Sample records for sol-gel encapsulated metal

  1. 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.

  2. 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.

  3. 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…

  4. 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 ...

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. Direct electrochemistry and Raman spectroscopy of sol-gel-encapsulated myoglobin.

    Ray, Anandhi; Feng, Manliang; Tachikawa, Hiroyasu


    The direct electrochemistry of myoglobin (Mb) has been observed at a glassy carbon (GC) electrode coated with silica sol-gel-encapsulated Mb film. A well-behaved cyclic voltammogram is observed with a midpoint potential (E(1/2)) of -0.25 V vs Ag/AgCl in a pH 7.0 phosphate buffer. This potential, which is pH-dependent, is 70-90 mV more negative than the formal potential values obtained by using the spectroeletrochemical titration method at the same pH. Square wave voltametry (SWV) also shows a peak potential of -0.25 V for the reduction of Mb under the same experimental conditions. Both cathodic and anodic peak currents have a linear relationship with the scan rate. The midpoint potential decreases with pH, having a slope of -30 mV/pH. UV-vis and resonance Raman spectroscopic studies reveal that the sol-gel provides a bio-compatible environment where Mb retains a structure similar to its solution form, a 6-coordinated aquomet myoglobin. These results suggest that the silica sol-gel is a useful matrix for studying direct electrochemistry of other heme proteins.

  12. Phospholipid Fatty Acids as Physiological Indicators of Paracoccus denitrificans Encapsulated in Silica Sol-Gel Hydrogels

    Josef Trögl


    Full Text Available The phospholipid fatty acid (PLFA content was determined in samples of Paracoccus denitrificans encapsulated in silica hydrogel films prepared from prepolymerized tetramethoxysilane (TMOS. Immediately after encapsulation the total PLFA concentration was linearly proportional to the optical density (600 nm of the input microbial suspension (R2 = 0.99. After 7 days this relationship remained linear, but with significantly decreased slope, indicating a higher extinction of bacteria in suspensions of input concentration 108 cells/mL and higher. trans-Fatty acids, indicators of cytoplasmatic membrane disturbances, were below the detection limit. The cy/pre ratio (i.e., ratio of cyclopropylated fatty acids (cy17:0 + cy19:0 to their metabolic precursors (16:1ω7 + 18:1ω7, an indicator of the transition of the culture to a stationary growth-phase, decreased depending on co-immobilization of nutrients in the order phosphate buffer > mineral medium > Luria Broth rich medium. The ratio, too, was logarithmically proportional to cell concentration. These results confirm the applicability of total PLFA as an indicator for the determination of living biomass and cy/pre ratio for determination of nutrient limitation of microorganisms encapsulated in sol-gel matrices. This may be of interest for monitoring of sol-gel encapsulated bacteria proposed as optical recognition elements in biosensor construction, as well as other biotechnological applications.

  13. 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.

  14. Encapsulation of fluorescence vegetable extracts within a templated sol-gel matrix

    Lacatusu, Ioana; Badea, Nicoleta; Nita, Rodica; Murariu, Alina; Miculescu, Florin; Iosub, Ion; Meghea, Aurelia


    The sol-gel encapsulation of labile substances with specific properties and recognition functions within robust polymer matrices remains a challenging task, despite the considerable research that has been focused on this field. Numerous studies have been reported in the field of sol-gel processes regarding different physical and chemical packing of sensitive biomolecules encapsulated in silica matrix. In this paper the classical sol-gel synthesis has been used under mild conditions in order to minimize denaturizing effects on encapsulated active vegetable extracts from flavones class. The silica templated matrix was obtained by using two types of surfactants with different alkyl chain (didodecyldimethyl-ammonium bromide and trioctadecylmetilammonium bromide) as structure-directing agents for the silicon oxide framework. An organic precursor of silicic acid (triethoxymethylsilane) has been used and it was processed by competitive hydrolysis and polycondensation reactions under controlled directions assured by the presence of oriented template. Silica materials thus obtained are used for encapsulation of two flavonoid samples containing as active principles two sources: rutin and a vegetable extract from Begonia plant. The synthesis of encapsulated nanocompounds has been achieved taking into consideration the specific interaction between the colloidal gel precursors and molecular structures of selected biomolecules. The main objective was to improve the encapsulation conditions for specific biomolecules, searching for the highest stability and functionality without loosing the quality of the flavonoid properties, particularly optical properties like fluorescence. The structural properties of the encapsulated samples have been studied by FT-IR and UV-VIS spectroscopy, thermal analysis and SEM/EDX analysis. The fluorescence experiments showed that, in the case of all four encapsulated samples, the fluorescence spectra manifest a significant increase in intensity

  15. 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.

  16. Synthesis and luminescence properties of encapsulated sol-gel glass samarium complexes.

    Zaitoun, M A; Momani, K; Jaradat, Q; Qurashi, I M


    Luminescence efficiency of lanthanide complexes generally largely depend on the choice of the organic ligand and the host matrix in which these complexes are doped. Two Sm(III) complexes, namely: Sm(III) dithicarbamate - Sm(L1)3B [L1=(R)2NCS2B, R=C2H5 and B=1,10-phenanthroline] and Sm(III) complex with the polytonic ligand L2=N', N'(2)-bis[(1E)-1-(2-pyridyl)ethylidene]ethanedihydrazide {Sm2-L2-(CH3COO)2; L2=C16H16N6O2} are synthesized, these complexes are then trapped in sol-gel glass. Room temperature luminescence of Sm(L1)3B and {Sm2-L2-(CH3COO)2} complexes encapsulated in sol-gel glass are studied using a spectrofluorometer. Up on excitation by a UV light, ligand L1B absorbs this light and transfers it into the Sm(III) ions and emission bands were observed in the visible region and were attributed to f-f transitions of Sm(III). The observed emission indicated an efficient L1B ligand as a sensitizer, while ligand L2 shows no ability to work as a sensitizer. The branching ratio I4G5/2→6H9/2/I4G5/2→6H7/2) of electric dipole transition to magnetic dipole transition was used as an effective spectroscopic probe to predict symmetry of the site in which Sm(III) is located. The encapsulation of the Samaium complexes was performed for three reasons: (i) before rare earth (RE)-doped sol-gel glasses can be used in applications such as laser materials, several fluorescence quenching mechanisms must be overcome, we show in this work that lanthanide fluorescence is greatly enhanced by chelation and selecting a suitable host matrix (sol-gel) to accommodate the lanthanide complex, (ii) to improve the stability of the phosphor with efficient and high color-purity characteristics under ultraviolet excitation and (iii) this work provides a framework for preparing transparent composite glasses that are robust hosts to study the fundamental interactions between nano-materials and light.

  17. Improving the scratch resistance of sol-gel metal oxide coatings cured at 250 C through use of thermogenerated amines

    Langanke, J.; Arfsten, N.; Buskens, P.; Habets, R.; Klankermayer, J.; Leitner, W.


    Scratch resistant sol-gel metal oxide coatings typically require a thermal post-treatment step (curing process) at temperatures between 400 and 700 C. In this report, we demonstrate that the in situ generation of amines within sol-gel films facilitates the preparation of scratch resistant metal oxid

  18. Fast and efficient proteolysis by reusable pepsin-encapsulated magnetic sol-gel material for mass spectrometry-based proteomics applications.

    Kayili, H Mehmet; Salih, Bekir


    Hydrophobic silicon-based material having magnetic properties was fairly synthesized by a classical sol-gel approach. Pepsin enzyme was encapsulated in the sol-gel material and the enzyme activity was evaluated in consequence of the digestion of some common proteins such as α- and β-casein, cytochrome c, myoglobin, and bovine serum albumin (BSA) both in a single protein batch and in the protein mixture. The optimum digestion time of the studied proteins using pepsin-encapsulated magnetic sol-gel material was found to be 20min. To produce the magnetic sol-gel material for convenient and easy proteomics applications, Fe3O4 was doped inside sol-gel material during the gelation step. It was observed that the activity of encapsulated pepsin was not affected by the amount of Fe3O4. Poly(ethylene glycol) was also inserted in sol-gel bulk to obtain suitable roughness and increase the hydrophilicity of the material surface to let protein molecules reach to the sol-gel material easily. The digestion of the protein mixture and non-fat bovine milk was performed with the pepsin-encapsulated magnetic sol-gel material and the digested solutions were analyzed using SDS-PAGE, MALDI-TOF-MS and LC-MS/MS for the protein identification. Reusability of the pepsin-encapsulated sol-gel material was examined and it was determined that they could be used at least 20 times. Finally, IgG digestions with a fast incubation time period were carried out using pepsin-encapsulated sol-gel material for generation of (Fab)2 product to evaluate the kinetic performance of the material.

  19. Sol-gel deposition of buffer layers on biaxially textured metal substances

    Shoup, Shara S.; Paranthamam, Mariappan; Beach, David B.; Kroeger, Donald M.; Goyal, Amit


    A method is disclosed for forming a biaxially textured buffer layer on a biaxially oriented metal substrate by using a sol-gel coating technique followed by pyrolyzing/annealing in a reducing atmosphere. This method is advantageous for providing substrates for depositing electronically active materials thereon.

  20. 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.

  1. Silica sol-gel encapsulated methylotrophic yeast as filling of biofilters for the removal of methanol from industrial wastewater.

    Kamanina, Olga A; Lavrova, Daria G; Arlyapov, Viacheslav A; Alferov, Valeriy A; Ponamoreva, Olga N


    This research suggests the use of new hybrid biomaterials based on methylotrophic yeast cells covered by an alkyl-modified silica shell as biocatalysts. The hybrid biomaterials are produced by sol-gel chemistry from silane precursors. The shell protects microbial cells from harmful effects of acidic environment. Potential use of the hybrid biomaterials based on methylotrophic yeast Ogataea polymorpha VKM Y-2559 encapsulated into alkyl-modified silica matrix for biofilters is represented for the first time. Organo-silica shells covering yeast cells effectively protect them from exposure to harmful factors, including extreme values of pH. The biofilter based on the organic silica matrix encapsulated in the methylotrophic yeast Ogataea polymorpha BKM Y-2559 has an oxidizing power of 3 times more than the capacity of the aeration tanks used at the chemical plants during methyl alcohol production. This may lead to the development of new and effective industrial wastewater treatment technologies.

  2. Encapsulation of biomaterials in porous glass-like matrices prepared via an aqueous colloidal sol-gel process

    Liu, Dean-Mo; Chen, I-Wei


    The present invention provides a process for the encapsulation of biologically important proteins into transparent, porous silica matrices by an alcohol-free, aqueous, colloidal sol-gel process, and to the biological materials encapsulated thereby. The process is exemplified by studies involving encapsulated cytochrome c, catalase, myoglobin, and hemoglobin, although non-proteinaceous biomaterials, such as active DNA or RNA fragments, cells or even tissues, may also be encapsulated in accordance with the present methods. Conformation, and hence activity of the biomaterial, is successfully retained after encapsulation as demonstrated by optical characterization of the molecules, even after long-term storage. The retained conformation of the biomaterial is strongly correlated to both the rate of gelation and the subsequent drying speed of the encapsulatng matrix. Moreover, in accordance with this process, gelation is accelerated by the use of a higher colloidal solid concentration and a lower synthesis pH than conventional methods, thereby enhancing structural stability and retained conformation of the biomaterials. Thus, the invention also provides a remarkable improvement in retaining the biological activity of the encapsulated biomaterial, as compared with those involved in conventional alkoxide-based processes. It further provides new methods for the quantitative and qualitative detection of test substances that are reactive to, or catalyzed by, the active, encapsulated biological materials.

  3. Ferroelectric-Like Properties of Amorphous Metal Oxide Thin Films Prepared by Sol-Gel Technique.

    Xu, Yuhuan


    Advances in the field of both optical and electrical integrated circuit devices require new thin film materials. Ferroelectric materials have attractive properties such as hysteresis behavior, pyroelectricity, piezoelectricity and nonlinear optical properties. Many ferroelectric thin films have been successfully prepared from metal organic compounds via sol-gel processing. Thus far, research has concentrated upon polycrystalline or epitaxial ferroelectric films. For amorphous ferroelectric thin films, preliminary experimental results in our laboratory indicated that these amorphous films possessed good ferroelectric -like properties. The purpose of this research is (1) to fabricate amorphous metal oxide thin films by the sol-gel technique, (2) to determine whether these amorphous metal oxide thin films have ferroelectric-like properties and (3) to propose a theoretical model ("ferrons model") to explain the ferroelectric-like properties of amorphous thin films, which deals with a structure of permanent dipoles of "partially ordered clusters" (ferrons) in the amorphous films. The theoretical model is based on our experimental results of thin films of two amorphous materials (barium titanite and lead zirconate titanate). This research may provide a new functional material which could be useful for producing integrated electronic and electrooptic devices.

  4. Sol-Gel Synthesis and Characterization of Selected Transition Metal Nano-Ferrites

    Aurelija GATELYTĖ


    Full Text Available In the present work, the sinterability and formation of nanosized yttrium iron garnet (Y3Fe5O12, yttrium perovskite ferrite (YFeO3, cobalt, nickel and zinc iron spinel (CoFe2O4, NiFe2O4 and ZnFe2O4, respectively powders by an aqueous sol-gel processes are investigated. The metal ions, generated by dissolving starting materials of transition metals in the diluted acetic acid were complexed by 1,2-ethanediol to obtain the precursors for the transition metal ferrite ceramics. The phase purity of synthesized nano-compounds was characterized by infrared spectroscopy (IR and powder X-ray diffraction analysis (XRD. The microstructural evolution and morphological features of obtained transition metal ferrites were studied by scanning electron microscopy (SEM.

  5. Encapsulation of Eu(TTA)3 into MCM-41 Mesoporous Molecular Sieve by Sol-Gel Method


    The rare earth complex Eu(TTA)3 was successfully encapsulated into MCM-41 mesoporous molecular sieve by the addition of the complex into the sol-gel mixture for the synthesis of MCM-41 mesoporous material under microwave radiation. The as-synthesized MCM-41-hosted Eu(TTA)3 mesophase was confirmed to possess hexagonally ordered mesostructure and a uniform crystal size of about 30 nm with XRD and HRTEM techniques. Moreover, the IR spectrum, photoluminescence effect and fluorescence lifetime of the Eu(TTA)3/MCM-41 hybrid were also studied. An increase in Stokes' shift and no change in luminescence lifetime were observed to the resultant mesophase in comparison with Eu(TTA)3 in ethanol solution.

  6. Effects of the sol-gel route on the structural characteristics and antibacterial activity of silica-encapsulated gentamicin.

    Corrêa, G G; Morais, E C; Brambilla, R; Bernardes, A A; Radtke, C; Dezen, D; Júnior, A V; Fronza, N; Santos, J H Z Dos


    The effects of sol-gel processes, i.e., acid-catalyzed gelation, base-catalyzed gelation and base-catalyzed precipitation routes, on the encapsulation of gentamicin were investigated. The resulting xerogels were characterized using a series of complementary instrumental techniques, i.e., the adsorption/desorption of nitrogen, small-angle X-ray scattering, Fourier transform infrared spectroscopy, diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy and scanning electron microscopy. The encapsulated gentamicin samples were tested against a series of Gram-positive and Gram-negative bacterial strains. The best antimicrobial activity was observed with the encapsulated gentamicin that was prepared via the precipitation route, even in comparison with the neat antibiotic, especially in the case of the Gram-positive strain Staphylococcus aureus. The gentamicin concentration on the outermost surface and the zeta potential were identified as factors that affected the highest efficiency, as observed in the case of encapsulation via the base-catalyzed process.

  7. 过渡金属醇盐溶胶-凝胶化学进展%Progress on Sol-Gel Chemistry of Transitional Metal Alkoxides

    王家芳; 章文贡


    介绍过渡金属醇盐(TMA)溶胶-凝胶(sol-gel)化学基本知识,着重讨论在TMAsol-gel过程中化学控制方法和分子改性方法,并指出其研究的重要意义和前景。%The basic sol-gel chemistry is introduced, the chemical controlin sol-gel process of transitional metal alkoxides (TMA) and the molecular modification is discussed in detail. The significance and prospective of the study on TMA sol-gel chemistry are pointed out.

  8. Modified Sol-Gel Technique as a Cost-Effective Method of Ultradispersed Metal Oxide Powders Production

    Vokhmintcev, K. V.; Konstantinov, O. V.; Belousov, V. V.


    A modified sol-gel technique was developed for fabrication of ultradispersed metal oxides powders of Bi2O3, CeO2, Cr2O3, Y2O3, ZnO2 and ZrO2. Hexamethylenetetramine, monoethanolamine and acetylacetone were used for the sol formation and gel stabilization.

  9. 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.


    Hansen, E; Eric Frickey, E; Leung Heung, L


    An external gelation process was developed to produce spherical granules that contain metal hydride particles in a sol-gel matrix. Dimensionally stable granules containing metal hydrides are needed for applications such as hydrogen separation and hydrogen purification that require columns containing metal hydrides. Gases must readily flow through the metal hydride beds in the columns. Metal hydrides reversibly absorb and desorb hydrogen and hydrogen isotopes. This is accompanied by significant volume changes that cause the metal hydride to break apart or decrepitate. Repeated cycling results in very fine metal hydride particles that are difficult to handle and contain. Fine particles tend to settle and pack making it more difficult to flow gases through a metal hydride bed. Furthermore, the metal hydrides can exert a significant force on the containment vessel as they expand. These problems associated with metal hydrides can be eliminated with the granulation process described in this report. Small agglomerates of metal hydride particles and abietic acid (a pore former) were produced and dispersed in a colloidal silica/water suspension to form the feed slurry. Fumed silica was added to increase the viscosity of the feed slurry which helped to keep the agglomerates in suspension. Drops of the feed slurry were injected into a 27-foot tall column of hot ({approx}70 C), medium viscosity ({approx}3000 centistokes) silicone oil. Water was slowly evaporated from the drops as they settled. The drops gelled and eventually solidified to form spherical granules. This process is referred to as external gelation. Testing was completed to optimize the design of the column, the feed system, the feed slurry composition, and the operating parameters of the column. The critical process parameters can be controlled resulting in a reproducible fabrication technique. The residual silicone oil on the surface of the granules was removed by washing in mineral spirits. The granules were

  11. Sol-gel encapsulation of pullulanase in the presence of hybrid magnetic (Fe3O4-chitosan) nanoparticles improves thermal and operational stability.

    Long, Jie; Li, Xingfei; Zhan, Xiaobei; Xu, Xueming; Tian, Yaoqi; Xie, Zhengjun; Jin, Zhengyu


    Pullulanase was sol-gel encapsulated in the presence of magnetic chitosan/Fe3O4 nanoparticles. The resulting immobilized pullulanase was characterized by scanning electron microscopy, vibrating sample magnetometry, Fourier transform infrared spectroscopy and thermogravimetric analysis. The results showed that the addition of pullulanase created a more regular surface on the sol-gel matrix and an enhanced magnetic response to an applied magnetic field. The maximal activity retention (83.9%) and specific activity (291.7 U/mg) of the immobilized pullulanase were observed under optimized conditions including an octyltriethoxysilane:tetraethoxysilane (OTES:TEOS) ratio of 1:2 and enzyme concentration of 0.484 mg/mL sol. The immobilized enzyme exhibited good thermal stability. When the temperature was above 60 °C, the immobilized pullulanase showed significantly higher activity than the free enzyme (p sol-gel encapsulation and co-immobilized by crosslinking-encapsulation retained 52 and 69% of their initial activity after 5 h at 62 °C, respectively, compared to 11% for the free enzyme. Moreover, the stability of the pullulanase was improved by crosslinking-encapsulation, as the enzyme retained more than 85 and 81% of its original activity after 5 and 6 consecutive reuses, respectively, compared to 80 and 72% of its original activity for simple sol-gel encapsulated enzymes. This indicated the leakage of enzyme molecules through the pores of the gel was substantially abated by cross-linking. Such immobilized pullulanase provides high stability and ease of enzyme recovery, characteristics that are advantageous for applications in the food industry that involve continuous starch processing.

  12. 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.

  13. Direct electrochemical immunoassay based on a silica nanoparticles/sol-gel composite architecture for encapsulation of immunoconjugate.

    Wang, Fu-Chang; Yuan, Ruo; Chai, Ya-Qin


    A highly hydrophobic and non-toxic colloidal silica nanoparticle/polyvinyl butyral sol-gel composite membrane was prepared on a platinum wire electrode. With diphtheria-toxoid (D-Ag) as a model antigen and encapsulation of diphtheria antibody (D-Ab) in the composite architecture, this membrane could be used for reagentless electrochemical immunoassay. It displayed a porous and homogeneous composite architecture without the aggregation of the immobilized protein molecules. The formation of immunoconjugate by a simple one-step immunoreaction between D-Ag in sample solution and the immobilized D-Ab introduced the change in the potential. Under optimal conditions, the D-Ag analyte could be determined in the linear ranges from 10 to 800 ng ml(-1) with a relatively low detection limit of 2.3 ng ml(-1) at 3delta. The D-Ag immunosensor exhibited good precision, high sensitivity, acceptable stability, accuracy, and reproducibility. This composite membrane could be used efficiently for the entrapment of different biomarkers and clinical applications.

  14. Stabilization of neutral polyfluorene in aqueous solution through their interaction with phospholipids and sol-gel encapsulation.

    Mallavia, Ricardo; Martínez-Tomé, Maria José; Vázquez-Guilló, Rebeca; Kahveci, Zehra; Estepa, Amparo; Mateo, C Reyes


    Interaction between poly[9,9-bis(6'-bromohexyl)-2,7-fluorene-co-alt-1,4-phenylene] (PFPBr2), a neutral conjugated polyfluorene which is completely insoluble in water, and zwitterionic phospholipids has been investigated in order to generate new fluorescent structures which are stable in aqueous media as a means of extending the biological applications of these kinds of polymers. Two types of differently shaped and composed fluorescent structures were identified and then isolated and characterized separately using different biophysical techniques. The first structure type, corresponding to liposomal complexes, showed a fluorescence band centered around 405 nm and maximum absorption at 345 nm, while the second, corresponding to polymer-phospholipid aggregates of variable sizes with lower lipid content, absorbed at longer wavelengths and displayed a well resolved fluorescence spectrum with a maximum centered at 424 nm. Both structures were stable in a large range of pH, and their fluorescence intensity remained practically unaltered for 10 days; it then began to decrease, which was probably because of aggregation. Encapsulation of these structures within the pores of a sol-gel matrix did not affect their fluorescent properties but increased their stability, avoiding further aggregation and subsequent precipitation.

  15. The chemical and catalytic properties of nanocrystalline metal oxides prepared through modified sol-gel synthesis

    Carnes, Corrie Leigh

    The goal of this research was to synthesize, characterize and study the chemical properties of nanocrystalline metal oxides. Nanocrystalline (NC) ZnO, CuO, NiO, Al2O3, and the binary Al2O 3/MgO and ZnO/CuO were prepared through modified sol gel methods. These NC metal oxides were studied in comparison to the commercial (CM) metal oxides. The samples were characterized by XRD, TGA, FTIR, BET, and TEM. The NC samples were all accompanied by a significant increase in surface area and decrease in crystallite size. Several chemical reactions were studied to compare the NC samples to the CM samples. One of the reactions involved a high temperature reaction between carbon tetrachloride and the oxide to form carbon dioxide and the corresponding metal chloride. A similar high temperature reaction was conducted between the metal oxide and hydrogen sulfide to form water and the corresponding metal sulfide. A room temperature gas phase adsorption was studied where SO2 was adsorbed onto the oxide. A liquid phase adsorption conducted at room temperature was the destructive adsorption of paraoxon (a toxic insecticide). In all reactions the NC samples exhibited greater activity, destroying or adsorbing a larger amount of the toxins compared to the CM samples. To better study surface area effects catalytic reactions were also studied. The catalysis of methanol was studied over the nanocrystalline ZnO, CuO, NiO, and ZnO/CuO samples in comparison to their commercial counterparts. In most cases the NC samples proved to be more active catalysts, having higher percent conversions and turnover numbers. A second catalytic reaction was also studied, this reaction was investigated to look at the support effects. The catalysis of cyclopropane to propane was studied over Pt and Co catalysts. These catalysts were supported onto NC and CM alumina by impregnation. By observing differences in the catalytic behavior, support effects have become apparent.

  16. Direct ArF laser photopatterning of metal oxide nanostructures prepared by the sol-gel route

    Ridaoui, Hassan; Wieder, Fernand; Ponche, Arnaud; Soppera, Olivier, E-mail: [Institut de Science des Materiaux de Mulhouse (IS2M), CNRS-LRC 7228, Universite de Haute Alsace, 15 rue Jean Starcky, Mulhouse (France)


    We developed specific negative tone resists suitable for preparing periodic inorganic nanostructures by ArF photolithography. This approach is based on the sol-gel chemistry of modified metal alkoxides followed by DUV laser irradiation. Patterning at the nanoscale was demonstrated by using an achromatic interferometer operating at 193 nm. In a second step, thermal treatment could be used to obtain metal oxide nanostructures (ZrO{sub 2}, TiO{sub 2}). Such thermal treatment did not affect the integrity of the nanostructures. The DUV-induced modifications of the physico-chemical properties of the sol-gel thin film were followed by ellipsometry, XPS and AFM. The crystalline structure of the material after thermal treatment was proved by DRX analysis. Examples of periodic nanostructures are given in order to illustrate the possibilities opened by this new route that provides a convenient method to create transparent, robust, high refractive index nanostructures compatible with a wide variety of substrates.

  17. 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.

  18. 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.

  19. Biodiesel production using alkali earth metal oxides catalysts synthesized by sol-gel method

    Majid Mohadesi


    Full Text Available Biodiesel fuel is considered as an alternative to diesel fuel. This fuel is produced through transesterification reactions of vegetable oils or animal fat by alcohols in the presence of different catalysts. Recent studies on this process have shown that, basic heterogeneous catalysts have a higher performance than other catalysts. In this study different alkali earth metal oxides (CaO, MgO and BaO doped SiO2 were used as catalyst for the biodiesel production process. These catalysts were synthesis by using the sol-gel method. A transesterification reaction was studied after 8h by mixing corn oil, methanol (methanol to oil molar ratio of 16:1, and 6 wt. % catalyst (based on oil at 60oC and 600rpm. Catalyst loading was studied for different catalysts ranging in amounts from 40, 60 to 80%. The purity and yield of the produced biodiesel for 60% CaO/SiO2 was higher than other catalysts and at 97.3% and 82.1%, respectively.

  20. 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.

  1. Encapsulation of β-Sitosterol in Polyurethane by Sol-Gel Electrospinning.

    Amina, Musarat; Amna, Touseef; Al-Musayeib, Nawal; Zabin, Sami A; Hassan, M Shamshi; Khil, Myung-Seob


    Pristine β-sitosterol or in combination with other phytosterols is utilized in an array of enriched commercial foods. Considering the presence of β-sitosterol in different functional foods and its potential role in prevention and cure of neurodegenerative diseases, the aims of our investigation were to encapsulate β-sitosterol in nanofibers and to estimate influence of β-sitosterol on proliferation of fibroblasts. Electrospun nanofibers have widely been used as scaffolds to mimic natural extracellular matrix. Herein, our group for the first time establishes an innovative scaffold based on β-sitosterol and polyurethane using electrospinning. β-Sitosterol promotes epithelialization and possesses anti-oxidant and anti-inflammatory activities, whereas polyurethane, besides possessing biomedical uses, also enhances epithelial growth. We optimized the concentration (5%) of β-sitosterol in polyurethane to obtain homogenous solution, which can be spun without difficulty for the synthesis of β-sitosterol amalgamated scaffold. The resulted twisted nanofibers have been characterized via scanning electron microscopy and Fourier transform infrared spectroscopy. The viability of cells on twisted scaffold was examined using NIH 3T3 fibroblasts as model cell line. Incorporation of β-sitosterol in polyurethane changed the structure and size of nanofibers, and the twisted scaffolds were non-cytotoxic. Thus, the twisted nanoribbons, which contain anti-inflammatory β-sitosterol, can be utilized as a promising future material, which will help to ease inflammation and also aid in wound healing. In conclusion, the outcome of the preliminary research evidently points out the potential of twisted scaffold in biomedical applications.

  2. A review of hydroxyapatite-based coating techniques: Sol-gel and electrochemical depositions on biocompatible metals.

    Asri, R I M; Harun, W S W; Hassan, M A; Ghani, S A C; Buyong, Z


    New promising techniques for depositing biocompatible hydroxyapatite-based coatings on biocompatible metal substrates for biomedical applications have continuously been exploited for more than two decades. Currently, various experimental deposition processes have been employed. In this review, the two most frequently used deposition processes will be discussed: a sol-gel dip coating and an electrochemical deposition. This study deliberates the surface morphologies and chemical composition, mechanical performance and biological responses of sol-gel dip coating as well as the electrochemical deposition for two different sample conditions, with and without coating. The review shows that sol-gel dip coatings and electrochemical deposition were able to obtain the uniform and homogeneous coating thickness and high adherent biocompatible coatings even in complex shapes. It has been accepted that both coating techniques improve bone strength and initial osseointegration rate. The main advantages and limitations of those techniques of hydroxyapatite-based coatings are presented. Furthermore, the most significant challenges and critical issues are also highlighted.

  3. 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.

  4. Encapsulation of biomolecules for bioanalytical purposes: Preparation of diclofenac antibody-doped nanometer-sized silica particles by reverse micelle and sol-gel processing

    Tsagkogeorgas, Fotios [Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, National Technical University of Athens, Iroon Polytechniou 9, 157 73 Athens (Greece); Institute of Hydrochemistry, Technical University of Munich, Marchioninistrasse 17, D-81377 Munich (Germany); Ochsenkuehn-Petropoulou, Maria [Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, National Technical University of Athens, Iroon Polytechniou 9, 157 73 Athens (Greece); Niessner, Reinhard [Institute of Hydrochemistry, Technical University of Munich, Marchioninistrasse 17, D-81377 Munich (Germany); Knopp, Dietmar [Institute of Hydrochemistry, Technical University of Munich, Marchioninistrasse 17, D-81377 Munich (Germany)]. E-mail:


    In recent years, the sol-gel technique has attracted increasing interest as a unique approach to immobilize biomolecules for bioanalytical applications as well as biochemical and biophysical studies. For this purpose, crushed biomolecule-doped sol-gel glass monoliths have been widely used. In the present work, for the first time, the encapsulation of anti-diclofenac antibodies in silica nanoparticles was carried out by a combination of reverse micelle and sol-gel technique. Cyclohexane was used for the preparation of the microemulsion as organic solvent, while surfactant Igepal CO-520 was found to be the optimal stabilizer. The antibody source was a purified IgG fraction originating from a polyclonal rabbit antiserum. Tetramethyl orthosilicate (TMOS) was used as precursor. Rather uniform, monodispersed and spherical silica particles of about 70 nm diameter size were fabricated, as was demonstrated by transmission electron microscopy (TEM) and scanning electron microscopy/energy dispersive X-ray fluorescence analysis (SEM/EDX). The biological activity of the encapsulated antibodies was evaluated by incubation of the nanoparticles with a diclofenac standard solution and analysis of the filtrate and followed washing solutions by a highly sensitive enzyme-linked immunosorbent assay (ELISA), using non-doped particles as blanks. While only about 6% of the added diclofenac was nonspecifically retained by the blank, the corresponding amount of about 66% was much higher with the antibody-doped particles. An obvious advantage of this approach is the general applicability of the developed technique for a mild immobilization of different antibody species.

  5. 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...

  6. 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.


    Yucheng Wu; Yong Zhang; Lide Zhang


    Nanosized palladium particles were incorporated into mesoporous silica matrix to obtain nanocomposites using the sol-gel technique. Effects of the finely dispersed metallic palladium on the microstructure and properties of the nanocomposites were investigated. By means of X-ray diffraction and optical absorption, it was found that palladium particles were 5~9 nm in diameter and their uniform dispersion in the mesoporous silica depended on both the content of the palladium and the structural features of the silica matrix. The results showed that the mixing method of preparation led to wider size distribution of the nanosized particles as compared to the immersion method, but dispersed degree was reduced. Although the incorporation of nanosized palladium particles could not substantially induce significant structural changes of the matrix, the apparent red-shifted optical absorptions for the nanocomposites were observed as compared to the parent monolithic silica, particularly with increase in palladium loading and calcination temperature.

  8. 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.

  9. Large-Scale Precise Printing of Ultrathin Sol-Gel Oxide Dielectrics for Directly Patterned Solution-Processed Metal Oxide Transistor Arrays.

    Lee, Won-June; Park, Won-Tae; Park, Sungjun; Sung, Sujin; Noh, Yong-Young; Yoon, Myung-Han


    Ultrathin and dense metal oxide gate di-electric layers are reported by a simple printing of AlOx and HfOx sol-gel precursors. Large-area printed indium gallium zinc oxide (IGZO) thin-film transistor arrays, which exhibit mobilities >5 cm(2) V(-1) s(-1) and gate leakage current of 10(-9) A cm(-2) at a very low operation voltage of 2 V, are demonstrated by continuous simple bar-coated processes.

  10. Sol-gel encapsulation of binary Zn(II) compounds in silica nanoparticles. Structure-activity correlations in hybrid materials targeting Zn(II) antibacterial use.

    Halevas, E; Nday, C M; Kaprara, E; Psycharis, V; Raptopoulou, C P; Jackson, G E; Litsardakis, G; Salifoglou, A


    In the emerging issue of enhanced multi-resistant properties in infectious pathogens, new nanomaterials with optimally efficient antibacterial activity and lower toxicity than other species attract considerable research interest. In an effort to develop such efficient antibacterials, we a) synthesized acid-catalyzed silica-gel matrices, b) evaluated the suitability of these matrices as potential carrier materials for controlled release of ZnSO4 and a new Zn(II) binary complex with a suitably designed well-defined Schiff base, and c) investigated structural and textural properties of the nanomaterials. Physicochemical characterization of the (empty-loaded) silica-nanoparticles led to an optimized material configuration linked to the delivery of the encapsulated antibacterial zinc load. Entrapment and drug release studies showed the competence of hybrid nanoparticles with respect to the a) zinc loading capacity, b) congruence with zinc physicochemical attributes, and c) release profile of their zinc load. The material antimicrobial properties were demonstrated against Gram-positive (Staphylococcus aureus, Bacillus subtilis, Bacillus cereus) and negative (Escherichia coli, Pseudomonas aeruginosa, Xanthomonas campestris) bacteria using modified agar diffusion methods. ZnSO4 showed less extensive antimicrobial behavior compared to Zn(II)-Schiff, implying that the Zn(II)-bound ligand enhances zinc antimicrobial properties. All zinc-loaded nanoparticles were less antimicrobially active than zinc compounds alone, as encapsulation controls their release, thereby attenuating their antimicrobial activity. To this end, as the amount of loaded zinc increases, the antimicrobial behavior of the nano-agent improves. Collectively, for the first time, sol-gel zinc-loaded silica-nanoparticles were shown to exhibit well-defined antimicrobial activity, justifying due attention to further development of antibacterial nanotechnology.

