:Ce.The optimum concentration of Ce3+ was 1.0 mol.%,and the concentration quenching was derived from the reciprocity between electric dipole and electric quadrupole (d-q).Especially,the pH value of the solution was a key factor to obtain a stable sol-gel system and then obtain pure and homogeneous rare earth ions doped YAG phosphors at a lower temperature.The Y3Al5O12:Ce0.03 phosphor with optimized synthesis-condition and composition had a similar luminescence intensity with the commercial phosphor YAG:Ce.

  10. Sol-gel synthesis and characterization of undoped and Al-doped ZnO thin films for memristive application

    Dawit G. Ayana


    Full Text Available The Sol-gel route is a versatile method to fabricate multi-layer, dense and homogeneous ZnO thin films with a controlled thickness and defects for a memristive application. In this work, sol-gel derived multi-layer undoped and Al-doped ZnO thin films were prepared by a spin-coating technique on SiO2/Ti/Pt and silica glass substrates. The effect of both Al doping and curing conditions on the structural and morphological features of ZnO films was investigated by complementary techniques, including electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, micro-Raman spectroscopy, and X-ray diffraction analysis. Electrical measurements were performed on SiO2/Ti/Pt/ZnO/Pt(dishes and SiO2/Ti/Pt/ZnO(Al/Pt(dishes fabricated memristive cells and preliminary current-voltage curves were acquired.

  11. Sol-gel synthesis and characterization of undoped and Al-doped ZnO thin films for memristive application

    Ayana, Dawit G.; Prusakova, Valentina; Collini, Cristian; Nardi, Marco V.; Tatti, Roberta; Bortolotti, Mauro; Lorenzelli, Leandro; Chiappini, Andrea; Chiasera, Alessandro; Ferrari, Maurizio; Lunelli, Lorenzo; Dirè, Sandra


    The Sol-gel route is a versatile method to fabricate multi-layer, dense and homogeneous ZnO thin films with a controlled thickness and defects for a memristive application. In this work, sol-gel derived multi-layer undoped and Al-doped ZnO thin films were prepared by a spin-coating technique on SiO2/Ti/Pt and silica glass substrates. The effect of both Al doping and curing conditions on the structural and morphological features of ZnO films was investigated by complementary techniques, including electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, micro-Raman spectroscopy, and X-ray diffraction analysis. Electrical measurements were performed on SiO2/Ti/Pt/ZnO/Pt(dishes) and SiO2/Ti/Pt/ZnO(Al)/Pt(dishes) fabricated memristive cells and preliminary current-voltage curves were acquired.

  12. Magnetic nanosized rare earth iron garnets R3Fe5O12: Sol-gel fabrication, characterization and reinspection

    Opuchovic, Olga; Kareiva, Aivaras; Mazeika, Kestutis; Baltrunas, Dalis


    The magnetic nanosized rare earth iron garnets (R3Fe5O12, where R=Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) were prepared by an aqueous sol-gel method. Herein we present, that all these garnets can be obtained by this effective synthesis method simply by changing the temperature of the final annealing. It was also demonstrated, that a different annealing temperature leads to a different particle size distribution of the final product. The SEM analysis results revealed that the smallest particles were formed in the range of 75-130 nm. The phase purity and structure of the rare earth iron garnets were estimated using XRD analysis and Mössbauer spectroscopy. Magnetic properties were determined by magnetization measurements. The relation between the particle size, composition and magnetic properties of the sol-gel derived garnets were also discussed in this study.

  13. Ceria nanoparticles vis-à-vis cerium nitrate as corrosion inhibitors for silica-alumina hybrid sol-gel coating

    Lakshmi, R. V.; Aruna, S. T.; Sampath, S.


    The present work provides a comparative study on the corrosion protection efficiency of defect free sol-gel hybrid coating containing ceria nanoparticles and cerium nitrate ions as corrosion inhibitors. Less explored organically modified alumina-silica hybrid sol-gel coatings are synthesized from 3-glycidoxypropyltrimethoxysilane and aluminium-tri-sec-butoxide. The microemulsion derived nanoparticles and the hybrid coatings are characterized and compared with coatings containing cerium nitrate. Corrosion inhibiting capability is assessed using electrochemical impedance spectroscopy. Scanning Kelvin probe measurements are also conducted on the coatings for identifying the apparent corrosion prone regions. Detailed X-ray photoelectron spectroscopy (XPS) analysis is carried out to comprehend the bonding and corrosion protection rendered by the hybrid coatings.

  14. Construction of bienzyme biosensors based on combination of the one-step electrodeposition and covalent-coupled sol-gel process


    Horseradish peroxidase (HRP) and glucose oxidase (GOD) bienzyme biosensor was constructed by in-situ formation of the organic-inorganic biocomposite film based on the one-step electrodeposition and covalent-coupled sol-gel process. The electrodeposition was performed in the solution containing functional inorganic precursor possessing the epoxy groups,γ-glycidoxypropyltrimethoxysiloxane (GPTMS),a biopolymer chitosan (CS),HRP and GOD. The covalent-coupled sol-gel process was formed by self-hydrolysis and self-condensation of GPTMS,followed by in-situ covalent cross-linking of CS,HRP and GOD through covalent reaction between amino groups and epoxy groups. The developed bienzyme biosensor presented high stability in acidic solution owing to the covalent-coupled organic-inorganic hybridization. Compared with the non-hybrid HRP-GOD/CS/Au electrode,the bienzyme biosensor of HRP-GOD/GPTMS/CS/Au showed improved sensitivity and a wider linear range for the determination of glucose. The linear response of the developed HRP-GOD/GPTMS/ CS/Au biosensor for the determination of glucose ranged from 1 to 351 μmol/L with a detection limit of 0.3 μmol/L.

  15. High-coercivity CoFe2O4 thin films on Si substrates by sol-gel

    Tang, Xianwu; Jin, Linghua; Wei, Renhuai; Zhu, Xiaoguang; Yang, Jie; Dai, Jianming; Song, Wenhai; Zhu, Xuebin; Sun, Yuping


    CoFe2O4 (CFO) thin films with high coercivity HC are desirable in applications. The difficulty in achieving large-area CFO thin films with high coercivity by sol-gel has hindered the development of CFO thin films. Herein, polycrystalline CFO thin films with the room temperature out-of-plane and in-plane coercivity HC respectively reached ~5.9 and 3.6 kOe has been achieved on the silicon substrate by sol-gel. The room-temperature maximum magnetic energy product (BH)max and remanence ratio Mr/Ms are of 1.66 MG Oe and 0.58 respectively, which are also the largest values amongst the CFO thin films prepared by solution methods. At the same time, annealing temperature and thickness effects on the HC, (BH)max and Mr/Ms of the derived CFO thin films have been investigated. It is observed that grain size and residual tensile strain in the derived films play an important role in the variations of HC and Mr/Ms. These results will provide an effective route for fabricating larger-area high-coercivity CFO thin films with low-cost by sol-gel on silicon wafers.

  16. Processing and Characterization of Sol-Gel Cerium Oxide Microspheres

    McClure, Zachary D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Padilla Cintron, Cristina [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)


    Of interest to space exploration and power generation, Radioisotope Thermoelectric Generators (RTGs) can provide long-term power to remote electronic systems without the need for refueling or replacement. Plutonium-238 (Pu-238) remains one of the more promising materials for thermoelectric power generation due to its high power density, long half-life, and low gamma emissions. Traditional methods for processing Pu-238 include ball milling irregular precipitated powders before pressing and sintering into a dense pellet. The resulting submicron particulates of Pu-238 quickly accumulate and contaminate glove boxes. An alternative and dust-free method for Pu-238 processing is internal gelation via sol-gel techniques. Sol-gel methodology creates monodisperse and uniform microspheres that can be packed and pressed into a pellet. For this study cerium oxide microspheres were produced as a surrogate to Pu-238. The similar electronic orbitals between cerium and plutonium make cerium an ideal choice for non-radioactive work. Before the microspheres can be sintered and pressed they must be washed to remove the processing oil and any unreacted substituents. An investigation was performed on the washing step to find an appropriate wash solution that reduced waste and flammable risk. Cerium oxide microspheres were processed, washed, and characterized to determine the effectiveness of the new wash solution.

  17. Sol-gel applications for ceramic membrane preparation

    Erdem, I.


    Ceramic membranes possessing superior properties compared to polymeric membranes are more durable under severe working conditions and therefore their service life is longer. The ceramic membranes are composed of some layers. The support is the layer composed of coarser ceramic structure and responsible for mechanical durability under filtration pressure and it is prepared by consolidation of ceramic powders. The top layer is composed of a finer ceramic micro-structure mainly responsible for the separation of components present in the fluid to be filtered and sol-gel method is a versatile tool to prepare such a tailor-made ceramic filtration structure with finer pores. Depending on the type of filtration (e.g. micro-filtration, ultra-filtration, nano-filtration) aiming separation of components with different sizes, sols with different particulate sizes should be prepared and consolidated with varying precursors and preparation conditions. The coating of sol on the support layer and heat treatment application to have a stable ceramic micro-structure are also important steps determining the final properties of the top layer. Sol-gel method with various controllable parameters (e.g. precursor type, sol formation kinetics, heat treatment conditions) is a practical tool for the preparation of top layers of ceramic composite membranes with desired physicochemical properties.

  18. Formation of Ultrafine Apatite Fibers by Sol-gel/Electrospinning

    DING Ya-mei; YUAN Xiao-yan; ZHAO Jin; GUO Wan-chun; WANG Xiu-kui


    Ultrafine apatite fibers were prepared by electrospinning of sol-gel precursor/poly(vinyl pyrrolidone)(PVP) solutions followed by subsequent calcination. The as-electrospun and calcinated fibers were observed under a scanning electron microscope and an optical polarizing microscope. Results show that the morphology and the diameter of as-electrospun fibers strongly depend on the viscosity and the surface tension of sol-gel precursor/PVP solutions. After calcination, the smooth as-electrospun fibers shrink and the fiber diameter decreases because of the removal of the polymer. The chemical evolution upon the transformation of the precursor from a gel to the final apatite fibers was investigated by thermogravimetric-differential thermal analysis, X-ray diffraction, and Fourier transform infrared spectroscopy. It is thus suggested that the crystalline structure of the calcined fibers is largely influenced by the calcination temperature. After being calcined at 600 ℃, the apatite fibers with a diameter of about 280 nm containing β-tricalcium phosphate were obtained.

  19. Sol-gel based sensor for selective formaldehyde determination.

    Bunkoed, Opas; Davis, Frank; Kanatharana, Proespichaya; Thavarungkul, Panote; Higson, Séamus P J


    We report the development of transparent sol-gels with entrapped sensitive and selective reagents for the detection of formaldehyde. The sampling method is based on the adsorption of formaldehyde from the air and reaction with beta-diketones (for example acetylacetone) in a sol-gel matrix to produce a yellow product, lutidine, which was detected directly. The proposed method does not require preparation of samples prior to analysis and allows both screening by visual detection and quantitative measurement by simple spectrophotometry. The detection limit of 0.03 ppmv formaldehyde is reported which is lower than the maximum exposure concentrations recommended by both the World Health Organisation (WHO) and the Occupational Safety and Health Administration (OSHA). This sampling method was found to give good reproducibility, the relative standard deviation at 0.2 and 1 ppmv being 6.3% and 4.6%, respectively. Other carbonyl compounds i.e. acetaldehyde, benzaldehyde, acetone and butanone do not interfere with this analytical approach. Results are provided for the determination of formaldehyde in indoor air.

  20. Novel hybrid sol-gel materials for smart sensor windows

    Wencel, Dorota; Higgins, Clare; Guckian, Adrian; McDonagh, Colette; MacCraith, Brian D.


    Current sensor trends, such as multianalyte capability, miniaturisation and patternability are important drivers for materials requirements in optical chemical sensors. In particular, issues such as enhanced sensitivity and printablity are key in developing optimised sensor materials for smart windows for bioprocessing applications. This study focuses on combining novel sol-gel-based hybrid matrices with engineered luminescent complexes to produce stable luminescence-based optical sensors with enhanced sensitivity for a range of analytes including oxygen, pH and carbon dioxide. As well as optimising sensor performance, issues such as surface modification of the plastic substrate and compatibility with different deposition techniques were addressed. Hybrid sol-gel matrices were developed using a range of precursors including tetraethoxysilane (TEOS), methyltriethoxysilane (MTEOS), ethyltriethoxysilane (ETEOS), n-propyltriethoxysilane (PTEOS), phenyltriethoxysilane (PhTEOS), and n-octyltriethoxysilane (C8TEOS). Oxygen sensing, based on luminescence quenching of ruthenium phenanthroline complexes, has been realised with each of these hybrid materials. Furthermore, the possibility of immobilising pH-indicators for pH and carbon dioxide sensing has been investigated with some success. In the context of in-situ monitoring of bioprocesses, issues such as humidity interference as well as the chemical robustness of the multianalyte platform, were addressed.

  1. Sol - Gel synthesis and characterization of magnesium peroxide nanoparticles

    Jaison, J.; Ashok raja, C.; Balakumar, S.; Chan, Y. S.


    Magnesium peroxide is an excellent source of oxygen in agriculture applications, for instance it is used in waste management as a material for soil bioremediation to remove contaminants from polluted underground water, biological wastes treatment to break down hydrocarbon, etc. In the present study, sol-gel synthesis of magnesium peroxide (MgO2) nanoparticles is reported. Magnesium peroxide is odourless; fine peroxide which releases oxygen when reacts with water. During the sol-gel synthesis, the magnesium malonate intermediate is formed which was then calcinated to obtain MgO2 nanoparticles. The synthesized nanoparticles were characterized using Thermo gravimetric -Differential Thermal Analysis (TG- DTA), X-Ray Diffraction studies (XRD) and High Resolution Transmission Electron Microscope (HRTEM). Our study provides a clear insight that the formation of magnesium malonate during the synthesis was due to the reaction between magnesium acetate, oxalic acid and ethanol. In our study, we can conclude that the calcination temperature has a strong influence on particle size, morphology, monodispersity and the chemistry of the particles.

  2. Nanostructured Energetic Materials with Sol-Gel Methods

    Gash, A; Satcher, J; Simpson, R; Clapsaddle, B


    The utilization of sol-gel chemical methodology to prepare nanostructured energetic materials as well as the concepts of nanoenergetics is described. The preparation and characterization of two totally different compositions is detailed. In one example, nanostructured aerogel and xerogel composites of sol-gel iron (III) oxide and ultra fine grained aluminum (UFG Al) are prepared, characterized, and compared to a conventional micron-sized Fe{sub 2}O{sub 3}/Al thermite. The exquisite degree of mixing and intimate nanostructuring of this material is illustrated using transmission and scanning electron microscopies (TEM and SEM). The nanocomposite material has markedly different energy release (burn rate) and thermal properties compared to the conventional composite, results of which will be discussed. Small-scale safety characterization was performed aerogels and xerogels of the nanostructured thermite. The second nanostructured energetic material consists of a nanostructured hydrocarbon resin fuel network with fine ammonium perchlorate (NH{sub 4}ClO{sub 4}) oxidizer present.

