Vapor phase modification of sol-gel derived titania (TiO{sub 2}) surfaces

Energy Technology Data Exchange (ETDEWEB)

Piwonski, Ireneusz [University of Lodz, Department of Chemical Technology and Environmental Protection, Pomorska 163, 90-236 Lodz (Poland)]. E-mail: irek@uni.lodz.pl; Ilik, Aneta [University of Lodz, Department of Chemical Technology and Environmental Protection, Pomorska 163, 90-236 Lodz (Poland)

2006-12-30

Chemical vapor deposition (CVD) method was used in titania surface modification. Titania layers were obtained in sol-gel process and prepared as thin films on silicon wafers in dip-coating method. In order to define the influence of modification on titania surface properties (e.g., friction), various types of fluoroalkylsilanes were used. The effectiveness of the modification was monitored by FT-IR spectroscopy. The topography and frictional measurements were investigated with the use of atomic force microscopy (AFM)

Equipment for production of hydrogel by sol-gel method

International Nuclear Information System (INIS)

Urbanek, V.

1975-01-01

The method of uranyl gel preparation is described by the sol-gel process of the internal gelation type. A laboratory-scale equipment with an output of 1.5 kg of gel per hour was built at the Nuclear Research Institute, Rez; the diameter of the microspheres produced may vary between 0.5 and 4.0 mm. The reliability of the equipment was verified by producing several tens of kilograms of uranyl gels and of gels based on other non-nuclear materials. (author)

Fabrication of hydrophobic compressed oil palm trunk surface by sol-gel process

Science.gov (United States)

Muzakir, Syafiqah; Salim, Nurjannah; Huda Abu Bakar, Nurul; Roslan, Rasidi; Sin, Lim Wan; Hashim, Rokiah

2018-04-01

Improvement of the robustness of hydrophobic surfaces is crucial to achieving commercial applications of these surfaces in such various areas as self-cleaning, water repellency and corrosion resistance. Compressed oil palm trunk (OPT) panel is one of potential product which can be used as panelling and indoor furniture application. By adding hydrophobic properties to compressed oil palm trunk panel might increase the application of compressed oil palm trunk especially for outdoor application. In this study, fabrication is using the sol-gel technique. Sol-gel was prepared by adding ethanol with Hexadecyl Trimethyl Ammonium Bromide (CTAB) solution with Tetraethyl Orthosilicate (TEOS) with surface modification of chlorotrimethylsilane (CTMS). The surface with hydrophobic coating was undergone surface analysis with contact angle machine with the aid of software SCA 20 and the determined of the morphology of surface with scanning electron microscope (SEM). The produced compressed oil palm trunk surfaces exhibited promising hydrophobic properties with a contact angle of 104° and the relatively better mechanical robustness.

Investigation of sol-gel transition by rheological methods. Part I. Experimental methods.

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KUDRYAVTSEV Pavel Gennadievich

2017-08-01

Full Text Available In this work rheological studies of the gelling process were carried out. We have developed a measuring system for studying the rheology of the gelation process. It consisted of several measuring cells of the Weiler-Rebinder type, system for automatic regulation of the composition of the medium and hermostabilization system. This complex is designed to measure the dependence of the value of the ultimate shear stress as a function of time, from the start of the sol-gel transition to the complete conversion of the sol to the gel. The developed device has a wide range of measured values of critical shear stresses τ0 = (0,05÷50000 Dyne/cm2. Using the developed instrument, it was possible to establish the shape of the initial section of the curve τ0 = f(t and develop a methodology for more accurate determination of gelation time. The developed method proved that the classical method for determining the start time of the sol-gel transition using the point of intersection of the tangent to the linear part of the rheological curve τ0 = f(t,gives significantly distorted results. A new phenomenon has been discovered: the kinetic curves in the coordinates of the Avrami-Erofeev-Bogolyubov equation have an inflection point which separates the kinetic curve into two parts, the initial and the final. It was found that the constant k in the Avrami–Erofeev–Bogolyubov quation does not depend on the temperature and is the same for both the initial and final parts of the kinetic curve. It depends only on the chemical nature of the reacting system. It was found that for the initial section of the kinetic curves, the value of the parameter n in the Avrami-Erofeev-Bogolyubov equation was n = 23,4±2,8 and, unlike the final section of the rheological curve, does not depend on temperature. A large value of this parameter can be interpreted as the average number of directions of growth of a fractal aggregate during its growth. The value of this parameter depends

Study of silica sol-gel materials for sensor development

Science.gov (United States)