  11. Rational Synthesis of Imprinted Organofunctional Sol-Gel Materials for Toxic Metal Separation - Final Report - 09/15/1997 - 09/14/2001

    Xue, Ziling (Ben); Barnes, Craig E.; Dai, Shang


    Current cost estimates for the environmental remediation of contaminated installations under the auspices of the Department of Energy (DOE) are staggering. On this basis alone, there is a critical need to develop the scientific basis for new approaches to the treatment and disposal of toxic metal ions from wastes or contaminated areas at many DOE sites. The overall goal of this project is to rationally design and synthesize imprinted, hybrid inorganic-organic sol-gel materials containing metal binding sites through template approaches, and to develop a scientific basis for metal ion binding and recognition by such tailored hybrid inorganic-organic materials. After removal of the template M, functionalized cavities are created which contain both grafted binding sites and functionality inherent to the silica network (Si-OH, Si-O-Si). These cavities are expected to ''recognize'' and bind the target metal ions through the high affinities between the binding sites and M, and their retained shapes. Our approaches utilize both the metal ion binding and the tailored impressions of the template metal ions in the imprinted cavities. Such imprinted organofunctional sol-gel networks are expected to exhibit both high selectivity and capacity for binding targeted ions in fluid waste streams. The principles of sol-gel chemistry and imprinting techniques will guide our approaches to optimize the chemical and physical properties of the imprinted organofunctional sol-gel materials. Cold isotopes or non-radioactive surrogate ions of similar size and charge will be used in imprinting investigations to minimize hazardous waste production. The design strategy we will follow is based on imprinted binding sites cross-linked by rigid, hydrophilic inorganic SiO{sub 2} or MiO{sub 2} networks. These hydrophilic metal oxide-based materials are expected to exhibit fast ion mass transfer and binding kinetics in comparison to functionalized hydrophobic organic polymers

  12. 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.

  13. A new approach to prepare nanoscopic rare earth metal fluorides: the fluorolytic sol-gel synthesis of ytterbium fluoride.

    Schmidt, L; Dimitrov, A; Kemnitz, E


    A new approach for the preparation of approx. 5 nm sized ytterbium fluoride nanoparticles based on the fluorolytic sol-gel route is reported. DLS, TEM, IR and XRD were used to characterize the particles as well as the aging behavior of the sols. Furthermore, a new Yb(III) complex was isolated from the precursor solution and characterized by X-ray single crystal structure determination.

  14. 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.

  15. 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.

  16. 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.

  17. Preparation and characterization of (metal, nitrogen)-codoped TiO2 by TiCl4 sol-gel auto-igniting synthesis

    LIU Zhongqing; ZHOU Yanping; LI Zhenhua; WANG Yichao; GE Changchun


    The nitrogen-doped and (metal, nitrogen)-codoped TiO2 photocatalysts (metal = Ag, Ce, Fe, La) were synthesized by sol-gel auto-igniting synthesis (SAS) with the complex compound sol of TiCl4-NH4NO3-citri acid-metal nitrateNH3.H2O as a precursor. The products were characterized by means of XRD, XPS, and UV-Vis diffuse reflectance spectra,and their photocatalytic activity was investigated under visible light. It was found that all the synthesized powders showed good absorption for visible light, and that the radius and alterable valence states of doping metallic cations played important roles on their photocatalytic activity. These results were discussed in detail.

  18. Study of Photocatalytic Activity and Properties of Transition Metal Ions Doped Nanocrystalline TiO2 Prepared by Sol-Gel Method

    K. S. Siddhapara


    Full Text Available Transition metal (Mn, Fe, Co, doped TiO2 nanoparticles were synthesized by the sol-gel method. All the prepared samples were calcined at different temperatures like 200°C to 800°C and characterized by X-ray diffraction (XRD and energy dispersive X-ray (EDX analysis. The studies revealed that transition metal (TM doped nanoparticles have smaller crystalline size and higher surface area than pure TiO2. Dopant ions in the TiO2 structure caused significant absorption shift into the visible region. The results of photodegradation of formaldehyde in aqueous medium under UV light showed that photocatalytic activity of TiO2 nanoparticles was significantly enhanced by the presence of some transition metal ions. Chemical oxygen demand (COD of formaldehyde solutions done at regular intervals gave a good idea about mineralization of formaldehyde.

  19. 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)

  20. 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.

  1. AFM studies and electrochemical characterization of boron-doped diamond surfaces modified with metal oxides by the Sol-Gel method

    Suffredini Hugo B.


    Full Text Available Continuing previous investigations, direct surface modifications of boron-doped diamond (BDD electrodes with metal oxides (PtOx, RuO2, IrO2 and PbO2 and with some mixed composites were carried out by the Sol-Gel technique. The materials were studied by atomic force microscopy (AFM to determine their surface topologies and by electrochemical techniques to establish the catalytic activity towards the oxygen evolution reaction (OER and also, for the PtOx and PtOx-RuO2 composites, the ethanol oxidation reactions in acid media. The stability of PtOx coating covered by a Nafion® film was also tested by long-term operation. The AFM results indicated sites of heterogeneous deposition and the electrochemical studies demonstrated that the active surface area changed considerably with the proposed method of modification. The IrO2/BDD electrode showed the best performance to the OER with the onset of the oxidation current at ~1.4 V, a value 200 mV lower than for the PtOx/BDD electrode. The enhanced stability of PtOx/BDD electrodes achieved by the application of a Nafion® film and already reported in acid media was further proved using the ethanol oxidation reaction. Only a small loss of activity (6% was observed after 4-hours electrolysis while one-thousand voltammetric cycles left the surface practically unchanged. In addition, preliminary studies for the same reaction on PtOx/BDD and PtOx-RuO2/BDD electrodes demonstrated the excellent activity of these mixed Sol-Gel coatings on the BDD surface and the possibility of further investigations for practical applications.

  2. 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...

  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. 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.

  5. 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.

  6. The Preparation of Porous Sol-Gel Silica with Metal Organic Framework MIL-101(Cr) by Microwave-Assisted Hydrothermal Method for Adsorption Chillers

    Uma, Kasimayan; Pan, Guan-Ting; Yang, Thomas C.-K.


    Metal organic framework (MOF) of MIL-101(Cr)-Silica (SiO2) composites with highly mesoporous and uniform dispersions were synthesized by a microwave-assisted hydrothermal method followed by the sol-gel technique. Water vapor adsorption experiments were conducted on the MIL-101(Cr)-SiO2 composites for industrial adsorption chiller applications. The effects of MIL-101(Cr)-SiO2 mixing ratios (ranging from 0% to 52%), the surface area and amount of Lewis and Brønsted sites were comprehensively determined through water vapor adsorption experiments and the adsorption mechanism is also explained. The BET and Langmuir results indicate that the adsorption isotherms associated with the various MIL-101(Cr)-SiO2 ratios demonstrated Type I and IV adsorption behavior, due to the mesoporous structure of the MIL-101(Cr)-SiO2. It was observed that the increase in the amount of Lewis and Brønsted sites on the MIL-101(Cr)-SiO2 composites significantly improves the water vapor adsorption efficiency, for greater stability during the water vapor adsorption experiments. PMID:28772969

  7. 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##

  8. 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##

  9. 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...

  10. 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.

  11. Solvent-Directed Sol-Gel Assembly of 3-Dimensional Graphene-Tented Metal Oxides and Strong Synergistic Disparities in Lithium Storage

    Ye, Jianchao; An, Yonghao; Montalvo, Elizabeth; Campbell, Patrick G.; Worsley, Marcus A.; Tran, Ich C.; Liu, Yuanyue; Wood, Brandon C.; Biener, Juergen; Jiang, Hanqing; Tang, Ming; Wang, Y. Morris


    Graphene/metal oxide (GMO) nanocomposites promise a broad range of utilities for lithium ion batteries (LIBs), pseudocapacitors, catalysts, and sensors. When applied as anodes for LIBs, GMOs often exhibit high capacity, improved rate capability and cycling performance. Numerous studies have attributed these favorable properties to a passive role played by the exceptional electronic and mechanical properties of graphene in enabling metal oxides (MOs) to achieve near-theoretical capacities. In contrast, the effects of MOs on the active lithium storage mechanisms of graphene remain enigmatic. Via a unique two-step solvent-directed sol-gel process, we have synthesized and directly compared the electrochemical performance of several representative GMOs, namely Fe2O3/graphene, SnO2/graphene, and TiO2/graphene. We observe that MOs can play an equally important role in empowering graphene to achieve large reversible lithium storage capacity. The magnitude of capacity improvement is found to scale roughly with the surface coverage of MOs, and depend sensitively on the type of MOs. We define a synergistic factor based on the capacity contributions. Our quantitative assessments indicate that the synergistic effect is most achievable in conversion-reaction GMOs (Fe2O3/graphene and SnO2/graphene) but not in intercalation-based TiO2/graphene. However, a long cycle stability up to 2000 cycles was observed in TiO2/graphene nanocomposites. We propose a surface coverage model to qualitatively rationalize the beneficial roles of MOs to graphene. Our first-principles calculations further suggest that the extra lithium storage sites could result from the formation of Li2O at the interface with graphene during the conversion-reaction. These results suggest an effective pathway for reversible lithium storage in graphene and shift design paradigms for graphene-based electrodes.

  12. 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

  13. Synthesis and Characterization of Fluoro- and Chlorobimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

    ATHAR, Taimur; SEOK, Sang II; KWON, Jeong Oh


    Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern.SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.

  14. Synthesis and characterization of metallic Pd embedded TiO2 nanoparticles by reverse micelle and sol-gel processing

    Jeoung-Ho JIN; Min-Cheol CHU; Seong-Jai CHO; Dong-Sik BAE


    Metallic Pd clusters were embedded into TiO2 nanoparticles that were synthesized within reverse micelle via a solution reduction of Pd(NO3)2 by hydrazine hydrate. The size of the particles can be controlled by manipulating the relative rates of the hydrolysis and condensation reactions of titanium tetra-isopropoxide within the micro-emulsion. The spherical equivalent size for the Pd clusters formed in TiO2 matrix was estimated to be around (3±1) nm. The presence of Pd in the matrix was demonstrated by EDS spectroscopy. The effects of synthesis parameters, such as the concentration of Pd solution, the molar ratio of water to TIP, and the molar ratio of water to surfactant, were discussed.%This research was financially supported by the Ministry of Education, Science Technology(MEST) and Korea Industrial Technology Foundation(KOTEF) through the Human Resource Training Project for Regional Innovation.

  15. 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.

  16. 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...

  17. 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.

  18. Structural Technology and Analysis Program (STAP). Delivery Order 0010: Sol-Gel Technology for Surface Preparation of Metal Alloys for Adhesive Bonding and Sealing Operations


    46 iv 4.8 VACUUM CURING ......................................................................................................................................47...blasted Figure 4.7-3. Total crack length for specimens primed with Cytec BR 6757 4.8 Vacuum Curing The effects of a vacuum cure cycle versus an...reduction in performance of the sol-gel surface preparations due to vacuum curing . 25% coh 15% coh 70% coh 10% coh 30% coh 0% coh 97% coh 97

  19. 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.

  20. Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment.

    Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha


    Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol-gel SiO2 is non-toxic and safe, whereas the sol-gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped active agents, thereby broadening the practical utilization of chemically unstable essential oils (EOs). Reviewing progress in the fabrication of diverse odorant and flavored sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

  1. 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.)

  2. Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment

    Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha


    .... The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties...

  3. Progress in sol-gel auto combustion synthesis of metals and alloys%溶胶凝胶自燃烧法合成金属与合金材料研究进展∗

    张新伟; 华正和; 蒋毓文; 杨绍光


    本文综述了溶胶凝胶自燃烧法制备金属与合金材料的研究进展,详细介绍了该方法的实验原理和技术路线,通过实例介绍了该方法在制备金属和合金材料中的具体应用。通过这一系列的工作介绍,我们证实可以把传统的溶胶凝胶法制备氧化物材料的技术拓展到金属与合金材料的制备,希望能够对材料研究的实验工作有所帮助。%This paper is an overview of the progress of sol-gel autocombustion synthesis of metals and metal alloys. Sol-gel is a convenient method to synthesize a variety of oxides by mixing of different elements at an atomic level. Autocombustion synthesis is a self-sustaining process caused by the heat generated from its exothermic reaction. By combining these two methods, the sol-gel autocombustion method is introduced in the synthesis of metals and metal alloys. The experimental principle and technological route are introduced in detail in this review. By using metal nitrate, citric acid etc. as starting materials, the dried gels are prepared through sol-gel routine. Under the protection of inert gas, the autocombustion could be activated at low temperature in a tube furnace. After the autocombustion was activated, the gel burned violently, and a large amount of white gas was released. During heating the gel, mass spectrum shows that the H2, CO and CH4 are evidently identified near the combustion temperature. They are well known reducing agents, which can be used in the redox reaction for synthesizing metals from oxides. Based on the data obtained from the TG-DTA and mass spectrum analysis, it is speculated that there are mainly five reactions appearing during the burning of the gel at high temperature: exothermic reaction between fuel and oxidant; metal oxide(s) formation by decomposition of the nitrate(s); generation of CH4, CO and H2 by the decomposition of CHx containing groups of complexing agent;exothermic reaction between CH4/CO/H2 and

  4. 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].

  5. Chlorobenzene, chloroform, and carbon tetrachloride adsorption on undoped and metal-doped sol-gel substrates (SiO{sub 2}, Ag/SiO{sub 2}, Cu/SiO{sub 2} and Fe/SiO{sub 2})

    Hernandez, M.A. [Postgrado de Ciencias Ambientales and Departamento de Investigacion en Zeolitas, Instituto de Ciencias, Universidad Autonoma de Puebla, Edificio 76, Complejo de Ciencias, Ciudad Universitaria, CP 72570 Puebla (Mexico)], E-mail:; Gonzalez, A.I.; Corona, L.; Hernandez, F. [Postgrado de Ciencias Ambientales and Departamento de Investigacion en Zeolitas, Instituto de Ciencias, Universidad Autonoma de Puebla, Edificio 76, Complejo de Ciencias, Ciudad Universitaria, CP 72570 Puebla (Mexico); Rojas, F.; Asomoza, M.; Solis, S. [Departamento de Quimica, Universidad Autonoma Metropolitana-Iztapalapa, P.O. Box 55-534, D.F. Mexico (Mexico); Portillo, R.; Salgado, M.A. [Facultad de Ciencias Quimicas, Universidad Autonoma de Puebla (Mexico)


    Adsorption isotherms of chlorobenzene, chloroform and carbon tetrachloride vapors on undoped SiO{sub 2}, and metal-doped Ag/SiO{sub 2}, Cu/SiO{sub 2} and Fe/SiO{sub 2} substrates were measured in the temperature range of 398-593 K. These substrates were prepared from a typical sol-gel technique in the presence of metal dopants that rendered an assortment of microporous-mesoporous solids. The relevant characteristic of these materials was the different porosities and micropore to mesopore volume ratios that were displayed; this was due to the effect that the cationic metal valence exerts on the size of the sol-gel globules that compose the porous solid. The texture of these SiO{sub 2} materials was analyzed by X-ray diffraction (XRD), FTIR, and diverse adsorption methods. The pore-size distributions of the adsorbents confirmed the existence of mesopores and supermicropores, while ultramicropores were absent. The Freundlich adsorption model approximately fitted the chlorinated compounds adsorption data on the silica substrates by reason of a heterogeneous energy distribution of adsorption sites. The intensity of the interaction between these organic vapors and the surface of the SiO{sub 2} samples was analyzed through evaluation of the isosteric heat of adsorption and standard adsorption energy; from these last results it was evident that the presence of metal species within the silica structure greatly affected the values of both the amounts adsorbed as well as of the isosteric heats of adsorption.

  6. One-pot preparation of silica-supported hybrid immobilized metal affinity adsorbent with macroporous surface based on surface imprinting coating technique combined with polysaccharide incorporated sol--gel process.

    Li, Feng; Li, Xue-Mei; Zhang, Shu-Sheng


    A simple and reliable one-pot approach using surface imprinting coating technique combined with polysaccharide incorporated sol-gel process was established to synthesize a new organic-inorganic hybrid matrix possessing macroporous surface and functional ligand. Using mesoporous silica gel being a support, immobilized metal affinity adsorbent with a macroporous shell/mesoporous core structure was obtained after metal ion loading. In the prepared matrix, covalently bonded coating and morphology manipulation on silica gel was achieved by using one-pot sol-gel process starting from an inorganic precursor, -glycidoxypropyltrimethoxysiloxane (GPTMS), and a functional biopolymer, chitosan (CS) at the atmosphere of imprinting polyethylene glycol (PEG). Self-hydrolysis of GPTMS, self-condensation, and co-condensation of silanol groups (Si-OH) from siloxane and silica gel surface, and in situ covalent cross-linking of CS created an orderly coating on silica gel surface. PEG extraction using hot ammonium hydroxide solution gave a chemically and mechanically stabilized pore structure and deactivated residual epoxy groups. The prepared matrix was characterized by using X-ray energy dispersion spectroscopy (EDX), scanning electron microscopy (SEM) and mercury intrusion porosimetry. The matrix possessed a high capacity for copper ion loading. Protein adsorption performance of the new immobilized metal affinity adsorbent was evaluated by batch adsorption and column chromatographic experiment using bovine serum albumin (BSA) as a simple model protein. Under the optimized coating conditions, the obtained macroporous surface resulted in a fast kinetics and high capability for protein adsorption, while the matrix non-charged with metal ions offered a low non-specific adsorption.

  7. 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.

  8. 溶胶-凝胶法制备金属铂高分散的二氧化钛薄膜%Preparation of Titania Thin Film with Highly-Dispersed Platinum Metal by Sol-Gel Method

    黄妙良; 伴隆幸; 大矢丰; 高桥康隆


    Uniform and crack-free TiO2 thin films with highly-dispersed platinum were p repared from i-PrOH-TTIP-DEA-H2O system containing H2PtCl6*6H 2O as metal source by sol-gel method. The microstructure and morphology of th e films were characterized by TEM and XRD respectively. It was found that the Pt particles dispersed in the films and had a homogeneous distribution in the shap e of sphere with an average size of about 5 nm. This study also showed that the doping with few percent of Pt resulted in the formation of pure rutile phase at a temperature as low as 550 ℃, whereas the same pure phase was formed at the te mperature higher than 650 ℃ in TiO2 or Au/TiO2 thin films.

  9. 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.

  10. Studies of (3-mercaptopropyl)trimethoxylsilane and bis(trimethoxysilyl)ethane sol-gel coating on copper and aluminum.

    Li, Ying-Sing; Lu, Weijie; Wang, Yu; Tran, Tuan


    Bis(trimethoxysilyl)ethane (BTMSE) and (3-mercaptopropyl)trimethoxysilane (MPTMS) have been used as precursors to prepare sol-gels and hybrid sol-gel under acidic condition. From the X-ray photoelectron spectroscopy data on MPTMS sol-gel coated aluminum and copper, it has been shown that the silane film is covalently bonded to Al surface through the interfacial condensation. There is no evidence of bonding interaction between the thiol group and the Cu. The recorded reflection adsorption IR (RAIR) spectrum has provided evidence that the coating BTMSE film covalently interacts with Al. Vibrational assignments have been suggested for pure BTMSE, BTMSE sol-gel, BTMSE xerogel, and BTMSE coated Al panel based on the group frequencies and the variation of frequencies with the sample treatment conditions. The progression of condensation reaction has been observed from the IR spectra of the BTMSE sol-gel and the sol-gel coated film after the treatments at different temperatures with different lengths of time. The corrosion protection of the sol-gel coated Al and Cu has been characterized in NaCl solutions by cyclic voltammetric, potentiodynamic polarization and impedance spectroscopy methods. All these electrochemical measurements indicate that the sol-gel coated metals have better corrosion protection than the corresponding uncoated metals.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. Hybrid inorganic-organic materials: Novel poly(propylene oxide)-based ceramers, abrasion-resistant sol-gel coatings for metals, and epoxy-clay nanocomposites, with an additional chapter on: Metallocene-catalyzed linear polyethylene

    Jordens, Kurt


    The sol-gel process has been employed to generate hybrid inorganic-organic network materials. Unique ceramers were prepared based on an alkoxysilane functionalized soft organic oligomer, poly(propylene oxide (PPO), and tetramethoxysilane (TMOS). Despite the formation of covalent bonds between the inorganic and organic constituents, the resulting network materials were phase separated, composed of a silicate rich phase embedded in a matrix of the organic oligomer chains. The behavior of such materials was similar to elastomers containing a reinforcing filler. The study focused on the influence of initial oligomer molecular weight, functionality, and tetramethoxysilane, water, and acid catalyst content on the final structure, mechanical and thermal properties. The sol-gel approach has also been exploited to generate thin, transparent, abrasion resistant coatings for metal substrates. These systems were based on alkoxysilane functionalized diethylenetriamine (DETA) with TMOS, which generated hybrid networks with very high crosslink densities. These materials were applied with great success as abrasion resistant coatings to aluminum, copper, brass, and stainless steel. In another study, intercalated polymer-clay nanocomposites were prepared based on various epoxy networks montmorillonite clay. This work explored the influence of incorporated clay on the adhesive properties of the epoxies. The lap shear strength decreased with increasing day content This was due to a reduction in the toughness of the epoxy. Also, the delaminated (or exfoliated) nanocomposite structure could not be generated. Instead, all nanocomposite systems possessed an intercalated structure. The final project involved the characterization of a series of metallocene catalyzed linear polyethylenes, produced at Phillips Petroleum. Polyolefins synthesized with such new catalyst systems are becoming widely available. The influence of molecular weight and thermal treatment on the mechanical, rheological

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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).

  14. Fabrication and characterization of sol-gel based nanoparticles for drug delivery

    Yadav, Reeta

    Nanogels are cross linked polymeric sol-gel based nanoparticles that offer an interior network for incorporation and protection of biomolecules, exhibiting unique advantages for polymer based delivery systems. We have successfully synthesized stable sol-gel nanoparticles by means of [a] silicification reactions using cationic peptides like polylysine as gelating agents, and [b] lyophilization of sol-gels. Macromolecules such as Hemoglobin and Glucose Oxidase and small molecules such as Sodium Nitroprusside (SNP) and antibiotics were encapsulated within the nanogels. We have used transmission electron microscopy, dynamic light scattering, zeta potential analysis, and spectroscopy to perform a physicochemical characterization of the nanogels resulting from the two approaches. Our studies have indicated that the nanogel encapsulated proteins and small molecules remain intact, stable and functional. A Hydrogen Peroxide (H2O2) and Nitric Oxide (NO) generating drug carrier was synthesized using these nanogels and the effect of generation of H2O2 from Glucose Oxidase encapsulated nanogels and NO from SNP encapsulated nanogels was tested on E.coli. The results show that the nanoparticles exert antimicrobial activity against E.Coli, in addition NO generating nanogels potentiated H2O2 generating nanogels induced killing. These data suggest that these NO and H2O2 releasing nanogels have the potential to serve as a novel class of antimicrobials for the treatment of multidrug resistant bacteria. The unique properties of these protein/drug incorporated nanogels raise the prospect of fine tailoring to specific applications such as drug delivery and bio imaging.

  15. 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)

  16. Photoresist-Free Fully Self-Patterned Transparent Amorphous Oxide Thin-Film Transistors Obtained by Sol-Gel Process

    Lim, Hyun Soo; Rim, You Seung; Kim, Hyun Jae


    We demonstrated self-patterned solution-processed amorphous oxide semiconductor thin-film transistors (TFTs) using photosensitive sol-gels. The photosensitive sol-gels were synthesized by adding β-diketone compounds, i.e., benzoylacetone and acetylacetone, to sol-gels. The chemically modified photosensitive sol-gels showed a high optical absorption at specific wavelengths due to the formation of metal chelate bonds. Photoreactions of the modified solutions enabled a photoresist-free process. Moreover, Zn-Sn-O with a high Sn ratio, which is hard to wet-etch using conventional photolithography due to its chemical durability, was easily patterned via the self-patterning process. Finally, we fabricated a solution-processed oxide TFT that included fully self-patterned electrodes and an active layer.

  17. Secondary Crystal Growth on a Cracked Hydrotalcite-Based Film Synthesized by the Sol-Gel Method.

    Lee, Wooyoung; Lee, Chan Hyun; Lee, Ki Bong


    The sol-gel synthesis method is an attractive technology for the fabrication of ceramic films due to its preparation simplicity and ease of varying the metal composition. However, this technique presents some limitations in relation to the film thickness. Notably, when the film thickness exceeds the critical limit, large tensile stresses occur, resulting in a cracked morphology. In this study, a secondary crystal growth method was introduced as a post-treatment process for Mg/Al hydrotalcite-based films synthesized by the sol-gel method, which typically present a cracked morphology. The cracked hydrotalcite-based film was hydrothermally treated for the secondary growth of hydrotalcite crystals. In the resulting film, hydrotalcite grew with a vertical orientation, and the gaps formed during the sol-gel synthesis were filled with hydrotalcite after the crystal growth. The secondary crystal growth method provides a new solution for cracked ceramic films synthesized by the sol-gel method.

  18. 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...

  19. 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...

  20. 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.

  1. Characterisation and thermal properties of titanium dioxide nanoparticles-containing biodegradable polylactide composites synthesized by sol-gel method.

    Mhlanga, Nikiwe; Ray, Suprakas Sinha


    This study reports the synthesis, characterisation and thermal properties of polylactide (PLA)/titanium dioxide nanoparticles (TiO2 NPs) composites using the sol-gel method. The percentage weight of TiO2 NP sol was varied from 3, 8, 11 and 14. The synthesised composites were characterised using scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction, energy dispersive X-ray spectroscopy (EDS), thermogravimetric analysis and dynamic mechanical analysis. Encapsulation of the TiO2 into the PLA matrix was attainable based on the SEM images and the FTIR and EDS results. The thermal stability of the composites was shifted to lower temperatures due to photodegradation induced by the metal oxide on the PLA chain. Both PLA and TiO2 NPs have potential in drug delivery because of their biocompatibility and biodegradability.

  2. Temperature Dependent Electrical Transport in Al/Poly(4-vinyl phenol/p-GaAs Metal-Oxide-Semiconductor by Sol-Gel Spin Coating Method

    Şadan Özden


    Full Text Available Deposition of poly(4-vinyl phenol insulator layer is carried out by applying the spin coating technique onto p-type GaAs substrate so as to create Al/poly(4-vinyl phenol/p-GaAs metal-oxide-semiconductor (MOS structure. Temperature was set to 80–320 K while the current-voltage (I-V characteristics of the structure were examined in the study. Ideality factor (n and barrier height (ϕb values found in the experiment ranged from 3.13 and 0.616 eV (320 K to 11.56 and 0.147 eV (80 K. Comparing the thermionic field emission theory and thermionic emission theory, the temperature dependent ideality factor behavior displayed that thermionic field emission theory is more valid than the latter. The calculated tunneling energy was 96 meV.

  3. 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

  4. 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

  5. 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.

  6. 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.

  7. 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...

  8. Encapsulating Cytochrome c in Silica Aerogel Nanoarchitectures without Metal Nanoparticles while Retaining Gas-phase Bioactivity

    Harper-Leatherman, Amanda S.; Pacer, Elizabeth R.; Kosciuszek, Nina D.


    Applications such as sensors, batteries, and fuel cells have been improved through the use of highly porous aerogels when functional compounds are encapsulated within the aerogels. However, few reports on encapsulating proteins within sol–gels that are processed to form aerogels exist. A procedure for encapsulating cytochrome c (cyt. c) in silica (SiO2) sol-gels that are supercritically processed to form bioaerogels with gas-phase activity for nitric oxide (NO) is presented. Cyt. c is added to a mixed silica sol under controlled protein concentration and buffer strength conditions. The sol mixture is then gelled and the liquid filling the gel pores is replaced through a series of solvent exchanges with liquid carbon dioxide. The carbon dioxide is brought to its critical point and vented off to form dry aerogels with cyt. c encapsulated inside. These bioaerogels are characterized with UV-visible spectroscopy and circular dichroism spectroscopy and can be used to detect the presence of gas-phase nitric oxide. The success of this procedure depends on regulating the cyt. c concentration and the buffer concentration and does not require other components such as metal nanoparticles. It may be possible to encapsulate other proteins using a similar approach making this procedure important for potential future bioanalytical device development. PMID:26967257

  9. 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

  10. /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.

  11. Ultrapure glass optical waveguide development in microgravity by the sol-gel process


    Containerless melting of glasses in space for the preparation of ultrapure homogeneous glass for optical waveguides is discussed. The homogenization of the glass using conventional raw materials is normally achieved on Earth either by the gravity induced convection currents or by the mechanical stirring of the melt. Because of the absence of gravity induced convection currents, the homogenization of glass using convectional raw materials is difficult in the space environment. Multicomponent, homogeneous, noncrystalline oxide gels can be prepared by the sol-gel process and these gels are promising starting materials for melting glasses in the space environment. The sol-gel process is based on the polymerization reaction of alkoxysilane with other metal alkoxy compounds or suitable metal salts. Many of the alkoxysilanes or other metal alkoxides are liquids and thus can be purified by distillation.

  12. 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...

  13. 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.

  14. 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...

  15. 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.

  16. Synthesis of hexagonal barium ferrite nanoparticle by sol-gel method

    DONG Limin; HAN Zhidong; ZHANG Yaoming; WU Ze; ZHANG Xianyou


    M-type Ba hexaferrites were successfully synthesized by sol-gel method. Several synthesizing factors, such as pH value, citric acid/metal ion ratio, and dispersion agent were mainly discussed. Fine and pure powders of BaFe12O19 were optimally synthesized under the conditions of the pH value is 7 and citricacid/metal ion ratio is 3. The X-ray diffraction analysis demonstrates that no impurity is observed in the synthesized powders after presintered at 450 ℃ and calcinated at 1100 ℃. SEM observations indicate that the size of the synthesized BaFe12O19 powders is small and uniform distribution. It can also be learned from SEM that the co-synthesizing sol-gel method can be in favor ofthe formation of finer particles.

  17. 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.

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

    张翔; 李书润; 翟文韬; 曹莹泽; 齐宏旭; 吉岩; 危岩


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

  19. 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...

  20. Revêtements polyesters hybrides organiques-inorganiques par voie sol-gel


    This study focuses on coatings based on news O/I hybrid coatings having a specific morphology to improve resistance to heat, abrasion and scratch as well as mechanical properties. To obtain and control the hybrid morphology, inorganic domains are generated in-situ via sol-gel chemistry based on hydrolysis/condensation reactions of metal alcoxydes (TEOS) into an organic polymer: hyperbranched polyesters (HBP Boltorn H20 and H40) and branched oligoesters (Synthoester, tannic acids). Which ones ...

  1. 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...

  2. 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:

  3. Thin-film silica sol-gels doped with ion responsive fluorescent lipid bilayers

    Sasaki, D.Y.; Shea, L.E.; Sinclair, M.B.


    A metal ion sensitive, fluorescent lipid-b i layer material (5oA PSIDA/DSPC) was successfully immobilized in a silica matrix using a tetramethoxysilane (TMOS) sol-gel procedure. The sol-gel immobilization method was quantitative in the entrapment of seif-assembled Iipid-bilayers and yielded thin films for facile configuration to optical fiber piatforms. The silica matrix was compatible with the solvent sensitive lipid bilayers and provided physical stabilization as well as biological protection. Immobilization in the silica sol-gel produced an added benefit of improving the bilayer's metal ion sensitivity by up to two orders of magnitude. This enhanced performance was attributed to a preconcentrator effect from the anionic surface of the silica matrix. Thin gels (193 micron thickness) were coupled to a bifurcated fiber optic bundle to produce a metal ion sensor probe. Response times of 10 - 15 minutes to 0.1 M CUCIZ were realized with complete regeneration of the sensor using an ethylenediarninetetraacetic acid (EDTA) solution.

  4. Effect of chelating agent acetylacetone on corrosion protection properties of silane-zirconium sol-gel coatings

    Yu, Mei; Liang, Min; Liu, Jianhua; Li, Songmei; Xue, Bing; Zhao, Hao


    The hybrid sol-gel coatings on AA2024-T3 were prepared with a silane coupling agent 3-glycidoxypropyltrimethoxysilane (GPTMS) and a metal alkoxide tetra-n-propoxyzirconium (TPOZ) as precursors. The effect of acetylacetone (AcAc) as a chelating agent on the corrosion protection properties of sol-gel coatings were evaluated and the optimal AcAc/TPOZ molar ratio was obtained. The sol-gel coatings were characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The corrosion protection properties of the coatings were evaluated by means of potentiodynamic polarization study (PDS) and electrochemical impedance spectroscopy (EIS). It is demonstrated that AcAc avoids fast hydrolysis of TPOZ and benefits to form stable sols. The coating with AcAc/TPOZ molar ratio of 3 shows the best corrosion protection performance in 0.05 M NaCl solution.

  5. 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.

  6. 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.

  7. 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.

  8. Electrochemical behaviour of ceramic yttria stabilized zirconia on carbon steel synthesized via sol-gel process

    Crespo, M.A. Dominguez, E-mail: mdominguezc@ipn.m [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Murillo, A. Garcia; Torres-Huerta, A.M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Yanez-Zamora, C. [Estudiante del postgrado en Tecnologia Avanzada del CICATA-IPN, Unidad Altamira, km 14.5, Carr. Tampico-Puerto Industrial. C.P. 89600, Altamira, Tamaulipas (Mexico); Carrillo-Romo, F. de J [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira (CICATA-IPN) km 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico)


    Chromate conversion coatings have been widely applied for the corrosion of different metallic substrates. However, the waste containing Cr{sup 6+} has many limitations due to the environmental consideration and health hazards. An interesting alternative seems to be the deposition on metallic surface of thin layers of yttria or zirconia or both by the sol-gel process. In this study, Ytttria and Yttria stabilized zirconia (YSZ, 8% Y{sub 2}O{sub 3}) thin films were used for coating commercial carbon steel substrates by sol-gel method and the dip-coating process. The evolution of organic compounds up to crystallization process as a function of heat treatments was study by FT-IR spectroscopy. The structure and morphology of the coatings were analysed using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The anticorrosion performance of the coatings has been evaluated by using electrochemical techniques in an aggressive media (3.5 wt.% NaCl). The corrosion behaviour of sol-gel method was compared with traditional chromate conversion coatings. Differences in the electrochemical behaviour of YSZ coatings are related to the development of microcracks during the sintering process and to the presence of organic compounds during growth film. Electrochemical results showed that sol-gel YSZ and Y{sub 2}O{sub 3} coatings can act as protective barriers against wet corrosion; however yttria films displayed low adhesion to substrate. The corrosion parameters provide an explanation of the role of each film and show a considerable increase in the corrosion resistance for coated samples in comparison to the bare steel samples.

  9. 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.

  10. 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.

  11. Effectiveness of silica based Sol-gel microencapsulation Method for odorants and flavours leading to sustainable Environment

    Muhammad Aqeel eAshraf


    Full Text Available Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol–gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol–gel SiO2 is non-toxic and safe, whereas the sol–gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped actives, thereby broadening the practical utilization of chemically unstable essential oils. Reviewing progress in the fabrication of diverse odorant and flavoured sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

  12. 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.

  13. 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.

  14. 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.)

  15. Sol-gel synthesis and structure of cordierite/tialite glass-ceramics

    Lachezar Radev


    Full Text Available In the present work the results of the research on the sol-gel synthesis and structure of cordierite (2MgO·2Al2O3·5SiO2, tialite (Al2O3·TiO2 and cordierite/tialite glass-ceramics as well cordierite containing 2 wt.% of Co and Co+Cu have been described and discussed. The sol-gel synthesis was carried out using different kind of precursors as follows: Al(NO3×9H2O, Si(OC2H54 , Ti(OC4H94 , Mg(NO32×6H2O, chlorides or nitrates of corresponding metals, H2O, C2H5OH, Aqua Regia, NH4F and PEG. The synthesized gels were dried and thermally treated in the temperature range from 800°C to 1200°C. The sol-gel processes and structure of the cordierite, tialite and cordierite/tialite glass-ceramics have been investigated by means of XRD, FTIR, TEM, SEM and EPMA.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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...

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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

  10. Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

    Sibille, L.; Gavira-Gallardo, J. A.; Hourlier-Bahloul, D.


    Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil similar JSC-1 in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. Characterization of the precursor molecules and efforts to further concentrate and hydrolyze the products to obtain gel materials will be presented for evaluation as ceramic precursors.

  11. Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

    Sibille, L.; Gavira-Gallardo, J. A.; Hourlier-Bahloul, D.


    Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil similar JSC-1 in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. Characterization of the precursor molecules and efforts to further concentrate and hydrolyze the products to obtain gel materials will be presented for evaluation as ceramic precursors.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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...