  3. Aero-sol-gel Reactor for Nano-powder Synthesis

    Beaucage, G.; Hyeon-Lee, J.; Kohls, D.J. [University of Cincinnati, Department of Materials Science and Engineering (United States); Pratsinis, S.E. [University of Cincinnati, Department of Chemical Engineering (United States)


    This paper discusses a new approach to the synthesis of nano-structured oxides where sol-gel reactions are carried out in aerosol droplets. This aero-sol-gel (ASG) reactor allows for manipulation of the structure, chemical composition and surface area of silica powders through variation of process parameters. ASG powders differ in nanostructure from other continuous process powders such as pyrolytic and solution-route powders. ASG powders contain mesopores (>2-nm) and micropores (<2-nm), the mesopores being responsible for high surface areas measured by nitrogen adsorption using BET theory. Primary particles of close to molecular scale are believed to lead to exceedingly large specific surface areas on the order of 600-m{sup 2}/g. These primary particles aggregate into nanometer scale mass-fractal aggregates that cluster in micron scale agglomerates. Under controlled reaction conditions the powder structure is reproducible as measured by small-angle X-ray scattering, SAXS, analysis. The ASG reactor displays transport effects similar to those previously seen in laminar flame reactors as evidenced by the effect of reactor geometry and reactant concentration on product structure.

  4. Titanium (IV) sol-gel chemistry in varied gravity environments

    Hales, Matthew; Martens, Wayde; Steinberg, Theodore

    Sol-gel synthesis in reduced gravity is a relatively new topic in the literature and further inves-tigation is essential to realise its potential and application to other sol-gel systems. The sol-gel technique has been successfully applied to the synthesis of silica systems of varying porosity for many diverse applications [1-5]. It is proposed that current methods for the synthesis of silica sol-gels in reduced gravity may be applied to titanium sol-gel processing in order to enhance desirable physical and chemical characteristics of the final materials. The physical and chemical formation mechanisms for titanium alkoxide based sol-gels, to date, is not fully understood. However, various authors [6-9] have described potential methods to control the hydrolysis and condensation reactions of titanium alkoxides through the use of chemical inhibitors. A preliminary study of the reaction kinetics of titanium alkoxide sol-gel reaction in normal gravity was undertaken in order to determine reactant mixtures suitable for further testing under varied gravity conditions of limited duration. Through the use of 1H Nuclear Magnetic Resonance spectroscopy (NMR) for structural analysis of precursor materials, Ultra-Violet-Visible spectroscopy (UV-VIS) and viscosity measurements, it was demonstrated that not only could the rate of the chemical reaction could be controlled, but directed linear chain growth within the resulting gel structure was achievable through the use of increased inhibitor concentrations. Two unique test systems have been fabricated to study the effects of varied gravity (reduced, normal, high) on the formation of titanium sol-gels. Whilst the first system is to be used in conjunction with the recently commissioned drop tower facility at Queensland University of Technology in Brisbane, Australia to produce reduced gravity conditions. The second system is a centrifuge capable of providing high gravity environments of up to 70 G's for extended periods of time

  5. Sol-gel based oxidation catalyst and coating system using same

    Watkins, Anthony N. (Inventor); Leighty, Bradley D. (Inventor); Oglesby, Donald M. (Inventor); Patry, JoAnne L. (Inventor); Schryer, Jacqueline L. (Inventor)


    An oxidation catalyst system is formed by particles of an oxidation catalyst dispersed in a porous sol-gel binder. The oxidation catalyst system can be applied by brush or spray painting while the sol-gel binder is in its sol state.

  6. Development of sol-gel formulations for slow release of phermones

    A new type of dispenser for slow-release of semiochemicals and sex pheromones was developed based on sol-gel polymers that can be useful in monitoring, mass trapping, and mating disruption in integrated pest management (IPM). Sol-gel matrices exhibit glass characteristics and allow control of the de...

  7. Bactericidal micron-thin sol-gel films prevent pin tract and periprosthetic infection.

    Qu, Haibo; Knabe, Christine; Burke, Megan; Radin, Shula; Garino, Jonathan; Schaer, Thomas; Ducheyne, Paul


    Orthopedic injuries constitute the majority of wounds sustained by U.S. soldiers in recent conflicts. The risk of infection is considerable with fracture fixation devices. In this pilot study, we examined the use of unique bactericidal micron-thin sol-gel films on fracture fixation devices and their ability to prevent and eradicate infections. External fixation was studied with micron-thin sol-gel coated percutaneous pins releasing triclosan and inserted medially into rabbit tibiae. A total of 11 rabbits received percutaneous pins that were either uncoated or sol-gel/triclosan coated. Internal fracture fixation was also studied using sol-gel coated intramedullary (IM) nails releasing vancomycin in the intramedullary tibiae. Six sheep received IM nails that were coated with a sol-gel film that either contained vancomycin or did not contain vancomycin. All animals were challenged with Staphylococcus aureus around the implant. Animals were euthanized at 1 month postoperative. Rabbits receiving triclosan/sol-gel coated percutaneous pins did not show signs of infection. Uncoated percutaneous pins had a significantly higher infection rate. In the sheep study, there were no radiographic signs of osteomyelitis with vancomycin/sol-gel coated IM nails, in contrast to the observations in the control cohort. Hence, the nanostructured sol-gel controlled release technology offers the promise of a reliable and continuous delivery system of bactericidals from orthopedic devices to prevent and treat infection.

  8. Polymer sol-gel composite inverse opal structures.

    Zhang, Xiaoran; Blanchard, G J


    We report on the formation of composite inverse opal structures where the matrix used to form the inverse opal contains both silica, formed using sol-gel chemistry, and poly(ethylene glycol), PEG. We find that the morphology of the inverse opal structure depends on both the amount of PEG incorporated into the matrix and its molecular weight. The extent of organization in the inverse opal structure, which is characterized by scanning electron microscopy and optical reflectance data, is mediated by the chemical bonding interactions between the silica and PEG constituents in the hybrid matrix. Both polymer chain terminus Si-O-C bonding and hydrogen bonding between the polymer backbone oxygens and silanol functionalities can contribute, with the polymer mediating the extent to which Si-O-Si bonds can form within the silica regions of the matrix due to hydrogen-bonding interactions.

  9. Manufacture of Regularly Shaped Sol-Gel Pellets

    Leventis, Nicholas; Johnston, James C.; Kinder, James D.


    An extrusion batch process for manufacturing regularly shaped sol-gel pellets has been devised as an improved alternative to a spray process that yields irregularly shaped pellets. The aspect ratio of regularly shaped pellets can be controlled more easily, while regularly shaped pellets pack more efficiently. In the extrusion process, a wet gel is pushed out of a mold and chopped repetitively into short, cylindrical pieces as it emerges from the mold. The pieces are collected and can be either (1) dried at ambient pressure to xerogel, (2) solvent exchanged and dried under ambient pressure to ambigels, or (3) supercritically dried to aerogel. Advantageously, the extruded pellets can be dropped directly in a cross-linking bath, where they develop a conformal polymer coating around the skeletal framework of the wet gel via reaction with the cross linker. These pellets can be dried to mechanically robust X-Aerogel.

  10. Moment scaling at the sol-gel transition

    Botet, R. [Paris-11 Univ., 91 - Orsay (France). Lab. de Physique des Solides; Ploszajczak, M. [Grand Accelerateur National d`Ions Lourds, 14 - Caen (France)


    Two standard models of sol-gel transition are revisited here from the point of view of their fluctuations in various moments of both the mass-distribution and the gel-mass. Bond-percolation model is an at-equilibrium system and undergoes a static second-order phase transition, while Monte-Carlo Smoluchowski model is an off-equilibrium one and shows a dynamical critical phenomenon. It is shown that the macroscopic quantities can be splitted into the three classes with different scaling properties of their fluctuations, depending on whether they correspond to: (i) non-critical quantities, (ii) critical quantities or to (iii) an order parameter. (author) 15 refs.

  11. Photochromic gratings in sol gel films containing diazo sulfonamide chromophore

    Kucharski, Stanisław; Janik, Ryszard


    The photochromic sol-gel hybrid materials were prepared by incorporation of an azo chromophore containing sulfonamide fragment into polysiloxane cross-linked network. The materials were used to form transparent films on glass by spin-coating and/or casting. The reversible change of refraction index of the films on illumination with white light was observed by ellipsometry. The experiments with two beam coupling (TBC) and four wave mixing (4 WM) arrangement with green or blue laser beams as writing beams showed formation of a diffraction grating. The diffraction efficiency of the first order was 0.025-0.038 which yielded refraction index modulation in the range of up to 0.0066.

  12. Multifunctional bioinspired sol-gel coatings for architectural glasses

    Cannavale, Alessandro; Fiorito, Francesco; Tortorici, Giovanni [Politecnico di Bari, Dipartimento di Architettura e Urbanistica, Via E. Orabona, 4, 70126, Bari (Italy); Manca, Michele; Cingolani, Roberto; Gigli, Giuseppe [Center for Biomolecular Nanotechnologies (CBN) of the Italian Institute of Technology (IIT), Via Barsanti 1, 73010, Arnesano (LECCE) (Italy)


    Although several multinational companies have recently released products incorporating bioinspired functional coatings, their practical integration in building envelopes is still an open issue. High production costs associated to the existing vacuum deposition technologies, as well as the difficulties in extending the number of functions achievable by a single coating, represent to date the main limitations to their diffusion on a large scale. This review summarizes the key topics in the field of functional coatings for architectural glasses, focusing in particular on the potential applications of sol-gel based antireflective and self-cleaning coatings, that have received a tremendous attention in the last years. It provides an overview of the recent research efforts aimed to improve their properties and to extend their range of applicability. The bioinspired principles, upon which such coatings are based, are also described and are related to the chemical and morphological properties of such surfaces. (author)

  13. Sol-Gel Glass Holographic Light-Shaping Diffusers

    Yu, Kevin; Lee, Kang; Savant, Gajendra; Yin, Khin Swe (Lillian)


    Holographic glass light-shaping diffusers (GLSDs) are optical components for use in special-purpose illumination systems (see figure). When properly positioned with respect to lamps and areas to be illuminated, holographic GLSDs efficiently channel light from the lamps onto specified areas with specified distributions of illumination for example, uniform or nearly uniform irradiance can be concentrated with intensity confined to a peak a few degrees wide about normal incidence, over a circular or elliptical area. Holographic light diffusers were developed during the 1990s. The development of the present holographic GLSDs extends the prior development to incorporate sol-gel optical glass. To fabricate a holographic GLSD, one records a hologram on a sol-gel silica film formulated specially for this purpose. The hologram is a quasi-random, micro-sculpted pattern of smoothly varying changes in the index of refraction of the glass. The structures in this pattern act as an array of numerous miniature lenses that refract light passing through the GLSD, such that the transmitted light beam exhibits a precisely tailored energy distribution. In comparison with other light diffusers, holographic GLSDs function with remarkably high efficiency: they typically transmit 90 percent or more of the incident lamp light onto the designated areas. In addition, they can withstand temperatures in excess of 1,000 C. These characteristics make holographic GLSDs attractive for use in diverse lighting applications that involve high temperatures and/or requirements for high transmission efficiency for ultraviolet, visible, and near-infrared light. Examples include projectors, automobile headlights, aircraft landing lights, high-power laser illuminators, and industrial and scientific illuminators.

  14. Mayenite Synthesized Using the Citrate Sol-Gel Method

    Ude, Sabina N [ORNL; Rawn, Claudia J [ORNL; Meisner, Roberta A [University of Tennessee (UTK) and Oak Ridge National Laboratory (ORNL); Kirkham, Melanie J [ORNL; Jones, Gregory L. [University of Tennessee, Knoxville (UTK); Payzant, E Andrew [ORNL


    A citrate sol-gel method has been used to synthesize mayenite (Ca12Al14O33). X-ray powder diffraction data show that the samples synthesized using the citrate sol-gel method contained CaAl2O4 and CaCO3 along with mayenite when fired ex-situ in air at 800 C but were single phase when fired at 900 C and above. Using high temperature x-ray diffraction, data collected in-situ in air at temperatures of 600 C and below showed only amorphous content; however, data collected at higher temperatures indicated the first phase to crystallize is CaCO3. High temperature x-ray diffraction data collected in 4% H2/96% N2 does not show the presence of CaCO3, and Ca12Al14O33 starts to form around 850 C. In comparison, x-ray powder diffraction data collected ex-situ on samples synthesized using traditional solid-state synthesis shows that single phase was not reached until samples were fired at 1350 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method suggest the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is very different depending on the environment. Brunauer-Emmett-Teller (BET) measurements showed a slightly higher surface area of 7.4 0.1 m2/g in the citrate gel synthesized samples compared to solid-state synthesized sample with a surface area of 1.61 0.02 m2/g. SEM images show a larger particle size for samples synthesized using the solid-state method compared to those synthesized using the citrate gel method.

  15. Sol-Gel processing of silica nanoparticles and their applications.

    Singh, Lok P; Bhattacharyya, Sriman K; Kumar, Rahul; Mishra, Geetika; Sharma, Usha; Singh, Garima; Ahalawat, Saurabh


    Recently, silica nanoparticles (SNPs) have drawn widespread attention due to their applications in many emerging areas because of their tailorable morphology. During the last decade, remarkable efforts have been made on the investigations for novel processing methodologies to prepare SNPs, resulting in better control of the size, shape, porosity and significant improvements in the physio-chemical properties. A number of techniques available for preparing SNPs namely, flame spray pyrolysis, chemical vapour deposition, micro-emulsion, ball milling, sol-gel etc. have resulted, a number of publications. Among these, preparation by sol-gel has been the focus of research as the synthesis is straightforward, scalable and controllable. Therefore, this review focuses on the recent progress in the field of synthesis of SNPs exhibiting ordered mesoporous structure, their distribution pattern, morphological attributes and applications. The mesoporous silica nanoparticles (MSNPs) with good dispersion, varying morphology, narrow size distribution and homogeneous porous structure have been successfully prepared using organic and inorganic templates. The soft template assisted synthesis using surfactants for obtaining desirable shapes, pores, morphology and mechanisms proposed has been reviewed. Apart from single template, double and mixed surfactants, electrolytes, polymers etc. as templates have also been intensively discussed. The influence of reaction conditions such as temperature, pH, concentration of reagents, drying techniques, solvents, precursor, aging time etc. have also been deliberated. These MSNPs are suitable for a variety of applications viz., in the drug delivery systems, high performance liquid chromatography (HPLC), biosensors, cosmetics as well as construction materials. The applications of these SNPs have also been briefly summarized. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Sol-gel synthesis and densification of aluminoborosilicate powders. Part 1: Synthesis

    Bull, Jeffrey; Selvaduray, Guna; Leiser, Daniel


    Aluminoborosilicate powders high in alumina content were synthesized by the sol-gel process utilizing various methods of preparation. Properties and microstructural effects related to these syntheses were examined. After heating to 600 C for 2 h in flowing air, the powders were amorphous with the metal oxides comprising 87 percent of the weight and uncombusted organics the remainder. DTA of dried powders revealed a T(sub g) at approximately 835 C and an exotherm near 900 C due to crystallization. Powders derived from aluminum secbutoxide consisted of particles with a mean diameter 5 microns less than those from aluminum isopropoxide. Powders synthesized with aluminum isopropoxide produced agglomerates comprised of rod shaped particulates while powders made with the secbutoxide precursor produced irregular glassy shards. Compacts formed from these powders required different loadings for equivalent densities according to the method of synthesis.