  1. 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...

  2. 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...

  3. 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.

  4. 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.)

  5. 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 ...

  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. 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. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Sol-gel zirconia nanopowders with {alpha}-cyclodextrin as organic additive

    Raileanu, M., E-mail: [' Ilie Murgulescu' Institute of Physical Chemistry, Roumanian Academy, Splaiul Independentei 202, 060021 Bucharest (Romania); Todan, L., E-mail: [' Ilie Murgulescu' Institute of Physical Chemistry, Roumanian Academy, Splaiul Independentei 202, 060021 Bucharest (Romania); Crisan, D.; Dragan, N.; Crisan, M.; Stan, C.; Andronescu, C.; Voicescu, M. [' Ilie Murgulescu' Institute of Physical Chemistry, Roumanian Academy, Splaiul Independentei 202, 060021 Bucharest (Romania); Vasile, B.S.; Ianculescu, A. [Department of Oxide Materials Science and Engineering, ' Politehnica' University of Bucharest, 1-7 Gh. Polizu, P.O. Box 12-134, 011061 Bucharest (Romania)


    Highlights: Black-Right-Pointing-Pointer The sol-gel synthesis of a zirconia powder has been performed, in the presence of {alpha}-cyclodextrin as organic additive. Black-Right-Pointing-Pointer A crystalline powder consisting from a mixture of monoclinic and tetragonal zirconia phases has resulted after the thermal treatment. Black-Right-Pointing-Pointer The organic additive acted the role of metal oxides used as doppants for zirconia powders, avoiding phase transformations. Black-Right-Pointing-Pointer The {alpha}-cyclodextrin made particles to assume spherical shape and reach fairly uniform size and prevented their agglomeration. Black-Right-Pointing-Pointer The organic additive led to a certain porous morphology of the zirconia particles that is pores embedded within grains. - Abstract: Nanomaterials present unique structural and physicochemical properties due to their ultra fine size of particles that make them very useful in many domains. The most spectacular applications of nanosized zirconia include ceramics, piezoelectrics, refractories, pigments, solid electrolytes, oxygen sensors, catalysts, ultrafiltration membranes, and chromatography packing materials. Nanostructured zirconia powders can be prepared using various methods, such as sol-gel process, coprecipitation, hydrothermal synthesis, and reverse micelle method. The aim of the present work was to prepare zirconia nanopowders through the sol-gel method, using {alpha}-cyclodextrin as organic additive and to establish its influence on the structural and textural properties of the obtained product. A white, amorphous ZrO{sub 2} powder containing {alpha}-cyclodextrin was prepared, which became a crystalline, stable one, after removing the organic matter by thermal treatment. The resulted nanocrystalline powder contains both monoclinic and tetragonal zirconia phases and is very stable. It presents a relatively reduced tendency of agglomeration of particles and contains closed pores which are embedded in

  13. 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.

  14. Sol-gel prepared active ternary oxide coating on titanium in cathodic protection



    Full Text Available The characteristics of a ternary oxide coating, on titanium, which consisted of TiO2, RuO2 and IrO2 in the molar ratio 0.6:0.3:0.1, calculated on the metal atom, were investigated for potential application for cathodic protection in a seawater environment. The oxide coatings on titanium were prepared by the sol gel procedure from a mixture of inorganic oxide sols, which were obtained by forced hydrolysis of metal chlorides. The morphology of the coating was examined by scanning electron microscopy. The electrochemical properties of activated titanium anodes were investigated by cyclic voltammetry and polarization measurements in a H2SO4- and NaCl-containing electrolyte, as well as in seawater sampled on the Adriatic coast in Tivat, Montenegro. The anode stability during operation in seawater was investigated by the galvanostatic accelerated corrosion stability test. The morphology and electrochemical characteristics of the ternary coating are compared to that of a sol-gel-prepared binary Ti0.6Ru0.4O2 coating. The activity of the ternary coating was similar to that of the binary Ti0.6Ru0.4O2 coating in the investigated solutions. However, the corrosion stability in seawater is found to be considerably greater for the ternary coating.

  15. Silica doped with lanthanum sol-gel thin films for corrosion protection

    Abuin, M. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Serrano, A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); Llopis, J. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Garcia, M.A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); IMDEA Nanoscience, Fco. Tomas y Valiente 7, 28049 Madrid (Spain); Carmona, N., E-mail: [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain)


    We present here anticorrosive silica coatings doped with lanthanum ions for the protection of metallic surfaces as an alternative to chromate (VI)-based conversion coatings. The coatings were synthesized by the sol-gel method starting from silicon alkoxides and two different lanthanum precursors: La (III) acetate hydrate and La (III) isopropoxide. Artificial corrosion tests in acid and alkaline media showed their effectiveness for the corrosion protection of AA2024 aluminum alloy sheets for coating prepared with both precursors. The X-ray absorption Near Edge Structure and X-ray Absorption Fine Structure analysis of the coatings confirmed the key role of lanthanum in the structural properties of the coating determining its anticorrosive properties. - Highlights: Black-Right-Pointing-Pointer Silica sol-gel films doped with lanthanum ions were synthesized. Black-Right-Pointing-Pointer Films from lanthanum-acetate and La-alkoxide were prepared for comparison purposes. Black-Right-Pointing-Pointer La-acetate is an affordable chemical reactive preferred for the industry. Black-Right-Pointing-Pointer Films properties were explored by scanning electron microscopy and X-Ray absorption spectroscopy. Black-Right-Pointing-Pointer An alternative to anticorrosive pre-treatments for metallic surfaces is suggested.

  16. Preparation of gas-tight strontium-doped lanthanum cobaltate by an aqueous sol-gel process

    Chen, C.H.; Kruidhof, H.; Bouwmeester, H.J.M.; Burggraaf, A.J.


    Gas-tight dense membranes of highly Sr-doped LaCoO3 (such as the composition La0.3Sr0.7CoO3 chosen in this study) are difficult to prepare using usual synthesis processes. This report presents an aqueous sol-gel route using metal acetates as precursors to achieve this goal. Hydrogen peroxide and amm

  17. 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

  18. Improvement of barrier properties of a hybrid sol-gel coating by incorporation of synthetic talc-like phyllosilicates for corrosion protection of a carbon steel


    International audience; Sol-gel coatings for corrosion protection of metals are a good alternative to toxic chromate treatments. The present work focussed on the incorporation of inorganic fillers in a sol-gel coating to improve the barrier properties of the film. Talc-like phyllosilicates obtained by hydrothermal synthesis at 160°C, 260°C and 350°C, called T160, T260 and T350 respectively, were selected as inorganic fillers. The synthetic materials showed talc lamellar structure but, in cont...

  19. Adhesion and Long-Term Barrier Restoration of Intrinsic Self-Healing Hybrid Sol-Gel Coatings.

    Abdolah Zadeh, Mina; van der Zwaag, Sybrand; Garcia, Santiago J


    Self-healing polymeric coatings aiming at smart and on-demand protection of metallic substrates have lately attracted considerable attention. In the present paper, the potential application of a dual network hybrid sol-gel polymer containing reversible tetrasulfide groups as a protective coating for the AA2024-T3 substrate is presented. Depending on the constituent ratio, the developed polymer exhibited a hydrophobic surface, high adhesion strength, and an effective long-term corrosion protection in 0.5 M NaCl solution. Upon thermal treatment, the healable hybrid sol-gel coating demonstrated full restoration of the barrier properties as well as recovery of the coating adhesion and surface properties (e.g., hydrophobicity and surface topology) necessary for lifetime extension of corrosion protective coatings. Excellent long-term barrier restoration of the coating was only obtained if the scratch width was less than the coating thickness.

  20. Inkjet printing of sol-gel synthesized hydrated tungsten oxide nanoparticles for flexible electrochromic devices.

    Costa, Cláudia; Pinheiro, Carlos; Henriques, Inês; Laia, César A T


    Tungsten oxide nanoparticles were synthesized via a sol-gel route using metallic tungsten as precursor, and were printed on a flexible electrode using inkjet printing in order to build solid-state electrochromic cells. Several spectroscopic techniques were used to characterize and compare tungsten oxide particles obtained from different origins. FTIR, Raman and X-ray diffraction spectroscopic measurements showed that the sol-gel synthesis described here produces nanoparticles mainly in an amorphous state with hexagonal crystalline domains and allowed the analysis of the hydration extent of those nanoparticles. The size was measured combining dynamic light scattering, sedimentation, and microscopic techniques (AFM), showing a consistent size of about 200 nm. The tungsten oxide nanoparticles were used to produce an ink formulation for application in inkjet printing. Solid-state electrochromic devices were assembled at room temperature, without sintering the tungsten oxide printed films, showing excellent contrast between on/off states. Electrochemical characterization of those films is described using cyclic voltammetry. The devices were then tested through spectroelectrochemistry by Visible/NIR absorption spectroscopy (400-2200 nm range), showing a dual spectroscopic response depending on the applied voltage. This phenomenon is attributed to the presence of two different crystalline states in accordance with results obtained from the spectroscopic characterization of the nanoparticles. The electrochromic cells had a good cycling stability showing high reversibility and a cyclability up to more than 50,000 cycles with a degradation of 25%. © 2012 American Chemical Society

  1. Synthesis of ZnO-CuO Nanocomposite Aerogels by the Sol-Gel Route

    Rula M. Allaf


    Full Text Available The epoxide addition sol-gel method has been utilized to synthesize porous zinc-copper composite aerogels in the zinc-to-copper molar ratios of 50 : 50 to 90 : 10. A two-step mixing approach has been employed to produce aerogels composed of nano- to micrometer sized particles. The aerogels were characterized by ultrahigh resolution scanning electron microscopy, transmission electron microscopy, and powder X-ray diffraction. The as-synthesized aerogels had a thin flake- or petal-like microstructure comprised of clustered flakes on two size scales; they were identified as being crystalline with the crystalline species identified as copper nitrate hydroxide, zinc hydroxide chloride hydrate, and zinc hydroxide nitrate hydrate. Annealing of the aerogel materials at a relatively low temperature (400°C resulted in a complete phase transition of the material to give highly crystalline ZnO-CuO aerogels; the aerogels consisted of networked nanoparticles in the ~25–550 nm size range with an average crystallite size of ~3 nm and average crystallinity of 98%. ZnO-CuO aerogels are of particular interest due to their particular catalytic and sensing properties. This work emphasizes the versatility of this sol-gel route in synthesizing aerogels; this method offers a possible route for the fabrication of aerogels of different metal oxides and their composites.

  2. Energy harvesting using piezoelectric thick films fabricated by a sol-gel process

    Shih, J.L. [McGill Univ., Montreal, PQ (Canada). Dept. of Electrical and Computer Engineering; Kobayashi, M.; Moisan, J.F.; Jen, C.K. [National Research Council of Canada, Boucherville, PQ (Canada). Industrial Materials Inst.


    Energy harvesting has been touted as a promising technology to power wireless devices. One of the common energies to be harvested is induced by mechanical vibrations. Piezoelectric materials are often used to get such energy. This study focused on a vibration-based energy harvesting device. Very flexible vibrators using lead-zirconate-titanate (PZT) ceramics were needed. Therefore, a sol-gel spray technology was used to fabricate PZT thick film directly onto metal membranes to serve as mechanical vibrators. The sol-gel process is an economical approach with excellent mass production appeal for both unimorph and bimorph sensors. For this study, the density of the PZT film was less than 85 per cent of the bulk PZT. Using a 20 mm diameter unimorph, the voltage generated from a 5 mm deflection displacement was 13.6 volts peak-to-peak at 10 Hz. With a load resistance of 150 K ohms, the measured average power generated by this sensor was estimated to be 41 {mu}W. A vibration test that lasted for 60 days with a frequency of 10 Hz and at a displacement of approximately 1 mm showed that the sensor is both durable and rugged. 14 refs., 7 figs.

  3. 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.

  4. 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.

  5. Synthesis of Nanocrystalline La1-xSrxCrO3 by Sol-Gel Method

    Ao Qing; Zhao Xinming; Li Dehui; Sun Liangcheng


    The nanocrystalline La1-xSrxCrO3 was prepared by sol-gel method using La( NO3 )3 · 6H2O, Sr( NO3 )2 and respectively. The phase transformation from dry-gel to crystal was investigated by means of TG, DSC and XRD. Influences of temperature and Sr quantity on particle-diameters were observed by HREM. The experimental results show that the best calcined temperature is near 800 ℃. The particle-diameters decrease with the increase of Sr quantity. The chromite phase formed continuously during crystallization process, which is mainly composed of four steps: ( 1 ) Carbonates first formed by decomposing metal citrates. (2) The decomposition of carbonates occurred metal oxides. (3) La0. 9Sr0.1 CrO4 were synthesized by the reaction of metal oxides. (4) Chromite phase formed lastly due to the decomposition of chromate phase.

  6. Preparation and characterization of quercetin-loaded silica microspheres stabilized by combined multiple emulsion and sol-gel processes

    Kim Young Ho


    Full Text Available Despite exhibiting a wide spectrum of cosmeceutical properties, flavonoids and related compounds have some limitations related to their stability and solubility in distilledwater. In this project, we prepared silica microspheres using a novel method that uses polyol-in-oil-in-water (P/O/W emulsion and sol-gel methods as techniques for stabilizing quercetin. A stable microsphere suspension was successfully preparedusing a mixed solvent system comprising a polyol-phase medium for performing the sol-gel processing of tetraethyl orthosilicate (TEOS as an inorganic precursor with outer water phase. The morphology of the microsphere was evaluated using a scanning electron microscope (SEM, which showed a characteristic spherical particle shape with a smooth surface. Furthermore, SEM/EDSanalysis of a representative microsphere demonstrated that the inner structure of the silica microspheres was filled with quercetin. The mean diameter of the microsphere was in the range 20.6-35.0 μm, and the encapsulation efficiency ranged from 17.8% to 27.5%. The free and encapsulated quercetin samples were incubated in separateaqueous solutions at 25 and 42°C for 28 days. The residualcontent of the quercetin encapsulated by silica microspheres was 82% at 42°C. In contrast, that of the free quercetin stored at 42°C decreased to ~24%.

  7. 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...

  8. 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.

  9. 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.

  10. Reactive Molecular Dynamics Investigations of Alkoxysilane Sol-Gel and Surface Coating Processes

    Deetz, Joshua David

    The ability to generate nanostructured materials with tailored morphology or chemistry is of great technological interest. One proven method of generating metal-oxide materials, and chemically modifying metal-oxide surfaces is through the reactions of molecular building blocks known as alkoxysilanes. Alkoxysilanes are a class of chemicals which contain one or more organic alkoxy groups bonded to silicon atoms. Alkoxysilane (Si-O-R) chemical groups can undergo reactions to form bridges (Si-O-M) with metal oxides. Due to their ability to "attach" to metal-oxides through condensation reactions, alkoxysilanes have a number of interesting applications, such as: the generation of synthetic siloxane materials through the sol-gel process, and the formation of functionalized surface coatings on metal-oxide surfaces. Despite widespread study of sol-gel and surface coatings processes, it is difficult to predict the morphology of the final products due to the large number of process variables involved, such as precursor molecule structure, solvent effects, solution composition, temperature, and pH. To determine the influence of these variables on the products of sol-gel and coatings processes reactive molecular dynamics simulations are used. A reactive force field was used (ReaxFF) to allow the chemical bonds in simulation to dynamically form and break. The force field parameters were optimized using a parallel optimization scheme with a combination of experimental information, and density functional theory calculations. Polycondensation of alkoxysilanes in mixtures of alcohol and water were studied. Steric effects were observed to influence the rates of hydrolysis and condensation in solutions containing different precursor monomers. By restricting the access of nucleophiles to the central silicon atom, the nucleation rate of siloxanes can be controlled. The influence of solution precursor, water, and methanol composition on reaction rates was explored. It was determined that

  11. 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.

  12. Biosorption of uranium and copper by Bacillus Sphaericus JG-A12 cells, spores and S-layer proteins embedded in sol-gel ceramics

    Raff, J.; Soltmann, U.; Boettcher, H. [Arbeitsgruppe Funktionelle Schichten, GMBU e.V., Dresden (Germany); Matys, S.; Pompe, W. [Inst. fuer Materialwissenschaft, Technische Univ. Dresden (Germany); Selenska-Pobell, S.


    Vegetative cells, spores and stabilized S-layer sheets of B. sphaericus JG-A12 were embedded in SiO{sub 2} bulk particles using sol-gel techniques. In sorption experiments the metal binding capacity of the free biocomponents and the corresponding biological ceramics were compared. (orig.)

  13. 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.

  14. Probing sol-gel matrices microenvironments by PGSE HR-MAS NMR.

    Ferreira, Ana S D; Barreiros, Susana; Cabrita, Eurico J


    We applied Pulsed Gradient Spin Echo diffusion with high-resolution magic angle spinning NMR to study sol-gel matrices used to encapsulate enzymes for biocatalysis (TMOS/MTMS and TMOS/BTMS) to gain insight into the local chemical microenvironment. Transport properties of solvents with different polarities (1-pentanol, acetonitrile and n-hexane) were studied through their apparent self-diffusion coefficients. The spin echo attenuation of the solvents shows two distinct diffusion domains, one with fast diffusion (Dfast ) associated with interparticle diffusion and another with slow diffusion (Dslow ) corresponding to the displacement inside the pores within the sol-gel particles. The analysis of the root mean square displacements at different diffusion times showed that the Dfast domain has a free diffusion regime in both matrices (the root mean square displacement is linearly dependent of the diffusion time), while the Dslow domain shows a different regime that depends on the matrix. We investigated the exchange regime between the two diffusion sites. In both matrices, n-hexane was in intermediate exchange between diffusion domains, while the polar solvents were in slow exchange in TMOS/BTMS and in intermediate exchange in TMOS/MTMS. Data were fitted for TMOS/BTMS with the Kärger model, and the physical parameters were obtained. The results add to the evidence that the pores are a hydrophobic environment but that the presence of some free hydrophilic groups inside the pore, as observed in the TMOS/BTMS, has a key role in slowing down the exchange of polar solvents and that this is relevant to explain previously reported enzyme activity in these materials. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  15. Comparing nanostructured hydroxyapatite coating on AZ91 alloy samples via sol-gel and electrophoretic deposition for biomedical applications.

    Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan


    Magnesium is one of the most critical elements in hard tissues regeneration and therefore causes speeding up the restoration of harmed bones, while high deterioration rate of magnesium in body fluid restricts it to be used as biodegradable implants. Alloying magnesium with some relatively nobler metals such as aluminium, zinc, rare earth elements, magnesium-bioceramics composites, and surface modification techniques are some of the routes to control magnesium corrosion rate. In this study AZ91 magnesium alloy had been coated by nanostructured hydroxyapatite via sol-gel dip coating and electrophoretical methods to survey the final barricade properties of the obtained coatings. In order to perform electrophoretic coating, powders were prepared by sol-gel method, and then the powders deposited on substrates utilizing direct current electricity. Zeta potentials of the electrophoresis suspensions were measured to determine a best mode for good quality coatings. Transmission Electron Microscopy (TEM), and Scanning Electron Microscopy (SEM) were used to confirm nanoscale dimension, and the uniformity of the nanostructured hydroxyapatite coating, respectively. Fourier Transform-Infrared and X-ray diffraction analysis were utilized for functional group and phase structure evaluation of the prepared coatings, correspondingly. Electrochemical corrosion tests were performed in SBF at 37±1 (°)C which revealed considerable increase in corrosion protection resistivity and corrosion current density for electrophoretic coated specimens versus sol-gel coated specimens. Results showed that both sol-gel and electrophoretical techniques seem to be suitable to coat magnesium alloys for biomedical applications but electrophoretic coating technique is a better choice due to the more homogeneity and more crystalline structure of the coating.

  16. Sol-Gel Synthesis and Luminescent Characteristic of Doped Eu3+ Silicate-Silica Phosphor

    Yang Liangzhun; Yu Xibin; Yang Shiping; Zhou Pingle; Tang Jinfeng; Peng Xiudong


    Eu-doped silicate complex gel nano-particles was obtained by sol-gel process and characterized with TEM, XRD, PL, etc. The well dispersed particles have particle size about 60~70 nm with specific surface area 98.3 m2·g-1. The complex gel phosphor gives a broad and strong luminescent emission originating from Eu2+ ions centered at 425 nm. The emission band shifts to shorter wavelengths with the increase of the ion radius of the alkali earth metals, but the band becomes red-shifted gradually with the increase of the ion radius of the alkali metals(except Li+). These divalent Eu2+ ions originate in inequivalent substitution of the alkaline earth ions. The presence of alkaline ions is favorable for the increasing emission intensity of the Eu2+ and lowering crystalline temperature of the silicate complex gel.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. Formulation and Performance of Novel Energetic Nanocomposites and Gas Generators Prepared by Sol-Gel Methods

    Clapsaddle, B J; Zhao, L; Prentice, D; Pantoya, M L; Gash, A E; Satcher Jr., J H; Shea, K J; Simpson, R L


    In the field of composite energetic materials, properties such as ingredient distribution, particle size, and morphology affect both sensitivity and performance. Since the reaction kinetics of composite energetic materials are typically controlled by the mass transport rates between reactants, one would anticipate new and potentially exceptional performance from energetic nanocomposites. We have developed a new method of making nanostructured energetic materials, specifically explosives, propellants, and pyrotechnics, using sol-gel chemistry. A novel sol-gel approach has proven successful in preparing nanostructured metal oxide materials. By introducing a fuel metal, such as aluminum, into the nanostructured metal oxide matrix, energetic materials based on thermite reactions can be fabricated. Two of the metal oxides are tungsten trioxide and iron(III) oxide, both of which are of interest in the field of energetic materials. Due to the versatility of the preparation method, binary oxidizing phases can also be prepared, thus enabling a potential means of controlling the energetic properties of the subsequent nanocomposites. Furthermore, organic additives can also be easily introduced into the nanocomposites for the production of nanostructured gas generators. The resulting nanoscale distribution of all the ingredients displays energetic properties not seen in its micro-scale counterparts due to the expected increase of mass transport rates between the reactants. The unique synthesis methodology, formulations, and performance of these materials will be presented. The degree of control over the burning rate of these nanocomposites afforded by the compositional variation of a binary oxidizing phase will also be discussed. These energetic nanocomposites have the potential for releasing controlled amounts of energy at a controlled rate. Due to the versatility of the synthesis method, a large number of compositions and physical properties can be achieved, resulting in

  10. 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.

  11. 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...

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. Sol-gel fabrication of lithium doped zinc oxide thin films

    Oral, A.Y.; Bahsi, Z.B. [Dept. of Materials Science and Engineering, Gebze Inst. of Tech., Kocaeli (Turkey); Aslan, M.H.; Basaran, E. [Dept. of Physics, Gebze Inst. of Tech., Kocaeli (Turkey)


    Li doped zinc oxide thin films were deposited on glass substrates by a sol-gel technique. Acetates of zinc and lithium were used as metal sources. A homogeneous and stable solution was prepared by dissolving acetates in the solution of 2-propanol and ethanolamine. ZnO:Li thin films were obtained after preheating the spin coated films at 250 C for 1 minute after each coating. A post annealing between 450-600 C was applied after the deposition of the last layers. XRD analysis revealed ZnO with zincite structure (Card no: 36-1451) in all films. The thickness of the films was measured as 75 nm per layer. The optical band gap of the films increased as doping concentration of Li increased and decreased as the post-annealing temperature increased. (orig.)

  17. Integrated ultrasonic transducers made by the sol gel spray technique for structural health monitoring

    Kobayashi, M.; Jen, C.-K.; Moisan, J.-F.; Mrad, N.; Nguyen, S. B.


    Integrated piezoelectric-based ultrasonic transducers (UTs) have been developed for potential structural health monitoring. Fabrication techniques and performance evaluation of these transducers at selected monitoring sites are presented. Our novel transducer fabrication approach focuses on the use of handheld and readily accessible equipment to perform sol-gel spray coating, including the use of a heat gun or a torch, to carry out drying and firing, poling and electrode fabrication. The application of these integrated UTs for thickness measurement of graphite/epoxy composites, thickness monitoring of ice build up on aluminum plates at low temperatures, viscosity measurement of a cooling oil flow at temperatures up to 160 °C and monitoring metal debris in cooling oil engines is demonstrated.

  18. Sol-gel hybrid films based on organosilane and montmorillonite for corrosion inhibition of AA2024.

    Dalmoro, V; dos Santos, J H Z; Armelin, E; Alemán, C; Azambuja, D S


    The present work reports the production of films on AA2024-T3 composed of vinyltrimethoxysilane (VTMS)/tetraethylorthosilicate (TEOS) with incorporation of montmorillonite (sodium montmorillonite and montmorillonite modified with quaternary ammonium salt, abbreviated Na and 30B, respectively), generated by the sol-gel process. According to FT-IR analyses the incorporation of montmorillonite does not affect silica network. Electrochemical characterization was performed by electrochemical impedance spectroscopy measurement in 0.05 mol L(-1) NaCl solution. Results indicate that montmorillonite incorporation improves the corrosion protection compared to the non-modified system. Scanning electron microscopy micrographs reveal that high concentrations of montmorillonite provide agglomerations on the metallic surface, which is in detriment of the anticorrosive performance. The VTMS/TEOS/30B films with the lowest concentration (22 mg L(-1)) of embedded clay provide the highest corrosion protection.

  19. The morphological characterizations of titanium dioxide (TiO2) via sol-gel method

    Nordin, N. K. S.; Hashim, U.; Vijayakumaran, T.


    Titanium Dioxide (TiO2) has comes with many fascinating properties in environmental purification, photocatalytic activity and in sensor application. TiO2 is prepared by sol-gel method and been coated on the silicon oxide (SiO) and glasses for 1 layer, 3 layers, 5 layers and finally 7 layers to find the best layer for coating purpose. A few characterizations had been carried out such as Scanning Electron Microscope (SEM), Photoluminescence (PL) and Current-Voltage (I-V) measurement for TiO2. The I-V recorded for the presence of Interdigitated Electrode (IDE) is 2.46×10-10 at 1V increased from 2.24×10-10 without the coating of TiO2. TiO2 coated on IDE triggered more sensitive sensor compared to IDE without metal oxides coated.

  20. Ozonation and sol-gel method to obtain Cu/Cu O nanoparticles from cyanidation wastewater

    Soria A, M. J.; Puente S, D. M.; Carrillo P, F. R. [Universidad Autonoma de Coahuila, Facultad de Metalurgia, Carretera 57 Km 4.5, 25710 Monclova, Coahuila (Mexico); Garcia C, L. A. [Centro de Investigacion en Quimica Aplicada, Blvd. Enrique Reyna No. 140, Col. Los Pinos, 25253 Saltillo, Coahuila (Mexico); Velazquez S, J., E-mail: [University of Texas at San Antonio, Department of Physics and Astronomy, San Antonio TX 78249 (United States)


    The extraction process of gold and silver by cyanidation generates large amounts of effluent which also contain contaminants such as cyanide and significant metal values such as copper. This paper presents the results of the removal and recovery of copper from ozonation treatment of a residual aqueous cyanide. The residual solution was treated by ozonation-precipitation to obtain a precipitate of copper. From this, copper nano composites obtained by Pechini modified sol-gel method were obtained. The compounds obtained were characterized by X-ray diffraction, showing a dependence of the type of compounds formed over time of ozonation and heat treatment of the gel. The particle size was measured by scanning electron microscopy and calculated by the Scherrer equation, being between 50 and 120 nm. (Author)

  1. Sol-Gel Precursors for Ceramics from Minerals Simulating Soils from the Moon and Mars

    Sibille, Laurent; Gavira-Gallardo, Jose-Antonio; Hourlier-Bahloul, Djamila


    Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report some preliminary results on the production of sol-gel precursors for ceramic products using mineral resources available in Martian or Lunar soil. The presence of SiO2, TiO2, and A12O3 in both Martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and Lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from Lunar and Martian simulant soils. Clear sol-gel precursors have been obtained by dissolution of silica from Lunar simulant soil in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Thermogravimetric Analysis and X-ray Photoelectron Spectroscopy were used to characterize the elemental composition and structure of the precursor molecules. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors. In the second set of experiments, we used the same starting materials to synthesize silicate esters in acidified alcohol mixtures. Preliminary results indicate the presence of silicon alkoxides in the product of distillation.

  2. Fabrication of channel waveguides from sol-gel-processed polyvinylpyrrolidone/ SiO(2) composite materials.

    Yoshida, M; Prasad, P N


    Sol-gel-processed composite materials of polyvinylpyrrolidone (PVP) and SiO(2) were studied for optical waveguide applications. PVP is a polymer that can be crosslinked, so it is expected to have high thermal stability after crosslinking. However, thermal crosslinking and thermal decomposition of pure PVP take place around the same temperature, 200 °C, therefore pure PVP had a high optical propagation loss as a result of the absorption of the decomposed molecules after crosslinking. The incorporation of sol-gel-processed SiO(2) prevented the thermal decomposition of PVP and provided remarkably low optical propagation losses. The PVP/SiO(2)composite material also produced thick (>2-µm) crack-free films when the PVP concentration was 50% or higher. An optical propagation loss of 0.2 dB/cm was achieved at 633 nm in the 50% PVP/SiO(2) composite planar waveguide. Several aspects of the thermal stability of the waveguides were evaluated. The slab waveguide was then used for fabrication of channel waveguides with a selective laser-densification technique. This technique used metal lines fabricated with photolithography on the slab waveguide as a light absorbent, and these metal lines were heated by an Ar laser. The resultant channel waveguide had an optical propagation loss of 0.9 dB/ cm at 633 nm. This technique provides lower absorption loss and scattering loss compared with the direct laser-densification technique, which uses UV lasers, and produces narrow waveguides that are difficult to fabricate with a CO(2) laser.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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)

  11. 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.

  12. 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.

  13. 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.

  14. Hidrogenación de Metil Oleato con Catalizadores de Ru-Sn/Al2O3: Método Sol-gel vs. Impregnación Hydrogenation of Methyl Oleate over Ru-Sn/Al2O3 Catalysts: Sol-gel Method vs. Impregnation Method

    David A Echeverri


    Full Text Available En este trabajo se evalúa el efecto del método de preparación, sol-gel e impregnación, sobre la conversión y selectividad a alcohol oleílico en la hidrogenación de metil oleato comercial con catalizadores de Ru-Sn/Al2O3 a 270ºC y 5 MPa. Los catalizadores se caracterizaron mediante SEM con EDS, TPR, DRX y área superficial por adsorción de nitrógeno. Con el método sol-gel se logró una alta dispersión de los metales en el soporte, sin embargo los catalizadores sintetizados por ese método presentaron menor reducibilidad. Para ambos métodos se encontró una relación óptima Sn/Ru que permitió obtener mayor porcentaje de alcohol insaturado. En el caso del método de impregnación esta relación fue 2 y en el del sol-gel fue 1. No obstante con el método de impregnación se obtuvo mayores conversiones y mayor selectividad hacia el alcohol insaturado que con el sol-gel para la relación optima Sn/Ru.In this work, the effect of the preparation method (sol-gel vs. impregnation over conversion and selectivity to oleyl alcohol in the hydrogenation of methyl oleate over Ru-Sn/Al2O3 catalysts at 270ºC and 5 MPa was evaluated. The catalysts were characterized by SEM-EDS, TPR, XRD and surface area by nitrogen adsorption. The sol-gel method produced high dispersion of metals in the support, however catalysts prepared by sol-gel method were less reducible. For both methods an optimum Sn/Ru atomic ratio that allowed higher percentage of unsaturated alcohol was found. For the impregnation method this atomic ratio was 2 and for sol-gel method was 1. However, higher conversions and higher selectivity toward the oleyl alcohol were obtained with the impregnation method, using the optimum atomic ratio,

  15. Recobrimento da liga Ti-6Al-4V com hidroxiapatita pelo método sol-gel e sua aplicação a hastes femorais não-cimentadas Coating of Ti-6Al-4V alloy with hydroxyapatite by using sol-gel method and its application to non-cemented femoral stem

    E. P. Avés


    Full Text Available O recobrimento de ligas metálicas com cerâmicas bioativas visa acelerar a formação óssea ao redor do implante, contribuindo para a sua estabilização. Neste trabalho estudou-se a fase cerâmica de hidroxiapatita depositada pelo processo sol-gel em chapas da liga metálica Ti-6Al-4V. A camada de recobrimento foi caracterizada por microscopia eletrônica de varredura, por difração de raios X e sua adesão ao substrato foi avaliada pelo teste de cisalhamento O teste de citocompatibilidade mostrou que o processo de recobrimento por sol-gel não promoveu morte celular significativamente maior que o controle (p > 0,05. Além disso, hastes femorais removidas de pacientes (explantes foram adequadamente recobertas utilizando-se o processo sol-gel.The coating of metallic alloys with bioactive ceramics aims to accelerate bone formation around the implant, contributing to its fixation. In this paper, the deposition of hydroxyapatite ceramic on Ti-6Al-4V alloy sheets by the sol-gel method was studied. The coating layer was characterized by scanning electron microscopy, X-ray diffraction and its adhesion to substrate was evaluated by shear testing. The citocompatibility test shows that the sol-gel coating did not provoke the cell death significantly higher than the control (p > 0.05. Moreover, femoral stems removed from patient (explants were adequately coated using the sol-gel process.

  16. Low temperature sol-gel process for optical coatings based on magnesium fluoride and titanium dioxide; Niedertemperatur Sol-Gel Verfahren fuer optische Schichtsysteme auf Basis von Magnesiumfluorid und Titandioxid

    Krueger, Hannes


    This work deals with the development of a low temperature sol-gel spincoating process for thin films with thicknesses in the nanometer range based on metal oxides and metal fluorides. Optical films such as anti-reflective (AR) or high reflective coatings are of much interest and consist of alternating dielectric layers of low and high refractive index materials. Regarding the general procedure for the metal fluorides a novel nonaqueous sol-gel synthesis starting from metal alkoxides and alcohol-dissolved HF was used. The coatings were dried and calcined at 100 C. The morphology of these films was characterised with REM, TEM and AFM. EDX and XPS were used to identify the chemical composition and ellipsometry and UV-vis spectroscopy to determine the optical properties of the films. This new process allows the preparation of homogeneous magnesium fluoride and titanium dioxide layers with low roughness (R{sub a} {<=} 1,9 nm) on silicon and quartz substrates. The magnesium fluoride layers are partially amorphous or microcrystalline with crystallite sizes from 2 nm to 10 nm. The titanium dioxide layers are predominantly amorphous. The thicknesses of the magnesium fluoride and titanium dioxide single layers were adjustable between 25 nm and 500 nm depending on the number of coating steps and on the concentration of the used sols. The magnesium fluoride layers had a refractive index of n{sub 500} = 1,36 and the titanium dioxide layers a refraction index of n{sub 500} = 2,05. For the first time, an alternating metal fluoride and oxide multilayer system was produced with a low temperature sol-gel method (consisting of magnesium fluoride and titanium dioxide). Based on the determined optical constants of the magnesium fluoride and titanium dioxide single layers, AR and HR multilayer systems were calculated and fabricated. The transmission spectra of the designs and the corresponding multilayer were in good agreement. Similar results were obtained with the reflection spectra

  17. 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...