  17. Low temperature synthesis of magnesium oxide and spinel powders by a sol-gel process

    Li-Zhai Pei


    Full Text Available Magnesium oxide and magnesium aluminate (MgAl2O4 spinel (MAS powders have been synthesized by a simple aqueous sol-gel process using citrate polymeric precursors derived from magnesium chloride, aluminium nitrate and citrate. The thermal decomposition of the precursors and subsequent formation of cubic MgO and MAS were investigated by X-ray diffraction (XRD, scanning electron microscopy (SEM, thermogravimetry-differential scanning calorimetry (TG-DSC and Fourier transform infrared spectra (FTIR. The single phase cubic MgO powder and MAS powder form after heat treatment at 800 and 1200 °C, respectively. The particle size of the MgO and MAS powders is about 100 nm and several micrometers, respectively. Ball milling eliminates the size of MgO and MgAl2O4 spinel powders by decreasing the conglomeration of the powders.

  18. Sol-Gel-Coated Calix[4]arene Fiber for Solid-Phase Microextraction

    LiXiu-juan; XiaoRui-min; LiHai-bing; ZengZhao-rui


    5, 11, 17, 23-tetra-tert-butyl-25, 27-diethoxy-26, 28-dihydroxycalix [4] arene/hydroxy-terminated silicone oil coated fiber was first prepared and applied for solid-phase microextraction with sol-gel technology. The properties of the new coating were investigated by analysis of benzene derivatives, polycyclic aromatic hydrocarbons and aromatic amines.The fiber is characterized by good sensitivity and selectivity to these aromatics. The fiber has stable performance at a high temperature of 380℃ and after a long solvent immersing,thus its lifetime is very long. It shows good fiber-to-fiber and batch-to-batch reproducibility. Furthermore, broad linear ranges and low detection limits are also its characteristics.

  19. Sol-Gel-Coated Calix[4]arene Fiber for Solid-Phase Microextraction

    Li Xiu-juan; Xiao Rui-min; Li Hai-bing; Zeng Zhao-rui


    5,11,17,23-tetra-tert-butyl-25, 27-diethoxy-26, 28-dihydroxycalix [4] arene /hydroxy-terminated silicone oil coated fiber was first prepared and applied for solid-phase microextraction with sol-gel technology. The properties of the new coating were investigated by analysis of benzene derivatives, polycyclic aromatic hydrocarbons and aromatic amines. The fiber is characterized by good sensitivity and selectivity to these aromatics. The fiber has stable performance at a high temperature of 380℃ and after a long solvent immersing, thus its lifetime is very long. It shows good fiber-to-fiber and batch-to-batch reproducibility. Furthermore, broad linear ranges and low detection limits are also its characteristics.

  20. Wide colour gamut generated in triply lanthanide doped sol-gel nano-glass-ceramics

    Castillo, J. del, E-mail: fjvargas@ull.e [Universidad de La Laguna, Dpto. Fisica Basica (Spain); Mendez-Ramos, J. [Universidad de La Laguna, Dpto. Fisica Fundamental y Experimental, Electronica y Sistemas (Spain); Yanes, A. C. [Universidad de La Laguna, Dpto. Fisica Basica (Spain); Rodriguez, V. D. [Universidad de La Laguna, Dpto. Fisica Fundamental y Experimental, Electronica y Sistemas (Spain)


    The generation of a wide colour gamut, based on up-conversion of cheap near-infrared photons into the visible range, is of great importance for general lighting appliances and integrated optical devices. Here, we report for the first time on up-conversion luminescence under infrared excitation at 980 nm in Yb{sup 3+}-Er{sup 3+}-Tm{sup 3+} triply doped sol-gel derived SiO{sub 2}-LaF{sub 3} based nano-glass-ceramics (SOL-YET), containing LaF{sub 3} nanocrystals with a size about 13 nm. Efficient simultaneous up-conversion emission of the three primary colours (blue, green and red) gives rise to a balanced white overall emission. The ratio between up-conversion emission bands can be varied by changing pump power intensity resulting in colour tuneable up-conversion phosphor.

  1. Influence of precursor ratios on the properties of cotton coated with a sol-gel flame retardant

    Chapple, Stephen A


    Full Text Available and strength), coatings were applied to cotton fabrics using different ratios of sol-gel precursors. The results showed that the ratio of sol-gel precursors influenced fabric stiffness and strength but not flammability. The distribution of the sol-gel flame...

  2. An Alcohol-Free SiO2 Sol-Gel Matrix Functionalized with Acetic Acid as Drug Reservoir for the Controlled Release of Pentoxifylline

    Mayra Angélica Alvarez Lemus


    Full Text Available Pentoxifylline (PTX is a xanthine derivative, with hemorrheologic properties, that has been useful in the treatment of several diseases. However, a conventional route of administration implies high doses, what is unnecessary to the organism, seriously increasing the risk of toxicity because of side effects. Because of the facility to modify their surface, sol-gel materials have proved to be suitable reservoirs for a variety of molecules for biological applications. In this work we prepared alcohol-free SiO2 material by the sol-gel process using acetic acid as surface modifier and hydrolysis catalyst, the alkoxide/water ratio (Rw used was 1/16, and tetraethylorthosilicate was used as SiO2 precursor. Spectroscopic characterization was carried out by means of FTIR-ATR and UV-Visible spectroscopies; the results confirmed the presence of the drug and interactions between sol-gel matrix and PTX. BET specific surface area values of the sol-gel materials were 365 and 462 m2/g for SiO2 and PTX-SiO2, respectively. Synthesized SiO2 nanoparticles showed efficient entrapment of PTX since a controlled release of 83% of drug content was reached.

  3. A utilização de materiais obtidos pelo processo de sol-gel na construção de biossensores The utilization of materials obtained by the sol-gel process in biosensors construction

    Antonio A. S. Alfaya


    Full Text Available The use of sol-gel materials to develop new biosensors has received great attention due to its characteristics and versatility of sol-gel process. An overview is presented of the state-of-the-art of electrochemical biosensors employing sol-gel materials. Low-temperature, porous sol-gel ceramics represent a new class for the immobilization of biomolecules. The rational design of sol-gel sensing materials, based on the judicious choice of the starting alkoxide, encapsulated reagents, and preparation conditions, allows tailoring of material properties in a wide range, and offers great potential for the development of electrochemical biosensors.

  4. Formulation and evaluation of antimicrobial activity of Morus alba sol-gel against periodontal pathogens

    Shilpa Gunjal


    Full Text Available Background: Periodontitis has a multifactorial etiology, with primary etiologic agents being pathogenic bacteria that reside in the subgingival area. Recent advances in the field of alternative medicine introduced various herbal products for the treatment of periodontitis. Aim: To assess and compare the antimicrobial activity of Morus alba sol-gel with chlorhexidine sol-gel against ATCC standard strains of Aggregatibacter actinomycetemcomitans, Porphyromonas gingivalis, and Tannerella forsythia. Materials and Methods: Crude extract of Morus alba leaves was prepared by Soxhlet method by using ethanol as a solvent. Phytochemical screening of the crude extract of M. alba was performed to check the various chemical constituents. M. alba sol-gel and chlorhexidine sol-gel were formulated using Pluronic f127 and Pluronic f108 and compared for their antimicrobial activity. The minimum inhibitory concentration of both the gels was performed using agar well diffusion technique. Results: The minimum inhibitory concentration of M. alba sol-gel and chlorhexidine sol-gel against A. actinomycetemcomitans is 19 and 17 mm, T. forsythia is 12 and 21 mm, and P. gingivalis is 16 and 18 mm, respectively. Conclusion: Both M. alba and chlorhexidine sol-gel exhibited potent antimicrobial activity against periodontal pathogens.

  5. Macroporous Titania Monolith Prepared via Sol-gel Process with Polymer Foam as the Template

    REN, Jian; DU, Zhong-Jie; ZHANG, Chen; LI, Hang-Quan


    Macroporous titania monoliths were prepared via sol-gel method using polymer foam as templates. The polymer foam polymerized via concentrated emulsion polymerization was immerged in a solution of titanium(Ⅳ) isopropoxide in 2-propanol, which underwent a sol-gel process. The organic components were subsequently removed by calcination. The effects of various parameters, including the nature of the monomer, the volume fraction of dispersed phase of the concentrated emulsion, and concentration of the sol-gel solution were investigated. The SEM micrographs of the macroporous titania monoliths thus obtained showed that the porous structure of the final material was effectively controllable.

  6. Ultrasound-assisted sol-gel synthesis of ZrO2.

    Guel, Marlene Lariza Andrade; Jiménez, Lourdes Díaz; Hernández, Dora Alicia Cortés


    Synthesis of tetragonal ZrO2 by both conventional sol-gel and ultrasound-assisted sol-gel methods and using a non-ionic surfactant Tween-20, was performed. A porous microstructure composed of nanometric particles was observed. Tetragonal ZrO2 was obtained using a low heat treatment temperature of powders, 500°C by both methods. A higher crystallinity and a shorter reaction time were observed when ultrasound was used in the sol-gel method due to the cavitation phenomenon.

  7. Growth of two-dimensional KGd(WO 4) 2 nanorods by modified sol-gel Pechini method

    Thangaraju, D.; Samuel, P.; Moorthy Babu, S.


    KGd (WO 4) 2 nanocrystalline powder was obtained by modified sol-gel Pechini method. The synthesis procedure was optimized with TGA and DTA analyses. Synthesized polymeric resin was calcinated at 550 and 700 °C using resistive furnace in an open atmosphere. Crystallinity of annealed powder was confirmed using X-ray diffraction. Absorption peaks of FT-IR for gel and the annealed samples, at two different temperatures show the decomposition of citrate-ethylene glycol complex and formation of KGW particles. Raman analysis confirms that the derived particles have well constructed bridges of W-O-O-W. External morphology of the particles was analysed through SEM.

  8. Characterization of carbon cryogels synthesized by sol-gel polycondensation



    Full Text Available Resorcinol-formaldehyde (RF cryogels were synthesized by the sol-gel polycondensation of resorcinol (R with formaldehyde (F and freeze-drying was carried out with t-butanol. Carbon cryogels were obtained by pyrolyzing RF cryogels in an inert atmosphere. Characterization by nitrogen adsorption showed that the carbon cryogels were micro and mesoporous materials with high specific surface areas (SBET ~ 550 m2/g. Cyclic voltammetry experiments at various scan rates (2 to 200 mV s-1 were performed to study the electrical double-layer charging of carbon cryogel electrodes in 0.5 mol dm-3 HClO4 solution. It has been demonstrated that it is possible to sub-divide the total specific capacitance into the mesoporous and the microporous specific capacitance by analyzing the linear dependence of the charge (q on the reciprocal of the square root of the potential scan rate (v-1/2, and the linear dependence of the reciprocal charge (1/q on the square root of the potential scan rate (v-1/2. The specific capacitance was found to be constant over a wide range of sample weight (12.5 to 50.0 mg and a very promising specific capacitance value of 150 F/g, was found for this material operating in an acidic 0.5 mol dm-3 HClO4 solution at room temperature.

  9. /dopamine films prepared by sol-gel method

    Valverde-Aguilar, G.; Prado-Prone, G.; Vergara-Aragón, P.; Garcia-Macedo, J.; Santiago, Patricia; Rendón, Luis


    Dopamine was encapsulated into nanoporous amorphous TiO2 matrix by sol-gel method under atmospheric conditions. A second sample was obtained by the addition of the crown-ether 15C5 in this previous sample. Thin films were spin-coated on glass wafers. No heat treatment was employed in both films. All films were characterized using infrared spectroscopy, high resolution transmission electronic microscopy, X-ray diffraction, optical absorption and scanning electronic microscopy. Despite the films prepared with 15C5 were no calcined, a partial crystallization was identified. Anatase and rutile nanoparticles with sizes of 4-5 nm were obtained. Photoconductivity technique was used to determine the charge transport mechanism on these films. Experimental data were fitted with straight lines at darkness and under illumination wavelengths at 320, 400, and 515 nm. It indicates an ohmic behavior. Photovoltaic and photoconductivity parameters were determined from the current density vs. the applied-electrical-field results. Amorphous film has bigger photovoltaic and photoconductive parameters than the partially crystalline film. Results observed in the present investigation prove that the nanoporous TiO2 matrix can protect the dopamine inhibiting its chemical instability. This fact modifies the optical, physical and electrical properties of the film, and is intensified when 15C5 is added.

  10. Preparation of silica by sol-gel method using formamide

    R.F.S. Lenza


    Full Text Available In this work we obtained microporous and mesoporous silica gels by sol-gel processing. Tetraethylortosilicate (TEOS was used as precursor. Nitric acid and hydrofluoric acid were used as catalysts. In order to study the affect of formamide as drying additive, we used a molar ratio alkoxide/formamide of 1/1. The performance of formamide in obtaining crack-free gels was evaluated through monolithicity measurements. The structural evolution occurring in the interconnected network of the gels during thermal treatment was monitored by Fourier transform infrared spectroscopy (FTIR, shrinkage and density measurements and nitrogen gas sorption. We noted that in the presence of formamide, the Si-O-Si bonds are stronger and belong to a more cross-linked structure. The samples obtained in the presence of formamide have larger pore volume and its pore structure is in the range of mesoporosity. The samples obtained without additive are microporous. Formamide allowed the preparation of crack-free silica gels stabilized at high temperatures.

  11. Synthesis of Titania-Silica Materials by Sol-Gel

    Rubia F. S. Lenza


    Full Text Available In this work TiO2-SiO2 glasses containing as much as 20 mol % of TiO2 were prepared via sol-gel process using titanium and silicon alkoxides, in the presence of chlorine, in the form of titanium tetrachloride or HCl. The gels were heat-treated until 800 °C. X-ray diffraction and Fourier transform infrared spectroscopy were used to understand the structural properties of TiO2-SiO2 oxides calcined at different temperatures and to evaluate the homogeneity of these materials. The degree of the compactness of the silica network is inferred from the frequency of the asymmetric stretching vibrations of Si-O-Si bonds. Formation of Si-O-Ti bridges, as monitored by the intensity of characteristic 945 cm-1 ¾ 960 cm-1 vibration, is particularly prominent if the method of basic two-step prehydrolysis of silicon alkoxide, addition of titanium alkoxide and completion of hydrolysis was used.

  12. Mesoporous nanocomposite coatings for photonic devices: sol-gel approach

    Islam, Shumaila; Bidin, Noriah; Riaz, Saira; Suan, Lau Pik; Naseem, Shahzad; Sanagi, Mohd. Marsin


    Thermally stable, optically active inorganic nanocomposites, i.e., aluminum-silicate (AS) and silica-titania (ST), are synthesized via acid-catalyzed low-temperature sol-gel method in order to get stable, crack-free coating material for photonic devices. The samples are characterized by atomic force microscope, field emission scanning electron microscope (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett--Teller (BET) surface area, Barrett-Joyner-Halenda (BJH) pore size distribution surface analysis and UV-Vis spectroscopy. Microscopic results show good incorporation of ST and AS particles as composites with grain size within range of 12-17 and 62-109 nm, respectively. EDX analysis substantiated the stoichiometric formation of homogeneous nanocomposites. XRD of the films reveals primary polycrystalline anatase titania phase and mullite phase of ST and AS nanocomposites. FTIR confirms the heterogeneous bond linkage between titania, silica and alumina species. Furthermore, the fabricated samples have mesoporous nature with high surface area, large pore volume and diameter. The tunable refractive index of 1.33-1.35 with high transparency is obtained for synthesized nanocomposites. The experimental findings show that these physically modified and thermally stable alumina- and titania-doped silica-based composite coatings are promising for photonic devices modification.