  18. Rare Earth based Sol-Gel Materials: An Intra- and Inter- Collegiate Collaborative Research Project

    Silversmith, Ann


    Sol-gel glasses containing rare earth (RE) impurities form an exciting class of new optical materials with potential uses as phosphors and solid state laser media. The low temperature glass synthesis based on the liquid organic precursor tetramethoxysilane allows incorporation of higher RE concentrations than in traditional melt glasses without compromising the amorphous character of the material. The synthesis and spectroscopic characterization of these materials have together formed the basis for a fruitful interdisciplinary and multi-institutional research collaboration. All materials used in this project are made by Hamilton College chemistry students; spectroscopy experiments are performed by students and faculty in the physics departments at Hamilton, Franklin and Marshall, and Davidson Colleges. In this talk results from two ongoing spectroscopic investigations will be presented, both connected to the long-term goal of improving the low fluorescence efficiency of these materials. The first is the chelation of the RE metal to create an enhanced fluorescence excitation path and to physically separate the RE from the sol-gel matrix. Chelating molecules absorb strongly in the uv, and subsequent energy transfer can produce intense visible emission from the RE. Results are presented for the chelating agent 2,6-pyridine-dicarboxylic acid (PDC) bound to europium ions and incorporated into gels. Red emission from europium follows excitation into the PDC absorption band below 300nm. The second investigation focuses on fluorescence quenching of blue emission from trivalent terbium. Two separate mechanisms -energy transfer from terbium to residual hydroxide ions and among terbium ions - lead to reduced intensity of the blue emission lines relative to other longer wavelength signals.

  19. Application of ultrasound irradiation on sol-gel technique for corrosion protection of Al65Cu20Fe15 alloy powder

    Liang, Bo; Zhang, Baoyan; Wang, Guodong; Li, Di; Zhang, Xiaoming


    Al65Cu20Fe15 alloy powder was firstly encapsulated by the conventional sol-gel technique utilizing tetraethoxysilane (TEOS) as the precursor in order to improve its corrosion resistance. The optimization was based on nine well-planned orthogonal experiments (L9 (34)). Four main factors in the encapsulation process (i.e. reaction temperature, ethylenediamine concentration, TEOS concentration and feeding method) were investigated. According to the visual analyses of the result, the optimum condition was obtained. Based on the optimal condition in the conventional sol-gel technique, the encapsulation process was then conducted under ultrasonic irradiation. The effects of ultrasound amplitude and irradiation time on the encapsulation process were also studied. FTIR, XRD, SEM, DLS and EDS were also used to characterize the resulting sample. Finally, the corrosion inhibition efficiency of encapsulated powder attained 99.3% in the acidic condition of pH 1, and the average grain size (d50) of the encapsulated powder was just 4.8% larger than that of the raw powder, implying that there was a thin silica film on the surface of powder.

  20. 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.

  1. RBS and HIRBS studies of nanostructured AgSiO{sub 2} sol-gel thin coatings

    Kokkoris, M. E-mail:; Trapalis, C.C. E-mail:; Kossionides, S.; Vlastou, R.; Nsouli, B.; Groetzschel, R.; Spartalis, S.; Kordas, G.; Paradellis, Th


    In the present work, composite AgSiO{sub 2} thin coatings, containing metal nanoparticles, were prepared on glass substrates by the sol-gel route. The coatings were thermally treated in oxidative and reductive conditions up to 500 deg. C for metal nanoparticle formation. The coating structure and the nanoparticle formation were studied by atomic force microscopy and Rutherford backscattering spectroscopy (RBS) techniques. In the case of RBS, 1.4 MeV {sup 4}He{sup +} ions were used for all samples, and low energy {sup 16}O and {sup 12}C ions in selected ones (heavy ion RBS, HIRBS), in order to improve the depth resolution for the profiling of the metal component. The antibacterial activity against Escherichia coli is examined by antibacterial drop test. The coatings exhibited a high antibacterial activity, which was enhanced with the increase of the metal concentration and was reduced with the increase of the particle size of the metal nanoparticles. The possible correlation between the layer interdiffusion after the thermal treatment and the antibacterial activity is examined and analyzed. Although further studies are required, RBS and HIRBS seem to be excellent tools for the quality control in the production of sol-gel thin coatings.

  2. Computational investigation and synthesis of a sol-gel imprinted material for sensing application of some biologically active molecules

    Atta, Nada F., E-mail: [Department of Chemistry, Faculty of Science, University of Cairo, Post Code 12613, Giza (Egypt); Hamed, Maher M.; Abdel-Mageed, Ali M. [Department of Chemistry, Faculty of Science, University of Cairo, Post Code 12613, Giza (Egypt)


    A hybrid sol-gel material was molecularly imprinted with a group of neurotransmitters. Imprinted material is a sol-gel thin film that is spin coated on the surface of a glassy carbon electrode. Imprinted films were characterized electrochemically using cyclic voltammetry (CV) and the encapsulated molecules were extracted from the films and complementary molecular cavities are formed that enable their rebind. The films were tested in their corresponding template solutions for rebinding using square wave voltammetry (SWV). Computational approach for exploring the primary intermolecular forces between templates and hydrolyzed form of the precursor monomer, tetraethylorthosilicate (TEOS), were carried out using Hartree-Fock method (HF). Interaction energy values were computed for each adduct formed between a monomer and a template. Analysis of the optimized conformations of various adducts could explain the mode of interaction between the templates and the monomer units. We found that interaction via the amino group is the common mode among the studied compounds and the results are in good agreement with the electrochemical measurements.

  3. Immobilization of membrane-bounded (S)-mandelate dehydrogenase in sol-gel matrix for electroenzymatic synthesis.

    Mazurenko, Ievgen; Ghach, Wissam; Kohring, Gert-Wieland; Despas, Christelle; Walcarius, Alain; Etienne, Mathieu


    Membrane-bounded (S)-mandelate dehydrogenase has been immobilized on the surface of glassy carbon and carbon felt electrodes by encapsulation in a silica film obtained by sol-gel chemistry. Such bioelectrochemical system has been used for the first time for electroenzymatic conversion of (S)-mandelic acid to phenylglyoxylic acid. Apparent Km in this sol-gel matrix was 0.7 mM in the presence of ferrocenedimethanol, a value in the same order of magnitude as reported previously for vesicles in solution with other electron acceptors, i.e., Fe(CN)6(3-) or 2,6-dichloroindophenol. The bioelectrode shows very good operational stability for more than 6 days. This stability was definitively improved by comparison to a bioelectrode prepared by simple adsorption of the proteins on the electrode surface (fast activity decrease during the first 15 h of experiment). Optimal electroenzymatic reaction was achieved at pH9 and 40 °C. Apparent Km of the protein activity was 3 times higher in carbon felt electrode than on glassy carbon surface, possibly because of transport limitations in the porous architecture of the carbon felt. A good correlation was found between electrochemical data and chromatographic characterization of the reaction products in the bioelectrochemical reactor.

  4. Effect of Pt Concentration on the Grain Growth of TiO2sol-gel Films

    Jia Y.J.


    Full Text Available Pt metallic has been supported on TiO2 surface using different methods, Here, Pt doped TiO2 (Pt-TiO2 sol gel thin film were successfully produced by reducing chloroplatinc acid (H2PtCl6. The structures of prepared composites were investigated using X-ray diffraction (XRD. The physical morphologies of the composites were examined using transmission electron microscope (TEM. The grain size of Pt-TiO2 thin film after annealing was also measured by atomic force microscope (AFM images.

  5. Synthesis of titanates MTiO{sub 3} (M = Mn, Co, Ni) by the sol-gel method

    Moreno, J.; Tavizon, G.; Vicente, L. [UNAM, Mexico City (Mexico). Dept. de Fisica y Quimica Teorica; Viveros, T. [UAM-Iztapalapa, Mexico City (Mexico). Dept. de Ingenieria Quimica


    The titanates MTiO{sub 3} (M = Ni, Co, Mn) were prepared by a sol-gel method. The reaction between the metal solution and titanium butoxide leads to the formation of gels. The amorphous gels so obtained under different pH conditions, were calcined at temperatures between 750 C and 1,200 C to obtain in some cases high purity, crystalline MTiO{sub 3} powders. The characterization of the samples was done by X-ray powder diffraction, differential thermal analysis (DTA), thermal gravimetry (TG) and BET surface measurements.

  6. Effect of citric acid on formation of oxides of Cu and Zn in modified sol-gel process: A comparative study



    We report here the influence of citric acid concentration on the formation of sol-gel products ineach of Cu and Zn systems by using respective metal nitrate as precursor and citric acid as gelling agent. Thesynthesized sol-gel products were characterized by X-ray diffraction (XRD), scanning electron microscope(SEM), energy dispersive X-ray analysis (EDX), Fourier transform infra-red (FT-IR) spectroscopy and UVVisiblediffused reflectance spectroscopy (UV-Vis DRS). The influence of citric acid concentration on theformation of metal/metal oxide in each case was primarily investigated by varying the molar ratio of each metalnitrate (N) and citric (C) acid (N:C = 1:1, 1:2, 1:4, 1:6 and 1:8). It was observed that at low N:C molar ratios(1:1) and (1:2), the Cu system had only CuO and at high N:C molar ratio, lower oxidation state of copper(Cu2O and Cu) has resulted. Distinctly, irrespective of the N:C molar ratio, the sol-gel product of Zn systemwas only single phase of ZnO. The SEM observations confirmed that the grains of these two metal systemswere spherical in nature. In each metal system, at high N:C molar ratio, small grain size has resulted. At highN:C ratio, lower oxidation state of metal ion is resulted where the metal system is susceptible for reduction. Thesusceptibility of metal ions to undergo reduction controlled the formation of end products in the sol-gel process.

  7. 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.

  8. 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.

  9. Smart electrochemical sensor for some neurotransmitters using imprinted sol-gel films.

    Atta, Nada F; Abdel-Mageed, Ali M


    A hybrid sol-gel material formed by acid hydrolysis of a mixture of tetraethylorthosilicate (TEOS) and phenyltriethylorthosilicate (PTEOS) as functional monomers was imprinted by tyramine and dopamine as template molecules for the purpose of molecular recognition. Imprinted materials were spin coated as thin films on the surface of glassy carbon electrodes and then were characterized using cyclic voltammetry (CV). After extraction of the encapsulated molecules, imprinted films were tested in solutions of their templates and other molecules. Rebinding experiments were followed by electrochemical characterization using square wave voltammetry (SWV). Imprinted films showed higher affinities toward their template molecules compared to other structurally similar molecules especially for tyramine imprinted film. With the exception of tyramine and norepinephrine, the interference level did not exceed 5% for all compounds studied for dopamine-imprinted films. Tyramine-imprinted films however showed high affinity to tyramine with dopamine 40% interference. Some factors related to the rebinding ability process like pH of solution, concentration of template were studied. The sensing surface lifetime extended to 2 weeks with decay in response signal that ranged from 22%, 40% to 60% for dopamine, tyramine and norepinephrine, respectively. The standard deviation from the mean of measurements for the repeated experiments is 7.4%. Electrochemical impedance spectroscopy (EIS) measurements confirmed the results obtained by electrochemical measurements. Morphological characteristics of the imprinted thin films and their thickness were investigated using scanning electron microscope (SEM).

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. "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.

  18. 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.

  19. 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:

  20. 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.

  1. 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.

  2. Relationship between sol-gel conditions and enzyme stability: a case study with β-galactosidase/silica biocatalyst for whey hydrolysis.

    Escobar, Sindy; Bernal, Claudia; Mesa, Monica


    The sol-gel process has been very useful for preparing active and stable biocatalysts, with the possibility of being reused. Especially those based on silica are well known. However, the study of the enzyme behavior during this process is not well understood until now and more, if the surfactant is involved in the synthesis mixture. This work is devoted to the encapsulation of β-galactosidase from Bacillus circulans in silica by sol-gel process, assisted by non-ionic Triton X-100 surfactant. The correlation between enzyme activity results for the β-galactosidase in three different environments (soluble in buffered aqueous reference solution, in the silica sol, and entrapment on the silica matrix) explains the enzyme behavior under stress conditions offered by the silica sol composition and gelation conditions. A stable β-galactosidase/silica biocatalyst is obtained using sodium silicate, which is a cheap source of silica, in the presence of non-ionic Triton X-100, which avoids the enzyme deactivation, even at 40 °C. The obtained biocatalyst is used in the whey hydrolysis for obtaining high value products from this waste. The preservation of the enzyme stability, which is one of the most important challenges on the enzyme immobilization through the silica sol-gel, is achieved in this study.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Nanocrystalline nickel ferrite particles synthesized by non-hydrolytic sol-gel method and their composite with biodegradable polymer.

    Yin, H; Casey, P S; Chow, G M


    Targeted drug delivery has been one of the most important biomedical applications for magnetic particles. Such applications require magnetic particles to have functionalized surfaces/surface coatings that facilitate their incorporation into a polymer matrix to produce a polymer composite. In this paper, nanocrystalline nickel ferrite particles with an oleic acid surface coating were synthesized using a non-hydrolytic sol-gel method and incorporated into a biodegradable polymer matrix, poly(D,L-lactide) PLA prepared using a double emulsion method. As-synthesized nickel ferrite particles had a multi-crystalline structure with chemically adsorbed oleic acid on their surface. After forming the PLA composite, nickel ferrite particles were encapsulated in PLA microspheres. At low nickel ferrite concentrations, composites showed very similar surface charges to that of PLA. The composites were magnetically responsive and increasing the nickel ferrite concentration was found to increase magnetization of the composite.

  15. Preparation and Characterization of CuO Nanoparticles by Novel Sol-Gel Technique

    Y. Aparna


    Full Text Available Recent developments of nanosize materials of metal and metal oxide particles are intensively pursued because of their prominence in different fields of applications. Among all the transition metal oxides, CuO is a potential candidate for the application of magnetic storage devices, solar energy transfer, sensors, and super capacitors etc. Moreover CuO nanoparticles act as a good catalyst in some of the chemical reactions. CuO nanoparticles were prepared by novel sol-gel method. In this technique CuCl2.6H2O is added with acetic acid and heated to 100 °C with continuous stirring. To control the ph of the above solution, NaOH is added to the solution till ph reached desired value. The color of the solution changed from blue to black with precipitation. The black precipitation was washed 3 – 4 times with distilled water. Finally the solution was centrifuged and dried in air for one day. The CuO nanoparticles were characterized by studying their structure with X-ray diffraction and composition by energy dispersive X-ray analysis. The size of the nanoparticles is estimated by particle size analyzer and transmission electron microscopy. The optical studies were carried out with Uv-Vis spectrophotometer.

  16. 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

  17. X-ray diffraction line profile analysis of nano-sized cobalt in silica matrix synthesized by sol-gel method

    Sen, Ranjan, E-mail: [Department of Metallurgical and Materials Engineering, Jadavpur University, Kolkata 700032 (India); Das, Gopes Chandra; Mukherjee, Siddhartha [Department of Metallurgical and Materials Engineering, Jadavpur University, Kolkata 700032 (India)


    Nano-sized cobalt particles in silica matrix have been synthesized by sol-gel method to reduce the oxidation of metallic cobalt. Different techniques of the X-ray diffraction line profile analysis (XRDLPA) have been used to determine the microstructural parameters of the nano-sized cobalt. The domain size, microstrain and lattice parameters have been estimated by the modified Rietveld technique and classical Williamson-Hall technique.

  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 Sr_3Al_2O_6:Eu~(2+), Dy~(3+)phosphors prepared by sol-gel-combustion processing

    Huang Ping; Cui Cai-E; Wang Sen


    A type of red luminescent Sr_3Al_2O_6:Eu~(2+), Dy~(3+) phosphor powder is synthesised by sol-gel-combustion processing, with metal nitrates used as the source of metal ions and citric acid as a chelating agent of metal ions. By tracing the formation process of the sol-gel, it is found that it is necessary to reduce the amount of NO_3~- by dropping ethanol into the solution for forming a stable and homogeneous sol-gel. Thermogravimetric and Differential Scanning Calorimeter Analysis, x-ray diffractionmeter, scanning electron microscopy and pbotoluminescence spectroscopy are used to investigate the luminescent properties of the as-synthesised Sr_3Al_2O_6:Eu~(2+), Dy~(3+). The results reveal that the Sr_3Al_2O_6 crystallises completely when the combustion ash is sintered at 1250 ℃. The excitation and the emission spectra indicate that the excitation broadband lies mainly in a visible range and the phosphors emit a strong light at 618 nm under the excitation of 472 nm. The afterglow of (Sr_(0.94)Eu_(0.03)Dy_(0.03))_3Al_2O_6 phosphors sintered at 1250 ℃ lasts for over 1000s when the excited source is cut off.

  1. Sol-gel preparation of ion-conducting ceramics for use in thin films

    Steinhauser, M.I.


    A metal alkoxide sol-gel solution suitable for depositing a thin film of La{sub 0.6}Sr{sub 0.4}CoO{sub 3} on a porous substrate has been developed; such films should be useful in fuel cell electrode and oxygen separation membrane manufacture. Crack-free films have been deposited on both dense and porous substrates by dip-coating and spin-coating techniques followed by a heat treatment in air. Fourier transform infrared spectroscopy was used to determine the chemical structure of metal alkoxide solution system. X-ray diffraction was used to determine crystalline phases formed at various temperatures, while scanning electron microscopy was used to determine physical characteristics of the films. Surface coatings have been successfully applied to porous substrates through the control of the substrate pore size, deposition parameters, and firing parameters. Conditions have been defined for which films can be deposited, and for which the physical and chemical characteristics of the film can be improved. A theoretical discussion of the chemical reactions taking place before and after hydrolysis in the mixed alkoxide solutions is presented, and the conditions necessary for successful synthesis are defined. Applicability of these films as ionic and electronic conductors is discussed.

  2. Fabrication of LaAlO3 film by sol-gel process with corresponding inorganic

    殷明志; 汪敏强; 姚熹


    Well-cubic perovskite lanthanum aluminate (LaAlO3) film on (110) silicon substrate was fabricated by sol-gel method with corresponding inorganic salts. Lanthanum acetate and aluminum acetate glacial acetic acid solutions were prepared via ligand exchange starting from lanthanum nitrate hexahydrate and aluminum nitrate hexahydrate after being refluxed. (CH3CO)2O removed nitrates and the crystallized H2O completely, acetylacetone (AcAc) was partially bidentated with metallic ion of the metallic acetates and formed La(OAc)3(x(AcAc)x, which were hydrolyzed into La(AcAc)3(x(OH)x by adding 10 ml 0.4% methyl cellulose (MCL) solution. The La(AcAc)3(x(OH)x, polymerizing and combining with MCL, formed the LaAlO3 sol precursor with heteropolymeric structure and formed film easily. The epitaxial LaAlO3 film on Si(110) substrate was crystallized after being annealed in thermal annealing furnace for 650(750 (C/30 min. The morphologies and microstructures were characterized. The refractive index of the LAO film was 1.942 to 2.007; the dielectric constant and the dissipation factors were estimated to be 23(26 and 2.1(10(4 ( 2.4(10(4 respectively.

  3. Fabrication of LaAlO3 film by sol-gel process with corresponding inorganic

    殷明志; 汪敏强; 姚熹


    Well-cubic perovskite lanthanum aluminate (LaAl03) film on (110) silicon substrate was fabricated by sol-gel method with corresponding inorganic salts. Lanthanum acetate and aluminum acetate glacial acetic acid solutions were prepared via ligand exchange starting from lanthanum nitrate hexahydrate and aluminum nitrate hexahydrate after being refluxed. (CH3CO)2O removed nitrates and the crystallized H2O completely, acetylacetone (AcAc) was partially bidentated with metallic ion of the metallic acetates and formed La(OAc)3-x(AcAc)x, which were hydrolyzed into La(AcAc)3-x(OH)x by adding 10 ml 0.4% methyl cellulose (MCL) solution. The La(AcAc)3-x(OH)x, polymerizing and combining with MCL,formed the LaA1O3 sol precursor with heteropolymeric structure and formed film easily. The epitaxial LaA1O3 film on Si(110) substrate was crystallized after being annealed in thermal annealing furnace for 650-750 ℃/30 min. The morphologies and microstructures were characterized. The refractive index of the LAO film was 1.942 to 2.007; the dielectric constant and the dissipation factors were estimated to be 23-26 and 2.1×10-4-2.4x10-4 respectively.

  4. Mullite long fibres prepared by sol-gel method using water solvent systems

    Okada, K.; Yasohama, S.; Hayashi, S.; Yasumori, A. [Tokyo Inst. of Tech. (Japan). Dept. of Inorganic Materials


    Mullite long fibres, which are a candidate for high temperature applications were prepared by sol-gel method from water solvent systems. They were synthesized from three different combinations of raw materials as follows: (1):Al(O{sub 1}C{sub 3}H{sub 7}){sub 3}, Al-nitrate and Si(OC{sub 2}H{sub 5}){sub 4} (TEOS), (2):Al metal, Al-chloride and TEOS, (3):Al metal, Al-nitrate and TEOS. In the methods (1) and (2), very fine SiO{sub 2} aerosol particles were also used partially replacing TEOS. The prepared solutions were condensed and examined the spinability by a hand drawing method. Dense and crack free mullite fibres were prepared from the methods (1) and (3) by firing up to 1100 C. Whereas the fibres prepared from the method (2) were less SiO{sub 2} than mullite composition and were porous by the firing due to evaporation of residual Cl ions at high temperature. (orig.) 10 refs.

  5. Sol-Gel Synthesis and Characterization of Cubic Bismuth Zinc Niobium Oxide Nanopowders

    Ganchimeg Perenlei


    Full Text Available Bismuth zinc niobium oxide (BZN was successfully synthesized by a diol-based sol-gel reaction utilizing metal acetate and alkoxide precursors. Thermal analysis of a liquid suspension of precursors suggests that the majority of organic precursors decompose at temperatures up to 150°C, and organic free powders form above 350°C. The experimental results indicate that a homogeneous gel is obtained at about 200°C and then converts to a mixture of intermediate oxides at 350–400°C. Finally, single-phased BZN powders are obtained between 500 and 900°C. The degree of chemical homogeneity as determined by X-ray diffraction and EDS mapping is consistent throughout the samples. Elemental analysis indicates that the atomic ratio of metals closely matches a Bi1.5ZnNb1.5O7 composition. Crystallite sizes of the BZN powders calculated from the Scherrer equation are about 33–98 nm for the samples prepared at 500–700°C, respectively. The particle and crystallite sizes increase with increased sintering temperature. The estimated band gap of the BZN nanopowders from optical analysis is about 2.60–2.75 eV at 500-600°C. The observed phase formations and measured results in this study were compared with those of previous reports.

  6. Preparación de recubrimientos multicapa de base zirconia por vía sol-gel; caracterización microestructural y mecánica

    Caruso, R.


    Full Text Available Frequently, the total substitution of a specific material for a certain application can be avoided by improving their surface properties (resistance to erosion and corrosion, electric properties, etc.. In particular, surface protection with ceramic coatings can be the solution of many practical problems. For this reason, the development of new ceramics coatings is a research area of technological interest. Sol-gel is a very interesting route to obtain oxide thin films on different substrates. In this work, our interest is centred on the protection of metallic substrates by using sol-gel zirconia coatings. The precursor sol-gel solution was obtained by hydrolysis of zirconium n-propoxide in propanol and nitric acid. We developed a routine fabrication of free cracks multilayer dip-coatings, with total thickness in the range 200-3000 nm. A microstructural and mechanical characterisation, by using Berkovich ultramicrohardness tests, will be presented.

    En ocasiones, no es necesario sustituir completamente un material para una determinada aplicación, sino que bastaría con mejorar sus propiedades superficiales (resistencia a erosión y corrosión, propiedades eléctricas, ópticas, etc.. La protección superficial mediante recubrimientos cerámicos puede ser la solución de muchos problemas prácticos, por lo que su estudio y desarrollo constituye un área de gran interés tecnológico. Una de las rutas más interesantes para obtener películas delgadas de óxido sobre diferentes substratos es la vía sol-gel. En este trabajo, nuestro interés se centra en la protección de substratos metálicos mediante recubrimientos sol-gel de base zirconia depositados por inmersión (dip-coating. Las soluciones sol-gel se obtuvieron mediante la hidrólisis de n-propoxido de zirconio en propanol con ácido nítrico. El método de fabricación propuesto permite la obtención de recubrimientos multicapa libres de grietas y con espesores en el rango 200

  7. 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.

  8. Synthesis and characterization of cellulose-functionalized 3,4-dihydroxyphenylalanine(dopamine)/silica-gold nanomaterials by sol-gel process.

    Ramesh, Sivalingam; Kim, Joo-Hyung


    Cellulose-metal oxide nanomaterials were developed the technologies to manipulate self-assembly and multi-functionallity, of new technologies to the point where industry can produce advanced and cost-competitive cellulose and lignocellulose-based materials. The present investigation focused on cellulose-silica and cellulose functionalized 3,4-dihydroxy phenyl alanine(dopamine) silica/gold nanomaterials by in-situ sol-gel process. The tetraethoxysilane (TEOS) and gold precursors such as tetrachloroauricacid (HAuCl4) and γ- aminopropyltriethoxysilane (γ-APTES) as coupling agent were used for sol-gel crosslinking process. The chemical and morphological properties of cellulose/silica and cellulose /silica-gold nanomaterials via covalent crosslinking hybrids were investigated with FTIR, XRD, SEM and TEM analysis. The results show that cellulose/silica and cellulose functionalized dopamine-silica/gold hybrids form new macromolecular structures in the size of 20 nm.

  9. 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.

  10. 金属基掺杂水滑石自修复型溶胶-凝胶膜层制备及机理研究%Preparation of metal matrix-containing hydrotalcite sol-gel self-healing coating and its corrosion resistance

    李龙芹; 王韶音; 李青


    设计并实现了一种自修复溶胶-凝胶膜层。利用膜层中添加的水滑石颗粒的阴离子交换作用实现了自修复功能,并对其修复机理进行设想和论证。长期浸泡测试结果表明,膜层中水滑石颗粒的最佳添加量为10%(质量分数)。通过 X 射线衍射和扫描电子显微镜观察验证设想。此种膜层的自修复功能是通过膜层中添加的水滑石颗粒的阴离子交换作用实现的。%In this work,hydrotalcite (HT)powder was prepared by the classical co-precipitation method using magnesium and aluminum nitrates as precursors.Different weight percentages (5%,10% and 15wt%)of hydrotalcite were added to sols.The sol-gel coatings were deposited by spin-coating method on AZ91D magnesi-um alloy substrate.Scanning electronmicroscopy (SEM)revealed the distribution of the agglomerates.The cor-rosion performance was evaluated by electrochemical impedance spectroscopy (EIS).The results showed a marked improvement of the corrosion resistance on the sol-gel/magnesium system when hydrotalcite was added to the sol-gel coating.And the healing effects may be due to the anion exchange capacity of hydrotalcite.

  11. Room temperature ferromagnetism of Mn-doped SnO{sub 2} thin films fabricated by sol-gel method

    Xiao Yuhua [Key Laboratory for Magnetism and Magnetic Materials of Ministry of Education, Lanzhou University, Lanzhou 730000 (China)], E-mail:; Ge Shihui; Xi Li; Zuo Yalu; Zhou Xueyun; Zhang Bangmin; Zhang Li [Key Laboratory for Magnetism and Magnetic Materials of Ministry of Education, Lanzhou University, Lanzhou 730000 (China); Li Chengxian; Han Xiufeng; Wen Zhenchao [State Key Laboratory of Magnetism, Institute of Physics, Chinese Academy of Sciences, Beijing 100080 (China)


    Sn{sub 1-x}Mn{sub x}O{sub 2} (x {<=} 0.11) thin films spin-coated on Si (1 1 1) substrate were fabricated by sol-gel method. X-ray diffraction revealed that single-phase rutile polycrystalline structure was obtained for x up to about 0.078. Evolution of the lattice parameters and X-ray photoelectron spectroscopy studies confirmed the incorporation of Mn{sup 3+} cations into rutile SnO{sub 2} lattice. Magnetic measurements revealed that all Sn{sub 1-x}Mn{sub x}O{sub 2} thin films exhibit ferromagnetism at room temperature, which is identified as an intrinsic characteristic. Magnetization data showed that the average magnetic moment per Mn atom decreased and the coercivity increases with increasing Mn content. The origin of room temperature ferromagnetism can be understood in terms of the percolation of the bound magnetic polaron. Our experimental results prove that the sol-gel method is an effective method for fabrication of transition metal doped SnO{sub 2} nanostructures with room temperature ferromagnetism by chemical synthesis.

  12. Quantum dot based on tin/titanium mixed oxide doped with europium synthesized by protein sol-gel method

    Paganini, Paula P.; Felinto, Maria Claudia F.C., E-mail: paulapaganini@usp.b, E-mail: mfelinto@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Brito, Hermi F., E-mail: hefbrito@iq.usp.b [Universidade de Sao Paulo (IQ/USP), Sao Paulo, SP (Brazil). Inst. de Quimica. Lab. de Elementos do Bloco f


    Special luminescence biomarkers have been developed to find more sensitive fluoroimmunoassay methods. A new generation of these biomarkers is the semiconductors nanocrystals, known as quantum dots, doped with lanthanides. The use of lanthanides ions as luminescent markers has many advantages, for example a security method, low cost, high specificity and also the luminescence can be promptly measured with high sensibility and accuracy. The protein sol-gel is a modification of conventional method, in which the coconut water replacing the alkoxides normally used. The advantage is that, the proteins present in coconut water bind chemically with metal salts forming a polymer chain. This work presents nanoparticles based on tin/titanium mixed oxide doped with 3% of europium synthesized by protein sol-gel method. The nanoparticles were burned at 300 deg C, 500 deg C, 800 deg C and 1100 deg C. The samples were analyzed and characterized by thermal analysis, X-ray powder diffraction (XRD), infrared spectroscopy (IR) and scanning electron microscopy (SEM). The synthesis was effective and the nanoparticles showed nanometric size and structural differences with the annealing. To be used in the fluoroimmunoassays tests, these particles need to be functionalized before be connect with biological molecules and after this process, these nanoparticles going to be submitted at gamma radiation for sterilization. (author)

  13. 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.

  14. Preparation of YAG: Ce3+ phosphor by sol-gel low temperature combustion method and its luminescent properties

    YAN Xing-huang; ZHENG Song-sheng; YU Rui-min; CAI Jing; XU Zhi-wei; LIU Chun-jia; LUO Xue-tao


    YAG:Ce3+ phosphor was prepared by sol-gel low-temperature combustion method.The effects of the precursor properties and calcining temperature on the crystallization process,microscopic morphology and luminescent properties of phosphor were studied.The results indicate that the pure phase of YAG can be obtained at 800℃ by sol-gel low temperature combustion method,using citric acid as complexing agent.When the molar ratio of metal ion to citric acid is 2.0 and pH value is 2,the crystallinity increases and the phosphor particle size grows up gradually with the increase of the calcining temperature.The powders were characterized through thermal analysis,X-ray diffraction analysis and scanning electron microscope analysis.The excitation spectra of YAG: Ce3+ phosphor take on a double peak structure,and the peak value of the main excitation spectra occurs at 460nm and that of the emission spectra is near 530nm.With the gradual increase of the calcining temperature,the peak position of excitation and emission spectra remains basically unchanged,but its relative intensity increases gradually.

  15. 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.

  16. Infrared and Raman spectroscopic studies of tris-[3-(trimethoxysilyl)propyl] isocyanurate, its sol-gel process, and coating on aluminum and copper.

    Li, Ying-Sing; Church, Jeffrey S; Woodhead, Andrea L; Vecchio, Nicolas E; Yang, Johnny


    Tris-[3-(trimethoxysilyl)propyl] isocyanurate (TTPI) has been used as a precursor to prepare a sol using ethanol as the solvent under acidic conditions. The sol-gel was applied for the surface treatment of aluminum and copper. Infrared and Raman spectra have been recorded for pure TTPI and the TTPI sol, xerogel and TTPI sol-gel coated metals. From the vibrational spectra, TTPI is likely to have the C1 point group. Vibrational assignments are suggested based on group frequencies, the expected reactions in the sol-gel process and the vibrational studies of some related molecules. From the experimental infrared spectra of xerogels annealed at different temperatures and from the thermal-gravimetric analysis, it is found that the TTPI xerogel decomposes at around 450°C with silica being the major decomposition product. A cyclic voltammetric study of the metal electrodes coated with different concentrations of TTPI ranging from 5% to 42% (v/v) has shown that the films with high concentrations of sol would provide better corrosion protection for aluminum and copper.

  17. Synthesis of palladium-doped silica nanofibers by sol-gel reaction and electrospinning process

    San, Thiam Hui; Daud, Wan Ramli Wan; Kadhum, Abdul Amir Hassan; Mohamad, Abu Bakar; Kamarudin, Siti Kartom; Shyuan, Loh Kee; Majlan, Edy Herianto [Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia and Department of Chemical and Process Engineering, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia)


    Nanofiber is drawing great attention nowadays with their high surface area per volume and flexibility in surface functionalities that make them favorable as a proton exchange membrane in fuel cell application. In this study, incorporation of palladium nanoparticles in silica nanofibers was prepared by combination of a tetraorthosilane (TEOS) sol-gel reaction with electrospinning process. This method can prevent the nanoparticles from aggregation by direct mixing of palladium nanoparticles in silica sol. The as-produced electrospun fibers were thermally treated to remove poly(vinyl pyrrolidone) (PVP) and condensation of silanol in silica framework. PVP is chosen as fiber shaping agent because of its insulting and capping properties for various metal nanoparticles. Scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the silica fibers and Pd nanoparticles on the fibers. Spun fibers with average diameter ranged from 100nm to 400nm were obtained at optimum operating condition and distribution of Pd nanoparticles on silica fibers was investigated.

  18. Synthesis, structure and electromagnetic properties of Mn-Zn ferrite by sol-gel combustion technique

    Wang, Wenjie; Zang, Chongguang; Jiao, Qingjie


    The electromagnetic absorbing behaviors of a thin coating fabricated by mixing Mn-Zn ferrite with epoxy resin (EP) were studied. The spinel ferrites Mn1-xZnxFe2O4 (x=0.2, 0.5 and 0.8) were synthesized with citrate acid as complex agent by sol-gel combustion method. The microstructure and surface morphology of Mn-Zn ferrite powders were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The complex permittivity and complex permeability of the fabricated ferrite/EP composites were investigated in terms of their contributions to the absorbing properties in the low frequency (10 MHz to 1 GHz). The microwave absorption of the prepared ferrite/EP composites could be tailored by matching the dielectric loss and magnetic loss and by controlling the doped metal ratio. The composites with the ferrite composition x=0.2 are found to show higher reflection loss compared with the composites with other compositions. It is proposed that the prepared composites can potentially be applied in electromagnetic microwave absorbing field.

  19. 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.

  20. 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.

  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. 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.)

  3. 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.

  4. 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

  5. Architectural optimization of an epoxy-based hybrid sol-gel coating for the corrosion protection of a cast Elektron21 magnesium alloy

    Murillo-Gutiérrez, N. V.; Ansart, F.; Bonino, J.-P.; Kunst, S. R.; Malfatti, C. F.


    An epoxy-based hybrid sol-gel coating was prepared in various architectural configurations has been studied for the corrosion protection of a cast Elektron21 magnesium alloy. The creation of a single layer of this coating presents defects consisting of macro-pores and protuberances, which opens access for corrosive species to reach the metallic substrate. These defects are suspected to result from the high reactivity of the substrate, as well as to the irregular topography of the substrate disrupted by the microstructure of the own magnesium alloy. Hence, a sol-gel coating in bilayer architecture is proposed, where the first layer would “inert” the surface of the magnesium substrate, and the second layer would cover the defects of the first layer and also thickening the coating. The morphological characteristics of the sol-gel coatings were analyzed by scanning electron microscopy (SEM), and their corrosion behavior was evaluated by OCP (open circuit potential) monitoring and electrochemical impedance spectroscopy (EIS) in chloride media. It is shown that both the architectural arrangement and the individual thickness of the first and second layers have an important influence on the anticorrosion performances of the protective system, just as much as its global thickness.