  13. Hybrid silica-PVA nanofibers via sol-gel electrospinning.

    Pirzada, Tahira; Arvidson, Sara A; Saquing, Carl D; Shah, S Sakhawat; Khan, Saad A


    We report on the synthesis of poly(vinyl alcohol) (PVA)-silica hybrid nanofibers via sol-gel electrospinning. Silica is synthesized through acid catalysis of a silica precursor (tetraethyl orthosilicate (TEOS) in ethanol-water), and fibers are obtained by electrospinning a mixture of the silica precursor solution and aqueous PVA. A systematic investigation on how the amount of TEOS, the silica-PVA ratio, the aging time of the silica precursor mixture, and the solution rheology influence the fiber morphology is undertaken and reveals a composition window in which defect-free hybrid nanofibers with diameters as small as 150 nm are obtained. When soaked overnight in water, the hybrid fibers remain intact, essentially maintaining their morphology, even though PVA is soluble in water. We believe that mixing of the silica precursor and PVA in solution initiates the participation of the silica precursor in cross-linking of PVA so that its -OH group becomes unavailable for hydrogen bonding with water. FTIR analysis of the hybrids confirms the disappearance of the -OH peak typically shown by PVA, while formation of a bond between PVA and silica is indicated by the Si-O-C peak in the spectra of all the hybrids. The ability to form cross-linked nanofibers of PVA using thermally stable and relatively inert silica could broaden the scope of use of these materials in various technologies.

  14. "Non-hydrolytic" sol-gel synthesis of molybdenum sulfides

    Leidich, Saskia; Buechele, Dominique; Lauenstein, Raphael; Kluenker, Martin; Lind, Cora


    Non-hydrolytic sol-gel reactions provide a low temperature solution based synthetic approach to solid-state materials. In this paper, reactions between molybdenum chloride and hexamethyldisilthiane in chloroform were explored, which gave access to both MoS2 and Mo2S3 after heat treatment of as-recovered amorphous samples to 600-1000 °C. Interesting morphologies were obtained for MoS2, ranging from fused spherical particles to well-defined nanoplatelets and nanoflakes. Both 2H- and 3R-MoS2 were observed, which formed thin hexagonal and triangular platelets, respectively. The platelets exhibited thicknesses of 10-30 nm, which corresponds to 15-50 MoS2 layers. No attempts to prevent agglomeration were made, however, well separated platelets were observed for many samples. Heating at 1000 °C led to formation of Mo2S3 for samples that showed well-defined MoS2 at lower temperatures, while less crystalline samples had a tendency to retain the MoS2 structure.

  15. Functionalization of ceramic tile surface by sol-gel technique.

    Bondioli, F; Taurino, R; Ferrari, A M


    The aim of this investigation was the surface functionalization of industrial ceramic tiles by sol-gel technique to improve at the same time the cleanability of unglazed surfaces. This objective was pursued through the design and preparation of nanostructured coating that was deposited on polished unglazed tiles by air-brushing. In particular TiO(2)-SiO(2) binary film with 1, 2 or 5wt% of titania were prepared by using tetraethoxysilane and titania nanoparticles as precursors. The obtained films were characterized by scratch tests to verify the adhesion of the coatings to the polished tiles. To mainly evaluate the effect of the thermal treatment (temperature range 100-600 degrees C) on the photocatalicity of the coatings, the films were studied under UV exposure by contact angle measurements and cleanability test. Particular attention has been paid to preserve the aesthetical aspect of the final product and the obtained hue variation was evaluated by means of UV-visible spectroscopy and colorimetric analysis.

  16. Infrared Spectroscopy Studies on sol-gel prepared alumina Powders



    Full Text Available Gamma-alumina fine particles were synthesized by sol-gel process. Aluminum tri-sec-butoxide (ATB, anhydrous ethyl alcohol (EtOH, water (H2O and hydrochloric acid (HCl were used as starting materials. Different samples were synthesized with EtOH/ATB=60/1, HCl/ATB=0.08/1 and H2O/ATB=1/1 ratios and calcined at different temperatures. Molar ratios of H2O/ATB (from 1 to 25 and HCl/ATB (from 0.08 to 0.4 were changed for some other samples, during synthesizing process. The products were characterized by both XRD and FTIR measurements. Studies were carried out on the effect of calcination temperature and change of H2O/ATB and HCl/ATB ratios on structure and processes involved in phase transformations.DOI:

  17. Mechanisms of silk fibroin sol-gel transitions.

    Matsumoto, Akira; Chen, Jingsong; Collette, Adam L; Kim, Ung-Jin; Altman, Gregory H; Cebe, Peggy; Kaplan, David L


    Silk fibroin sol-gel transitions were studied by monitoring the process under various physicochemical conditions with optical spectroscopy at 550 nm. The secondary structural change of the fibroin from a disordered state in solution to a beta-sheet-rich conformation in the gel state was assessed by FTIR and CD over a range of fibroin concentrations, temperatures, and pH values. The structural changes were correlated to the degree of gelation based on changes in optical density at 550 nm. No detectable changes in the protein secondary structure (FTIR, CD) were found up to about 15% gelation (at 550 nm), indicating that these early stages of gelation are not accompanied by the formation of beta-sheets. Above 15%, the fraction of beta-sheet linearly increased with the degree of gelation. A pH dependency of gelation time was found with correlation to the predominant acidic side chains in the silk. Electrostatic interactions were related to the rate of gelation above neutral pH. The overall independencies of processing parameters including concentration, temperature, and pH on gel formation and protein structure can be related to primary sequence-specific features in the molecular organization of the fibroin protein. These findings clarify aspects of the self-assembly of this unique family of proteins as a route to gain control of material properties, as well as for new insight into the design of synthetic silk-biomimetic polymers with predictable solution and assembly properties.

  18. Sol-Gel Synthesis and Characterization of Nanoparticles

    S. Ramesh


    Full Text Available The nanoparticles have been synthesized by sol-gel technique. X-ray diffraction, scanning electron microscopy, optical absorption spectroscopy, and electron paramagnetic resonance spectroscopy were used to characterize the sample. The X-ray diffraction results indicate the formation of nanocrystalline materials in tetragonal lattice with P42/nnm space group. The identical distribution of elements were confirmed by scanning electron microscopy with energy dispersive X-ray spectrometry and X-ray mapping. Electron paramagnetic resonance lineshapes of the samples are obtained at various (13 K, 77 K, and 300 K temperatures. The isotropic lineshapes of the sample B1 are attributed to dipole-dipole interaction of Ti3+ ions. The incorporation of Al3+ ions into the sample B2–B5 the isotropic nature of the lineshapes are collapsed due to the distraction in crystal field. Optical absorption spectra results reveal the presence of Ag-TiO2 nanoparticles.

  19. Molecular receptors in metal oxide sol-gel materials prepared via molecular imprinting

    Sasaki, Darryl Y.; Brinker, C. Jeffrey; Ashley, Carol S.; Daitch, Charles E.; Shea, Kenneth J.; Rush, Daniel J.


    A method is provided for molecularly imprinting the surface of a sol-gel material, by forming a solution comprised of a sol-gel material, a solvent, an imprinting molecule, and a functionalizing siloxane monomer of the form Si(OR).sub.3-n X.sub.n, wherein n is an integer between zero and three and X is a functional group capable of reacting with the imprinting molecule, evaporating the solvent, and removing the imprinting molecule to form the molecularly imprinted metal oxide sol-gel material. The use of metal oxide sol-gels allows the material porosity, pore size, density, surface area, hardness, electrostatic charge, polarity, optical density, and surface hydrophobicity to be tailored and be employed as sensors and in catalytic and separations operations.

  20. Characterization and comparison of PZT powder synthesis by solid state and sol gel methods

    E Pakizeh


    Full Text Available   This paper describes the synthesis of Pb(Zr0.95Ti0.05O3 powder by sol gel and solid state methods. PZT powders were fabricated by solid-state reaction process using metal oxides and in sol gel method salts and organic compounds were employed. The powders were calcined at 700 and 950 oC in sol gel and solid state methods, respectively. The synthesized powders were analyzed by FTIR and XRD. The average crystal grain size of PZT powders determined by X-ray diffraction method using the Scherrer equation, and in sol gel and solid state methods measured 42 and 330 nm, respectively. The optical constants of powders were evaluated and compaed using FTIR transmittance spectroscopy and Kramers-Kronig analysis.

  1. Preparation of oxide glasses from metal alkoxides by sol-gel method

    Kamiya, K.; Yoko, T.; Sakka, S.


    An investigation is carried out on the types of siloxane polymers produced in the course of the hydrolysis of silicon tetraethoxide, as well as the preparation of oxide glasses from metal alkoxides by the sol-gel method.

  2. Amoeba-like self-oscillating polymeric fluids with autonomous sol-gel transition

    Onoda, Michika; Ueki, Takeshi; Tamate, Ryota; Shibayama, Mitsuhiro; Yoshida, Ryo


    In the field of polymer science, many kinds of polymeric material systems that show a sol-gel transition have been created. However, most systems are unidirectional stimuli-responsive systems that require physical signals such as a change in temperature. Here, we report on the design of a block copolymer solution that undergoes autonomous and periodic sol-gel transition under constant conditions without any on-off switching through external stimuli. The amplitude of this self-oscillation of the viscosity is about 2,000 mPa s. We also demonstrate an intermittent forward motion of a droplet of the polymer solution synchronized with the autonomous sol-gel transition. This polymer solution bears the potential to become the base for a type of slime-like soft robot that can transform its shape kaleidoscopically and move autonomously, which is associated with the living amoeba that moves forward by a repeated sol-gel transition.

  3. Optical pH detector based on LTCC and sol-gel technologies

    Tadaszak, R. J.; Łukowiak, A.; Golonka, L. J.


    This paper presents an investigation on using sol-gel thin film as a material for sensors application in LTCC (Low Temperature Co-fired Ceramics) technology. This material gives the opportunity to make new, low-cost highly integrated optoelectronic devices. Sensors with optical detection are a significant part of these applications. They can be used for quick and safe diagnostics of some parameters. Authors present a pH detector with the optical detection system made of the LTCC material. The main part of the device is a flow channel with the chamber and sol-gel active material. The silica sol-gel with bromocresol green indicator was used. As the absorbance of sol-gel layer changes with the pH value of a measured medium, the transmitted light power was measured. The pH detector was integrated with the electronic components on the LTCC substrate.

  4. Enhanced piezoelectric performance of composite sol-gel thick films evaluated using piezoresponse force microscopy.

    Liu, Yuanming; Lam, Kwok Ho; Kirk Shung, K; Li, Jiangyu; Zhou, Qifa


    Conventional composite sol-gel method has been modified to enhance the piezoelectric performance of ceramic thick films. Lead zirconate titanate (PZT) and lead magnesium niobate-lead titanate (PMN-PT) thick films were fabricated using the modified sol-gel method for ultrasonic transducer applications. In this work, piezoresponse force microscopy was employed to evaluate the piezoelectric characteristics of PZT and PMN-PT composite sol-gel thick films. The images of the piezoelectric response and the strain-electric field hysteresis loop behavior were measured. The effective piezoelectric coefficient (d33,eff) of the films was determined from the measured loop data. It was found that the effective local piezoelectric coefficient of both PZT and PMN-PT composite films is comparable to that of their bulk ceramics. The promising results suggest that the modified composite sol-gel method is a promising way to prepare the high-quality, crack-free ceramic thick films.

  5. Electrochemical Properties of Poly(ethylene oxide)(PEO) Doped TiO2-PEO Films Prepared by Sol-gel Dip Coating Technique


    PEO modified TiO2-PEO organic-inorganic hybrid thin films were prepared via sol-gel dipping process on glass substrate pre-coated with ITO. The preparation parameters were studied. Electrochemical and optical properties of the films were characterized by cyclic voltammetric response and visible transmittance. X-ray diffraction (XRD) was used to determined the crystalline structure of the gel. The results show the sols added with PEO have acceptable stable periods for practical use. The PEO modified optical transitivity of the hybrid films has heavy effects on the crystallization of TiO2 during structural evolution because of the interaction between PEO and TiO2. PEO- TiO2 films have better electrochemical activity than the TiO2 equivalent behaved as higher Li+ insertion/extraction current density and cyclic reversibility.

  6. Realization of MMI Power Splitter by UV-light Imprinting Technique Using Hybrid Sol-Gel SiO2 Materials

    WANG Yue; WU Yuan-Da; LI Jian-Guang; WANG Hong-Jie; HU Xiong-Wei


    An efficient fabrication scheme of buried ridge, waveguide devices is demonstrated by UV-light imprinting technique using organic-inorganic hybrid sol-gel Zr-doped SiO2 materials. The refractive indices of a guiding layer and a cladding layer for the buried ridge waveguide structure are 1.537 and 1.492 measured at 1550nm, respectively. The tested results show more circular mode profiles due to existence of the cladding layer. A buried ridge single-mode waveguide operating at 1550nm has a low propagation loss (O.088 dB/cm) and the 1 × 2 MMI power splitter exhibits uniform outputs, with a very low splitting loss of O.029dB at 1549nm.

  7. Strength of interactions between immobilized dye molecules and sol-gel matrices.

    Ismail, Fanya; Schoenleber, Monika; Mansour, Rolan; Bastani, Behnam; Fielden, Peter; Goddard, Nicholas J


    In this paper we present a new theory to re-examine the immobilization technique of dye doped sol-gel films, define the strength and types of possible bonds between the immobilized molecule and sol-gel glass, and show that the immobilized molecule is not free inside the pores as was previously thought. Immobilizing three different pH sensitive dyes with different size and functional groups inside the same sol-gel films revealed important information about the nature of the interaction between the doped molecule and the sol-gel matrix. The samples were characterized by means of ultraviolet-visible spectrophotometer (UV-VIS), thermal gravimetric analysis (TGA), mercury porosimetry (MP), nuclear magnetic resonance spectroscopy ((29)Si NMR) and field-emission environmental scanning electron microscopy (ESEM-FEG). It was found that the doped molecule itself has a great effect on the strength and types of the bonds. A number of factors were identified, such as number and types of the functional groups, overall charge, size, pK(a) and number of the silanol groups which surround the immobilized molecule. These results were confirmed by the successful immobilization of bromocresol green (BCG) after a completely polymerized sol-gel was made. The sol-gel consisted of 50% tetraethoxysilane (TEOS) and 50% methyltriethoxysilane (MTEOS) (w/w). Moreover, the effect of the immobilized molecule on the structure of the sol-gel was studied by means of a leaky waveguide (LW) mode for doped films made before and after polymerization of the sol-gel.

  8. Making MgO/SiO2 Glasses By The Sol-Gel Process

    Bansal, Narottam P.


    Silicon dioxide glasses containing 15 mole percent magnesium oxide prepared by sol-gel process. Not made by conventional melting because ingredients immiscible liquids. Synthesis of MgO/SiO2 glass starts with mixing of magnesium nitrate hexahydrate with silicon tetraethoxide, both in alcohol. Water added, and transparent gel forms. Subsequent processing converts gel into glass. Besides producing glasses of new composition at lower processing temperatures, sol-gel method leads to improved homogeneity and higher purity.

  9. Mixed Pyridine-phenol Boron Complex Encapsulated in Polymer/Silica Hybrid Sol-gel Matrix

    DONG Wei; TANG Jun; WANG Yue


    A novel pyridine-phenol boron complex[(dppy)BF]was encapsulated into polymer/silica composite matrix by sol-gel process.UV-Vis absorption spectra show that this process can control the aggregation structure of complex(dppy)BF.The results of photoluminescence of(dppy)BF in sol-gel composite film indicate that both fluorescence intensity and photostability are markedly increased using this method compared with other methods,which increases the practical significance of such composite film.

  10. Sol-Gel Optics: Proceedings SPIE-The International Society for Optical Engineering Held in San Diego, California on 11-13 July 1990. Volume 1328


    Physicochimie des Materiaux "CNRS (France); G. Le Flem, C. Parent. Lab. de Chimie du Solide’CNRS (France); C. L. Lurin, Kodak Pathe (France...Time Process Result 1 25C Mixing Produces colloidalə Hr Hydrolysis & Condensation) suspension (sol) Used for films, coatings 2 250CCsi Sol cast...metal-organic derived oxide coatings. 2. INTRODUCTION Sol-gel derived oxide films may be deposited either from colloidal suspensions or clear polymer

  11. Investigation on a Sol-gel Coating Containing Inhibitors on 2024-T3 Aluminum Alloy

    SHI Hong-wei; LIU Fu-chun; HAN En-hou; SUN Ming-cheng


    For a long time, chromate incorporated conversion coatings have been drawn special attention in corrosion protection of aircraft-used aluminum alloys. However,ever-increasing environmental pressures requires that non-chromate conversion coatings be developed because of the detrimental carcinogenic effects of the chromate compounds. In recent years, the sol-gel coatings doped with inhibitors were developed to replace chromate conversion coatings, and showed real promise. A sol-gel coating was prepared and its anti-corrosion behavior was investigated using the potentiodynamic scanning (PDS) and the electrochemical impedance spectroscopy (EIS). It is found that the sol-gel coating obtained by the hydrolysis and condensation of 3-glycidoxypropyltrimethoxysilane (GPTMS) and tetramethoxysilane (TMOS) is prone to form defects if cured at the room temperature, whereas if cured at a higher temperature (100 ℃), these flaws can be avoided. Furthermore, it can be seen that addition of anti-foam agents and surfactants will reduce the faults if cured at the room temperature. Effects of the corrosion inhibitors, CeCl3 and mercaptobenzothiazole (MBT), in the sol-gel coatings on 2024-T3 aluminum alloy were also investigated. Results show that the corrosion resistance of the sol-gel coatings containing CeCl3 proves to be better than that of the pure and MBT added sol-gel coatings by the electrochemical methods.

  12. Preparation and antioxidant capacity of element selenium nanoparticles sol-gel compounds.

    Bai, Yan; Qin, Biyin; Zhou, Yanhui; Wang, Yudong; Wang, Zi; Zheng, Wenjie


    This paper reported the preparation and antioxidant capacities of element selenium nanoparticles (nanoSe(0))-ascorbic acid (Vc) sol and nanSe(0)/Vc/selenocystine (SeCys) sol-gel compounds. NanoSe(0)-Vc sol was prepared by reduction of selenious dioxide (SeO2) with Vc. In the nanoSe(0)-Vc sol, highly concentrated Vc was also used as a modifier to modulate the diameter of Se(0) nanoparticles in the liquid phase. Then excellent nanoSe(0) sol-gel compounds were obtained by adding SeCys into the nanoSe(0)-Vc sol. The structure of the nanoSe(0)/Vc/SeCys sol-gel compounds was defined, which was constructed via C-Se, Se-H and O=C-Se valences and by interaction between SeCys and Vc via peptide bonds, esterification and dehydration. The antioxidant capacities of the nanoSe(0)-Vc sol and the nanoSe(0)Vc/SeCys sol-gel compounds were estimated by oxygen radical absorption capacity (ORAC) assay. The nanoSe(0)/Vc/SeCys sol-gel compounds possessed a strong antioxidant capacity due to forming the perfect three-dimensional (3D) frameworks structure. The results suggested that the nanoSe(0)-Vc sol and the nanoSe(0)Vc/SeCys sol-gel compounds might be potential medicine, especially antioxidant.

  13. Preparation and characterization of conductive and transparent ruthenium dioxide sol-gel films.

    Allhusen, John S; Conboy, John C


    RuO2 conductive thin films were synthesized using the sol-gel method and deposited onto transparent insulating substrates. The optical transmission, film thickness, surface morphology and composition, resistivity, and spectroelectrochemical performance have been characterized. The optical transmission values of these films ranged from 70 to 89% in the visible region and from 56 to 88% in the infrared region. Resistivity values of the RuO2 sol-gel films varied from 1.02 × 10(-3) to 1.13 Ω cm and are highly dependent on the initial solution concentration of RuO2 in the sol-gel. The RuO2 sol-gel films were used as electrodes for the electrochemical oxidation and reduction of ferrocenemethanol. The electrochemical behavior of our novel RuO2 sol-gel films was compared to that of a standard platinum disk electrode and showed no appreciable differences in the half-wave potential (E1/2). The mechanical and chemical stability of the coatings was tested by physical abrasion and exposure to highly acidic, oxidizing Piranha solution. Repeated exposure to these extreme conditions did not result in any appreciable decline in electrochemical performance. Finally, the use of the novel RuO2 sol-gel conductive and transparent films was demonstrated in a spectroelectrochemistry experiment in which the oxidation and reduction of ferrocenemethanol was monitored via UV-vis spectroscopy as the applied potential was cycled.

  14. Robust aptamer sol-gel solid phase microextraction of very polar adenosine from human plasma.

    Mu, Li; Hu, Xiangang; Wen, Jianping; Zhou, Qixing


    Conventional solid phase microextraction (SPME) has a limited capacity to extract very polar analytes, such as adenosine. To solve this problem, aptamer conjugating sol-gel methodology was coupled with an SPME fiber. According to the authors' knowledge, this is the first reported use of aptamer SPME. The fiber of aptamer sol-gel SPME with a mesoporous structure has high porosity, large surface area, and small water contact angle. Rather than employing direct entrapment, covalent immobilization was the dominant method of aptamer loading in sol-gel. Aptamer sol-gel fiber captured a specified analyte from among the analog molecules, thereby, exhibiting an excellent selective property. Compared with commercial SPME fibers, this aptamer fiber was suitable for extracting adenosine, presenting an extraction efficiency higher than 20-fold. The values of repeatability and reproducibility expressed by relative standard deviation were low (9.4%). Interestingly, the sol-gel network enhanced the resistance of aptamer SPME to both nuclease and nonspecific proteins. Furthermore, the aptamer sol-gel fiber was applied in human plasma with LOQ 1.5 μg/L, which is an acceptable level. This fiber also demonstrates durability and regeneration over 20-cycles without significant loss of efficiency. Given the various targets (from metal ions to biomacromolecules and cells) of aptamers, this methodology will extend the multi-domain applications of SPME.

  15. Investigation of bioactivity, biocompatibility and thermal behavior of sol-gel silica glass containing a high PEG percentage.

    Catauro, M; Renella, R A; Papale, F; Vecchio Ciprioti, S


    SiO2/PEG organic-inorganic hybrid materials, which contain 60 or 70 weight percentage of PEG, were synthesized by the sol-gel technique. The materials were characterized and subjected to various tests to assess their application in the biomedical field. The evaluation of their morphology by scanning electron microscopy (SEM) confirms the homogeneity of the samples on the nanometer scale. Fourier transform infrared spectroscopy (FT-IR) indicated that the two components of the hybrids (SiO2 and PEG) are linked by hydrogen bonds. This feature makes them class I hybrids. Simultaneous thermogravimetry/differential thermal analysis (TG/DTA) was used to investigate their thermal behavior and to establish the best temperatures for their pre-treatment. The fundamental properties that a material must have to be used in the biomedical field are biocompatibility and bioactivity. The formation of a hydroxyapatite layer was observed on the hybrid surface by SEM/EDX and FTIR after soaking in simulated body fluid. This indicates that the materials are able to bond to bone tissue. Moreover, the biocompatibility of SiO2/PEG hybrids was assessed by performing WST-8 cytotoxicity tests on fibroblast cell NIH 3T3 after 24h of exposure. The cytotoxicity tests highlight that the cell viability is affected by the polymer percentage. The results showed that the synthesized materials were bioactive and biocompatible. Therefore, the results obtained are encouraging for the use of the obtained hybrids in dental or orthopedic applications.

  16. Synthesis of Bioactive Chlorogenic Acid-Silica Hybrid Materials via the Sol-Gel Route and Evaluation of Their Biocompatibility.

    Catauro, Michelina; Pacifico, Severina


    Natural phenol compounds are gaining a great deal of attention because of their potential use as prophylactic and therapeutic agents in many diseases, as well as in applied science for their preventing role in oxidation deterioration. With the aim to synthetize new phenol-based materials, the sol-gel method was used to embed different content of the phenolic antioxidant chlorogenic acid (CGA) within silica matrices to obtain organic-inorganic hybrid materials. Fourier transform infrared (FTIR) measurements were used to characterize the prepared materials. The new materials were screened for their bioactivity and antioxidant potential. To this latter purpose, direct DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azinobis-(3-ethylbenzothiazolin-6-sulfonic acid) methods were applied: radical scavenging capability appeared strongly dependent on the phenol amount in investigated hybrids, and became pronounced, mainly toward the ABTS radical cation, when materials with CGA content equal to 15 wt% and 20 wt% were analyzed. The in vitro biocompatibility of the synthetized materials was estimated by using the MTT assay towards fibroblast NIH 3T3 cells, human keratinocyte HaCaT cells, and the neuroblastoma SH-SY5Y cell line. As cell viability and morphology of tested cell lines seemed to be unaffected by new materials, the attenuated total reflectance (ATR)-FTIR method was applied to deeply measure the effects of the hybrids in the three different cell lines.

  17. Organic/inorganic nanocomposite polymer electrolyte

    Li Qi; Shao Jun Dong


    The organic/inorganic nanocomposites polymer electrolytes were designed and synthesized. The organic/inorganic nanocom posites membrane materials and their lithium salt complexes have been found thermally stable below 200 ℃. The conductivity of the organic/inorganic nanocomposites polymer electrolytes prepared at room temperature was at magnitude range of 10-6 S/cm.

  18. Sol-gel preparation of silica and titania thin films

    Thoř, Tomáš; Václavík, Jan


    Thin films of silicon dioxide (SiO2) and titanium dioxide (TiO2) for application in precision optics prepared via the solgel route are being investigated in this paper. The sol-gel process presents a low cost approach, which is capable of tailoring thin films of various materials in optical grade quality. Both SiO2 and TiO2 are materials well known for their application in the field of anti-reflective and also highly reflective optical coatings. For precision optics purposes, thickness control and high quality of such coatings are of utmost importance. In this work, thin films were deposited on microscope glass slides substrates using the dip-coating technique from a solution based on alkoxide precursors of tetraethyl orthosilicate (TEOS) and titanium isopropoxide (TIP) for SiO2 and TiO2, respectively. As-deposited films were studied using spectroscopic ellipsometry to determine their thickness and refractive index. Using a semi-empirical equation, a relationship between the coating speed and the heat-treated film thickness was described for both SiO2 and TiO2 thin films. This allows us to control the final heat-treated thin film thickness by simply adjusting the coating speed. Furthermore, films' surface was studied using the white-light interferometry. As-prepared films exhibited low surface roughness with the area roughness parameter Sq being on average of 0.799 nm and 0.33 nm for SiO2 and TiO2, respectively.




    Full Text Available The objective of the submitted work was to prepare and to characterize two types of silicate coatings prepared by the sol-gel method using the dip-coating technique on a titanium substrate. Efforts have been made to use mechanical properties of bio-inert titanium and bioactive properties of a silicate layer enriched with an admixture of compounds identified below. The first group consisted of silicate coatings containing silver, brushite and monetite. The other group of silicate coatings contained calcium nitrate and triethyl phosphate. Mechanically and chemically treated titanium substrates were dipped into sols and dried and fired. Silicate coatings from the first group were also chemically treated in 10 mol.l-1 solution of sodium hydroxide. All coatings were measured to determine their adhesive and bioactive properties and furthermore the antibacterial properties were tested in the case of first group. Surfaces of the coated substrates were investigated after the firing and after the individual tests with optical and electron microscopy and X-ray microdiffraction. A tape test demonstrated excellent adhesive property of all coatings to the substrate, classified with degree 5. A static in vitro test demonstrated bioactivity of nearly all the coatings. The basic silicate coating from the first group and one type of coating from the second group were identified as inert. Antibacterial properties of silicate coatings containing silver showed to be different when tested against Escherichia coli bacteria. A complete inhibition of the growth of bacteria under our experimental conditions was observed for the coating containing silver and monetite and a partial inhibition of the growth of bacteria for coatings containing silver and silver in combination with brushite.

  20. Synthesis and Characterization of Sol-Gel Prepared Silver Nanoparticles

    Ahlawat, Dharamvir Singh; Kumari, Rekha; Rachna; Yadav, Indu


    Silver nanoparticles (SNPs) have been successfully prepared using sol-gel method by annealing the sample at 550°C for 30 min. The SNPs were not confirmed by X-ray diffraction (XRD) analysis when the annealing temperature was considered at 450°C. They were also not confirmed without calcination of the sample. The physical mechanism of silver clusters formation in the densified silica matrix with respect to thermal treatment has been understood. The presence of silver metal in the silica matrix was confirmed by XRD analysis and TEM image of the samples. The average size of nanoparticles dispersed in silica matrix was determined as 10.2 nm by the XRD technique. The synthesized nanocomposites were also characterized by UV-Visible spectroscopy with a peak in the absorption spectra at around 375 nm. The distribution of particle size has been reported here in the range from 8 nm to 25 nm by TEM observations of the sample prepared at 550°C. The spherically smaller size (≈10 nm) SNPs have reported the surface plasmons resonance (SPR) peak less than or near to 400 nm due to blue-shifting and effect of local refractive index. Without annealing the silica samples the absorption spectra does not show any peak around 375 nm. The FTIR spectroscopy of the three types of samples prepared at different temperatures (room temperature, 450°C and 550°C) has also been reported. This spectra have provided the identification of different chemical groups in the prepared samples. It has been predicted that the size of SNPs by XRD, UV-Visible and TEM results have agreed well with each other. It may be concluded that formation of SNPs is a function of annealing temperature.

  1. Two highly stable and selective solid phase microextraction fibers coated with crown ether functionalized ionic liquids by different sol-gel reaction approaches.