  6. The preparation of sol-gel materials doped with ionic liquids and trialkyl phosphine oxides for yttrium(III) uptake.

    Liu, Yinghui; Sun, Xiaoqi; Luo, Fang; Chen, Ji


    A new material (IL923SGs) composed of ionic liquids and trialkyl phosphine oxides (Cyanex 923) for Y(III) uptake was prepared via a sol-gel method. The hydrophobic ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate (C8mim+ PF6(-)) was used as solvent medium and pore templating material. The extraction of Y(III) by IL923SGs was mainly due to the complexation of metal ions with Cyanex 923 doped in the solid silica. Ionic liquid was stably doped into the silica gel matrix providing a diffusion medium for Cyanex 923, and this will result in higher removal efficiencies and excellent stability for metal ions separation. IL923SGs were also easily regenerated and reused in the subsequent removal of Y(III) in four cycles.

  7. The preparation of sol-gel materials doped with ionic liquids and trialkyl phosphine oxides for Yttrium(III) uptake

    Liu Yinghui [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100039 (China); Sun Xiaoqi [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Luo Fang [Key Laboratory of Polyoxometalates Science of Ministry of Education, College of Chemistry, Northeast Normal University, Changchun 130024 (China); Chen Ji [Key Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China)], E-mail:


    A new material (IL923SGs) composed of ionic liquids and trialkyl phosphine oxides (Cyanex 923) for Y(III) uptake was prepared via a sol-gel method. The hydrophobic ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate (C{sub 8}mim{sup +}PF{sub 6}{sup -}) was used as solvent medium and pore templating material. The extraction of Y(III) by IL923SGs was mainly due to the complexation of metal ions with Cyanex 923 doped in the solid silica. Ionic liquid was stably doped into the silica gel matrix providing a diffusion medium for Cyanex 923, and this will result in higher removal efficiencies and excellent stability for metal ions separation. IL923SGs were also easily regenerated and reused in the subsequent removal of Y(III) in four cycles.

  8. 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.

  9. 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.

  10. 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.)

  11. 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.

  12. 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.

  13. Study on the formation of self-assembled monolayers on sol-gel processed hafnium oxide as dielectric layers.

    Ting, Guy G; Acton, Orb; Ma, Hong; Ka, Jae Won; Jen, Alex K-Y


    High dielectric constant (k) metal oxides such as hafnium oxide (HfO2) have gained significant interest due to their applications in microelectronics. In order to study and control the surface properties of hafnium oxide, self-assembled monolayers (SAMs) of four different long aliphatic molecules with binding groups of phosphonic acid, carboxylic acid, and catechol were formed and characterized. Surface modification was performed to improve the interface between metal oxide and top deposited materials as well as to create suitable dielectric properties, that is, leakage current and capacitance densities, which are important in organic thin film transistors. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, contact angle goniometry, atomic force microscopy (AFM), and simple metal-HfO2-SAM-metal devices were used to characterize the surfaces before and after SAM modification on sol-gel processed hafnium oxide. The alkylphosphonic acid provided the best monolayer formation on sol-gel processed hafnium oxide to generate a well-packed, ultrathin dielectric exhibiting a low leakage current density of 2x10(-8) A/cm2 at an applied voltage of -2.0 V and high capacitance density of 0.55 microF/cm2 at 10 kHz. Dialkylcatechol showed similar characteristics and the potential for using the catechol SAMs to modify HfO2 surfaces. In addition, the integration of this alkylphosphonic acid SAM/hafnium oxide hybrid dielectric into pentacene-based thin film transistors yields low-voltage operation within 1.5 V and improved performance over bare hafnium oxide.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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...

  2. 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.

  3. 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.

  4. Fabrication of SWNT/silica composites by the sol-gel process.

    Babooram, Keshwaree; Narain, Ravin


    Single-walled carbon nanotubes (SWNTs) have successfully been incorporated into a silica matrix using the sol-gel process. The SWNTs were first functionalized with 3-aminopropyltriethoxysilane (APTES) through an amide linkage formed between the carboxylic acid groups already present on their surface and the amino group on APTES. The silane moieties were then used to form silica with and without the presence of tetramethylorthosilicate (TMOS) in a sol-gel reaction. The addition of TMOS was found to influence the molecular arrangement of the SWNT in the silica matrix and also to retard the degradation of the silica-SWNT composite.

  5. Sol-gel processed alumina based materials in microcalorimeter sensor device fabrication for automotive applications

    Nakouzi, S.R.; McBride, J.R.; Nietering, K.E.; Narula, C.K. [Ford Motor Co., Dearborn, MI (United States)


    The application of sol-gel processed materials in a variety of sensors has been proposed. The authors describe microcalorimeter sensor devices employing sol-gel processed alumina based materials which can be used to monitor pollutants in automotive exhaust. These sensors operate by measuring changes in resistance upon catalysis and are economically acceptable for automotive applications. It is important to point out that automobiles will be required to have a means of monitoring exhaust gases by on-board sensors as mandated by the EPA and the California Air Resources Board (OBD-II).

  6. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    Figus, Cristiana, E-mail:; Quochi, Francesco, E-mail:; Piana, Giacomo; Saba, Michele; Mura, Andrea; Bongiovanni, Giovanni [Dipartimento di Fisica, University of Cagliari, SS 554 Bivio per Sestu, I-09042, Monserrato-Cagliari (Italy); Artizzu, Flavia [Dipartimento di Fisica, University of Cagliari and Dipartimento di Scienze Chimiche e Geologiche, University of Cagliari, SS 554 Bivio per Sestu, I-09042, Monserrato-Cagliari (Italy); Mercuri, Maria Laura; Serpe, Angela; Deplano, Paola [Dipartimento di Scienze Chimiche e Geologiche, University of Cagliari, SS 554 Bivio per Sestu, I-09042, Monserrato-Cagliari (Italy)


    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ{sub 4}) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ{sub 4} are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution.

  7. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    Figus, Cristiana; Quochi, Francesco; Artizzu, Flavia; Piana, Giacomo; Saba, Michele; Mercuri, Maria Laura; Serpe, Angela; Deplano, Paola; Mura, Andrea; Bongiovanni, Giovanni


    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ4) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ4 are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution.

  8. Effect of vanadium on the obtaining of the titanium dioxide by Sol-Gel Method; Efeito do vanadio na obtencao de dioxido de titanio pelo Metodo Sol-Gel

    Granado, S.R.; Silva, D.W.; Lopes, S.A.; Cavalheiro, A.A., E-mail: [Universidade Estadual de Mato Grosso do Sul (CPTREN/UEMS), Navirai, MS (Brazil). Centro de Pesquisas Tecnologicas em Recursos Naturais


    The obtaining of transition metal modified titanium dioxide (TiO{sub 2}) can be a promising path to promote changes in crystal structure of anatase phase in order to displace the band gap toward frequencies near to visible region. The insertion of the heterovalent ions such as vanadium can be shift the titanium coordination number in the anatase matrix, leading to important changes in the photonic characteristics of the material. In Sol-Gel method, the presence of the non alkoxide precursors can affects the stability of the solution and the gelifying process, with consequences on the characteristics of the material. In this work, it was investigated the effect of 5mol% of vanadium by thermal analysis of the dried gel and XRD and adsorption isotherm in the samples obtained at different temperatures. The decomposition steps of the precursor were associated to phase formation in the material, leading to conclusion that the presence of vanadium affects the stability of anatase phase. (author)

  9. Characterization of silica particles prepared via urease-catalyzed urea hydrolysis and activity of urease in sol-gel silica matrix

    Kato, Katsuya, E-mail: [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya 463-8560 (Japan); Nishida, Masakazu [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya 463-8560 (Japan); Ito, Kimiyasu; Tomita, Masahiro [Division of Chemistry for Materials, Graduate School of Engineering, Mie University, 1577 Kurimamachiya-cho, Tsu, Mie 514-8570 (Japan)


    Highlights: Black-Right-Pointing-Pointer Silica precipitation occurred via urease-catalytic reactions. Black-Right-Pointing-Pointer Higher urease activity for silica synthesis enables mesostructure of silica-urease composites. Black-Right-Pointing-Pointer Urease encapsulating in silica matrix retained high activity. - Abstract: Urease templated precipitation of silica synthesized by sol-gel chemistry produces a composite material allowing high urease activity. This study investigates the structural properties of the composite material that allow for the retention of the urease hydrolysis activity. Scanning (SEM) and transmission (TEM) electron microscopy reveal that the composite has a mesoporous structure composed of closely packed spherical structures {approx}20-50 nm in diameter. Brunauer-Emmett-Teller (BET) analysis revealed that the surface area and pore volume of the composite prepared under the conditions of 50 mM urea and 25 Degree-Sign C is relatively high (324 m{sup 2}/g and 1.0 cm{sup 3}/g). These values are equivalent to those of usual mesoporous silica materials synthesized from the self-assembly of triblock copolymers as organic templates. In addition, after encapsulating in a sol-gel silica matrix, urease retained high activity ({approx}90% of the activity compared with native urease). Our results suggest a new method for synthesizing mesoporous silica materials with highly tunable pore sizes and shapes under mild conditions.

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

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


    Biofouling on ships and boats, characterized by aquatic bacteria and small organisms attaching to the hull, is an important global issue, since over 80000 tons of antifouling paint is used annually. This biofilm, which can form in as little as 48 hours depending on water temperature, increases drag on watercraft, which greatly reduces their fuel efficiency. In addition, biofouling can lead to microbially induced corrosion (MIC) due to H2S formed by the bacteria, especially sulfate-reducing bacteria. When the International Maritime Organization (IMO) international convention banned the use of effective but environmentally damaging coatings containing tributyl tin in 2008, the development of clean and effective antifouling systems became more important than ever. New nonbiocidal coatings are now in high demand. Scientists have developed new polymers, materials, and biocides, including new elastomeric coatings that they have obtained by improving the original silicone (polydimethylsiloxane) formulation patented in 1975. However, the high cost of silicones, especially of fluoropolymer-modified silicones, has generally prevented their large-scale diffusion. In 2009, traditional antifouling coatings using cuprous oxide formulated in copolymer paints still represented 95% of the global market volume of anti-fouling paints. The sol-gel nanochemistry approach to functional materials has emerged as an attractive candidate for creating low fouling surfaces due to the unique structure and properties of silica-based coatings and of hybrid inorganic-organic silicas in particular. Sol-gel formulations easily bind to all types of surfaces, such as steel, fiberglass, aluminum, and wood. In addition, they can cure at room temperature and form thin glassy coatings that are markedly different from thick silicone elastomeric foul-releasing coatings. Good to excellent performance against biofouling, low cure temperatures, enhanced and prolonged chemical and physical stability, ease of

  11. Physical properties and heavy metal uptake of encapsulated Escherichia coli expressing a metal binding gene (NCP).

    Bang, S S; Pazirandeh, M


    A recombinant Escherichia coli expressing the Neurospora crassa metallothionein gene (NCP) has previously been shown to remove low levels of Cd and other metals from solution. For further development as a biosorbent, the encapsulation of the NCP is investigated by various matrices. The NCP was encapsulated in alginate, chitosan-alginate or kappa-carrageenan, and its physical properties characterized. Results indicated that encapsulation in alginate resulted in fragile beads, whereas encapsulation in kappa-carrageenan or chitosan-alginate provided more physical and chemical integrity to the beads. Maximal heavy metal removal by cells encapsulated in carrageenan occurred within 3 h, while a gradual increase in removal was observed up to 24 h for cells encapsulated in chitosan-alginate. Metal removal by cells encapsulated in alginate beads was lower than those encapsulated in carrageenan or chitosan-alginate.

  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


    Recently, sol-gel methods employing ionic liquids (ILs) have shown significant implications for the synthesis of well-defined nanostructured inorganic materials. Herein, we synthesized nanocrystalline TiO2 particles via an alkoxide sol-gel method employing a water-immi...


    Recently, sol-gel methods employing ionic liquids (ILs) have shown significant implications for the synthesis of well-defined nanostructured inorganic materials. Herein, we synthesized nanocrystalline TiO2 particles via an alkoxide sol-gel method employing a water-immi...

  15. 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.


    Yucheng Wu; Xiaoye Hu; Ting Xie; Guanghai Li; Lide Zhang


    With Ti(OBu)4 as precursor, and HAc as complexing agent, pure and W-doped TiO2 gelatins were prepared by a sol-gel method. During the process of gel formation, metal ions were dispersed in the porous TiO2 matrix.Then, powders of nano-TiO2 and W-doped nano-TiO2 were prepared by drying, grinding and heat treatment at different temperatures. The grain size and structure of the samples, pure TiO2 and W-doped, and treated at different temperatures,were studied by X-ray diffraction (XRD), Beckman Coulter Sorption Analysis and TEM.Results showed that, with increasing temperature, the TiO2 transformed from anatase to rutile and the grain size increased. This transformation and grain growth of TiO2 could be retarded by doping with W.

  17. A facile synthesis of zinc oxide/multiwalled carbon nanotube nanocomposite lithium ion battery anodes by sol-gel method

    Köse, Hilal; Karaal, Şeyma; Aydın, Ali Osman; Akbulut, Hatem


    Free standing zinc oxide (ZnO) and multiwalled carbon nanotube (MWCNT) nanocomposite materials are prepared by a sol gel technique giving a new high capacity anode material for lithium ion batteries. Free-standing ZnO/MWCNT nanocomposite anodes with two different chelating agent additives, triethanolamine (TEA) and glycerin (GLY), yield different electrochemical performances. Field emission gun scanning electron microscopy (FEG-SEM), energy dispersive X-ray spectrometer (EDS), high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) analyses reveal the produced anode electrodes exhibit a unique structure of ZnO coating on the MWCNT surfaces. Li-ion cell assembly using a ZnO/MWCNT/GLY free-standing anode and Li metal cathode possesses the best discharge capacity, remaining as high as 460 mAh g-1 after 100 cycles. This core-shell structured anode can offer increased energy storage and performance over conventional anodes in Li-ion batteries.

  18. Sol-gel zinc oxide humidity sensors integrated with a ring oscillator circuit on-a-chip.

    Yang, Ming-Zhi; Dai, Ching-Liang; Wu, Chyan-Chyi


    The study develops an integrated humidity microsensor fabricated using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The integrated humidity sensor consists of a humidity sensor and a ring oscillator circuit on-a-chip. The humidity sensor is composed of a sensitive film and branch interdigitated electrodes. The sensitive film is zinc oxide prepared by sol-gel method. After completion of the CMOS process, the sensor requires a post-process to remove the sacrificial oxide layer and to coat the zinc oxide film on the interdigitated electrodes. The capacitance of the sensor changes when the sensitive film adsorbs water vapor. The circuit is used to convert the capacitance of the humidity sensor into the oscillation frequency output. Experimental results show that the output frequency of the sensor changes from 84.3 to 73.4 MHz at 30 °C as the humidity increases 40 to 90%RH.

  19. Sol-Gel Zinc Oxide Humidity Sensors Integrated with a Ring Oscillator Circuit On-a-Chip

    Ming-Zhi Yang


    Full Text Available The study develops an integrated humidity microsensor fabricated using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS process. The integrated humidity sensor consists of a humidity sensor and a ring oscillator circuit on-a-chip. The humidity sensor is composed of a sensitive film and branch interdigitated electrodes. The sensitive film is zinc oxide prepared by sol-gel method. After completion of the CMOS process, the sensor requires a post-process to remove the sacrificial oxide layer and to coat the zinc oxide film on the interdigitated electrodes. The capacitance of the sensor changes when the sensitive film adsorbs water vapor. The circuit is used to convert the capacitance of the humidity sensor into the oscillation frequency output. Experimental results show that the output frequency of the sensor changes from 84.3 to 73.4 MHz at 30 °C as the humidity increases 40 to 90%RH.

  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. Increasing the activity and enantioselectivity of lipases by sol-gel immobilization: further advancements of practical interest.

    Tielmann, Patrick; Kierkels, Hans; Zonta, Albin; Ilie, Adriana; Reetz, Manfred T


    The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of the sol-gel approach.

  2. Sol-gel-modified boron-doped diamond surfaces for methanol and ethanol electro-oxidation in acid medium

    Salazar-Banda, G. R.; Suffredini, H. B.; Calegaro, M. L.; Tanimoto, S. T.; Avaca, L. A.

    Studies of the methanol and ethanol electro-oxidation reactions on boron-doped diamond (BDD) electrode surfaces modified with Pt, Pt-RuO 2 and Pt-RuO 2-RhO 2 by the sol-gel method are reported here. The materials were initially characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). The XRD analyses indicate that the sol-gel method produces nano-sized deposits on the BDD surfaces. These deposits also form nano-clusters with a size of ca. 100 nm as observed by SEM and AFM. The EDX maps showed that the metals are homogeneously distributed on the BDD surface and have a composition close to the expected one. Cyclic voltammetry experiments in acid medium revealed that the CO poisoning effect for the methanol and the ethanol oxidation reactions is largely inhibited on the Pt-RuO 2-RhO 2/BDD electrode showing the positive contribution of the rhodium oxide to the electrocatalysts performance in these reactions. Potentiostatic polarization curves and the corresponding Tafel plots showed that the addition of RuO 2 and RhO 2 to Pt/BDD produces a more reactive electrocatalyst that adsorbs methanol and ethanol more efficiently and changes the reactions onsets by 120 or 180 mV towards less positive potentials, respectively. Moreover, the stationary current density measured at a fixed potential for ethanol oxidation on the Pt-RuO 2-RhO 2/BDD composite electrode is more than one order of magnitude larger than on a Pt/BDD surface. In addition, chronoamperometric experiments indicate that on those composite electrodes the effect of CO poisoning only appears after a considerable amount of charge has passed through the interface. Consequently, the catalyst containing Pt, RuO 2 and RhO 2 deposited on BDD by the sol-gel method is a very promising composite material to be used in fuel cell anodes.

  3. Non isothermal decomposition of lanthanum titanates precursors prepared by sol gel process: A kinetic and thermodynamic study

    Bassil, S. [Université Lyon 1, CNRS, UMR 5256, IRCELYON, Institut de recherches sur la catalyse et l’environnement de Lyon, 2 avenue Albert Einstein, F-69626 Villeurbanne (France); Kaddouri, A., E-mail: [Université Lyon 1, CNRS, UMR 5256, IRCELYON, Institut de recherches sur la catalyse et l’environnement de Lyon, 2 avenue Albert Einstein, F-69626 Villeurbanne (France); Béguin, B.; Gélin, P. [Université Lyon 1, CNRS, UMR 5256, IRCELYON, Institut de recherches sur la catalyse et l’environnement de Lyon, 2 avenue Albert Einstein, F-69626 Villeurbanne (France)


    Highlights: ► Metal-propionates is a most promising route for the preparation of La{sub 0.8}Sr{sub 0.2}TiO{sub 3+δ} (LST) at a temperature substantially lower than that used for the preparation of the same solid by traditional methods. ► Activation energy and isothermal thermodynamic parameters calculated for the decomposition process are close to those observed for metal organic compounds. ► Sol gel-prepared LST presented low propensity to coke deposition and high stability with time during the critical long term exposure to methane and steam at high temperatures. - Abstract: The single phase La{sub 0.8}Sr{sub 0.2}TiO{sub 3+δ} was prepared via the sol gel process using propionic acid. Kinetics of the thermal decomposition of the precursors has been studied using differential thermogravimetry under non-isothermal conditions in different atmospheres (air and helium). Non isothermal kinetic (A and ΔE) and thermodynamic parameters (ΔH, ΔS and Cp) were determined using different heating rates. La{sub 2}O{sub 3}, SrO and TiO{sub 2} products crystallized at temperatures of ca. 730, 960 and 470 °C respectively while pure La{sub 0.8}Sr{sub 0.2}TiO{sub 3+δ} phase was obtained at 1200 °C, temperature substantially lower than that used for the preparation of La{sub 0.8}Sr{sub 0.2}TiO{sub 3+δ} by conventional solid state method. Precursors and/or final solids were characterized by thermogravimetric analysis (TG), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction, diffuse reflectance ultraviolet–visible spectroscopy (DR-UV–vis) and methane steam reforming under water deficient conditions.

  4. Silica-polyethylene glycol hybrids synthesized by sol-gel: Biocompatibility improvement of titanium implants by coating.

    Catauro, M; Bollino, F; Papale, F; Ferrara, C; Mustarelli, P


    Although metallic implants are the most used in dental and orthopaedic fields, they can early fail due to low tissue tolerance or osseointegration ability. To overcome this drawback, functional coatings can be applied on the metallic surface to provide a firm fixation of the implants. The objective of the present study was twofold: to synthesize and to characterize silica/polyethylene glycol (PEG) hybrid materials using sol-gel technique and to investigate their capability to dip-coat titanium grade 4 (Ti-gr4) substrates to improve their biological properties. Various hybrid systems have been synthesized by changing the ratio between the organic and inorganic phases in order to study the influence of the polymer amount on the structure and, thus, on the properties of the coatings. Fourier transform infrared (FTIR) spectroscopy and solid state Nuclear Magnetic Resonance (NMR) allowed us to detect the formation of hydrogen bonds between the inorganic sol-gel matrix and the organic component. SEM analysis showed that high PEG content enables to obtain crack free-coating. Moreover, the effective improvement in biological properties of Ti-gr4 implants has been evaluated by performing in vitro tests. The bioactivity of the hybrid coatings has been showed by the hydroxyapatite formation on the surface of SiO2/PEG coated Ti-gr4 substrates after soaking in a simulated body fluid and the lack of cytotoxicity by the WST-8 Assay. The results showed that the coated substrates are more bioactive and biocompatible than the uncoated ones and that the bioactivity is not significantly affected by PEG amount whereas its addition makes the films more biocompatible.

  5. Estado del arte del proceso sol-gel en México

    María Teresa Ramírez Palma


    Full Text Available A partir de una revisión bibliográfica, realizada por alumnos de la Maestría en Ciencia e Ingeniería de Materiales de la unam, se muestra el estado del arte del proceso sol-gel en México.


    Xia Wang; Jiang Li; Cheng-fen Long; Yun-zhao Yu


    Nano silica-modified epoxy resins were synthesized by the sol-gel process. The materials have the morphological structure of nano particales dispersed in the epoxy matrix. The dispersed phase formed a physical network in the resin and thus influenced the rheological behavior greatly. However, the nano silica did not show a significant influence on the mechanical properties of the cured resins.

  7. Sol-gel coatings on large area glass sheets for electrochromic devices

    Vroon, Z.A.E.P.; Spee, C.I.M.A.


    The preparation of vanadium and tungsten oxide coatings is described using vanadium oxide tri-2-propoxide/2-propanol and tungsten penta-ethoxide/2-propanol solutions. These solutions are dip coated onto K-glass substrates and cured. For vanadium oxide coatings it is shown that sol-gel/dip coat

  8. 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.

  9. 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.

  10. 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

  11. Sol-gel immunoaffinity chromatography for the clean up of ochratoxin A contaminated grains.

    Reiter, Elisabeth Viktoria; Cichna-Markl, Margit; Tansakul, Natthasit; Shim, Won-Bo; Chung, Duck-Hwa; Zentek, Jürgen; Razzazi-Fazeli, Ebrahim


    This paper describes the application of sol-gel immunoaffinity columns for clean up of ochratoxin A contaminated cereal crops. Monoclonal antibodies selective for OTA have been entrapped into the pores of a sol-gel matrix in order to prepare immunoaffinity columns. Different parameters such as amount of entrapped antibodies and loading conditions were optimized to obtain highest possible recoveries of OTA. The method has been found to be a suitable tool in sample preparation prior to HPLC-FLD determination and as selective as conventional commercially available immunoaffinity columns. In the clean up of different cereals mean recoveries of 82±5%, 90±6% and 91±3%, were obtained for wheat, barley and rye, respectively, with sol-gel columns containing 1mg of anti-OTA antibodies. The detection limit (signal-to-noise ratio, 3) was 0.5 μg/kg and the limit of quantification (signal-to-noise ratio, 10) determined to be 1 μg/kg. Sol-gel columns can be reused 7 times without significant loss of recovery. After 10 applications the recovery decreased to approx. 50%.

  12. Self-Protection of Electrochemical Storage Devices via a Thermal Reversible Sol-Gel Transition.

    Yang, Hui; Liu, Zhiyuan; Chandran, Bevita K; Deng, Jiyang; Yu, Jiancan; Qi, Dianpeng; Li, Wenlong; Tang, Yuxin; Zhang, Chenguang; Chen, Xiaodong


    Thermal self-protected intelligent electrochemical storage devices are fabricated using a reversible sol-gel transition of the electrolyte, which can decrease the specific capacitance and increase and enable temperature-dependent charging and discharging rates in the device. This work represents proof of a simple and useful concept, which shows tremendous promise for the safe and controlled power delivery in electrochemical devices.

  13. Foldable and Cytocompatible Sol-gel TiO2 Photonics

    Li, Lan; Zhang, Ping; Wang, Wei-Ming; Lin, Hongtao; Zerdoum, Aidan B.; Geiger, Sarah J.; Liu, Yangchen; Xiao, Nicholas; Zou, Yi; Ogbuu, Okechukwu; Du, Qingyang; Jia, Xinqiao; Li, Jingjing; Hu, Juejun


    Integrated photonics provides a miniaturized and potentially implantable platform to manipulate and enhance the interactions between light and biological molecules or tissues in in-vitro and in-vivo settings, and is thus being increasingly adopted in a wide cross-section of biomedical applications ranging from disease diagnosis to optogenetic neuromodulation. However, the mechanical rigidity of substrates traditionally used for photonic integration is fundamentally incompatible with soft biological tissues. Cytotoxicity of materials and chemicals used in photonic device processing imposes another constraint towards these biophotonic applications. Here we present thin film TiO2 as a viable material for biocompatible and flexible integrated photonics. Amorphous TiO2 films were deposited using a low temperature (sol-gel process fully compatible with monolithic integration on plastic substrates. High-index-contrast flexible optical waveguides and resonators were fabricated using the sol-gel TiO2 material, and resonator quality factors up to 20,000 were measured. Following a multi-neutral-axis mechanical design, these devices exhibit remarkable mechanical flexibility, and can sustain repeated folding without compromising their optical performance. Finally, we validated the low cytotoxicity of the sol-gel TiO2 devices through in-vitro cell culture tests. These results demonstrate the potential of sol-gel TiO2 as a promising material platform for novel biophotonic devices.

  14. Seed-assisted sol-gel synthesis and characterization of nanoparticular V2O5/anatase

    Kunov-Kruse, Andreas Jonas; Kristensen, Steffen Buus; Riisager, Anders


    Nanoparticular supported vanadia materials with crystalline anatase support with a narrow size distribution around 12 nm have been synthesized by a new facile sol-gel, co-precipitation method using decomposable ammonium chloride seed crystals. The materials have been characterized by means of X...

  15. Patterned transparent zinc oxide films produced by sol-gel embossing

    Rao, J.; Koh, L.H.K.; Crean, G.M. [Tyndall National Institute, Lee Maltings, Prospect Row, Cork (Ireland); Department of Microelectronic Engineering, University College Cork, Cork (Ireland); O' Brien, S. [Tyndall National Institute, Lee Maltings, Prospect Row, Cork (Ireland); Winfield, R.J.


    A low cost zinc oxide embossing technique is reported as a method of fabricating structures relevant to a variety of applications. A zinc based sol-gel material was prepared from zinc acetate[Zn(C{sub 2}H{sub 3}O{sub 2}){sub 2}], monoethanolamine[H{sub 2}NC{sub 2}H{sub 4}OH] and isopropanol. The sol-gel was cast into a polydimethylsiloxane (PDMS) mould a track design, placed in contact with the substrate and dried under vacuum at 70 C for 3 hours. The formed track pattern was further densified to provide a stable conductor film that retained the embossed shape. An optimum Zn sol-gel content of 0.6 M was identified. The embossed films had a transparency of greater than 83% in the visible region. The optical bandgap energy was evaluated to be 3.306 eV. The influence of ZnO sol-gel film synthesis and embossing parameters on the microstructure, morphology and optical transparency of fabricated structures is described. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  16. Sol-gel fabrication of one-dimensional photonic crystals with predicted transmission spectra

    Ilinykh, V. A.; Matyushkin, L. B.


    One-dimensional multilayer structures of periodically alternating low refractive index (silica) and high refractive index (titania) materials have been deposited by sol-gel spincoating. Experimental spectra of the structures are in agreement with spectra calculated by transfer matrix technique. As an example, theoretical and experimental spectra with a stop band corresponding 600 nm-reflection are shown.

  17. Hybrid Thin Film Organosilica Sol-Gel Coatings To Support Neuronal Growth and Limit Astrocyte Growth.

    Capeletti, Larissa Brentano; Cardoso, Mateus Borba; Dos Santos, João Henrique Zimnoch; He, Wei


    Thin films of silica prepared by a sol-gel process are becoming a feasible coating option for surface modification of implantable neural sensors without imposing adverse effects on the devices' electrical properties. In order to advance the application of such silica-based coatings in the context of neural interfacing, the characteristics of silica sol-gel are further tailored to gain active control of interactions between cells and the coating materials. By incorporating various readily available organotrialkoxysilanes carrying distinct organic functional groups during the sol-gel process, a library of hybrid organosilica coatings is developed and investigated. In vitro neural cultures using PC12 cells and primary cortical neurons both reveal that, among these different types of hybrid organosilica, the introduction of aminopropyl groups drastically transforms the silica into robust neural permissive substrate, supporting neuron adhesion and neurite outgrowth. Moreover, when this organosilica is cultured with astrocytes, a key type of glial cells responsible for glial scar response toward neural implants, such cell growth promoting effect is not observed. These findings highlight the potential of organo-group-bearing silica sol-gel to function as advanced coating materials to selectively modulate cell response and promote neural integration with implantable sensing devices.

  18. Influence of Calcium on the Initial Stages of the Sol-Gel Synthesis of Bioactive Glasses.

    Côté, Alexander S; Cormack, Alastair N; Tilocca, Antonio


    Understanding how calcium interacts with silica sources and influences their polycondensation in aqueous solutions is of central importance for the development of more effective biomaterials by sol-gel approaches. For this purpose, the atomic-scale evolutions of a calcium-containing precursor solution corresponding to a typical sol-gel bioactive glass and of a corresponding Ca-free solution were compared using reactive molecular dynamics simulations. The simulations highlight a significantly faster rate of condensation when calcium is present in the initial solution, resulting in the formation of large and ramified silica clusters within 5 ns, which are absent in the Ca-free system. This different behavior has been analyzed and interpreted in terms of the Ca-induced nanosegregation in calcium-rich and silica-rich regions, which promotes the condensation reactions within the latter. By identifying a possible mechanism behind the limited incorporation of calcium in the silica nanoclusters formed in the early stages of the sol-gel process, these results could guide further studies aimed at identifying favorable experimental conditions to enhance initial calcium incorporation and thus produce sol-gel biomaterials with improved properties.

  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. Non-cytotoxic antibacterial silver-coumarin complex doped sol-gel coatings.

    Jaiswal, Swarna; Bhattacharya, Kunal; Sullivan, Maeve; Walsh, Maureen; Creaven, Bernadette S; Laffir, Fathima; Duffy, Brendan; McHale, Patrick


    Microbial colonisation on clinical and industrial surfaces is currently of global concern and silane based sol-gel coatings are being proposed as potential solutions. Sol-gels are chemically inert, stable and homogeneous and can be designed to act as a reservoir for releasing antimicrobial agents over extended time periods. In the present study, silver nitrate (AgN) and a series of silver coumarin complexes based on coumarin-3-carboxylatosilver (AgC) and it is 6, 7 and 8 hydroxylated analogues (Ag6, Ag7, Ag8) were incorporated into sol-gel coatings. The comparative antibacterial activity of the coatings was determined against meticillin resistant Staphylococcus aureus (MRSA) and multidrug resistance Enterobacter cloacae WT6. The percentage growth inhibitions were found in the range of 9.2 (±2.7)-66.0 (±1.2)% at low silver loadings of 0.3% (w/w) with E. cloacae being the more susceptible. Results showed that among the Ag coumarin complexes, the Ag8 doped coating had the highest antibiofilm property. XPS confirmed the presence of silver in the nanoparticulate state (Ag(0)) at the coating surface where it remained after 4 days of exposure to bacterial culture. Comparative cytotoxicity studies revealed that the Ag-complex coatings were less toxic than the AgN coating. Thus, it can be concluded that a sol-gel matrix with Ag-coumarin complexes may provide non-toxic surfaces with antibacterial properties.

  1. Luminescent Thin Film of Doped Terbium Complex Obtained by Sol-Gel Method

    刘丰祎; 符连社; 王俊; 李焕荣; 张洪杰


    The transparent luminescent thin films of doped terbium complex were obtained by sol-gel method. The result indicates that rare earth carboxylates with poor solubility can be homogeneously doped into sol matrix in situ. The fluorescence spectra show that the thin film material emits the characteristic narrow band emission of Tb3+ under the UV excitation.

  2. Investigation of optical properties of anthocyanin doped into sol-gel based matrix

    Hashim, Hasrina; Abdul Aziz, Nik Mohd Azmi Nik; Isnin, Aishah


    Anthocyanin dye was extracted from petal of Hibiscus rosasinensis (Bunga Raya) and doped into sol-gel based matrix to investigate an effect of pH change on its optical properties. Sol-gel matrix based on Vinyl triethoxysilene (VTES) as a precursor was prepared through Sol-gel process at pH 7. The sol was doped with 0.1% of Anthocyanin and the same amount of dye was also dissolved in ethanol as a comparative sample. Hydrochloric Acid, HCl and Tetramethylammonium Hydroxide, TMAH were used to change the pH value by adding them at various concentrations into each sample. The emission spectra and chemical structures of the samples were measured by Spectrofluorometer and Fourier Transform Infrared (FTIR) respectively. When excited at 410 nm, two emission peaks at about 492 and 574 nm were observed for Anthocyanin in acidic environment both in ethanol and VTES sol. In base environment however, only Anthocyanin dissolved in ethanol produced emission peak with a single peak at about 539 nm. The sensitivity of Anthocyanin dye toward pH changes in VTES open a possibility to use it as sensing element in which sol-gel based matrix are known to have higher mechanical strength and thermal stability.

  3. [Sol-gel preparation of ultrathin nano-hydroxyapatite coating and its characterization].

    Yang, Jianhua; Guo, Linghong; Li, Hui


    Present study used dip-coating techniques to fabricate ultrathin nano-HA coating on titanium in organic sol-gel of Ca (NO3)2. 4H2O and PO(CH3)3 and inorganic sol-gel of Ca (NO3)2. 4H2O and (NH4)2HPO4. Scanning electron microscope (SEM) and grazing-incidence X-ray diffraction (XRD) were used to observe the morphology and distribution of crystallite size (D) and lattice strain (epsilon) of ultrathin nano-HA coating. After heated at 400 degrees C, the apatite structure of coatings on titanium began to appear. At heating temperature of 400 degrees C-600 degrees C, the effect of heating temperature on D and epsilon of both coatings was obvious. Precursor types significantly affected the particle diameters of nano-HA coatings, which were 25-40 nm for organic sol-gel and about 100 nm for inorganic sol. The thickness of ultrathin nano-HA coatings was 2.5 microm for organic sol-gel and 5 microm for inorganic sol and morphology of interfaces between coating and titanium was intact and homogenous.

  4. Sol-gel coating of inorganic nanostructures with resorcinol-formaldehyde resin.

    Li, Na; Zhang, Qiao; Liu, Jian; Joo, Jibong; Lee, Austin; Gan, Yang; Yin, Yadong


    A general sol-gel process has been developed to form a coating of resorcinol-formaldehyde (RF) resin on inorganic nanostructures of various compositions and morphologies. The RF shell can be conveniently converted into carbon through high temperature carbonization under an inert atmosphere.

  5. The increase in pH during aging of porous sol-gel silica spheres

    Titulaer, M.K.; Kegel, W.K.; Jansen, J.B.H.; Geus, John W.


    The increase in pH in the hydrothermal fluid is studied after hydrothermal aging of porous silica gel spheres of 1–3 mm diameter. The porous silica spheres are formed by the sol-gel process from a supersaturated silica solution. The increase of the pH of the hydrothermal solution affects the silica

  6. 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.