    Shu, Jianjun; Xie, Pengfei; Lin, Danni; Chen, Rongfeng; Wang, Jiang; Zhang, Beibei; Liu, Mingming; Liu, Hanlan; Liu, Fan


    In this work, two novel crown ether functionalized ionic liquid (FIL)-based solid phase microextraction (SPME) fibers were prepared by sol-gel technology using the synthesized 1-(trimethoxysily)propyl 3-(6'-oxo-benzo-15-crown-5 hexyl) imidazolium bis(trifluoromethanesulphonyl)imide ([TMSP(Benzo15C5)HIM][N(SO2CF3)2]) and 1-allyl-3-(6'-oxo-benzo-15-crown-5 hexyl) imidazolium bis(trifluoromethanesulphonyl)imide ([A(Benzo15C5)HIM][N(SO2CF3)2]) as selective stationary phases. Owing to the introduction of trimethoxysilypropyl to the imidazole cation, the [TMSP(Benzo15C5)HIM][N(SO2CF3)2] could be chemically bonded to the formed sol-gel silica substrate through the hydrolysis and polycondensation reaction. Similarly, the [A(Benzo15C5)HIM][N(SO2CF3)2] was able to participate in the formation of the organic-inorganic copolymer coatings through the free radical crosslinking reaction. These two fibers were determined to have "bubble-like" surface characteristics analogous to a previously prepared [A(Benzo15C5)HIM][PF6]-based fiber. Their thermal stabilities were much higher than that of the [A(Benzo15C5)HIM][PF6]-based coating. They were capable of withstanding temperatures as high as 400°C without evident loss of the crown ether FILs. They also had strong solvent, acid and alkali resistance, good coating preparation reproducibility and high selectivity for medium polar to polar compounds. The high selectivity of these two fibers could be attributed to the strong ion-dipole, hydrogen bonding and π-π interactions provided by the synergetic effect of ILs and benzo-15-crown-5 functionalities. Moreover, the selectivity of these two fibers was rather different although the structures of these two crown ether FILs were very similar. This is maybe because the relative contents of the crown ether FILs chemically bonded to the organic-inorganic copolymer coatings were quite different when prepared by different sol-gel reaction approaches.

  2. Lithium ceramics: sol-gel preparation and tritium release; Ceramiques lithiees: elaboration sol-gel et relachement du tritium

    Renoult, O.


    Ceramics based on lithium aluminate (LiA1O{sub 2}), lithium zirconate (Li{sub 2}ZrO{sub 3}) and lithium titanate (Li{sub 2}TiO{sub 3}) are candidates as tritium breeder blanket materials for forthcoming nuclear fusion reactors. Lithium silico-aluminate Li{sub 4+x}A1{sub 4-3x}Si{sub 2x}O{sub 8} (0 {<=} x {<=} 0,25) powders were synthetized from alkoxyde-hydroxyde sol-gel route. By direct sintering at 850-1100 deg C (without prior calcination), ceramics with controlled stoichiometry and homogenous microstructure were obtained. We have also prepared, using a comparable method, Li{sub 2}Zr{sub 1-x}Ti{sub x}O{sub 3} (x = 0, x = 0,1 et x = 1) materials. All these ceramics, with different microstructures and compositions, have been tested in out-of-reactor experiments. Concerning lithium aluminate microporous ceramics, the silicon substitution leads to a significant improvement of the tritrium release. Classical models taking into account independent surface mechanisms are not able to describe correctly the observed tritium release kinetics. We show, using a simple model, that the release kinetics is in fact limited by an intergranular diffusion followed by a desorption. The delay in tritium release, which occurs when the ceramic compacity increases, is explained in terms of an enhancement of the ionic T{sup +} diffusion path length. The energy required for desorption includes a leading term independent of hydrogen contained in the sweep gas. This term is attributed to the limiting recombination step of T{sup +} in molecular species HTO. For similar microstructures, the facility of tritium release for the different studied materials is explained by three properties: the crystal structure of the ceramic, the acidity of oxides and finally the presence of electronic non-stoichiometric defects. (author). 89 refs., 50 figs., 2 tabs., 1 annexe.

  3. Entrapment of subtilisin in ceramic sol-gel coating for antifouling applications.

    Regina, Viduthalai Rasheedkhan; Søhoel, Helmer; Lokanathan, Arcot Raghupathi; Bischoff, Claus; Kingshott, Peter; Revsbech, Niels Peter; Meyer, Rikke Louise


    Enzymes with antifouling properties are of great interest in developing nontoxic antifouling coatings. A bottleneck in developing enzyme-based antifouling coatings is to immobilize the enzyme in a suitable coating matrix without compromising its activity and stability. Entrapment of enzymes in ceramics using the sol-gel method is known to have several advantages over other immobilization methods. The sol-gel method can be used to make robust coatings, and the aim of this study was to explore if sol-gel technology can be used to develop robust coatings harboring active enzymes for antifouling applications. We successfully entrapped a protease, subtilisin (Savinase, Novozymes), in a ceramic coating using a sol-gel method. The sol-gel formulation, when coated on a stainless steel surface, adhered strongly and cured at room temperature in less than 8 h. The resultant coating was smoother and less hydrophobic than stainless steel. Changes in the coating's surface structure, thickness and chemistry indicate that the coating undergoes gradual erosion in aqueous medium, which results in release of subtilisin. Subtilisin activity in the coating increased initially, and then gradually decreased. After 9 months, 13% of the initial enzyme activity remained. Compared to stainless steel, the sol-gel-coated surfaces with active subtilisin were able to reduce bacterial attachment of both Gram positive and Gram negative bacteria by 2 orders of magnitude. Together, our results demonstrate that the sol-gel method is a promising coating technology for entrapping active enzymes, presenting an interesting avenue for enzyme-based antifouling solutions.

  4. Infrared Thermochromic Properties of VO2 Thin Films Prepared through Aqueous Sol-gel Process

    LIU Dongqing; CHENG Haifeng; ZHENG Wenwei; ZHANG Chaoyang


    The stoichiometric vanadium(Ⅳ) oxide thin films were obtained by controlling the temperature,time and pressure of annealing.The thermochromic phase transition and the IR thermochromic property of 400 nm and 900 nm VO2 thin films in the 7.5 μm-14 μm region were discussed.The derived VO2 thin film samples were characterized by Raman,XRD,XPS,AFM,SEM,and DSC.The resistance and infrared emissivity of VO2 thin films under different temperature were measured,and the thermal images of films were obtained using infrared imager.The results show that the VO2 thin film annealed at 550 ℃ for 10 hours through aqueous sol-gel process is pure and uniform.The 900 nm VO2 thin film exhibits better IR thermochromic property than the 400 nm VO2 thin film.The resistance of 900 nm VO2 film can change by 4orders of magnitude and the emissivity can change by 0.6 during the phase transition,suggesting the outstanding IR thermochromic property.The derived VO2 thin film can control its infrared radiation intensity and lower its apparent temperature actively when the real temperature increases,which may be applied in the field of energy saving,thermal control and camouflage.

  5. Preparation and applications of hybrid organic-inorganic monoliths: a review.

    Zhu, Tao; Row, Kyung Ho


    This review presents an overview of the properties of hybrid organic-inorganic monolithic materials and summarizes the recent developments in the preparation and applications of these hybrid monolithic materials. Hybrid monolithic materials with porosities, surface functionalities, and fast dynamic transport have developed rapidly, and have been used in a wide range of applications owing to the low cost, good stability, and excellent performance. Basically, these materials can be divided into two major types according to the chemical composition: hybrid silica-based monolith (HSM) and hybrid polymer-based monolith (HPM). Compared to the HPM, HSM monolith has been attracting most wide attentions, and it is commonly synthesized by the sol-gel process. The conventional preparation procedures of two type's hybrid organic-inorganic monoliths are addressed. Applications of hybrid organic-inorganic monoliths in optical devices, capillary microextraction (CME), capillary electrochromatography (CEC), high performance liquid chromatography (HPLC), and chiral separation are also reviewed. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Diamond nanoparticles as a way to improve electron transfer in sol-gel L-lactate biosensing platforms.

    Briones, M; Casero, E; Vázquez, L; Pariente, F; Lorenzo, E; Petit-Domínguez, M D


    In the present work, we have included for the first time diamond nanoparticles (DNPs) in a sol-gel matrix derived from (3-mercaptopropyl)-trimethoxysilane (MPTS) in order to improve electron transfer in a lactate oxidase (LOx) based electrochemical biosensing platform. Firstly, an exhaustive AFM study, including topographical, surface potential (KFM) and capacitance gradient (CG) measurements, of each step involved in the biosensing platform development was performed. The platform is based on gold electrodes (Au) modified with the sol-gel matrix (Au/MPTS) in which diamond nanoparticles (Au/MPTS/DNPs) and lactate oxidase (Au/MPTS/DNPs/LOx) have been included. For the sake of comparison, we have also characterized a gold electrode directly modified with DNPs (Au/DNPs). Secondly, the electrochemical behavior of a redox mediator (hydroxymethyl-ferrocene, HMF) was evaluated at the platforms mentioned above. The response of Au/MPTS/DNPs/LOx towards lactate was obtained. A linear concentration range from 0.053 mM to 1.6 mM, a sensitivity of 2.6 μA mM(-1) and a detection limit of 16 μM were obtained. These analytical properties are comparable to other biosensors, presenting also as advantages that DNPs are inexpensive, environment-friendly and easy-handled nanomaterials. Finally, the developed biosensor was applied for lactate determination in wine samples.

  7. Review and the state of the art: Sol-gel and melt quenched bioactive glasses for tissue engineering.

    Kaur, Gurbinder; Pickrell, Gary; Sriranganathan, Nammalwar; Kumar, Vishal; Homa, Daniel


    Biomaterial development is currently the most active research area in the field of biomedical engineering. The bioglasses possess immense potential for being the ideal biomaterials due to their high adaptiveness to the biological environment as well as tunable properties. Bioglasses like 45S5 has shown great clinical success over the past 10 years. The bioglasses like 45S5 were prepared using melt-quenching techniques but recently porous bioactive glasses have been derived through sol-gel process. The synthesis route exhibits marked effect on the specific surface area, as well as degradability of the material. This article is an attempt to provide state of the art of the sol-gel and melt quenched bioactive bioglasses for tissue regeneration. Fabrication routes for bioglasses suitable for bone tissue engineering are highlighted and the effect of these fabrication techniques on the porosity, pore-volume, mechanical properties, cytocompatibilty and especially apatite layer formation on the surface of bioglasses is analyzed in detail. Drug delivery capability of bioglasses is addressed shortly along with the bioactivity of mesoporous glasses. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 1248-1275, 2016.

  8. Inverted organic solar cells with sol-gel processed high work-function vanadium oxide hole-extraction layers

    Zilberberg, Kirill; Trost, Sara; Riedl, Thomas [Institute of Electronic Devices, University of Wuppertal, Rainer-Gruenter-Str. 21, 42119 Wuppertal (Germany); Meyer, Jens; Kahn, Antoine [Department of Electrical Engineering, Princeton University, Princeton, NJ (United States); Behrendt, Andreas; Luetzenkirchen-Hecht, Dirk; Frahm, Ronald [Physics of Condensed Matter, University of Wuppertal (Germany)


    For large-scale and high-throughput production of organic solar cells (OSCs), liquid processing of the functional layers is desired. We demonstrate inverted bulk-heterojunction organic solar cells (OSCs) with a sol-gel derived V{sub 2}O{sub 5} hole-extraction-layer on top of the active organic layer. The V{sub 2}O{sub 5} layers are prepared in ambient air using Vanadium(V)-oxitriisopropoxide as precursor. Without any post-annealing or plasma treatment, a high work function of the V{sub 2}O{sub 5} layers is confirmed by both Kelvin probe analysis and ultraviolet photoelectron spectroscopy (UPS). Using UPS and inverse photoelectron spectroscopy (IPES), we show that the electronic structure of the solution processed V{sub 2}O{sub 5} layers is similar to that of thermally evaporated V{sub 2}O{sub 5} layers which have been exposed to ambient air. Optimization of the sol gel process leads to inverted OSCs with solution based V{sub 2}O{sub 5} layers that show power conversion efficiencies similar to that of control devices with V{sub 2}O{sub 5} layers prepared in high-vacuum. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Asymmetric bioreduction of acetophenones by Baker's yeast and its cell-free extract encapsulated in sol-gel silica materials

    Kato, Katsuya; Nakamura, Hitomi; Nakanishi, Kazuma


    Baker's yeast (BY) encapsulated in silica materials was synthesized using a yeast cell suspension and its cell-free extract during a sol-gel reaction of tetramethoxysilane with nitric acid as a catalyst. The synthesized samples were fully characterized using various methods, such as scanning electron microscopy, nitrogen adsorption-desorption, Fourier transform infrared spectroscopy, thermogravimetry, and differential thermal analysis. The BY cells were easily encapsulated inside silica-gel networks, and the ratio of the cells in the silica gel was approximately 75 wt%, which indicated that a large volume of BY was trapped with a small amount of silica. The enzyme activity (asymmetric reduction of prochiral ketones) of BY and its cell-free extract encapsulated in silica gel was investigated in detail. The activities and enantioselectivities of free and encapsulated BY were similar to those of acetophenone and its fluorine derivatives, which indicated that the conformation structure of BY enzymes inside silica-gel networks did not change. In addition, the encapsulated BY exhibited considerably better solvent (methanol) stability and recyclability compared to free BY solution. We expect that the development of BY encapsulated in sol-gel silica materials will significantly impact the industrial-scale advancement of high-efficiency and low-cost biocatalysts for the synthesis of valuable chiral alcohols.

  10. Surface modification of stainless steel orthopedic implants by sol-gel ZrTiO4 and ZrTiO4-PMMA coatings.

    Salahinejad, E; Hadianfard, M J; Macdonald, D D; Sharifi Asl, S; Mozafari, M; Walker, K J; Rad, A Tahmasbi; Madihally, S V; Vashaee, D; Tayebi, L


    In this paper, the biocompatibility of a medical-grade stainless steel coated with sol-gel derived, nanostructured inorganic ZrTiO4 and hybrid ZrTiO4-PMMA thin films is correlated with surface characteristics. The surfaces of the samples are characterized by atomic force microscopy, the sessile drop technique, and electrochemical corrosion experiments. The viability of adult human mesenchymal stem cells on the surfaces after one day of culture is also assessed quantitatively and morphologically. According to the results, both of the coatings improve the hydrophilicity, corrosion resistance, and thereby cytocompatibility of the substrate. Despite the higher corrosion protection by the hybrid coating, the sample coated with the inorganic thin film exhibits a better cell response, suggesting the domination of wettability. In summary, the ZrTiO4-based sol-gel films can be considered to improve the biocompatibility of metallic implants.

  11. Preparation of new Calix[4]arene-immobilized biopolymers for enhancing catalytic properties of Candida rugosa lipase by sol-gel encapsulation.