  7. Foldable and Cytocompatible Sol-gel TiO2 Photonics.

    Li, Lan; Zhang, Ping; Wang, Wei-Ming; Lin, Hongtao; Zerdoum, Aidan B; Geiger, Sarah J; Liu, Yangchen; Xiao, Nicholas; Zou, Yi; Ogbuu, Okechukwu; Du, Qingyang; Jia, Xinqiao; Li, Jingjing; Hu, Juejun


    Integrated photonics provides a miniaturized and potentially implantable platform to manipulate and enhance the interactions between light and biological molecules or tissues in in-vitro and in-vivo settings, and is thus being increasingly adopted in a wide cross-section of biomedical applications ranging from disease diagnosis to optogenetic neuromodulation. However, the mechanical rigidity of substrates traditionally used for photonic integration is fundamentally incompatible with soft biological tissues. Cytotoxicity of materials and chemicals used in photonic device processing imposes another constraint towards these biophotonic applications. Here we present thin film TiO2 as a viable material for biocompatible and flexible integrated photonics. Amorphous TiO2 films were deposited using a low temperature (<250 °C) sol-gel process fully compatible with monolithic integration on plastic substrates. High-index-contrast flexible optical waveguides and resonators were fabricated using the sol-gel TiO2 material, and resonator quality factors up to 20,000 were measured. Following a multi-neutral-axis mechanical design, these devices exhibit remarkable mechanical flexibility, and can sustain repeated folding without compromising their optical performance. Finally, we validated the low cytotoxicity of the sol-gel TiO2 devices through in-vitro cell culture tests. These results demonstrate the potential of sol-gel TiO2 as a promising material platform for novel biophotonic devices.

  8. Highly Luminescent Hybrid SiO2-Coated CdTe Quantum Dots Retained Initial Photoluminescence Efficiency in Sol-Gel SiO2 Film.

    Sun, Hongsheng; Xing, Yugui; Wu, Qinan; Yang, Ping


    A highly luminescent silica film was fabricated using tetraethyl orthosilicate (TEOS) and 3-aminopropyltrimethoxysilane (APS) through a controlled sol-gel reaction. The pre-hydrolysis of TEOS and APS which resulted in the mixture of TEOS and APS in a molecular level is a key for the formation of homogenous films. The aminopropyl groups in APS play an important role for obtaining homogeneous film with high photoluminescence (PL). Red-emitting hybrid SiO2-coated CdTe nano-crystals (NCs) were fabricated by a two-step synthesis including a thin SiO2 coating via a sol-gel process and a subsequent refluxing using green-emitting CdTe NCs. The hybrid SiO2-coated CdTe NCs were embedded in a functional SiO2 film via a two-step process including adding the NCs in SiO2 sol with a high viscosity and almost without ethanol and a subsequent spinning coating. The hybrid SiO2-coated CdTe NCs retained their initial PL efficiency (54%) in the film. Being encapsulated with the hybrid NCs in the film, no change on the absorption and PL spectra of red-emitting CdTe NCs (632 nm) was observed. This indicates the hybrid NCs is stable enough during preparation. This phenomenon is ascribed to the controlled sol-gel process and a hybrid SiO2 shell on CdTe NCs. Because these films exhibited high PL efficiency and stability, they will be utilizable for potential applications in many fields.

  9. Investigations of the small-scale thermal behavior of sol-gel thermites.

    Warren, Mial E.; Farrow, Matthew; Tappan, Alexander Smith


    Sol-gel thermites, formulated from nanoporous oxides and dispersed fuel particles, may provide materials useful for small-scale, intense thermal sources, but understanding the factors affecting performance is critical prior to use. Work was conducted on understanding the synthesis conditions, thermal treatments, and additives that lead to different performance characteristics in iron oxide sol-gel thermites. Additionally, the safety properties of sol-gel thermites were investigated, especially those related to air sensitivity. Sol-gel thermites were synthesized using a variety of different techniques and there appear to be many viable routes to relatively equivalent thermites. These thermites were subjected to several different thermal treatments under argon in a differential scanning calorimeter, and it was shown that a 65 C hold for up to 200 minutes was effective for the removal of residual solvent, thus preventing boiling during the final thermal activation step. Vacuum-drying prior to this heating was shown to be even more effective at removing residual solvent. The addition of aluminum and molybdenum trioxide (MoO{sub 3}) reduced the total heat release per unit mass upon exposure to air, probably due to a decrease in the amount of reduced iron oxide species in the thermite. For the thermal activation step of heat treatment, three different temperatures were investigated. Thermal activation at 200 C resulted in increased ignition sensitivity over thermal activation at 232 C, and thermal activation at 300 C resulted in non-ignitable material. Non-sol-gel iron oxide did not exhibit any of the air-sensitivity observed in sol-gel iron oxide. In the DSC experiments, no bulk ignition of sol-gel thermites was observed upon exposure to air after thermal activation in argon; however ignition did occur when the material was heated in air after thermal treatment. In larger-scale experiments, up to a few hundred milligrams, no ignition was observed upon exposure to air

  10. Iron specificity of a biosensor based on fluorescent pyoverdin immobilized in sol-gel glass

    Kisaalita William S


    Full Text Available Abstract Two current technologies used in biosensor development are very promising: 1. The sol-gel process of making microporous glass at room temperature, and 2. Using a fluorescent compound that undergoes fluorescence quenching in response to a specific analyte. These technologies have been combined to produce an iron biosensor. To optimize the iron (II or III specificity of an iron biosensor, pyoverdin (a fluorescent siderophore produced by Pseudomonas spp. was immobilized in 3 formulations of porous sol-gel glass. The formulations, A, B, and C, varied in the amount of water added, resulting in respective R values (molar ratio of water:silicon of 5.6, 8.2, and 10.8. Pyoverdin-doped sol-gel pellets were placed in a flow cell in a fluorometer and the fluorescence quenching was measured as pellets were exposed to 0.28 - 0.56 mM iron (II or III. After 10 minutes of exposure to iron, ferrous ion caused a small fluorescence quenching (89 - 97% of the initial fluorescence, over the range of iron tested while ferric ion caused much greater quenching (65 - 88%. The most specific and linear response was observed for pyoverdin immobilized in sol-gel C. In contrast, a solution of pyoverdin (3.0 μM exposed to iron (II or III for 10 minutes showed an increase in fluorescence (101 - 114% at low ferrous concentrations (0.45 - 2.18 μM while exposure to all ferric ion concentrations (0.45 - 3.03 μM caused quenching. In summary, the iron specificity of pyoverdin was improved by immobilizing it in sol-gel glass C.

  11. Iron specificity of a biosensor based on fluorescent pyoverdin immobilized in sol-gel glass.

    Yoder, Michael F; Kisaalita, William S


    Two current technologies used in biosensor development are very promising: 1. The sol-gel process of making microporous glass at room temperature, and 2. Using a fluorescent compound that undergoes fluorescence quenching in response to a specific analyte. These technologies have been combined to produce an iron biosensor. To optimize the iron (II or III) specificity of an iron biosensor, pyoverdin (a fluorescent siderophore produced by Pseudomonas spp.) was immobilized in 3 formulations of porous sol-gel glass. The formulations, A, B, and C, varied in the amount of water added, resulting in respective R values (molar ratio of water:silicon) of 5.6, 8.2, and 10.8. Pyoverdin-doped sol-gel pellets were placed in a flow cell in a fluorometer and the fluorescence quenching was measured as pellets were exposed to 0.28 - 0.56 mM iron (II or III). After 10 minutes of exposure to iron, ferrous ion caused a small fluorescence quenching (89 - 97% of the initial fluorescence, over the range of iron tested) while ferric ion caused much greater quenching (65 - 88%). The most specific and linear response was observed for pyoverdin immobilized in sol-gel C. In contrast, a solution of pyoverdin (3.0 μM) exposed to iron (II or III) for 10 minutes showed an increase in fluorescence (101 - 114%) at low ferrous concentrations (0.45 - 2.18 μM) while exposure to all ferric ion concentrations (0.45 - 3.03 μM) caused quenching. In summary, the iron specificity of pyoverdin was improved by immobilizing it in sol-gel glass C.

  12. Fabrication of spherical CaO-SrO-ZnO-SiO₂ particles by sol-gel processing.

    Kim, Ill Yong; Towler, Mark R; Wren, Anthony; Ohtsuki, Chikara


    This study was concerned with the fabrication of ceramic CaO-SrO-ZnO-SiO(2) spherical particles, which are novel candidates for the glass phase in glass polyalkenoate cements (GPCs). GPCs made from these glasses have potential as bone cements because, unlike conventional GPCs, they do not contain aluminum ions, which inhibit the calcification of hydroxyapatite in the body. The glass phase of GPCs require a controllable glass morphology and particle size distribution. Sol-gel processing can potentially be used to fabricate homogenous ceramic particles with controlled morphology. However, a thorough study on preparation conditions of spherical CaO-SrO-ZnO-SiO(2) particles by sol-gel processing has, to date, not been reported. In this study, gels were prepared by hydrolysis and polycondensation of tetraethoxysilane (TEOS) in an aqueous solution containing polyethylene glycol and nitrates of calcium, strontium and zinc. It was possible to control the morphology and size of the gels by varying the H(2)O/TEOS molar ratio and the metal ion content in the starting compositions. An aliquot of 3-5 mum homogenous spherical particles were obtained at a H(2)O/TEOS molar ratio of 42.6 when the starting composition molar ratios were Sr(NO(3)):Ca(NO(3))(2):Zn(NO(3))(2):Si(OC(2)H(5))(4) = x:0.12:(0.40 - x):0.48 (0

  13. The sol-gel route: A versatile process for up-scaling the fabrication of gas-tight thin electrolyte layers

    Viazzi, Céline; Rouessac, Vincent; Lenormand, Pascal; Julbe, Anne; Ansart, Florence; Guizard, Christian


    Sol-gel routes are often investigated and adapted to prepare, by suitable chemical modifications, submicronic powders and derived materials with controlled morphology, which cannot be obtained by conventional solid state chemistry paths. Wet chemistry methods provide attractive alternative routes because mixing of species occurs at the atomic scale. In this paper, ultrafine powders were prepared by a novel synthesis method based on the sol-gel process and were dispersed into suspensions before processing. This paper presents new developments for the preparation of functional materials like yttria-stabilized-zirconia (YSZ, 8% Y2O3) used as electrolyte for solid oxide fuel cells. YSZ thick films were coated onto porous Ni-YSZ substrates using a suspension with an optimized formulation deposited by either a dip-coating or a spin-coating process. The suspension composition is based on YSZ particles encapsulated by a zirconium alkoxide which was added with an alkoxide derived colloidal sol. The in situ growth of these colloids increases significantly the layer density after an appropriated heat treatment. The derived films were continuous, homogeneous and around 20 μm thick. The possible up-scaling of this process has been also considered and the suitable processing parameters were defined in order to obtain, at an industrial scale, homogeneous, crack-free, thick and adherent films after heat treatment at 1400 °C.

  14. 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.

  15. Transport Properties of Polycrystalline La2/3Ca1/3Mn1-x CuxO3 Prepared by Sol-Gel

    YANG Ying-ping; YUAN Song-liu; XIA Zheng-cai; ZHANG Guo-hong; ZHANG Li-jiang


    The influence of Cu dopant (x) and sintering temperature (Ts) on the transport properties of La2/3 Ca1/3 Mn1- xCuxO3 series samples prepared by Sol-Gel technique was investigated. X-ray diffraction patterns show that all the samples with different Cu dopant and sintering temperatures (Ts) are of single phase without obvious lattice distortion. Experimental results indicate that the insulator-metal transition temperature is directly related to the sintering temperature and Cu dopant x. It is interesting to observe that a proper amount of Cu dopant can substantially improve magnetoresistance effects.

  16. Emission spectra of the sol-gel glass doped with europium(III) complexes of picolinic acid N-oxide-A new UV-light sensor

    Godlewska, P. [Department of Bioorganic Chemistry, Institute of Chemistry and Food Technology, Faculty of Engineering and Economics, Lower Silesian University of Economics, Wroclaw (Poland); Macalik, L. [Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Wroclaw (Poland); Hanuza, J. [Department of Bioorganic Chemistry, Institute of Chemistry and Food Technology, Faculty of Engineering and Economics, Lower Silesian University of Economics, Wroclaw (Poland); Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Wroclaw (Poland)], E-mail:


    New europium complexes of picolinic acid N-oxides have been synthesised and introduced into sol-gel matrices. Their application as UV-light sensors has been considered. The sequence of the electronic levels for Eu{sup 3+} ions has been determined from the absorption and emission studies and assigned to the respective electron transitions. The lifetimes of the excited states have been detected and analysed. The role of the CT transition inside the picolinic ligand and its influence on the ligand to metal charge transfer (LMCT) have been discussed.

  17. Antimony (V) Oxide Adsorbed on a Silica-Zirconia Mixed Oxide Obtained by the Sol-Gel Processing Method: Preparation and Acid Properties

    Zaitseva,Galina; Gushikem,Yoshitaka


    The preparation, degree of dispersion, thermal stability and Lewis and Brønsted acidity of antimony (V) oxide adsorbed on SiO2/ZrO2 mixed oxide, previously prepared by the sol-gel processing method, are described herein. The samples SiO2/ZrO2/Sb2O5, with compositions (in wt %): (a) Zr= 8.1 and Sb= 6.3; (b) Zr= 14.9 and Sb= 11.4, were prepared. Scanning electron microscopy images connected to a X-ray energy dispersive spectrometer showed that both metals, Zr and Sb, were highly dispersed ...

  18. Effect of PMMA impregnation on the fluorescence quantum yield of sol-gel glasses doped with quinine sulfate

    Meneses-Nava, M. A.; Barbosa-García, O.; Díaz-Torres, L. A.; Chávez-Cerda, S.; Torres-Cisneros, M.; King, T. A.


    The fluorescence quantum yield of quinine sulfate in sol-gel and PMMA impregnated glasses is measured. The observed quantum yield improvement in the sol-gel matrix, compared to ethanol, is interpreted as a reduction of non-radiative relaxation channels by isolation of the molecules by the cage of the glass. PMMA impregnated sol-gel glasses show an extra improvement of the fluorescence yield, which is interpreted as a reduction of the free space and the rigid fixation of the molecules to the matrix.

  19. Erosion and high temperature oxidation resistance of new coatings fabricated by a sol-gel route for a TBC application.

    Viazzi, Céline; Wellman , Richard; Oquab, Djar; Nicholls, John; Monceau, Daniel; Bonino, Jean-Pierre; Ansart, Florence


    This paper examines the erosion and cyclic oxidation performance of novel thermal barrier coatings produced via the sol-gel route. The ceramic top coat, with a thickness of 5-80 m, was deposited via a sol-gel route onto standard MCrAlY and PtAl bond coats. In both the erosion and the cyclic oxidation tests it was found that the bond coat had a profound affect on the results. The erosion of the sol-gel coatings were compared to standard EB PVD and PS TBCs and were found to be significantly...



    The aim of the experiment was the obtaining of thin silica coatings on titanium by sol-gel method, using mechanical (SiC - paper No.180) and chemical (leaching in HF) pretreatments of the titanium substrates. The solutions were based on TEOS. For the sol-gel dipping process 4 different solutions were prepared: silica, silica with AgNO3 and silica + AgNO3 with brushite (CaHPO4·2H2O) or monetite (CaHPO4) powders. The solutions were aged for 7 and 14 days at laboratory temperature. After sol-gel...

  1. Occlusion of chromophore oxides by Sol-Gel methods: Application to the synthesis of hematite-silica red pigments

    Vicent, J. B.


    Full Text Available Heteromorphic pigments present the chromophore particle occluded in an encapsulating matrix which is thermally stable and insoluble in glazes. The occluded chromophore compound is also insoluble in the host matrix. In this work the mechanisms of formation of this type of pigments are analyzed and the occlusion of hematite into silica matrix is discussed. The formation of this hematite-silica red pigment follows a sintering-coarsening mechanism, and, consequently, the control of both hematite particles nucleation and their crystal growth results to be decisive to obtain a good coloring effectiveness.

    En los pigmentos heteromórficos la partícula de cromóforo es ocluida en una matriz encapsuladora estable tanto termicamente como frente a los vidriados. El compuesto cromóforo ocluido y la matriz no coloreada son insolubles. En este trabajo se analiza los diferentes mecanismos de formación de estos pigmentos heteromórficos y se estudia la oclusión de hematita en sílice mediante métodos sol-gel acuoso. El pigmento sigue un mecanismo de sinterización-crecimiento cristalino por lo que es muy importante controlar el momento de nucleación y la velocidad de crecimiento de las partículas de hematita en el seno de la matriz.

  2. Electrochemically assisted deposition of sol-gel bio-composite with co-immobilized dehydrogenase and diaphorase

    Wang Zhijie [LCPME, UMR 7564, CNRS-Nancy University, 405, rue de Vandoeuvre, 54600 Villers-les-Nancy (France); Etienne, Mathieu, E-mail: [LCPME, UMR 7564, CNRS-Nancy University, 405, rue de Vandoeuvre, 54600 Villers-les-Nancy (France); Kohring, Gert-Wieland [Mikrobiologie, Universitaet des Saarlandes, Campus, Geb. A1.5, D-66123 Saarbruecken (Germany); Bon-Saint-Come, Yemima; Kuhn, Alexander [Universite Bordeaux, ISM, ENSCPB, 16 avenue Pey Berland, 33607 Pessac (France); Walcarius, Alain [LCPME, UMR 7564, CNRS-Nancy University, 405, rue de Vandoeuvre, 54600 Villers-les-Nancy (France)


    We report here that the electrochemically assisted deposition (EAD) of silica thin films can be a good strategy to co-encapsulate D-sorbitol dehydrogenase (DSDH) and diaphorase in an active form. This is achieved via the electrolysis of a hydrolyzed sol containing the biomolecules to initiate the poly-condensation of silica precursors upon electrochemically induced pH increase at the electrode/solution interface. DSDH was found to be very sensitive to the silica gel environment and the addition of a positively-charged polyelectrolyte was necessary to ensure effective operational behavior of the biomolecules. The composition of the sol and the conditions for electrolysis have been optimized with respect to the intensity of the electrochemical response to D-sorbitol oxidation. The K{sub m} of DSDH in the electrodeposited film was in the range of 3 mM, slightly better than the value determined biochemically in solution (6.5 mM). The co-immobilization of DSDH and diaphorase in this way led on the one hand to the possible reduction of NAD{sup +} to NADH (simultaneously to D-sorbitol oxidation) and on the other hand to the safe re-oxidation of the co-factor using a mediator (ferrocenedimethanol) as electron relay. The bioelectrocatalytic response looks promising for electro-enzymatic applications. To support this idea, the EAD of sol-gel bio-composite has been extended to macroporous electrodes displaying a much bigger electroactive surface area.

  3. A New Route to Liposil Formation by an Interfacial Sol-Gel Process Confined by Lipid Bilayer.

    Shen, Shukun; Yang, Lu; Lu, Yaxing; Chen, Jian-Gang; Song, Shaofei; Hu, Daodao; Parikh, Atul


    We report a new and simple approach to prepare a class of silica-reinforced liposomes with hybrid core-shell nanostructures. The amphiphilic natural structure of lipids was exploited to sequester hydrophobic molecules, namely precursor TEOS and pyrene, in the hydrophobic midplane of liposomal bilayer assemblies in the aqueous phase. Subsequent interfacial hydrolysis of TEOS at the bilayer/water interface and ensuing condensation within the hydrophobic interstices of the lipid bilayer drives silica formation in situ, producing a novel class of silica-lipid hybrid liposils. Structural characterization by scanning- and transmission electron microscopy confirm that the liposils so generated preserve closed topologies and size-monodipersity of the parent lecithin liposomes, and DSC-TGA and XRD measurements provide evidence for the silica coating. Monitoring fluorescence measurements using embedded pyrene yield detailed information on microenvironment changes, which occur during sol-gel process and shed light on the structural evolution during silica formation. We envisage that liposils formed by this simple, new approach, exploiting the hydrophobic core of the lipid bilayer to spatially localize silica-forming precursors enables preparation of stable liposils exhibiting capacity for cargo encapsulation, bicompatibility, and fluorescence monitoring, more generally opening a window for construction of stable, functional hybrid materials.

  4. High Cycling Performance Cathode Material: Interconnected LiFePO4/Carbon Nanoparticles Fabricated by Sol-Gel Method

    Zhigao Yang


    Full Text Available Interconnected LiFePO4/carbon nanoparticles for Li-ion battery cathode have been fabricated by sol-gel method followed by a carbon coating process involving redox reactions. The carbon layers coated on the LiFePO4 nanoparticles not only served as a protection layer but also supplied fast electrons by building a 3D conductive network. As a cooperation, LiFePO4 nanoparticles encapsulated in interconnected conductive carbon layers provided the electrode reactions with fast lithium ions by offering the lithium ions shortening and unobstructed pathways. Field emission scanning electron microscopy (FESEM and X-ray diffraction (XRD tests showed optimized morphology. Electrochemical characterizations including galvanostatic charge/discharge, cyclic voltammetry (CV, and electrochemical impedance spectroscopy (EIS tests, together with impedance parameters calculated, all indicated better electrochemical performance and excellent cycling performance at high rate (with less than 9.5% discharge capacity loss over 2000 cycles, the coulombic efficiency maintained about 100%.

  5. Biomolecules/gold nanowires-doped sol-gel film for label-free electrochemical immunoassay of testosterone.

    Liang, Ke-Zhong; Qi, Jun-Sheng; Mu, Wei-Jun; Chen, Zai-Gang


    A direct, rapid, and label-free electrochemical immunoassay method for testosterone has been described based on encapsulating testosterone antibody into polyvinyl butyral sol-gel film doped with gold nanowires. Gold nanowires prepared by using nanopore polycarbonate membrane were used to conjugate testosterone antibody onto the probe surface. The presence of gold nanowires provided a biocompatible microenvironment for biomolecules, greatly amplified the immobilized amount of biomolecules on the electrode surface, and improved the sensitivity of the immunosensor. In comparison with gold nanoparticle-conjugating probe, the gold nanowire-functionalized probe could avoid the leakage of biomolecules from the composite film, and enhanced the stability of the sensor. The performance and factors influencing the performance of the resulting immunosensor were investigated in detail. Under optimal conditions, the developed immunosensor exhibited a good linear relationship with testosterone ranging from 1.2 to 83.5 ng mL(-1) with a detection limit of 0.1 ng mL(-1) (at 3delta). Moreover, the proposed immunosensor exhibited high sensitivity, good reproducibility and long-term stability. The as-prepared immunosensors were used to analyze testosterone in human serum specimens. Analytical results suggest that the developed immunoassay has a promising alternative approach for detecting testosterone in the clinical diagnosis. Compared with the conventional ELISAs, the proposed immunoassay method was simple and rapid without multiple labeling and separation steps. Importantly, the route provides an alternative approach to incorporate gold nanowires into the solid matrix for biosensing application.

  6. Manufacture of amorphous and poly-crystalline materials with the sol-gel process; Fabricacion de materiales amorfos y policristalinos con la ruta sol-gel

    Castaneda-Contreras, J. [Centro Universitario de Los Lagos, Universidad de Guadalajara, Guadalajara, Jalisco (Mexico)


    The sun-gel process is a chemical route that allows the manufacture of amorphous and poly-crystalline materials in a relatively simple way. New materials can be obtained, materials that through the traditional manufacture methods, are very difficult to obtain, such as oxide combinations (SiO{sub 2}, TiO{sub 2}, ZrO{sub 2}, etc.), and that, when being produced by traditional methods, they run the risk of being contaminated with rare earth ions or organic dyes. The unique structures, micro- structures and compounds that can be made with the sun-gel process open many possibilities for practical applications, to name a few: the manufacture of optical components, preforms for optical fibers, dielectric coatings, superconductors, waveguides, nanoparticles, solar cells, etc. [Spanish] El proceso sol-gel es una ruta quimica que permite fabricar materiales amorfos y policristalinos de forma relativamente sencilla. Se pueden obtener nuevos materiales que a traves de los metodos tradicionales de fabricacion son muy dificiles de obtener, tales como combinaciones de oxidos (SiO{sub 2}, TiO{sub 2}, ZrO{sub 2}, etc.), y que, de ser producidos por metodos tradicionales corren el riesgo de contaminarse con iones de tierras raras o colorantes organicos. Las estructuras unicas, micro estructuras y compuestos que pueden hacerse con el proceso sol-gel abren muchas posibilidades para aplicaciones practicas, por nombrar algunas, la fabricacion de componentes opticos, preformas para fibras opticas, recubrimientos dielectricos, superconductores, guias de onda, nanoparticulas, celdas solares, etc.

  7. Pulsed electric field assisted sol-gel preparation of TiO2 nanoparticles

    Mani, Rajaboopathi; Han, Bing; Louhi-Kultanen, Marjatta


    This work studies the effect of a pulsed electric field (PEF) on the precipitation and properties of TiO2 nanoparticles. TiO2 nanoparticles were prepared using pulsed DC electric field assisted sol-gel method. The duration of the PEF treatment was varied to investigate its effect on the particle size of TiO2 nanoparticles. The nanoparticles were characterized by X-ray powder diffraction (XRD), Raman spectroscopy, UV diffuse reflectance spectroscopy (UV-DRS) and transmission electron microscopy (TEM). It was found that TiO2 particles prepared with pulsed electric field assisted sol-gel method had enhanced average crystallite size due to the effect of the pulsed electric field on primary nucleation. The effect of electric field on nanoparticle preparation is interesting which can be used to control the grain and crystallite size of nanoparticle.

  8. Incorporation of europium III complex into nanoparticles and films obtained by the Sol-Gel methodology

    Faley Jean de Sousa


    Full Text Available The sol-gel process is very effective for the preparation of new materials with potential applications in optics, sensors, catalyst supports, coatings, and specialty inorganic polymers that can be used as hosts for the accommodation of organic molecules. The low temperature employed in the process is the main advantage of this methodology. In this work, the europium (III complex with 1,10-phenantroline was prepared, and this luminescent complex was incorporated into silica nanoparticles and films by the sol-gel process. The nanoparticles were obtained by the modified Stöber methodology. The films were obtained by the dip-coating technique, at different deposition rates and numbers of layers. The nanoparticles and films were characterized by photoluminescence, thermal analysis, and Raman and infrared spectroscopies. Characterization revealed that the europium (III complex was not affected upon incorporation into the nanoparticles and films, opening a new field for the application of these materials.

  9. Three-phase microemulsion/sol-gel system for aqueous catalysis with hydrophobic chemicals.

    Abu-Reziq, Raed; Blum, Jochanan; Avnir, David


    A facile three-phase transport process is described that allows to carry out catalytic reactions in water, whereby all components are hydrophobic. According to this process a hydrophobic substrate is microemulsified in water and subjected to an organometallic catalyst, which is entrapped within a partially hydrophobized sol-gel matrix. The surfactant molecules, which carry the hydrophobic substrate, adsorb/desorb reversibly on the surface of the sol-gel matrix breaking the micellar structure, spilling their substrate load into the porous medium that contains the catalyst. A catalytic reaction then takes place within the ceramic material to form the desired products that are extracted by the desorbing surfactant, carrying the emulsified product back into the solution. The method is general and versatile and has been demonstrated with the catalytic hydrogenations of alkenes, alkynes, aromatic C=C bonds, and nitro and cyano groups.

  10. Preparation of nanometer MgO by sol-gel auto-combustion


    Nanometer MgO was prepared via a sol-gel auto-combustion technique using magnesium nitrate as raw material and citric acid as chelating agent.IR spectra of the dried gel were used to investigate the structure of the precursors.By studying the different TG curves of magnesium citrate gel prepared by different methods,we found that a combustion process occurred and the nitrate ions acted as an oxidant in the combustion process.TEM photographs of synthesized powders from the sol-gel auto-combustion showed that the crystallites were uniform in size.In addition,the XRD pattern of this sample showed that the particle size was 8.9 nm.The BET curves,in turn,showed that the specific surface of the sample was 26.34 m2/g.The mechanism of the frothing process in restraining agglomeration is discussed.

  11. Fluor-hydroxyapatite sol-gel coating on titanium substrate for hard tissue implants.

    Kim, Hae-Won; Kim, Hyoun-Ee; Knowles, Jonathan C


    Hydroxyapatite (HA) and fluor-hydroxyapatite (FHA) films were deposited on a titanium substrate using a sol-gel technique. Different concentrations of F- were incorporated into the apatite structure during the sol preparation. Typical apatite structures were obtained for all coatings after dipping and subsequent heat treatment at 500 degrees C. The films obtained were uniform and dense, with a thickness of approximately 5 microm. The dissolution rate of the coating layer decreased with increasing F- incorporation within the apatite structure, which demonstrates the possibility of tailoring the solubility by a functional gradient coating of HA and FHA. The cell proliferation rate on the coating layer decreased slightly with increasing F- incorporation. The alkaline phosphatase (ALP) activity of the cells on all the HA and FHA coated samples showed much higher expression levels compared to pure Ti. This confirmed the improved activity of cell functions on the substrates with the sol-gel coating treatment.

  12. Reversible Sol-Gel Transitions in Aqueous Solutions of N-Isopropylacrylamide Ionic Copolymers

    Krzyminski, Karol J.; Jasionowski, Marek; Gutowska, Anna


    Ionic copolymers of N-isopropylacrylamide (NIPA) exhibiting sol-gel transitions in aqueous solutions were investigated. The studies were aimed at understanding of the structure-property relationship in design of injectable, in situ forming gels for potential biomedical applications in delivery of therapeutics and tissue engineering. Aqueous solutions of NIPA ionic copolymers were found to flow freely at ambient temperatures and formed soft gels with controlled syneresis above 32°C, the lower critical solution temperature of NIPA. The sol-gel transitions and temperature dependent properties of the resulting gels were analyzed using dynamic rheometry, UV and IR spectrometry, and were found to be controlled by the molecular weight and composition of copolymers, ionization state of comonomers, and composition of aqueous solvent.

  13. 3D Printed PEG-Based Hybrid Nanocomposites Obtained by Sol-Gel Technique.

    Chiappone, Annalisa; Fantino, Erika; Roppolo, Ignazio; Lorusso, Massimo; Manfredi, Diego; Fino, Paolo; Pirri, Candido Fabrizio; Calignano, Flaviana


    In this work, three-dimensional (3D) structured hybrid materials were fabricated combining 3D printing technology with in situ generation of inorganic nanoparticles by sol-gel technique. Those materials, consisting of silica nanodomains covalently interconnected with organic polymers, were 3D printed in complex multilayered architectures, incorporating liquid silica precursors into a photocurable oligomer in the presence of suitable photoinitiators and exposing them to a digital light system. A post sol-gel treatment in acidic vapors allowed the in situ generation of the inorganic phase in a dedicated step. This method allows to build hybrid structures operating with a full liquid formulation without meeting the drawbacks of incorporating inorganic powders into 3D printable formulations. The influence of the generated silica nanoparticle on the printed objects was deeply investigated at macro- and nanoscale; the resulting light hybrid structures show improved mechanical properties and, thus, have a huge potential for applications in a variety of advanced technologies.

  14. 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...

  15. Ion beam photography in sol-gel NiO-SiO{sub 2} films

    Canut, B. E-mail:; Merlen, A.; Teodorescu, V.; Ghica, C.; Sandu, C.S.; Ramos, S.M.M.; Bovier, C.; Espiau de la Maestre, R.; Broniatowski, A.; Bernas, H


    Composite oxide films (NiO-SiO{sub 2}) were deposited on silicon wafers using the sol-gel dip coating technique. The average stoichiometry [NiO]/[SiO{sub 2}], adjusted from the molar ratio of the two starting precursors, was typically 10%. Single and multilayer coatings were used to obtain film thicknesses from 70 to 400 nm. The samples were then irradiated at room temperature with MeV ions in the 10{sup 12}-10{sup 14} cm{sup -2} fluence range and further annealed at low temperature in argon atmosphere. Our first cross-sectional transmission electron microscopy studies show that such a treatment induces the nucleation and growth of pure Ni clusters. Some information is obtained on the specific features due to the sol-gel fabrication process.

  16. 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.

  17. A Review of Photocatalysts Prepared by Sol-Gel Method for VOCs Removal

    Ting Ke Tseng


    Full Text Available The sol-gel process is a wet-chemical technique (chemical solution deposition, which has been widely used in the fields of materials science, ceramic engineering, and especially in the preparation of photocatalysts. Volatile organic compounds (VOCs are prevalent components of indoor air pollution. Among the approaches to remove VOCs from indoor air, photocatalytic oxidation (PCO is regarded as a promising method. This paper is a review of the status of research on the sol-gel method for photocatalyst preparation and for the PCO purification of VOCs. The review and discussion will focus on the preparation and coating of various photocatalysts, operational parameters, and will provide an overview of general PCO models described in the literature.

  18. 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.

  19. Versatile technique to functionalize optical microfibers via a modified sol-gel dip-coating method.

    Xu, Z Y; Li, Y H; Wang, L J


    We present a convenient and versatile technique to functionalize microfibers by depositing sol-gel jackets via a modified dip-coating method. This was elucidated by gain-functionalizing microfibers with erbium-ytterbium codoped silica sol-gel jackets. For a 4.5-cm-long coated microfiber, an internal gain of 1.8 dB and a net gain of 0.8 dB for a 1550 nm signal were observed, when combing together the gain of the doped jackets and low loss of microfibers. With benefits of convenience and versatility, this technique can be used for functionalizing microfibers with jackets showing gains in other spectral ranges, high nonlinearity, high sensitivity, and many other functions.

  20. The role of temperature in forming sol-gel biocomposites containing polydopamine

    Dyke, Jason Christopher; Hu, Huamin; Lee, Dong Joon; Ko, Ching-Chang; You, Wei


    To further improve the physical strength and biomedical applicability of bioceramicsbuilt on hydroxyapatite-gelatin (HAp-Gel) and siloxane sol-gel reactions, we incorporated mussel adhesive inspired polydopamine (PD) into our original composite based on HAp-Gel cross-linked with siloxane. Surprisingly, with the addition of PD, we observed that the processing conditions and temperatures play an important role in the structure and performance of these materials. A systematic study to investigate this temperature dependence behavior discloses that the rate of crosslinking of silane during the sol-gel process is significantly influenced by the temperature, whereas the polymerization of the dopamine only shows minor temperature dependence. With this discovery, we report an innovative thermal process for the design and application of these biocomposites. PMID:25485111

  1. Microstructure Control of Nanoporous Silica Thin Film Prepared by Sol-gel Process


    Nanoporous silica films were prepared by sol-gel process with base, acid and base/acid two-step catalysis.Transmission electron microscope (TEM) and particle size analyzer were used to characterize the microstructure and the particle size distribution of the sols. Scanning electron microscopy (SEM), atomic force microscopy (AFM) and spectroscopic ellipsometer were used to characterize the surface microstructure and the optical properties of the silica films. Stability of the sols during long-term storage was investigated. Moreover,the dispersion relation of the optical constants of the silica films, and the control of the microstructure and properties of the films by changing the catalysis conditions during sol-gel process were also discussed.

  2. Performance of astronomical beam combiner prototypes fabricated by hybrid sol-gel technology.

    Ghasempour, Askari; Leite, A M P; Alexandre, D; Reynaud, F; Marques, P V S; Garcia, P J V; Moreira, P J


    Integrated optics coaxial two, three and four telescope beam combiners have been fabricated by hybrid sol-gel technology for astronomical applications. Temporal and spectral analyses of the output interferometric signal have been performed, and their results are in mutual good agreement. The results of the characterization method employed are cross-checked using contrast measurements obtained independently, demonstrating that the chromatic differential dispersion is the main contributer to contrast reduction. The mean visibility of the fabricated devices is always higher than 95 %, obtained using a source with spectral bandwidth of 50 nm. These results show the capability of hybrid sol-gel technology for fast prototyping of complex chip designs used in astronomical applications.

  3. A sol-gel method to synthesize indium tin oxide nanoparticles

    Xiuhua Li; Xiujuan xu; Xin Yin; Chunzhong Li; Jianrong Zhang


    Transparent conductive indium tin oxide (ITO) nanoparticles were synthesized by a novel sol-gel method.Granulated indium and tin were dissolved in HNO3 and partially complexed with citric acid.A sol-gel process was induced when tertiary butyl alcohol was added dropwise to the above solution.ITO nanoparticles with an average crystallite size of 18.5 nm and surface area of 32.6 m2/g were obtained after the gel was heat-treated at 700 C.The ITO nanoparticles showed good sinterability,the starting sintering temperature decreased sharply to 900 C,and the 1400 C sintered pellet had a density of 98.1 % of theoretical density (TD).

  4. Tunable erbium-doped microbubble laser fabricated by sol-gel coating

    Yang, Yong; Kasumie, Sho; Xu, Linhua; Ward, Jonathan; Yang, Lan; Chormaic, Síle Nic


    In this work, we show that the application of a sol-gel coating renders a microbubble whispering gallery resonator into an active device. During the fabrication of the resonator, a thin layer of erbium-doped sol-gel is applied to a tapered microcapillary, then a microbubble with a wall thickness of 1.3 $\\mu$m is formed with the rare earth diffused into its walls. The doped microbubble is pumped at 980 nm and lasing in the emission band of the Er$^{3+}$ ions with a wavelength of 1535 nm is observed. The laser wavelength can be tuned by aerostatic pressure tuning of the whispering gallery modes of the microbubble. Up to 240 pm tuning is observed with 2 bar of applied pressure. It is shown that the doped microbubble could be used as a compact, tunable laser source. The lasing microbubble can also be used to improve sensing capabilities in optofluidic sensing applications.

  5. Comparative study of ZnO thin films prepared by different sol-gel route

    F Esmaieli Ghodsi


    Full Text Available   Retraction Notice    The paper "Comparative study of ZnO thin films prepared by different sol-gel route" by H. Absalan and F. E. Ghodsi, which appeared in Iranian Journal of Physics Research, Vol. 11, No. 4, 423-428 (in Farsi is translation of the paper "Comparative Study of ZnO Thin Films Prepared by Different Sol-Gel Route" by F. E. Ghodsi and H. Absalan, which appeared in ACTA PHYSICA POLONICA A, Vol 118 (2010 (in English and for this reason is retracted from this journal.The corresponding author  (and also the first author is the only responsible person for this action.   

  6. 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.

  7. Biological influence of Ca/P ratio on calcium phosphate coatings by sol-gel processing

    Catauro, M., E-mail: [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Papale, F. [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Sapio, L.; Naviglio, S. [Department of Biochemistry, Biophysics and General Pathology, Second University of Naples, Via L. De Crecchio 7, 80138 Naples (Italy)


    The objective of this work has been to develop low temperature sol-gel glass coatings to modify the substrate surface and to evaluate their bioactivity and biocompatibility. Glasses, based on SiO{sub 2}·CaO·P{sub 2}O{sub 5}, were synthesized by the sol-gel technique using tetraethyl orthosilicate, calcium nitrate tetrahydrate and triethyl phosphate as precursors of SiO{sub 2}, CaO and P{sub 2}O{sub 5}, respectively. Those materials, still in the sol phase, have been used to coat substrates by means of the dip-coating technique. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) has been used for characterize coatings and a microstructural analysis has been obtained using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated substrate was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. In order to study the cell behavior and response to our silica based materials, prepared via the sol-gel method, with various Ca/P ratio and coating substrate, we have used the human osteoblast-like U2OS cell line. - Highlights: • Coatings consisting of SiO{sub 2}·CaO·P{sub 2}O{sub 5} glasses were prepared via sol-gel dip coating. • Ca/P molar ratio affects the film morphology and biocompatibility. • Higher cell proliferation was found in response to higher Ca/P ratios coatings. • A growth cell proliferation inhibition was observed in response to lower Ca/P ratio.

  8. Ultrapure glass optical waveguide: Development in microgravity by the sol gel process

    Mukherjee, S. P.; Debsikdar, J. C.; Beam, T.


    The sol-gel process for the preparation of homogeneous gels in three binary oxide systems was investigated. The glass forming ability of certain compositions in the selected oxide systems (SiO-GeO2, GeO2-PbO, and SiO2-TiO2) were studied based on their potential importance in the design of optical waveguide at longer wavelengths.

  9. Production and characterization of spodumene dosimetric pellets prepared by a sol-gel route

    Lima, H. R. B. R.; Nascimento, D. S.; Bispo, G. F. C.; Teixeira, V. C.; Valério, M. E. G.; Souza, S. O.


    Spodumene is an aluminosilicate that has shown good results for high-dose TL dosimetry for beta or gamma rays. Due to its chemical composition (LiAlSi2O6) it has potential to be used as a neutron dosimeter. The synthetic spodumene is usually produced by solid state reaction and conventional sol-gel, whose shortcomings arise from the need to employ high temperatures and high cost reagents, respectively. Proteic sol-gel method is promising, because it can reduce production costs and the possibility of environmental contamination. This work reports the production of the spodumene by the proteic sol-gel method using edible unflavored gelatin as a precursor. The product is characterized physically and morphologically, and investigated its applicability as a TL dosimeter. Two sets of samples were prepared using different sources of silicon, one with TEOS (Si(OC3H5)4) and one with SILICA (SiO2). The materials produced were characterized by X-ray diffraction, differential thermal analysis and thermogravimetry in order to evaluate the structural properties, as well as possible changes in physical or chemical properties depending on the temperature. The production of spodumene was successful, with generation of the crystals in the β-phase with tetragonal structure. Sintered pellets produced from these crystals were irradiated with a 90Sr-90Y source and their TL glow curves were evaluated. Although the samples prepared by the proteic sol-gel method with TEOS presented a lower forming temperature, the samples produced with SILICA showed higher sensitivity to radiation.

  10. Sol-gel Transition of Methylcellulose Solution in the Coexistence of Hexadecyltrimethylammonium Bromide and Sodium Chloride

    Shah Zhou; Hai-yang Yang; Yong-jun Xie; Hua-zhen Li; Guang-ming Liu


    The sol-gel transition of methylcellulose (MC) solution in the presence of NaCl and hexadecyltrimethylammonium bromide (HTAB),together with MC/NaCl solution in the presence of HTAB and MC/HATB solution in the presence of NaCl,was investigated by the rheological measurements.It has been found that the sol-gel transition temperature of MC solution decreases linearly with the concentration of NaCl in solution but increases linearly with the concentration of HTAB in solution,respectively.However,the sol-gel transition temperature of MC/NaCl solution in the presence of HTAB keeps the same value,independent of the concentration of HTAB in solution.On the other hand,the sol-gel transition temperature of MC/HTAB solution decreases linearly with the concentration of NaCl in solution.The experimental results suggest that,for MC/NaCl solution in the presence of HTAB,the saltinduced spherical micelles of HTAB should have formed in bulk solution.For MC solution in the absence of NaCl,no spherical micelles have been formed in bulk solution,though the concentration of HTAB in our experiment is almost one order of magnitude higher than the critical micelle concentration of HTAB in polymer-free solution.In fact,due to adsorption of HTAB on MC chains,the realconcentration of HTAB in bulk solution,is much less than the apparent concentration of HTAB dissolved in MC solution.

  11. In situ ion-beam analysis and modification of sol-gel zirconia thin films

    Levine, T.E. [Cornell Univ., Ithaca, NY (United States). Dept. of Materials Science and Engineering; Yu, Ning; Kodali, P.; Walter, K.C.; Nastasi, M.; Tesmer, J.R.; Maggiore, C.J. [Los Alamos National Lab., NM (United States); Mayer, J.W. [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemical, Bio and Materials Science Engineering


    We report the investigation of ion-beam-induced densification of sol-gel zirconia thin films via in situ ion backscattering spectrometry. We have irradiated three regions of a sample with neon, argon, and krypton ions. For each ion species, a series of irradiation and analysis steps were performed using an interconnected 3 MV tandem accelerator. The technique offers the advantages of minimizing the variation of experimental parameters and sequentially monitoring the densification phenomenon with increasing ion dose.

  12. Microstructures of nanosized alumina powders synthesized by sol-gel method

    王晶; 张波


    The microstructures of nanosized alumina powders prepared by sol-gel routine were systematically studied with transmission electron microscopy and X-ray diffractometer. It was found that the morphologies of alumina gel powders change in the orders of caterpillar- thorn- granular-dumbbell shaped structures during calcining at temperatures from 20℃ to 800℃, 1200℃ and 1300℃. The caterpillar shaped structure composed of strings with a diameter of 5nm.

  13. Sol-Gel Synthesis of Ordered β-Cyclodextrin-Containing Silicas

    Trofymchuk, Iryna Mykolaivna; Roik, Nadiia; Belyakova, Lyudmila


    New approaches for β-cyclodextrin-containing silicas synthesis were demonstrated. Materials with hexagonally ordered mesoporous structure were prepared by postsynthesis grafting and by co-condensation methods. β-Cyclodextrin activated by a N,N′-carbonyldiimidazole was employed for postsynthesis treatment of 3-aminopropyl-modified MCM-41 support as well as for sol-gel synthesis with β-cyclodextrin-containing organosilane and tetraethyl orthosilicate participation in the presence of cetyltrimet...

  14. 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.

  15. 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...

  16. Sol-Gel Synthesis of Carbon Xerogel-ZnO Composite for Detection of Catechol


    Carbon xerogel-zinc oxide (CXZnO) composites were synthesized by a simple method of sol-gel condensation polymerization of formaldehyde and resorcinol solution containing zinc salt followed by drying and thermal treatment. ZnO nanoparticles were observed to be evenly dispersed on the surfaces of the carbon xerogel microspheres. The as-prepared CXZnO composites were mixed with laccase (Lac) and Nafion to obtain a mixture solution, which was further modified on an electrode surface to construct...



    Nanosized Zinc Oxide (ZnO) was synthesized using sol-gel method. The nanomaterials with structure were annealed at different temperatures ranging from 500 to 700°C which were chosen based on the Thermogravimetric (TGA) Analysis. The structure and morphology were characterized by Powder X-Ray Diffraction (PXRD) and Transmission Electron Microscope (TEM), respectively. The PXRD shows the increasing tendency in crystallite size when the annealing temperature increases and the hexagonal struc...



    Nanosized Zinc Oxide (ZnO) was synthesized using sol-gel method. The nanomaterials with structure were annealed at different temperatures ranging from 500 to 700°C which were chosen based on the Thermogravimetric (TGA) Analysis. The structure and morphology were characterized by Powder X-Ray Diffraction (PXRD) and Transmission Electron Microscope (TEM), respectively. The PXRD shows the increasing tendency in crystallite size when the annealing temperature increases and the hexagonal structure...

  19. Chemical sensing of copper phthalocyanine sol-gel glass through organic vapors

    Ridhi, R.; Gawri, Isha; Abbas, Saeed J.; Saini, G. S. S.; Tripathi, S. K. [Department of Physics, Center of Advanced Study in Physics, Panjab University, Chandigarh-160 014 (INDIA) Fax: +91-172-2783336; Tel.:+91-172-2544362 (India)


    The sensitivities of metallophthalocyanine to vapor phase electron donors has gained significance in many areas and disciplines due to their sensing properties and ease of operation. In the present study the interaction mechanism of organic vapors in Copper Phthalocyanine (CuPc) sol-gel glass has been studied. The interaction mechanism is affected by many factors like morphology, electrical or optical properties of film. CuPc sol-gel glass has been synthesized using chemical route sol-gel method. Its structural characterization was conducted using XRD and the amorphous nature of the silicate glass was observed with characteristic α polymorph phase of CuPc at around 6.64° with 13.30Å interplanar spacing. The size of the particle as determined using Debbye Scherre’s formula comes out around 15.5 nm. The presence of α phase of CuPc was confirmed using FTIR with the appearance of crystal parameter marker band at 787 cm-1. Apart from this A2u and Eu symmetry bands of CuPc have also been observed. The UV absorption spectrum of CuPc exhibits absorption peaks owing to π→ π* and n→ π* transitions. A blue shift in the prepared CuPc glass has been observed as compared to the dopant CuPc salt indicating increase of band gap. A split in B (Soret) band and Q band appears as observed with the help of Lorentzian fitting. CuPc sol gel glass has been exposed with chemical vapors of Methanol, Benzene and Bromine individually and the electrical measurements have been carried out. These measurements show the variation in conductivity and the interaction mechanism has been analyzed.

  20. Synthesis and Characterization of NASICON Nanoparticles by Sol-gel Method

    WANG Biao; LIANG Xi-shuang; LIU Feng-min; ZHONG Tie-gang; ZHAO Chun; LU Ge-yu; QUAN Bao-fu


    Na superionic conductor(NASICON) nanoparticles were synthesized by a modified sol-gel method and sintered at a temperature range of 800-1000 ℃. The performance of the samples was characterized by the analysis methods of X-ray diffraction(XRD), Fourier transform infrared spectroscopy(FTIR), and transmission electron microscopy(TEM) as well as conductivity measurement. Compared with those sintered at other temperatures, the NASICON material sintered at 900 ℃ had the best crystalline structure and higher conductivity.

  1. Photochromic properties of a silylated spirooxazine in sol-gel coatings

    Hou, Lisong; Schmidt, Helmut K.


    For the first time a silylated spirooxazine was introduced into organically modified ceramics (Ormocer) coatings by the sol-gel method and its photochromic properties are studied and compared with the free (non-silylated) spirooxazine. The results reveal that the silylation has little influence on the spectroscopic properties and the photochromic intensity of the silylated dye in Ormocer coatings is at the same level as that of the free dye, though the decolouration rate of the dye is reduced...

  2. An Experimental Exploration on the Characterization of TiO2 Using Sol-Gel

    Suman Malik


    Full Text Available TiO2 is defined as the photo catalyst and the poor adsorption so that the improvement of TiO2 decomposition is performed for the purification of the organic pollutants in water and air. In this paper, the TiO2 is defined and explored under the structure analysis. It also includes the deposition optimization using sol-gel approach. The works also include the relative experimentation for the purification process.:

  3. Sol-gel coatings as active barriers to protect ceramic reinforcement in aluminum matrix composites

    Rams, J.; Urena, A.; Campo, M. [Departamento de Tecnologia Quimica, Ambiental y de los Materiales, ESCET, Universidad Rey Juan Carlos C/ Tulipan s/nMostoles 28933 Madrid (Spain)


    Silica obtained through a sol-gel process is used as a coating for ceramic reinforcements (SiC) in aluminium matrix composite materials. The interaction between molten aluminium and the coated particles during material casting can be controlled by means of the thermal treatment given to the coating. Wettability is increased because the coating reacts with molten aluminium, and the formation of the degrading aluminium carbide is inhibited. (Abstract Copyright [2004], Wiley Periodicals, Inc.)

  4. AFM and XPS Study of Glass Surface Coated with Titania Nanofilms by Sol-Gel Method

    JI Guo-Jun; SHI Zhi-Ming


    @@ Ce3+-doped and undoped TiO2 nanofilms are prepared on glass surface using a sol-gel method.Crystal structure,surface morphology,chemical composition and element distribution of both glass substrates and TiO2 films were characterized by x-ray diffractometer(XRD),atomic force microscopy(AFM)and x-ray photoelectron spectroscopy(XPS).

  5. Free-standing coating patterns fabricated by ultraviolet contact lithography using photosensitive sol-gel coatings

    Xiang, Youlai; Du, Ai; Li, Xiaoguang; Sun, Wei; Wu, Shuai; Li, Tiemin; Liu, Mingfang; Zhou, Bin


    Photosensitive ZrO2-SiO2 hybrid sol-gel coatings containing large contents of chelating rings were prepared by using the zirconium n-butoxide (TBOZ) and methyltriethoxysilane (MTES) as hybrid precursors, and benzoylacetone (BZAC) as chelating agent. The change of ultraviolet (UV) absorption spectra, chemical composition, and optical properties of ZrO2-SiO2 hybrid sol-gel coatings were analyzed before and after UV exposure and calcination. The refractive index of the ZrO2-SiO2 hybrid gel coatings decreased from 1.673 to 1.561 with the increase of the molar content of MTES in precursors. The sol-gel coating patterns with the periods of 20.24 μm, 10.11 μm and 3.99 μm on the PAMS substrates were firstly obtained by using the photosensitive ZrO2-SiO2 hybrid sol-gel films as fundamental materials through a process of UV contact lithography with photo masks and etching with ethanol. Finally, the free-standing gel coating patterns supported by copper grids, with the period of 12.70 μm and line width of 4.93 μm, and the period of 14.20 μm and line width of 3.82 μm, were obtained by removing the PAMS thermal degradation sacrifice layer after being calcined at 330 °C. Micrometer-periodic free-standing gel coating patterns with different structure have potential applications in the laser physical experiments.

  6. A Novel Approach for Entrapment of Biopolymers in Silica Matrix by Sol-gel Technique



    1 Results The entrapment of biopolymers into silica by the sol-gel technique meets with incompatibility of inorganic and bioorganic components. The aim was to develop a compatible procedure biomimicking the biomineralization processes in the living nature. A suggested solution in Ref.[1-2] for the biopolymer entrapment into silica matrix is based on a novel silica precursor. The developed approach is distinguished from the common technique for fabrication of hybrid biopolymer-silica nanocomposite materi...

  7. Sol-gel synthesis of 45S5 bioglass – Prosthetic coating by electrophoretic deposition

    Faure Joel


    Full Text Available In this work, the 45S5 bioactive glass has been prepared by the sol-gel process using an organic acid catalyst instead of nitric acid usually used. The physico-chemical and structural characterizations confirmed and validated the elemental composition of the resulting glass. In addition, the 45S5 bioactive glass powder thus obtained was successfully used to elaborate by electrophoretic deposition a prosthetic coating on titanium alloy Ti6Al4V.

  8. Tailoring the oxidation state of cobalt through halide functionality in sol-gel silica

    Gianni Olguin; Christelle Yacou; Simon Smart; Diniz da Costa, João C.


    The functionality or oxidation state of cobalt within a silica matrix can be tailored through the use of cationic surfactants and their halide counter ions during the sol-gel synthesis. Simply by adding surfactant we could significantly increase the amount of cobalt existing as Co3O4 within the silica from 44% to 77%, without varying the cobalt precursor concentration. However, once the surfactant to cobalt ratio exceeded 1, further addition resulted in an inhibitory mechanism whereby the alt...

  9. 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.

  10. All-silica nanofluidic devices for DNA-analysis fabricated by imprint of sol-gel silica with silicon stamp

    Mikkelsen, Morten Bo Lindholm; Letailleur, Alban A; Søndergård, Elin


    We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination of the imprin......We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination...... of the imprinted hybrid sol-gel material produces purely inorganic silica, which has very low autofluorescence and can be fusion bonded to a glass lid. Compared to top-down processing of fused silica or silicon substrates, imprint of sol-gel silica enables fabrication of high-quality nanofluidic devices without...

  11. Modified thermoresponsive Poloxamer 407 and chitosan sol-gels as potential sustained-release vaccine delivery systems

    Kojarunchitt, Thunjiradasiree; Baldursdottir, Stefania; Dong, Yao-Da


    Thermoresponsive, particle-loaded, Poloxamer 407 (P407)-Pluronic-R® (25R4) or chitosan-methyl cellulose (MC) formulations were developed as single-dose, sustained release vaccines. The sol-gels, loaded either with a particulate vaccine (cubosomes) or soluble antigen (ovalbumin) and adjuvants (Quil...... the chitosan-MC sol-gels sustained the release of antigen up to at least 14 days after administration. The chitosan-MC sol-gels stimulated both cellular and humoral responses. The inclusion of cubosomes in the sol-gels did not provide a definitive beneficial effect. Further analysis of the formulations...... with small-angle X-ray scattering (SAXS) revealed that while cubosomes were stable in chitosan-MC gels they were not stable in P407-25R4 formulations. The reason for the mixed response to cubosome-loaded vehicles requires more investigation, however it appears that the cubosomes did not facilitate...

  12. Thermodynamic analysis of sol-gel transition of gelatin in terms of water activity in various solutions.

    Miyawaki, Osato; Omote, Chiaki; Matsuhira, Keiko


    Sol-gel transition of gelatin was analyzed as a multisite stoichiometric reaction of a gelatin molecule with water and solute molecules. The equilibrium sol-gel transition temperature, Tt , was estimated from the average of gelation and melting temperature measured by differential scanning calorimetry. From Tt and the melting enthalpy, ΔHsol , the equilibrium sol-to-gel ratio was estimated by the van't Hoff equation. The reciprocal form of the Wyman-Tanford equation, which describes the sol-to-gel ratio as a function of water activity, was successfully applied to obtain a good linear relationship. From this analysis, the role of water activity on the sol-gel transition of gelatin was clearly explained and the contributions of hydration and solute binding to gelatin molecules were separately discussed in sol-gel transition. The general solution for the free energy for gel-stabilization in various solutions was obtained as a simple function of solute concentration.

  13. Brilliant molecular nanocrystals emerging from sol-gel thin films: towards a new generation of fluorescent biochips

    Dubuisson, E; Monnier, V; Sanz-Menez, N; Ibanez, A [Institut Neel, CNRS and Universite Joseph Fourier, UPR 2940, BP166, F-38042 Grenoble Cedex 9 (France); Boury, B [Universite Montpellier 2, Departement de Chimie, Institut Charles Gerhardt, UMR 5253 CNRS, cc 1701, Place E Bataillon, F-34095 Montpellier Cedex 5 (France); Usson, Y [TIMC-IMAG, UMR 5525 CNRS, Universite Joseph Fourier, Domaine de la Merci, F-38706 La Tronche Cedex (France); Pansu, R B, E-mail: alain.ibanez@grenoble.cnrs.f [Laboratoire de Photophysique et de Photochimie Supramoleculaire et Macromoleculaire, CNRS, UMR 8531, ENS Cachan, F-94235 Cachan Cedex (France)


    To develop highly sensitive biosensors, we made directly available to biological aqueous solutions organic nanocrystals previously grown in the pores of sol-gel films. Through the controlled dissolution of the sol-gel surface, we obtained emerging nanocrystals that remained strongly anchored to the sol-gel coating for good mechanical stability of the final sensing device. We demonstrated that in the presence of a solution of DNA functionalized with a molecular probe, the nanocrystal fluorescence is strongly quenched by Foerster resonance energy transfer thus opening the way towards very sensitive fluorescent biosensors through biomolecules grafted onto fluorescent nanocrystals. Finally, this controlled dissolution, involving weak concentrated NaOH solution, is a generic process that can be used for the thinning of any kind of sol-gel layer.

  14. Lithium Ferrite as the Cathode of the Electrochemical Power Sources: the Perspectives of Sol-gel Synthesis Method

    O.M. Uhorchuk


    Full Text Available Synthesis of highly dispersed systems of lithium-ferrite oxide spinel, obtained by the low-temperature sol-gel method, with the subsequent auto combustion and the comparison of these systems’ characteristics with the analogous ones of the conventional ceramic method are performed. It is shown that the systems synthesized by solid-phase and sol-gel methods are the single phase structures with the space group P4332. The sol-gel method of auto combustion made it possible to increase the size of crystallites in more than 4 times and the specific area of the surface in 20 times. Obtained by sol-gel method lithium pentaferrit is suggested to be used as the cathode of lithium power sources.

  15. Nanoscale morphology for high hydrophobicity of a hard sol gel thin film

    Wu, Y. L.; Chen, Z.; Zeng, X. T.


    It is challenging to obtain a hydrophobic smooth coating with high optical and mechanical properties at the same time because the hydrophobic additives are soft in nature resulting in reduced hardness and durability. This paper reports a durable hydrophobic transparent coating on glass fabricated by sol-gel technology and a low volume medium pressure (LVMP) spray process. The sol-gel formula consists of a pre-linked hydrophobic nano-cluster from hydroxyl-terminated polydimethylsiloxane, titanium tetraisopropoxide and a silica-based sol-gel matrix with silica hard fillers. Polydimethylsiloxane (PDMS) is uniformly distributed throughout the coating layer providing durable hydrophobic property. Mechanical properties are achieved by the hard matrix and hard fillers with the nano-structures. Due to the surface nano-morphology, a high degree of hydrophobicity was maintained with only 10 vol.% PDMS, while the hardness and abrasion resistance of the coatings were not significantly compromised. Chemical analyses by FTIR confirmed the uniform distribution of the PDMS and surface morphology analyses by atomic force microscopy (AFM) displayed the nano-surface structures that enhanced the hydrophobicity. The special surface nanostructures can be quantified using surface Kurtosis and ratio between asperity peak height to distance between peaks. The LVMP process influences the spray droplet size resulting in different surface structures.

  16. Preparation and Characterization of Nanosized LiCoO2 by Sol-Gel Process

    ZHOU; YingKe


    In the intense search for high-energy density cathode materials for use in lithium-ion rechargeable battery technology, LiCoO2 has become the first, and one of the most promising, for commercial applications1. Sol-gel chemistry has recently evolved as a powerful approach for preparing inorganic materials such as glasses and ceramics2. The improved sol-gel process is based on the ability of certain weak acids to form polybasic acid chelates with various cations. These chelates can undergo polyesterification when heated in a polyhydroxyl alcohol to form a solid polymeric resin through which the cations are uniformly distributed. Thus the resin retains homogeneity on the atomic scale and may be calcined at low temperature to yield fine particulate oxides. Using this method, it is possible to obtain phase-pure ultrafine crystalline nanophases after firing the ploymeric precursors at some appointed temperature for several hours. In this work we reported that nanosized LiCoO2 were prepared by the improved sol-gel process.  ……

  17. High quality factor Er-doped Fabry-Perot microcavities by sol-gel processing

    Li Yigang; Fortes, Luis M; Almeida, Rui M [Departamento de Engenharia de Materiais/ICEMS, Instituto Superior Tecnico/TULisbon, Av. Rovisco Pais, 1049-001 Lisboa (Portugal); Chiappini, Andrea; Ferrari, Maurizio, E-mail:, E-mail: rui.almeida@ist.utl.p [CNR-IFN, Istituto di Fotonica e Nanotecnologie, CSMFO Lab., Via alla Cascata 56/C, Povo, 38123 Trento (Italy)


    An optimized sol-gel process was developed to fabricate 1D photonic bandgap structures. Several erbium-doped Fabry-Perot microcavities were prepared and characterized. The thickest sample contained two Bragg mirrors, each having 12 distributed Bragg reflector periods of alternating silicate glass and titania layers. The total thickness of this sample reached {approx}12 {mu}m. The Er{sup 3+} photoluminescence spectra at 1.5 {mu}m were measured for the microcavities. A quality factor of 250 and an Er{sup 3+} photoluminescence enhancement of 96 times at 1.5 {mu}m have been reached. The sol-gel processing details, the crystallization of the titania films and the refractive index of the deposited materials are discussed in detail. The simulated optical spectra of the microcavities were found to agree well with the actually measured curves. These results demonstrate that the present sol-gel processing technique is of potential interest for low cost fabrication of 1D photonic bandgap devices.

  18. Disinfection studies on TiO2 thin films prepared by a sol-gel method.

    Kambala, Venkata Subba Rao; Naidu, Ravi


    Transparent anatase TiO2 nanometer thin films were prepared by dip-coating on soda-lime glass plates via the sol-gel method. The un-calcined and the calcined films were characterized by X-ray diffraction (XRD), AFM, Nano-indentation (hardness and Young's modulus), UV-vis spectrometry, thickness and hydrophilicity (contact angle measurements). The photocatalytic activity of the thin films was evaluated by performing disinfection studies on the Gram-negative microorganisms like Escherichia coli, and Staphylococcus Aureus, a Gram-positive organism. The photocatalytic activity for both groups of organisms was studied in saline and nutrient broth. The leakage of potassium from the bacteria was observed parallel to cell viability. The activity of the sol-gel prepared TiO2 thin films were compared under UV lamps and natural day light (ND) lamps with Degussa P-25 TiO2 thin films prepared on soda-lime glass using a polymer support and the commercial self-cleaning glass (SC). The sol-gel prepared thin films which were annealed at 450 degrees C, show highest photocatalytic activity, the slowest conversion rate from hydrophilic to a hydrophobic state, light-induced hydrophilicity, and also higher disinfection activities compared to P-25 films and commercial self-cleaning glass. The films also show excellent activities when continuously reused for more than a month.

  19. Sol gel TiO2 antireflection coatings for silicon solar cells

    L.A. Dobrzański


    Full Text Available Purpose: The aim of this paper was to investigate changes in surface morphology and optical reflection of thin films of titanium dioxide. Thin films were prepared using sol gel spin coating method.Design/methodology/approach: The microanalysis have been investigated by the Energy-dispersive X-ray spectroscopy EDS. The changes in surface topography was observed by the atomic force microscope AFM and scanning electron microscope SEM. The results of roughness have been prepared in the software XEI Park Systems and optical reflection by the spectrometer UV/VIS.Findings: Results and their analysis allow to conclude that the titanium isopropoxide concentration in solution and spin speed, which is an important factor in spin coating technology has a significant influence on surface morphology and optical reflection of thin films titanium dioxide.Practical implications: Known sol gel titanium dioxide optical parameters and the possibility of obtaining a uniform thin films show that it can be good material for photovoltaic application.Originality/value: The paper presents some researches of titanium dioxide thin films deposited by sol gel spin coating method on monocrystalline silicon.

  20. Preparation and Characterization of Nanosized LiCoO2 by Sol-Gel Process


    @@ In the intense search for high-energy density cathode materials for use in lithium-ion rechargeable battery technology, LiCoO2 has become the first, and one of the most promising, for commercial applications1. Sol-gel chemistry has recently evolved as a powerful approach for preparing inorganic materials such as glasses and ceramics2. The improved sol-gel process is based on the ability of certain weak acids to form polybasic acid chelates with various cations. These chelates can undergo polyesterification when heated in a polyhydroxyl alcohol to form a solid polymeric resin through which the cations are uniformly distributed. Thus the resin retains homogeneity on the atomic scale and may be calcined at low temperature to yield fine particulate oxides. Using this method, it is possible to obtain phase-pure ultrafine crystalline nanophases after firing the ploymeric precursors at some appointed temperature for several hours. In this work we reported that nanosized LiCoO2 were prepared by the improved sol-gel process.

  1. Relative brookite and anatase content in sol-gel-synthesized titanium dioxide nanoparticles.

    Isley, Sara L; Penn, R Lee


    Sol-gel synthesis of titania typically produces a mixture of brookite and anatase. Rietveld refinements were used to systematically track the brookite content and particle size as functions of synthetic variables. Results demonstrate that brookite content and anatase particle size decrease with decreasing Ti/H(2)O ratios. In syntheses at pH 3, the addition of HCl resulted in increased amorphous content compared to samples synthesized using HNO(3). Similar amorphous contents were observed for particles prepared at pH 6-9. Hydrothermal aging for 4 h at 200 degrees C of sol-gel products containing substantial amorphous titania resulted in higher brookite content than did hydrothermal aging of sol-gel products containing little to no amorphous titania. Finally, dialysis prior to hydrothermal aging appeared to inhibit phase transformation from brookite to anatase in aged materials. Results presented demonstrate that considerable control over the relative anatase and brookite contents can be achieved through control of synthetic variables.

  2. Surface modification of quartz fibres for dental composites through a sol-gel process.

    Wang, Yazi; Wang, Renlin; Habib, Eric; Wang, Ruili; Zhang, Qinghong; Sun, Bin; Zhu, Meifang


    In this study, quartz fibres (QFs) surface modification using a sol-gel method was proposed and dental posts reinforced with modified QFs were produced. A silica sol (SS) was prepared using tetraethoxysilane (TEOS) and 3-methacryloxypropyltrimethoxysilane (γ-MPS) as precursors. The amount of γ-MPS in the sol-gel system was varied from 0 to 24wt.% with a constant molar ratio of TEOS, ethanol, deionized water, and HCl. Thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), and contact angle (CA) measurements were used to characterize the modified QFs, which confirmed that SS had successfully coated the surface of QFs. SEM images showed good interfacial bonding between the modified QFs and the resin matrix. The results of three-point bending tests of the fibre reinforced composite (FRC) posts showed that the QFs modified by SS with 12wt.% γ-MPS presented the best mechanical properties, demonstrating improvements of 108.3% and 89.6% for the flexural strength and flexural modulus, respectively, compared with untreated QFs. Furthermore, the sorption and solubility of the prepared dental posts were also studied by immersing the posts in artificial saliva (AS) for 4weeks, and yielded favourable results. This sol-gel surface modification method promises to resolve interfacial bonding issues of fibres with the resin matrix, and produce FRC posts with excellent properties.

  3. Biological influence of Ca/P ratio on calcium phosphate coatings by sol-gel processing.

    Catauro, M; Papale, F; Sapio, L; Naviglio, S


    The objective of this work has been to develop low temperature sol-gel glass coatings to modify the substrate surface and to evaluate their bioactivity and biocompatibility. Glasses, based on SiO2·CaO·P2O5, were synthesized by the sol-gel technique using tetraethyl orthosilicate, calcium nitrate tetrahydrate and triethyl phosphate as precursors of SiO2, CaO and P2O5, respectively. Those materials, still in the sol phase, have been used to coat substrates by means of the dip-coating technique. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) has been used for characterize coatings and a microstructural analysis has been obtained using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated substrate was immersed in simulated body fluid (SBF) for 21days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. In order to study the cell behavior and response to our silica based materials, prepared via the sol-gel method, with various Ca/P ratio and coating substrate, we have used the human osteoblast-like U2OS cell line.

  4. Sol-Gel Material-Enabled Electro-Optic Polymer Modulators.

    Himmelhuber, Roland; Norwood, Robert A; Enami, Yasufumi; Peyghambarian, Nasser


    Sol-gels are an important material class, as they provide easy modification of material properties, good processability and are easy to synthesize. In general, an electro-optic (EO) modulator transforms an electrical signal into an optical signal. The incoming electrical signal is most commonly information encoded in a voltage change. This voltage change is then transformed into either a phase change or an intensity change in the light signal. The less voltage needed to drive the modulator and the lower the optical loss, the higher the link gain and, therefore, the better the performance of the modulator. In this review, we will show how sol-gels can be used to enhance the performance of electro-optic modulators by allowing for designs with low optical loss, increased poling efficiency and manipulation of the electric field used for driving the modulator. The optical loss is influenced by the propagation loss in the device, as well as the losses occurring during fiber coupling in and out of the device. In both cases, the use of sol-gel materials can be beneficial due to the wide range of available refractive indices and low optical attenuation. The influence of material properties and synthesis conditions on the device performance will be discussed.

  5. Improvement in Tensile Strength of Bamboo Knitted Fabric by Sol-Gel Coating

    Awais Khatri


    Full Text Available Textiles made of bamboo regenerated fibre are reported to have lower tensile strength than the other cellulosic fibres, due to high porosity of the fibre. This paper was aimed to modify the bamboo knitted fabric by the sol-gel coating to improve the tensile strength with minimum effect on its inherent morphology and ultimate relevant properties such as good absorbency and air permeability. The paddry- bake process was employed for the coating where tetraethyl-orthosilicate and nano-titanium-dioxide were used as the active ingredients. The treated fabrics were tested for the tensile behaviour in terms of breaking strength and elongation and the sol-gel process recipe and parameters were optimised. The absorbency, air-permeability and washing durability of the coating were also tested for the optimised process. Results showed the increase in tensile strength of the fabric by sol-gel coating, whereas absorbency and air-permeability were almost unaffected. The coating results were unaffected even after a washing treatment (equivalent to 5 industrial washings. Additionally, the wrinkle recovery angle of the coated fabric was also tested and found improved.