    Ozyilmaz, Elif; Sayin, Serkan


    The article describes preparation of new calixarene biopolymers consisting of the immobilization of convenience calixarene derivative onto cellulose and chitosan biopolymers, and the encapsulation of these calixarene biopolymers with Candida rugosa lipase within a chemical inert sol-gel supported by polycondensation with tetraethoxysilane and octyltriethoxysilane. The catalytic properties of immobilized lipase were evaluated into model reactions employing the hydrolysis of p-nitrophenylpalmitate and the enantioselective hydrolysis of naproxen methyl esters from racemic prodrugs in aqueous buffer solution/isooctane reaction system. The resolution studies using sol-gel support have observed more improvement in the enantioselectivity of naproxen E = 300 with Cel-Calix-E than with encapsulated lipase without calixarene-based materials. Furthermore, the encapsulated lipase (Cel-Calix-E) was still retained about 39 % of their conversion ratios after the fifth reuse in the enantioselective reaction.

  12. FeS2@C nanowires derived from organic-inorganic hybrid nanowires for high-rate and long-life lithium-ion batteries

    Zhang, Feifei; Wang, Chunli; Huang, Gang; Yin, Dongming; Wang, Limin


    One-dimensional (1D) porous FeS2@C nanowires as a high cathode material for lithium-ion batteries (LIBs) are synthesized on a large-scale from an organic-inorganic hybrid nanowire precursor. The FeS2@C nanowires not only provide a continuous and fast electron transport pathway, favorable diffusion kinetics, but also provide the protection buffer the volume expansion and effectively prevent the polysulfides from dissolving in the electrolyte during cycling. Attributing to the synergistic advantages of both 1D porous nanostructure and the encapsulation of thin amorphous carbon layers, the FeS2@C nanowires exhibit remarkable lithium storage performance with a high specific capacity of 889 mA h g-1 at 0.1 A g-1 and 521 mA h g-1 at 10 A g-1. Moreover, a discharge energy density of 1225 Wh kg-1 is obtained at 2 A g-1 and remains as high as 637 Wh kg-1 after 1000 cycles, which is even higher than the LiCoO2 cathode. The results demonstrate that the potential for applications in LIBs with high power density and long cycling life.

  13. Synthesis of partial-stabilized cement (PSC) via sol-gel process.

    Wang, Wen-Hsi; Lee, Yuan-Ling; Lin, Chun-Pin; Lin, Feng-Huei


    The traditional method of preparing partial-stabilized cement (PSC), which is a kind of calcium silicate cement, is through power mixing method. Low reaction efficiency and initial strength limited the application of PSC as a dental root-end filling material. This study provides a one-step sol-gel process for the synthesis of PSC. A complexing ligand is used for tuning down the activity of aluminum sec-butoxide (ASB) in order to avoid possible self-polymerization. After the modification with complex ligand, there is no residue of reactant observed on the analysis of SDT, and bonding between metal atoms is observed in the FTIR spectrum. Each component of PSC is identified using XRD. The hydration product, which is called portlandite, of sol-gel-synthesized PSC is observed after 1 day of hydration, and crystallinity of portlandite increases much faster than that of traditional PSC. The initial strength of sol-gel-synthesized PSC achieves detectable level 24 h earlier than that of traditional PSC; microhardness value of sol-gel-synthesized PSC at 7th day is 2.98 HV, which is much higher than that of traditional PSC (2.05 HV). PSC is successfully synthesized and the initial strength of PSC is improved by this modified sol-gel process.

  14. Wear characteristics of second-phase-reinforced sol-gel corundum abrasives

    Mayer, Joachim [Central Facility for Electron Microscopy (GFE), RWTH Aachen University, 52056 Aachen (Germany)]. E-mail:; Engelhorn, Robert [Laboratory for Machine Tools and Production Engineering (WZL), RWTH Aachen University, 52056 Aachen (Germany); Bot, Rosemarie [Laboratory for Machine Tools and Production Engineering (WZL), RWTH Aachen University, 52056 Aachen (Germany); Weirich, Thomas [Central Facility for Electron Microscopy (GFE), RWTH Aachen University, 52056 Aachen (Germany); Herwartz, Cleo [Central Facility for Electron Microscopy (GFE), RWTH Aachen University, 52056 Aachen (Germany); Klocke, Fritz [Laboratory for Machine Tools and Production Engineering (WZL), RWTH Aachen University, 52056 Aachen (Germany)


    The use of sol-gel technologies makes it possible to manufacture new corundum-based abrasives with superior performance in terms of grinding processes. The aim of the present work is to reveal the detailed wear mechanisms on a nanometre scale and relate them to the particular microstructure of these new materials. A commercial sol-gel corundum (Cubitron 321{sup TM}) was used. In the grinding experiments, wheels consisting of four different mixtures with 0%, 30%, 50% and 100% of sol-gel corundum were used to machine a tool steel (100Cr6V) by plane grinding. Changes to the contact zone were studied after controlled abrasion experiments on hard steel substrates using a pin-on-wheel tribometer, in single grit scratch tests and after tests of resistance to heat shock. Cross-sections through contact areas of a sol-gel grain were prepared using a focused ion beam workstation and investigated using conventional and analytical transmission electron microscopy. The results indicate that the combined effect of controlled propagation of subsurface shear cracks and plastic deformation leads to the formation of flat contact zones. On these contact zones, a nanocrystalline FeO debris layer adheres to the alumina. The results of our investigations were verified in grinding experiments and give insight into the physical reasons of the superior tribological properties of the sol-gel corundum abrasives.

  15. Carbon nanotube-coated solid-phase microextraction metal fiber based on sol-gel technique.

    Jiang, Ruifen; Zhu, Fang; Luan, Tiangang; Tong, Yexiang; Liu, Hong; Ouyang, Gangfeng; Pawliszyn, Janusz


    A novel carbon nanotube (CNT)-coated solid-phase microextraction fiber was prepared based on sol-gel technique. Commonly used fragile fused silica fiber was replaced with stainless steel wire, which made the fiber unbreakable. An approach was also proposed for batch producing, and good reproducibilities for fiber to fiber and between fibers were achieved. Experiments showed that the sol-gel-CNT fiber exhibited high thermal stability to resist 350 degrees C and excellent solvent durability in methanol and acetonitrile. Compared to commercial polydimethylsiloxane (PDMS) fiber, the sol-gel-CNT fiber represented significantly improved extraction efficiencies for both polar (phenols) and non-polar (benzene, toluene, ethylbenzene, and o-xylene) compounds. Meanwhile, no replacement effect, low carry-over and wide linear range demonstrated that the newly prepared sol-gel-CNT coating has liquid properties, which allow a relatively easy quantification procedure. Moreover, the characterization of the sol-gel-CNT coating was also evaluated with McReynold probe solutes. The results showed that the coating has better affinity for all the five types of solutes compared to commercial 7microm PDMS fiber, which suggested that the coating has the potential to be developed as GC stationary phase.

  16. Optical Characterization of Chemically Etched Nanoporous Silicon Embedded in Sol-Gel Matrix

    A. S. Al Dwayyan


    Full Text Available Nanoporous (NPs silicon fabricated by chemical etching process in HF acid was first separated in tetrahydrofuran (THF solvent and then incorporated into SiO2 matrix. The matrix was prepared by sol gel process in which dimethylformamide (DMF was used as drying chemical control additive (DCCA to form crack-free dried sample. We examined the optical properties of NPs in three medium which are solvent, sol, and dried sol gel. Our observations reveal that absorption spectra of NPs silicon in THF are modified with respect to the spectra in sol gel. Significant stability in PL of NPs silicon in the sol gel is observed. Influence of matrix environment on peaks of NPs is also discussed. Surface morphology is characterized by field emission scanning electron microscopy (FESEM which shows that the NPs silicon in THF is similar to the sol gel but becomes aggregation particle to particle. Presence of Si nanoparticles in THF and sol is confirmed by Transmission electron microscopy (TEM. The NPs silicons have mono dispersive and high crystalline nature with spherical shape of around 5 nm in sizes.

  17. Preparation and rapid analysis of antibacterial silver, copper and zinc doped sol-gel surfaces.

    Jaiswal, Swarna; McHale, Patrick; Duffy, Brendan


    The colonisation of clinical and industrial surfaces with microorganisms, including antibiotic-resistant strains, has promoted increased research into the development of effective antibacterial and antifouling coatings. This study describes the preparation of metal nitrate (Ag, Cu, Zn) doped methyltriethoxysilane (MTEOS) coatings and the rapid assessment of their antibacterial activity using polyproylene microtitre plates. Microtitre plate wells were coated with different volumes of liquid sol-gel and cured under various conditions. Curing parameters were analysed by thermogravimetric analysis (TGA) and visual examination. The optimum curing conditions were determined to be 50-70°C using a volume of 200 μl. The coated wells were challenged with Gram-positive and Gram-negative bacterial cultures, including biofilm-forming and antibiotic-resistant strains. The antibacterial activities of the metal doped sol-gel, at equivalent concentrations, were found to have the following order: silver>zinc>copper. The order is due to several factors, including the increased presence of silver nanoparticles at the sol-gel coating surface, as determined by X-ray photoelectron spectroscopy, leading to higher elution rates as measured by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The use of microtitre plates enabled a variety of sol-gel coatings to be screened for their antibacterial activity against a wide range of bacteria in a relatively short time. The broad-spectrum antibacterial activity of the silver doped sol-gel showed its potential for use as a coating for biomaterials.

  18. Mechanical compatibility of sol-gel annealing with titanium for orthopaedic prostheses.

    Greer, Andrew I M; Lim, Teoh S; Brydone, Alistair S; Gadegaard, Nikolaj


    Sol-gel processing is an attractive method for large-scale surface coating due to its facile and inexpensive preparation, even with the inclusion of precision nanotopographies. These are desirable traits for metal orthopaedic prostheses where ceramic coatings are known to be osteoinductive and the effects may be amplified through nanotexturing. However there are a few concerns associated with the application of sol-gel technology to orthopaedics. Primarily, the annealing stage required to transform the sol-gel into a ceramic may compromise the physical integrity of the underlying metal. Secondly, loose particles on medical implants can be carcinogenic and cause inflammation so the coating needs to be strongly bonded to the implant. These concerns are addressed in this paper. Titanium, the dominant material for orthopaedics at present, is examined before and after sol-gel processing for changes in hardness and flexural modulus. Wear resistance, bending and pull tests are also performed to evaluate the ceramic coating. The findings suggest that sol-gel coatings will be compatible with titanium implants for an optimum temperature of 500 °C.

  19. Efficacy of a new tan doped sol-gel sorbent for uptake of zinc

    Khan, A.; Ahmed, S.; Riaz, M. [Nuclear Chemistry Div., Pakistan Inst. of Nuclear Science and Technology, Islamabad (Pakistan); Mahmood, F.; Younas Khokhar, M. [Dept. of Chemistry, Bahauddin Zakariya Univ., Multan (Pakistan)


    A TAN (1-(2-Thiazolylazo)-2-naphthol) doped sol gel silica sorbent (reddish colour, porous, stable, hard, non-swelling) were prepared and investigated for the removal of Zn (II) from aqueous solutions. The kinetics, adsorption isotherm, equilibration time and pH effect on the removal were studied from non competitive aqueous solution to optimize the conditions to be utilized on a large scale. Fast equilibration was observed and adsorption equilibria were reached within 30 minutes. Adsorption of zinc ions on the blank (un-doped) sol gel was found negligible. The maximum adsorption of Zn (II) ions onto the TAN doped sol-gel from single solutions were 2.33 mg/g (0.035 mmol/g). TAN doped sol gel can be regenerated through washing with a solution of 0.1 M HCl solution. The maximum regeneration value was as high as 99.0%. The TAN-doped sol gel silica is suitable at least for four adsorption-desorption cycles without experiencing considerable loss of adsorption capacity. The uptake route and the nature of the Zn-TAN complex have been discussed. (orig.)

  20. Vibrational spectroscopic studies of triethoxy(4-(trifluoromethyl)-phenyl) silane and its sol-gel coating.

    Li, Ying-Sing


    We have prepared a silica sol-gel using triethoxy (4-(trifluoromethyl)-phenyl) silane (TETFMPS) as a precursor in ethanol solution under acidic condition. The prepared sol-gel was applied to the surface treatment of aluminum for corrosion prevention. Infrared and Raman spectra of the silane coupling agent, sol-gel and sol-gel films on metal have been collected. Infrared spectroscopy has been used to study the thermal effect on the chemical composition of xerogel. Results suggested that TETFMPS molecule has a C(s) point group symmetry with the plane of reflection orthogonal to the phenyl ring and the organic part of the sol-gel film remains essentially unchanged at or below 450 °C but decomposes at or above 550 °C. After the decomposition of the organic branch, the remaining film is composed of silica. Vibrational assignments were suggested by using the collected spectroscopic data in different states along with the group vibrational frequencies and other related references.

  1. Optical sensing of HCl with phenol red doped sol-gels

    Wang Enju [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States)]. E-mail:; Chow, Kwok-Fan [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Wang Wenqun [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Wong, Crystal [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Yee, Cynthia [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Persad, Alvin [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Mann, Jonathan [Department of Chemistry, Princeton University, Princeton, NJ 08540 (United States); Bocarsly, Andrew [Department of Chemistry, Princeton University, Princeton, NJ 08540 (United States)


    A dye doped sol-gel for the sensing of hydrochloric acid in solution and/or gaseous phase is described. The sol-gel is obtained by acidic hydrolysis of tetraethoxysilane (TEOS) and phenyltriethoxysilane (Ph-TriEOS) in the presence of phenol red (PR) and further spin-coating onto glass slides. The sensitive response is based on an increase of the absorption band at 510 nm of phenol red entrapped in the sol-gel casting when exposed to HCl solution or gas, due to protonation of the dye. The detection limit of the sol-gel response to moisturized gaseous HCl is below 12 ppm, and its response to HCl in solution falls in the range of 0.01-6 M. The sol-gel coating has a response time of less than 40 s in steady-state, and life-time of more than a year. Weak acids such as acetic acid, benzoic acid, salicylate acid, citrate acid, and carbonic acid do not interfere the response. The responses in acid solutions are completely reversible. In the gaseous phase, response of HCl appears to be moisture sensitive.

  2. Preparation and optical characteristics of ZnO films by chelating sol-gel method

    YANG Lirong; JIN Zhengguo; BU Shaojing; SUN Yingchun; CHENG Zhijie


    The effect of different annealing temperatures on the structure, morphology, and optical properties of ZnO thin films prepared by the chelating sol-gel method was investigated. Zinc-oxide thin films were coated on quartz glass substrates by dip coating. Zinc nitrate, absolute ethanol, and citric acid were used as precursor, solvent, and chelating agent, respectively. The results show that ZnO films derived from zinc-citrate have lower crystallization temperature (below 400°C),and that the crystal structure is wurtzite. The films, treated over 500°C, consist of nano-particles and show to be porous at 600°C. The particle size of the film increases with the increase of the annealing temperature. The largest particle size is 60 nm at 600°C. The optical transmittances related to the annealing temperatures become 90% higher in the visible range. The film shows a starting absorption at 380 nm, and the optical band-gap of the thin film (fired at 500°C) is 3.25 eV and close to the intrinsic band-gap of ZnO (3.2 eV).