  6. Sol-Gel Material-Enabled Electro-Optic Polymer Modulators

    Roland Himmelhuber


    Full Text Available Sol-gels are an important material class, as they provide easy modification of material properties, good processability and are easy to synthesize. In general, an electro-optic (EO modulator transforms an electrical signal into an optical signal. The incoming electrical signal is most commonly information encoded in a voltage change. This voltage change is then transformed into either a phase change or an intensity change in the light signal. The less voltage needed to drive the modulator and the lower the optical loss, the higher the link gain and, therefore, the better the performance of the modulator. In this review, we will show how sol-gels can be used to enhance the performance of electro-optic modulators by allowing for designs with low optical loss, increased poling efficiency and manipulation of the electric field used for driving the modulator. The optical loss is influenced by the propagation loss in the device, as well as the losses occurring during fiber coupling in and out of the device. In both cases, the use of sol-gel materials can be beneficial due to the wide range of available refractive indices and low optical attenuation. The influence of material properties and synthesis conditions on the device performance will be discussed.

  7. Hybrid titanium dioxide/PS-b-PEO block copolymer nanocomposites based on sol-gel synthesis

    Gutierrez, J; Tercjak, A; Garcia, I; Peponi, L; Mondragon, I [' Materials-Technologies' Group, Departamento Ingenieria Quimica y Medio Ambiente, Escuela Politecnica, Universidad PaIs Vasco/Euskal Herriko Unibertsitatea, Plaza Europa 1, E-20018 Donostia-San Sebastian (Spain)], E-mail:


    The poly(styrene)-b-poly(ethylene oxide) (SEO) amphiphilic block copolymer, with two different molecular weights, has been used as a structure directing agent for generating nanocomposites of TiO{sub 2}/SEO via the sol-gel process. SEO amphiphilic block copolymers are designed with a hydrophilic PEO-block which can interact with inorganic molecules, as well as a hydrophobic PS-block which builds the matrix. The addition of different amounts of sol-gel provokes strong variations in the self-assembled morphology of TiO{sub 2}/SEO nanocomposites with respect to the neat block copolymer. As confirmed by atomic force microscopy (AFM), TiO{sub 2}/PEO-block micelles get closer, forming well-ordered spherical domains, in which TiO{sub 2} nanoparticles constitute the core surrounded by a corona of PEO-blocks. Moreover, for 20 vol% sol-gel the generated morphology changes to a hexagonally ordered structure for both block copolymers. The cylindrical structure of these nanocomposites has been confirmed by the two-dimensional Fourier transform power spectrum of the corresponding AFM height images. Affinity between titanium dioxide precursor and PEO-block of SEO allows us to generate hybrid inorganic/organic nanocomposites, which retain the optical properties of TiO{sub 2}, as evaluated by UV-vis spectroscopy.

  8. Synthesis of polymeric fluorinated sol-gel precursor for fabrication of superhydrophobic coating

    Li, Qianqian; Yan, Yuheng; Yu, Miao; Song, Botao; Shi, Suqing; Gong, Yongkuan


    A fluorinated polymeric sol-gel precursor (PFT) is synthesized by copolymerization of 2,3,4,5,5,5-hexafluoro-2,4-bis(trifluorinated methyl)pentyl methacrylate (FMA) and 3-methacryloxypropyltrimethoxysilane (TSMA) to replace the expensive long chain fluorinated alkylsilanes. The fluorinated silica sol is prepared by introducing PFT as co-precursor of tetraethyl orthosilicate (TEOS) in the sol-gel process with ammonium hydroxide as catalyst, which is then used to fabricate superhydrophobic coating on glass substrate through a simple dip-coating method. The effects of PFT concentrations on the chemical structure of the formed fluorinated silica, the surface chemical composition, surface morphology, wetting and self-cleaning properties of the resultant fluorinated silica coatings were studied by using X-ray powder diffraction (XRD), Fourier transform infrared spectrometer (FTIR), X-ray photoelectron spectrophotometer (XPS), scanning electron microscopy (SEM) and water contact angle measurements (WCA). The results show that the fluorinated silica sols are successfully obtained. The size and size distribution of the fluorinated silica particles are found greatly dependent on the concentration of PFT, which play a crucial role in the surface morphology of the corresponding fluorinated silica coatings. The suitable PFT concentration added in the sol-gel stage, i.e. for F-sol-1 and F-sol-2, is helpful to achieve both the low surface energy and multi-scaled microstructures, leading to the formation of the superhydrophobic coatings with bio-mimicking self-cleaning property similar to lotus leaves.

  9. The effect of silica-coating by sol-gel process on resin-zirconia bonding.

    Lung, Christie Ying Kei; Kukk, Edwin; Matinlinna, Jukka Pekka


    The effect of silica-coating by sol-gel process on the bond strength of resin composite to zirconia was evaluated and compared against the sandblasting method. Four groups of zirconia samples were silica-coated by sol-gel process under varied reagent ratios of ethanol, water, ammonia and tetraethyl orthosilicate and for different deposition times. One control group of zirconia samples were treated with sandblasting. Within each of these five groups, one subgroup of samples was kept in dry storage while another subgroup was aged by thermocycling for 6,000 times. Besides shear bond testing, the surface topography and surface elemental composition of silica-coated zirconia samples were also examined using scanning electron microscopy and X-ray photoelectron spectroscopy. Comparison of silica coating methods revealed significant differences in bond strength among the Dry groups (psol-gel deposition times also revealed significant differences in bond strength among the Dry groups (pcoating of zirconia by sol-gel process resulted in weaker resin bonding than by sandblasting.

  10. 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).

  11. Structural study of metastable tetragonal YSZ powders produced via a sol-gel route

    Viazzi, Celine [CIRIMAT, Paul Sabatier University, 118 Rte de Narbonne, 31 062 Toulouse Cedex 09 (France)], E-mail:; Bonino, Jean-Pierre; Ansart, Florence; Barnabe, Antoine [CIRIMAT, Paul Sabatier University, 118 Rte de Narbonne, 31 062 Toulouse Cedex 09 (France)


    Sol-gel yttria stabilized zirconia (YSZ) is investigated in this paper. The final aim is to process YSZ powders into stable slurries in order to prepare thick coatings for thermal barrier to be applied on hot turboengine components. In fact, this system is well-known for its excellent thermomechanical resistance at elevated temperatures but the relationship between these performances and the structural and microstructural characteristics of these materials is not fully understood. This paper reports a preliminary study concerning recent progress on the structural properties control of YSZ powders synthesized by sol-gel process and the main advantages of this process compared to conventional methods. As a first step towards this understanding, structural investigations of ZrO{sub 2} doped with various xmol%YO{sub 1.5} coatings, have been performed using X-ray diffraction, structural Rietveld refinement, Raman spectra analysis and transmission electron microscopy. The evolution of the crystallographic structure of YSZ powders after air annealing at various temperatures 1100 deg. C, 1200 deg. Cand 1400 deg. C was studied to well understand the conditions of the formation of desired metastable tetragonal phase (t'). Then, this work should allow to correlate chemical and thermomechanical parameters as YSZ formulation and sol-gel elaboration conditions, temperature and t' phase performances.

  12. Quasi-one-dimensional nanostructured cobalt (Co) intercalated vanadium oxide (V{sub 2}O{sub 5}): Peroxovanadate sol gel synthesis and structural study

    Langie da Silva, Douglas, E-mail: [Departamento de Física, Universidade Federal de Pelotas, Caixa Postal 354, Pelotas 96010-900 (Brazil); Moreira, Eduardo Ceretta [Laboratório de Espectroscopia, Universidade Federal do Pampa, Campus Bagé, Bagé 96400-970 (Brazil); Dias, Fábio Teixeira; Neves Vieira, Valdemar das [Departamento de Física, Universidade Federal de Pelotas, Caixa Postal 354, Pelotas 96010-900 (Brazil); Brandt, Iuri Stefani; Cas Viegas, Alexandre da; Pasa, André Avelino [Laboratório de Filmes Finos e Superfícies, Universidade Federal de Santa Catarina, Caixa Postal 476, Florianópolis 88.040-900 (Brazil)


    Nanostructured cobalt vanadium oxide (V{sub 2}O{sub 5}) xerogels spread onto crystalline Si substrates were synthesized via peroxovanadate sol gel route. The resulting products were characterized by distinct experimental techniques. The surface morphology and the nanostructure of xerogels correlate with Co concentration. The decrease of the structural coherence length is followed by the formation of a loose network of nanopores when the concentration of intercalated species was greater than 4 at% of Co. The efficiency of the synthesis route also drops with the increase of Co concentration. The interaction between the Co(OH{sub 2}){sub 6}{sup 2+} cations and the (H{sub 2}V{sub 10}O{sub 28}){sup 4−} anions during the synthesis was suggested as a possible explanation for the incomplete condensation of the V{sub 2}O{sub 5} gel. Finally the experimental results points for the intercalation of Co between the bilayers of the V{sub 2}O{sub 5}. In this scenario two possible preferential occupation sites for the metallic atoms in the framework of the xerogel were proposed. - Graphical abstract: Quasi-one-dimensional nanostructured cobalt (Co) intercalated vanadium oxide (V{sub 2}O{sub 5}) nanoribbons synthesized by peroxovanadate sol gel route. - Highlights: • Nanostructured cobalt V{sub 2}O{sub 5} gel spread onto c{sub S}i were synthesized via peroxovanadate sol gel route. • The micro and nanostructure correlates with the cobalt content. • The efficiency of the synthesis route shows to be also dependent of Co content. • The experimental results points for the intercalation of Co between the bilayers of the V{sub 2}O{sub 5} xerogel.

  13. Matrix molecularly imprinted mesoporous sol-gel sorbent for efficient solid-phase extraction of chloramphenicol from milk.

    Samanidou, Victoria; Kehagia, Maria; Kabir, Abuzar; Furton, Kenneth G


    Highly selective and efficient chloramphenicol imprinted sol-gel silica based inorganic polymeric sorbent (sol-gel MIP) was synthesized via matrix imprinting approach for the extraction of chloramphenicol in milk. Chloramphenicol was used as the template molecule, 3-aminopropyltriethoxysilane (3-APTES) and triethoxyphenylsilane (TEPS) as the functional precursors, tetramethyl orthosilicate (TMOS) as the cross-linker, isopropanol as the solvent/porogen, and HCl as the sol-gel catalyst. Non-imprinted sol-gel polymer (sol-gel NIP) was synthesized under identical conditions in absence of template molecules for comparison purpose. Both synthesized materials were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and nitrogen adsorption porosimetry, which unambiguously confirmed their significant structural and morphological differences. The synthesized MIP and NIP materials were evaluated as sorbents for molecularly imprinted solid phase extraction (MISPE) of chloramphenicol in milk. The effect of critical extraction parameters (flow rate, elution solvent, sample and eluent volume, selectivity coefficient, retention capacity) was studied in terms of retention and desorption of chloramphenicol. Competition and cross reactivity tests have proved that sol-gel MIP sorbent possesses significantly higher specific retention and enrichment capacity for chloramphenicol compared to its non-imprinted analogue. The maximum imprinting factor (IF) was found as 9.7, whereas the highest adsorption capacity of chloramphenicol by sol-gel MIP was 23 mg/g. The sol-gel MIP was found to be adequately selective towards chloramphenicol to provide the necessary minimum required performance limit (MRPL) of 0.3 μg/kg set forth by European Commission after analysis by LC-MS even without requiring time consuming solvent evaporation and sample reconstitution step, often considered as an integral part in solid phase extraction work-flow. Intra and

  14. 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.

  15. Sol-Gel Entrapped Levonorgestrel Antibodies: Activity and Structural Changes as a Function of Different Polymer Formats

    Moran Shalev


    Full Text Available The paper describes development of a sol-gel based immunoaffinity method for the steroid hormone levonorgestrel (LNG and the effects of changes in the sol-gel matrix format on the activity of the entrapped antibodies (Abs and on matrix structure. The best sol-gel format for Ab entrapment was found to be a tetramethoxysilane (TMOS based matrix at a TMOS:water ratio of 1:8, containing 10% polyethylene glycol (PEG of MW 0.4 kDa. Addition of higher percentages of PEG or a higher MW PEG did not improve activity. No activity was obtained with a TMOS:water ratio of 1:12, most likely because of the very dense polymer that resulted from these polymerization conditions. Only minor differences in the non-specific binding were obtained with the various formats. TMOS was found to be more effective than tetrakis (2-hydroxyethylorthosilicate (THEOS for entrapment of anti-levonorgestrel (LNG Abs. However, aging the THEOS-based sol-gel for a few weeks at 4 °C stabilized the entrapped Abs and increased its binding capacity. Confocal fluorescent microscopy with fluorescein isothiocyanate (FITC labeled immunoglobulines (IgGs entrapped in the sol-gel matrix showed that the entrapped Abs were distributed homogenously within the gel. Scanning electron microscopy (SEM images have shown the diverse structures of the various sol-gel formats and precursors.

  16. 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.

  17. Hydrogen Gas Sensing Based on SnO2 Nanostructure Prepared by Sol-Gel Spin Coating Method

    Kadhim, Imad H.; Abu Hassan, H.


    A novel H2 gas sensor based on a SnO2 nanostructure was operated at room temperature (RT) (25°C). The SnO2 nanostructure was grown on Al2O3 substrates by a sol-gel spin coating method. The structural characteristics, surface morphology, and gas sensing properties of the SnO2 nanostructure were investigated. Thin film annealing at 500°C produced a high-quality SnO2 nanostructure with a crystallite size of 33.98 nm. A metal-semiconductor-metal gas sensor was fabricated using the SnO2 nanostructure and palladium metal. The gas sensor exhibited a sensitivity of 2570% to 1000 ppm H2 gas at RT. The sensing measurements for H2 gas at different temperatures (RT to 125°C) were repeatable for 50 min. Sensor sensitivity was tested under different H2 concentrations (150 ppm, 250 ppm, 375 ppm, 500 ppm, and 1000 ppm) at different operating temperatures. Adding glycerin to the sol solution increased the porosity of the SnO2 nanostructure surface, which increased the adsorption/desorption of gas molecules which leads to the high sensitivity of the sensor. Therefore, this H2 gas sensor is a suitable portable RT gas sensor.

  18. Hydrogen Gas Sensing Based on SnO2 Nanostructure Prepared by Sol-Gel Spin Coating Method

    Kadhim, Imad H.; Abu Hassan, H.


    A novel H2 gas sensor based on a SnO2 nanostructure was operated at room temperature (RT) (25°C). The SnO2 nanostructure was grown on Al2O3 substrates by a sol-gel spin coating method. The structural characteristics, surface morphology, and gas sensing properties of the SnO2 nanostructure were investigated. Thin film annealing at 500°C produced a high-quality SnO2 nanostructure with a crystallite size of 33.98 nm. A metal-semiconductor-metal gas sensor was fabricated using the SnO2 nanostructure and palladium metal. The gas sensor exhibited a sensitivity of 2570% to 1000 ppm H2 gas at RT. The sensing measurements for H2 gas at different temperatures (RT to 125°C) were repeatable for 50 min. Sensor sensitivity was tested under different H2 concentrations (150 ppm, 250 ppm, 375 ppm, 500 ppm, and 1000 ppm) at different operating temperatures. Adding glycerin to the sol solution increased the porosity of the SnO2 nanostructure surface, which increased the adsorption/desorption of gas molecules which leads to the high sensitivity of the sensor. Therefore, this H2 gas sensor is a suitable portable RT gas sensor.

  19. Synthesis of sub-10 nm VO2 nanoparticles films with plasma-treated glass slides by aqueous sol-gel method

    Lan, Shi-Di; Cheng, Chih-Chia; Huang, Chi-Hsien; Chen, Jem-Kun


    This paper describes an aqueous sol-gel synthesis of thermochromic thin films consisted of vanadium dioxide nanoparticles (VNPs) on glass slides. The glass slides were treated by argon/oxygen plasma to generate dispersedly negative charge sites on the surface to attract VO2+ from a sol-gel solution. After heat treatment in a low-pressure carbon monoxide/carbon dioxide (CO/CO2) atmosphere, the VNPs could be generated in sub-10 nm of particle size on the surface. Various levels of doping were achieved by adding small quantities of a water-soluble tungsten compound to the sol; however, the particle size increased slightly with the tungsten doping levels. The change in electrical conductivity with temperature for VNP films were measured and compared to VO2 crystalline films. VNP films exhibited the lower transition temperature of the semiconductor to metal phase change; at a doping level of 4 wt% the transition temperature was measured at 32.2 ± 1.2 and 24.1 ± 1.2 °C for the VO2 and VNP films, respectively. The VNP films showed excellent visible transparency and a large change in transmittance at near-infrared (NIR) wavelengths before and after the metal-insulator phase transition (MIT). The current method is a landmark in the development of nanostructured material toward applications in energy-saving smart windows.

  20. 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...

  1. 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.

  2. Properties of Zn O/Cr thin films prepared by Sol-Gel; Propiedades de peliculas delgadas ZnO/Cr preparadas por Sol-Gel

    Tirado G, S.; Olvera A, R., E-mail: [IPN, Escuela Superior de Fisica y Matematicas, Edificio 9, Unidad Profesional A. L. M., San Pedro Zacatenco, 07788 Mexico D. F. (Mexico)


    Zn O films and those superficially modified with chromium were deposited on substrates of soda-lime glass, using the Sol-Gel process and the repeated immersion method. Starting from dehydrated zinc acetate was prepared a solution to 0.6 M to ambient temperature in 2-methoxyethanol and monoethanolamine (Mea) stirring magnetically. The Sol was prepared with an aging to seven days and was used to grow a films group with thickness to eight immersions. These same films were superficially modified with several depositions of a chromium nitrate Sol dissolved in ethanol to low concentration. The Zn O films were structurally characterized by X-ray diffraction, its chemical composition by energy dispersive X-ray spectroscopy and its morphology by scanning electron microscopy and atomic force microscopy, as well as their optical properties by UV-vis. Of the obtained results are proposed possible applications. (author)

  3. Synthesis of ZNO nanoparticles by Sol-Gel processing; Obtencao de nanoparticulas de ZnO a partir de processamento Sol-Gel

    Savi, B.M.; Rodrigues, L.; Uggioni, E.; Bernardin, A.M., E-mail: [Universidade do Extremo Sul Catarinense (UNESC), Criciuma, SC (Brazil). Grupo de Materiais Ceramicos e Vitreos


    The aim of this study was to obtain and characterize ZnO nanoparticles by Sol-Gel technique. ZnCl{sub 2}, Zn(NO{sub 3}){sub 2}, NaOH were used as precursors for the synthesis. NaOH was dissolved in distilled water at a concentration of 1.0 M with agitation to the desired reaction temperature (50°C and 90°C). 0.5 M ZnCl{sub 2} and 0.5 M Zn(NO3)2 were added by dripping (60 and 30 min). The powder was characterized by XRD (Cu Kα), UV-Vis, and HR-TEM. Nano ZnO particles were obtained with crystallite size between 20 and 40 nm (HR-TEM and XRD). The results of UV-Vis spectrometry show that the band gap energy, given by the absorbance at 300 nm depends on the precursor used. (author)

  4. 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

  5. Effective Sol-Gel Nanocoatings on ZnO Electrodes for Suppressing Recombination in Dye-Sensitized Solar Cells

    Shintaro Ueno


    Full Text Available Attempts have been made to improve the performance of dye-sensitized solar cells by forming metal-oxide nanocoating layers on ZnO electrodes by a sol-gel transformation. SiO2, Nb2O5, TiO2, or ZrO2 nanocoating layers could be formed by dipping ZnO films into metal alkoxide solutions of low concentrations and subsequent heat treatments. The performance of DSSCs using the coated ZnO electrodes depends strongly on the structure of coating layers such as the thickness and the surface coverage, which are significantly influenced by the coating conditions. In particular, SiO2 and Nb2O5 coating layers are effective to suppress the recombination by constructing the energy barrier at the ZnO/electrolyte interface and enhance energy conversion efficiency. It is found that the coating layers also hinder the grain growth of ZnO, contributing to the enhanced cell performance as well.

  6. Synthesis and Characterization of Fe₂(MoO₄)₃Nano-Photocatalyst by Simple Sol-Gel Method.

    Umapathy, V; Manikandan, A; Ramu, P; Antony, S Arul; Neeraja, P


    Ferric molybdate (Fe₂(MoO₄)₃) nanorods (NRs) were successfully synthesized using metal nitrates, citric acid and ethyl cellulose by a simple sol-gel method. Structural, morphological, optical and magnetic properties of the obtained powder were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, high resolution scanning electron microscope (HR-SEM), energy dispersive X-ray (EDX), UV-Visible diffuse reflectance spectra (DRS), photoluminescence (PL) spectra and vibrating sample magnetometer (VSM). XRD results indicated that the resultant powder was pure single phase crystalline with monoclinic structure. FT-IR spectra indicate the type of bonds between metals and oxygen. HR-SEM images shows that the morphology of the powder consist with well defined nanorods (NRs) structure. VSM results showed ferromagnetic behavior. The addition of TiO₂ catalyst, it enhanced the photo-catalytic activity of Fe₂(MoO₄)₃. The mixed oxide catalyst of Fe₂(MoO₄)₃-TiO₂ nano-composites (NCs) were also tested for the photocatalytic degradation (PCD) of 4-chlorophenol (4-CP). It was found that the PCD efficiency of Fe₂(MoO₄)₃ NCs is higher than pure Fe₂(MoO₄)₃ and TiO₂ catalysts.

  7. One pot synthesis of exchange coupled Nd2Fe14B/alpha-Fe by pechini type sol-gel method.

    Hussain, Abid; Jadhav, Abhijit P; Baek, Yeon Kyung; Choi, Hul Jin; Lee, Jaeho; Kang, Young Soo


    In this work, a combination of nanoparticles of Nd2Fe14B hard magnetic phase and alpha-Fe soft magnetic phase were synthesized by one pot chemical synthesis technique using sol-gel method. A gel of Nd-Fe-B was prepared using NdCl3 x 6H2O, FeCl3 x 6H2O, H3BO3, citric acid, and ethylene glycol by pechini type sol-gel method. The gel was subsequently calcined and annealed to obtain the mixed oxide powders. The produced metal oxide particles were identified with XRD, SEM, TEM to obtain the crystal structure, shape and domain structure of them. The nanoparticles of mixed phase of Nd2Fe14B/alpha-Fe were obtained from these oxides by a process of reduction-diffusion in vacuum by employing CaH2 as reducing agent. During this process it was optimized by controlling temperature, reaction time and concentration of the reducing agent (CaH2). The phase formation of Nd2Fe14B was resulted by the direct diffusion of NdH2, Fe and B. The magnetic property of produced hard and soft phases was successfully identified with vibrating sample magnetometer (VSM). The mixed domains of the hard and soft phases were identified with selected area electron diffraction method (SAED) patterns.

  8. Photoluminescent properties of Ca2Gd8(SiO4)6O2: Dy3+ phosphor films prepared by sol-gel process

    HAN Xiumei; LIN Jun; LI Zhe; QI Xiwei; LI Mingya; WANG Xiaoqiang


    There are growing interests on phosphor thin films owing to their potential application in high-resolution devices such as cathode ray tubes and fiat panel display devices. The solution-based sol-gel method is one of the most important techniques for the synthesis of vari-ous functional coating films. Compounds with the apatite structure are very suitable host lattices for various luminescent ions. Ca2RE8(SiO4)6O2 (RE=Y, Gd, La) is a kind of ternary rare-earth-metal silicate with oxyapatite structure, which has been used as host mate-rial for the luminescence of various rare earth and mercury-like ions. In this article, Ca2Gd8(SiO4)6O2:Dy3+phosphor films were dip-coated on quartz glass substrates through the sol-gel process. X-ray diffraction (XRD), atomic force microscopy (AFM), photoluminescence (PL) spectra, as well as lifetimes were used to characterize the resulting films. AFM study revealed that the phosphor films consisted of homoge-neous particles. The Dy3+ showed its characteristic emission in crystalline phosphor films, i.e., 4F9/2-6H15/2 and 4F9/2-613/2.

  9. Effect of ZrN coating by magnetron sputtering and sol-gel processed silica coating on titanium/porcelain interface bond strength.

    Xia, Yang; Zhou, Shu; Zhang, Feimin; Gu, Ning


    In this study, a coating technique was applied to improve the bond strength of titanium (Ti) porcelain. ZrN coating was prepared by magnetron sputtering, and silica coating was processed by a sol-gel method. The treated surfaces of the specimens were analyzed by X-ray diffraction, and the Ti/porcelain interface was investigated by scanning electron microscopy (SEM) and energy dispersive spectroscopy. The coated specimens appeared fully coherent to the Ti substrate. The fractured bonding surface was also investigated by SEM. The residual porcelain on the metal surface could be observed in the ZrN group and silica group, but there was no obvious porcelain remaining in the control group. A three-point-bending test showed that the bonding strength of the ZrN group (45.99 ± 0.65 MPa) was higher than the silica group (37.77 ± 0.78 MPa) (P coatings resulted in a stronger Ti/porcelain bond. ZrN coating by magnetron sputtering was a more effective way to improve the bond strength between Ti and porcelain compared with sol-gel processed silica coating in this study.

  10. A new sol-gel synthesis of 45S5 bioactive glass using an organic acid as catalyst.

    Faure, J; Drevet, R; Lemelle, A; Ben Jaber, N; Tara, A; El Btaouri, H; Benhayoune, H


    In this paper a new sol-gel approach was explored for the synthesis of the 45S5 bioactive glass. We demonstrate that citric acid can be used instead of the usual nitric acid to catalyze the sol-gel reactions. The substitution of nitric acid by citric acid allows to reduce strongly the concentration of the acid solution necessary to catalyze the hydrolysis of silicon and phosphorus alkoxides. Two sol-gel powders with chemical compositions very close to that of the 45S5 were obtained by using either a 2M nitric acid solution or either a 5mM citric acid solution. These powders were characterized and compared to the commercial Bioglass®. The surface properties of the two bioglass powders were assessed by scanning electron microscopy (SEM) and by Brunauer-Emmett-Teller method (BET). The Fourier transformed infrared spectroscopy (FTIR) and the X-ray diffraction (XRD) revealed a partial crystallization associated to the formation of crystalline phases on the two sol-gel powders. The in vitro bioactivity was then studied at the key times during the first hours of immersion into acellular Simulated Body Fluid (SBF). After 4h immersion into SBF we clearly demonstrate that the bioactivity level of the two sol-gel powders is similar and much higher than that of the commercial Bioglass®. This bioactivity improvement is associated to the increase of the porosity and the specific surface area of the powders synthesized by the sol-gel process. Moreover, the nitric acid is efficiently substituted by the citric acid to catalyze the sol-gel reactions without alteration of the bioactivity of the 45S5 bioactive glass.

  11. Sol-gel-CVD组合技术制备纳米复合膜自洁净玻璃的研究%Composite technology of sol - gel - CVD for preparation of self- cleaning glass with nano - composite film

    张敬畅; 胡博; 曹维良


    采用溶胶-凝胶法(sol-gel)、化学气相沉积法(CVD)法及sol-gel-CVD组合技术制备自洁净玻璃,对光降解膜的化学组分进行了优化,通过以甲基橙为降解物对光催化性能进行考察,测试了其浸润角、膜厚,采用SEM技术对表面结构进行了表征,并对sol-gel,CVD以及sol-gel-CVD的组合技术3种方法进行比较.结果表明,采用sol-gel-CVD的组合技术制得Ti-Ce膜的洁净玻璃表面致密性最好,具有很好的亲水性,光催化性能最高,1.5 h时的降解率最好达到96.2%.

  12. Evaluation of hybrid sol-gel incorporated with nanoparticles as nano paint

    Jameel, Zainab N.; Haider, Adawiya J.; Taha, Samar Y.; Gangopadhyay, Shubhra; Bok, Sangho


    A coating with self-cleaning characteristics has been developed using a TiO2/SiO2 hybrid sol-gel, TiO2 nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO2 nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO2 nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO2 phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO2 NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

  13. Preparation and mechanical properties of silicon oxycarbide fibers from electrospinning/sol-gel process

    Wang, Xiaofei [School of Materials Sciences and Engineering, Tianjin University, 300072 Tianjin (China); Gong, Cairong, E-mail: [School of Materials Sciences and Engineering, Tianjin University, 300072 Tianjin (China); Fan, Guoliang [School of Materials Sciences and Engineering, Tianjin University, 300072 Tianjin (China)


    Graphical abstract: Ceramic fibers, silicon oxycarbide (SiOC) fibers were demonstrated and showed higher mechanical properties from electrospinning/sol-gel process at 1000 Degree-Sign C. Highlights: Black-Right-Pointing-Pointer SiOC fibers with low cost are promising to substitute the non-oxide fibers. Black-Right-Pointing-Pointer Successful preparation of SiOC fibers by electrospinning/sol-gel process. Black-Right-Pointing-Pointer Confirmation of the designed product using material characterization methods. Black-Right-Pointing-Pointer The SiOC fibers prepared at 1000 Degree-Sign C possess higher strength (967 MPa). -- Abstract: Silicon oxycarbide (SiOC) fibers were produced through the electrospinning of the solution containing vinyltrimethoxysilane and tetraethoxysilane in the course of sol-gel reaction with pyrolysis to ceramic. The effect of the amount of spinning agent Polyvinylpyrrolidone (PVP) on the dope spinnability was investigated. At a mass ratio of PVP/alkoxides = 0.05, the spinning sol exhibited an optimal spinnable time of 50 min and generated a large quantity of fibers. Electrospun fibers were characterized by Fourier transform infrared spectroscopy (FTIR), thermo gravimetric analysis-differential scanning calorimetry (TGA-DSC), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The SEM results revealed that the SiOC fibers had a smooth surface and dense cross-section, free of residue pores and cracks. The XPS results gave high content of SiC (13.99%) in SiOC fibers. The SiOC fibers prepared at 1000 Degree-Sign C had a high tensile strength of 967 MPa and Young's modulus of 58 GPa.

  14. Evaluation of hybrid sol-gel incorporated with nanoparticles as nano paint

    Jameel, Zainab N., E-mail:; Haider, Adawiya J., E-mail: [Nanotechnology and Advanced Materials Research Center, The University of Technology, Baghdad (Iraq); Taha, Samar Y., E-mail: [College of Science for Women, University of Baghdad, Baghdad (Iraq); Gangopadhyay, Shubhra, E-mail:; Bok, Sangho, E-mail: [Department of Electrical and Computer, University of Missouri, Engineering, Building West, Columbia, Missouri 65211 (United States)


    A coating with self-cleaning characteristics has been developed using a TiO{sub 2}/SiO{sub 2} hybrid sol-gel, TiO{sub 2} nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO{sub 2} nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO{sub 2} nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO{sub 2} phases. The NPs size as determined by Dynamic Light Scattering (DLS) ranges within of (3-4) and (20-42) nm, which was also confirmed by Scanning Electron Microscopy (SEM). The nanoparticles showed surface charge (zeta-potential, ζ) of +35 and +25.62 mV for the methods, respectively, and ζ values of +41.31 and 34.02 mV for anatase and rutile phases, respectively. The NPs were mixed with the coating solution (i.e., hybrid sol-gel and OSNP) in different concentrations and thin films were prepared by spin coating. Self-cleaning tests were performed using Rhodamine B (RhB) as a pollution indicator. The effect of UV-irradiation on the films was also studied. Anatase and rutile incorporated as a mixture with different ratios in local paint and washability as well as a contrast ratio tests were performed. It was found that the addition of TiO{sub 2} NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

  15. Electrophoretically active sol-gel processes to backfill, seal, and/or densify porous, flawed, and/or cracked coatings on electrically conductive material

    Panitz, Janda K.; Reed, Scott T.; Ashley, Carol S.; Neiser, Richard A.; Moffatt, William C.


    Electrophoretically active sol-gel processes to fill, seal, and/or density porous, flawed, and/or cracked coatings on electrically conductive substrates. Such coatings may be dielectrics, ceramics, or semiconductors and, by the present invention, may have deposited onto and into them sol-gel ceramic precursor compounds which are subsequently converted to sol-gel ceramics to yield composite materials with various tailored properties.

  16. Electrophoretically active sol-gel processes to backfill, seal, and/or densify porous, flawed, and/or cracked coatings on electrically conductive material

    Panitz, J.K.; Reed, S.T.; Ashley, C.S.; Neiser, R.A.; Moffatt, W.C.


    Electrophoretically active sol-gel processes to fill, seal, and/or density porous, flawed, and/or cracked coatings on electrically conductive substrates. Such coatings may be dielectrics, ceramics, or semiconductors and, by the present invention, may have deposited onto and into them sol-gel ceramic precursor compounds which are subsequently converted to sol-gel ceramics to yield composite materials with various tailored properties. 6 figs.

  17. Sol-gel methyl coating in capillary microextraction hyphenated on-line with high-performance liquid chromatography Counterintuitive extraction behavior for polar analytes.

    Segro, Scott S; Malik, Abdul


    A sol-gel coating with anchored methyl groups was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). This was accomplished by using methyltrimethoxysilane as the sol-gel precursor. The methyl group on the sol-gel precursor ultimately turned into a pendant group on the created sol-gel coating and was primarily responsible for the extraction of nonpolar analytes. A 40-cm segment of 0.25mm I.D. fused silica capillary containing the sol-gel methyl coating on the inner surface was installed as a sampling loop in an HPLC injection port. The analytes were extracted by the coating when an aqueous sample containing the analytes was passed through this capillary. The extracted analytes were then transferred to the HPLC column using isocratic elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for polycyclic aromatic hydrocarbons and ketones. Unexpectedly, this coating also provided good extraction for polar analytes, including aromatic phenols, alcohols, and amines. Considering the fact that the methyl group is nonpolar in nature, such an extraction behavior of sol-gel methyl coating toward polar analytes is counterintuitive. Thus, sol-gel sorbents with short alkyl side chains have the potential to offer a polymer-free alternative to traditional sol-gel capillary microextraction (CME) media commonly prepared with the use of polymers in the sol solution. Elimination of polymers from the sol-gel coating solution is conducive to improving thermal stability and solvent tolerance of the created sol-gel extracting phase. This also makes the preparation of sol-gel coatings facile and cost-effective. Possessing excellent solvent stability, such sol-gel coatings offer the opportunity for effective on-line hyphenation of capillary microextraction with HPLC and other liquid-phase separation techniques that employ organo-aqueous mobile phases.

  18. Free volume effects on the fluorescence characteristics of sol-gel glasses doped with quinine sulphate

    Meneses-Nava, M. A.; Barbosa-García, O.; Díaz-Torres, L. A.; Chávez-Cerda, S.; King, T. A.


    The broadening of the absorption and fluorescence spectra and the red shift of the fluorescence maximum of quinine sulfate doped sol-gel glasses, before and after PMMA polymer impregnation, are investigated at different concentrations. The fluorescence decay of the quinine sulfate doped samples does not fit to a single exponential, as it does in ethanol solutions. We found that a double exponential gives a good fit to the obtained results. Introduction of solvent to fill the pores of the matrix does not only have the same effect as the polymer, but also reveals the strong attachment of the molecules to the pore walls and the influence of the interaction with the cage.

  19. 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.

  20. Dielectric function of sol-gel prepared nano-granular zinc oxide by spectroscopic ellipsometry

    Gilliot, Mickaël, E-mail:; Hadjadj, Aomar [LISM, Université de Reims Champagne-Ardenne, Reims (France); Eypert, Céline [HORIBA Jobin Yvon S.A.S., Palaiseau (France)


    ZnO thin films have been prepared by sol gel and deposited by spin coating. The dielectric function has been determined by spectroscopic ellipsometry. Ellipsometric spectra are inverted by a direct numerical method without using the standard fitting procedures. The obtained dielectric function presents a broad excitonic effect. The dielectric function is studied using Elliot excitonic theory including exciton plus band-to-band Coulomb interactions with standard Lorentzian broadening. A modification of this model dielectric function with independent bound and unbound exciton contributions is empirically proposed to improve modelling of the band gap excitonic peak.