  3. Bioactive sol-gel glass added ionomer cement for the regeneration of tooth structure.

    Choi, Jung-Young; Lee, Hae-Hyoung; Kim, Hae-Won


    Dental cements including the glass ionomer cement (GIC) have found widespread use in restoring tooth structures. In this study, a sol-gel derived glass (SG) with a bioactive composition (70SiO(2).25CaO.5P(2)O(5)) was added to the commercial GIC (GC, Fuji I) to improve the bioactivity and tooth regeneration capability. The SG powders prepared with sizes in the range of a few micrometers were mixed with GIC at SG/GC ratios of 10 and 30 wt%. The setting time, diametral tensile strength, and in vitro bioactivity of the GC-SG cements were examined. The setting time of the GC-SG cements increased with increasing amount of SG. However, the addition of SG did not significantly alter the diametral tensile strength of the GC. GC-SG induced the precipitation of an apatite bone-mineral phase on the surface after immersion in a simulated body fluid (SBF), showing in vitro bone bioactivity. However, no mineral induction in SBF was observed in the commercial GIC after the immersion. The in vitro cell assay confirmed that the GC-SG samples produced higher cell viability than the GC sample with cell culturing for up to 7 days.

  4. Proton Conduction in Sulfonated Organic-Inorganic Hybrid Monoliths with Hierarchical Pore Structure.

    von der Lehr, Martin; Seidler, Christopher F; Taffa, Dereje H; Wark, Michael; Smarsly, Bernd M; Marschall, Roland


    Porous organic-inorganic hybrid monoliths with hierarchical porosity exhibiting macro- and mesopores are prepared via sol-gel process under variation of the mesopore size. Organic moieties in the pore walls are incorporated by substituting up to 10% of the silicon precursor tetramethylorthosilicate with bisilylated benzene molecules. After functionalization with sulfonic acid groups, the resulting sulfonated hybrid monoliths featuring a bimodal pore structure are investigated regarding proton conduction depending on temperature and relative humidity. The hierarchical pore system and controlled mesopore design turn out to be crucial for sulfonation and proton conduction. These sulfonated hybrid hierarchical monoliths containing only 10% organic precursor exhibit higher proton conduction at different relative humidities than sulfonated periodic mesoporous organosilica made of 100% bisilylated precursors exhibiting solely mesopores, even with a lower concentration of sulfonic acid groups.

  5. Organic/inorganic hybrid materials formed from TiO2 nanoparticles and polyaniline

    Schnitzler Danielle C.


    Full Text Available This paper describes the synthesis and characterization of organic/inorganic hybrid materials formed from TiO2 nanoparticles and polyaniline (PANI. The preparation method is based on a sol-gel technique using titanium tetra-isopropoxide as oxide precursor, and two synthetic routes to the hybrids formation were employed, based on the addition of aniline after or before the sol formation. Different amounts of aniline were used to verify this effect on the characteristics of the formed materials. Samples were characterized by electronic spectroscopy, Raman spectroscopy, Fourier transformed infrared spectroscopy, thermal analysis, X-ray diffractometry and cyclic voltammetry. Results show that the different experimental routes are successful to produce hybrids formed by oxides nanoparticles and polyaniline in its conducting form, the emeraldine salt. There are no strong differences between the samples obtained by the two synthetic routes employed, except by the amount of polymer in the final material.

  6. Organic-inorganic hybrid protonic polymeric electrolytes grafted by sulfonic acid/sulfonamide moieties

    Depre, L.; Poinsignon, C.; Popall, M.


    Thin proton conducting membranes of an organic-inorganic polymer electrolyte bearing sulphonamide and sulfonic groups are prepared by sol-gel process. Polycondensation of alkoxysilanes provides the inorganic silicate backbone whereas the organic network is formed from reactive functional groups R{prime}(({minus}DH{sub 2}){sub 3}-SO{sub 3}H) and [({minus}CH{sub 2}){sub 3}-SO{sub 2}NH{sub 2}] of alkoxysilanes of R{prime}Si[OR{sub 3}] type. Proton conductivity measured in the dry and wet state under controlled Temperature and Relative Humidity increases from 10{sup {minus}4} S/cm under vacuum to 6 10{sup {minus}2} S/cm at 70 C and 96% RH. Conductivity dependence on temperature and associated conduction mechanisms are discussed in both states.

  7. Preparation and characterization of bismuth ruthenate pyrochlore via solid state reaction and sol-gel methods

    Mayuree Sansernnivet


    Full Text Available Bismuth ruthenate pyrochlores, potential cathode materials for intermediate temperature solid oxide fuel cells(ITSOFCs, were prepared via solid-state and sol-gel method. Effects of the preparation routes and conditions on the phase and microstructures of the materials were investigated in this study using XRD and SEM. The study showed that the preparation method and the adding sequence of the starting meterials have a significant effect on the crystal phase and the particle size obtained. Sol-gel synthesis could yield a material with only pyrochlore structure, i.e. Bi2Ru2O7, while the solid state method yielded powder with a small amount of the secondary RuO2 phase. The sol-gel synthesis resulted in materialswith a finer particle size (~0.3-1.0 μm compared to powder synthesized via the solid state reaction method.

  8. Zinc oxide films prepared by sol-gel spin coating technique

    Kamaruddin, Sharul Ashikin; Chan, Kah-Yoong; Yow, Ho-Kwang [Multimedia University, Faculty of Engineering, Cyberjaya, Selangor (Malaysia); Zainizan Sahdan, Mohd; Saim, Hashim [Universiti Tun Hussein Onn Malaysia, Faculty of Electrical and Electronics Engineering, Batu Pahat, Johor (Malaysia); Knipp, Dietmar [Jacobs University Bremen, School of Engineering and Science, Bremen (Germany)


    Zinc oxide (ZnO) thin films and micro- and nanostructures are very promising candidates for novel applications in emerging thin-film transistors, solar cells, sensors and optoelectronic devices. In this paper, a low-cost sol-gel spin coating technique was used to fabricate ZnO films on glass substrates. The sol-gel fabrication process of the ZnO films is described. The influence of precursor concentration on the material properties of the ZnO films was investigated. Atomic force microscopy and X-ray diffractometry were employed to examine the structural properties of the ZnO films. The optical properties of the ZnO films were characterized with ultraviolet-visible spectroscopy. The experimental results reveal that the precursor concentration in the sol-gel spin coating process exerts a strong influence on the properties of the ZnO films. The effects of the precursor concentration are discussed. (orig.)

  9. Emission of Eu3+in sol-gel oxyfluoride glass materials obtained by different preparation methods

    M. Żądło; B. Szpikowska-Sroka; L. Żur; R. Czoik; W.A. Pisarski


    Silica glasses doped with Eu3+ions prepared by sol-gel methods were investigated. The X-ray diffraction (XRD) was used to verify the nature of the studied systems. Excitation and emission spectra of Eu3+ ions in sol-gel glass materials were detected. Red-to-orange luminescence intensity ratios R/O related to integrated intensities of 5D0→7F2 to 5D0→7F1 transitions and luminescence lifetimes for 5D0 state of Eu3+ions were determined. The results indicated that spectroscopic parameters for Eu3+ions strongly de-pended on reagents and their relative ratios used for sol-gel glass preparation.

  10. Characterization of Sr{beta}-alumina prepared by sol-gel and spray pyrolysis methods

    Kalaignan, G. Paruthimal; Seo, Dae Jong; Park, Seung Bin


    Eu{sup 2+} doped {beta}-alumina, Sr{sub 1-x}MgAl{sub 10}O{sub 17} Eu{sub x}{sup 2+} (x=0.01-0.07) were successfully prepared by sol-gel and spray pyrolysis techniques with the same precursor materials. Sr{beta}-alumina doped with Eu{sup 2+} (SrMgAl{sub 10}O{sub 17}:Eu{sup 2+}) prepared from sol-gel method showed three photoluminescence (PL) peaks at 390, 418 and 459 nm after excitation wavelength at 254 nm and one PL peak at 461 nm when excitation was at 365 nm. The same powder was prepared from spray pyrolysis technique showed the six PL peaks at 323, 397, 415, 443, 480 and 508 nm after excitation at 254 nm. Also two PL peaks at 440 and 480 nm were observed after the excitation at 365 nm. These PL peaks were dependent on the excitation wavelength. The effect of different annealing temperatures of sol-gel powders, preparation conditions of spray pyrolysis powders and reduction atmospheres of both sol-gel and spray pyrolysis powders of various compositions of Eu{sup 2+} doped Sr{beta}-alumina were also studied. Both the powders were characterized by scanning electron microscopy, X-ray diffraction and PL techniques and comparison between the two preparation methods. Sol-gel prepared powder had eight times higher PL intensity and brightness than the spray pyrolysis prepared powder. The suggested good composition of Sr{beta}-alumina is Sr{sub 0.93}MgAl{sub 10}O{sub 17}:Eu{sub 0.07} for both sol-gel and spay pyrolysis methods.

  11. Preparation of A New Fiber by Sol-gel Technology in Solid-phase Microextraction (SPME)

    Li Ming WEI; Qing Yu OU; Ju Bai LI


    The sol-gel technology is applied for the preparation of solid-phase microextraction (SPME) fiber. The fiber demonstrates high thermal stability, efficient extraction rate and the selectivity for non-polar or low-polar analytes. Efficient SPME-GC-FID analyses of benzene- toluene-ethylbenzene-xylenes (BTEXs) and low-polar halocarbon were achieved by the sol-gel coated DSDA-DDBT-TiO2 fiber. Some parameters of the SPME fiber for the determination of halocarbon in aqueous sample were investigated.

  12. Sol-gel process for the manufacture of high power switches

    Landingham, Richard L.; Satcher, Jr, Joe; Reibold, Robert


    According to one embodiment, a photoconductive semiconductor switch includes a structure of nanopowder of a high band gap material, where the nanopowder is optically transparent, and where the nanopowder has a physical characteristic of formation from a sol-gel process. According to another embodiment, a method includes mixing a sol-gel precursor compound, a hydroxy benzene and an aldehyde in a solvent thereby creating a mixture, causing the mixture to gel thereby forming a wet gel, drying the wet gel to form a nanopowder, and applying a thermal treatment to form a SiC nanopowder.

  13. Fundamental electrochemiluminescence characteristics of fluorine-doped tin oxides synthesized by sol-gel combustion.

    Moon, B H; Chaoumead, A; Sung, Y M


    Fluorine-doped tin oxide (FTO) materials synthesized by sol-gel combustion method were investigated for electrochemical luminescence (ECL) application. Effects of sol-gel combustion conditions on the structures and morphology of the porous FTO (p-FTO) materials were studied. ECL efficiency of p-FTO-based cell was about 251 cd/m2 at 4 V bias, which is higher than the sell using only FTO electrodes (102.8 cd/m2). The highest intensity of the emitting light was obtained at the wavelength of about 610 nm. The porous FTO layer was effective for increasing ECL intensities.

  14. Porous Silica Sol-Gel Glasses Containing Reactive V2O5 Groups

    Stiegman, Albert E.


    Porous silica sol-gel glasses into which reactive vanadium oxide functional groups incorporated exhibit number of unique characteristics. Because they bind molecules of some species both reversibly and selectively, useful as chemical sensors or indicators or as scrubbers to remove toxic or hazardous contaminants. Materials also oxidize methane gas photochemically: suggests they're useful as catalysts for conversion of methane to alcohol and for oxidation of hydrocarbons in general. By incorporating various amounts of other metals into silica sol-gel glasses, possible to synthesize new materials with broad range of new characteristics.

  15. Biocompatible Nb2O5 thin films prepared by means of the sol-gel process.

    Velten, D; Eisenbarth, E; Schanne, N; Breme, J


    Thin biocompatible oxide films with an optimised composition and structure on the surface of titanium and its alloys can improve the implant integration. The preparation of these thin oxide layers with the intended improvement of the surface properties can be realised by means of the sol-gel process. Nb2O5 is a promising coating material for this application because of its extremely high corrosion resistance and thermodynamic stability. In this study, thin Nb2O5 layers ( TiO2 sol-gel coated cp-titanium concerning the spreading of cells, collagen I synthesis and wettability.

  16. The Recent Uses of Sol-Gel Doped Catalysts in Fine Chemistry

    Mario Pagliaro; Rosaria Ciriminna


    @@ 1Introduction A variety of sol-gel entrapped catalysts is available on the chemical market due to the unique advantages offered by these highly porous oxides doped with transition metal catalyst, enzymes or even living cells[1].Catalytic sol-gel lipase immobilizates were rapidly commercialized by Fluka after their invention by Reetz and coworkers in 1995 and have now reached a 2nd generation level of performance[2]. Besides esterification reactions these materials are also excellent catalysts in the kinetic resolution of chiral alcohols and amines, and are recyclable without any substantial loss in enantioselectivity (residual activity of 70% even after 20 reaction cycles).

  17. Double component long period waveguide grating filter in sol-gel material.

    Moujoud, Abderrafia; Kim, Hyun Jae; Kang, Sung Ho; Oh, Gyong-Jin; Kim, Woo-Soo; Bae, Byeong-Soo; Shin, Sang-Yung


    An efficient, tunable Long Period Waveguide Grating (LPWG) filter based on a new hybrid sol-gel material is demonstrated. The LPWG exhibits an attenuation of -22 dB and a high temperature sensitivity of ~3.3 nm/ degrees C. At room temperature the device shows an almost polarization independent wavelength. We took the advantage of the UV-curable sol-gel materials and used soft lithography to demonstrate a simple approach of integrating two LPWG filters on the same structure. The gratings were fabricated on the top and on the bottom of the same ridge waveguide and operate at communication wavelengths of 1550 and 1310 nm, respectively.

  18. Sol-gel fabrication and optical absorption properties of C-NiO nanocomposite coatings

    Tile, N


    Full Text Available of the sunlight as possible, then prevent thermal emittance The manufacturing process for most commercial thermal products is complicated C-NiO/Al has been fabricated using a simple and cheap sol-gel procedure combined with spin coating technique C... SOLUTION) Structure directing templateFinal C-NiO gel By suitable choice of precursor, we can engineer novel composite materials Sol-gel technique can be adapted to different coating methods coating substrate Spray coating Spin coating The material...

  19. Comparison of Characteristics of Sol-Gel and Precipitation Synthesis of Nanosized ZnO Powders

    Xiaoping Liang; Shaobo Xin; Xiaohui Wang; Yajin Liu


    Zinc oxide nanosized powders with different sizes and morphologies were obtained by the sol-gel method and the precipitation method, respectively. The effects of the sintering temperature on the characteristics of nanosized ZnO powders were discussed. ZnO particles were characterized by XRD and TEM. The results show that the powders prepared by both methods are of hexagon crystalline, and the average diameter of the particles prepared by the sol-gel method is smaller than that by the precipitation method.

  20. Microwave sintering of sol-gel composite films using a domestic microwave oven

    Kobayashi, Makiko; Matsumoto, Makoto


    Feasibility study of sol-gel composite microwave sintering using a domestic microwave oven was carried out. Two kinds of lead zirconate titanate (PZT) powders were mixed with PZT sol-gel solution and the mixture was sprayed onto 3-mm-thick titanium substrate. The films were sintered by 700 W domestic oven for 10 min. Ultrasonic measurement was carried out in pulse-echo mode and clear multiple echoes were confirmed. It would be suitable method to fabricate high frequency broadband focused ultrasonic transducers. Further research is required to improve sintering degree.