Lei, Qiong

Silica sol-gel is a transparent, highly porous silicon oxide glass made at room temperature by sol-gel process. The name of silica sol-gel comes from the observable physical phase transition from liquid sol to solid gel during its preparation. Silica sol-gel is chemically inert, thermally stable, and photostable, it can be fabricated into different desired shapes during or after gelation, and its porous structure allows encapsulation of guest molecules either before or after gelation while still retaining their functions and sensitivities to surrounding environments. All those distinctive features make silica sol-gel ideal for sensor development. Study of guest-host interactions in silica sol-gel is important for silica-based sensor development, because it helps to tailor local environments inside sol-gel matrix so that higher guest loading, longer shelf-life, higher sensitivity and faster response of silica gel based sensors could be achieved. We focused on pore surface modification of two different types of silica sol-gel by post-grafting method, and construction of stable silica hydrogel-like thin films for sensor development. By monitoring the mobility and photostability of rhodamine 6G (R6G) molecules in silica alcogel thin films through single molecule spectroscopy (SMS), the guest-host interactions altered by post-synthesis grafting were examined. While physical confinement remains the major factor that controls mobility in modified alcogels, both R6G mobility and photostability register discernable changes after surface charges are respectively reversed and neutralized by aminopropyltriethoxysilane (APTS) and methyltriethoxysilane (MTES) grafting. The change in R6G photostability was found to be more sensitive to surface grafting than that of mobility. In addition, silica film modification by 0.4% APTS is as efficient as that by pure MTES in lowering R6G photostability, which suggests that surface charge reversal is more effective than charge neutralization

Thoria sol-gel processes

International Nuclear Information System (INIS)

Matthews, R.B.

1978-10-01

Alternate fuel fabrication techniques are being developed at WNRE as part of the thorium fuel cycle program. The sol-gel techniques are attractive and this report assembles and summarizes information relating to thoria sol-gel fuels. Some background information on the behaviour and advantages of sol-gel fuel forms is presented, followed by a review of relevant colloid chemistry and an explanation of the fundamental steps of sol-gel processes. Finally, several variants to the basic process are reviewed and evaluated. (author)

Sol-gel processing with inorganic metal salt precursors

Science.gov (United States)

Hu, Zhong-Cheng

2004-10-19

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.

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

Directory of Open Access Journals (Sweden)

Manish Kumar

2011-06-01

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

Current and future possibilities of sol-gel process

International Nuclear Information System (INIS)

Sakka, Sumio

2004-01-01

The sol-gel method is characterized by the low temperature processing. Since this method starts from solutions, the product is essentially nanomaterials. So far, various kinds of microstructures, including dense, porous, hybrid, amorphous and crystalline microstructures have been realized. Accordingly, sol-gel materials cover a wide range of functions, such as optical, electronic, mechanical, chemical and bio-functions. Future perspectives of the sol-gel method are described in the article. (author)

Applications of sol gel ceramic coatings

International Nuclear Information System (INIS)

Barrow, D.

1996-01-01

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.)

Thermal stability of octadecylsilane hybrid silicas prepared by grafting and sol-gel methods

International Nuclear Information System (INIS)

Brambilla, Rodrigo; Santos, Joao H.Z. dos; Miranda, Marcia S.L.; Frost, Ray L.

2008-01-01

Hybrid silicas bearing octadecylsilane groups were prepared by grafting and sol-gel (SG) methods. The effect of the preparative route on the thermal stability was evaluated by means of thermal gravimetric analysis (TGA), infrared emission spectroscopy (IRES) and, complementary, by 13 C solid-state nuclear magnetic resonance ( 13 C NMR) and matrix assisted laser deionization time of flight mass spectroscopy (MALDI-TOF-MS). Silicas prepared by the grafting route seem to be slightly more stable than those produced by the sol-gel method. This behavior seems to be associated to the preparative route, since grafting affords a liquid-like conformation, while in the case of sol-gel a highly organized crystalline chain conformation was observed

Synthesis of uranium and thorium dioxides by Complex Sol-Gel Processes (CSGP). Synthesis of uranium oxides by Complex Sol-Gel Processes (CSGP)

International Nuclear Information System (INIS)

Deptula, A.; Brykala, M.; Lada, W.; Olczak, T.; Wawszczak, D.; Chmielewski, A.G.; Modolo, G.; Daniels, H.

2010-01-01

In the Institute of Nuclear Chemistry and Technology (INCT), a new method of synthesis of uranium and thorium dioxides by original variant of sol-gel method - Complex Sol-Gel Process (CSGP), has been elaborated. The main modification step is the formation of nitrate-ascorbate sols from components alkalized by aqueous ammonia. Those sols were gelled into: - irregularly agglomerates by evaporation of water; - medium sized microspheres (diameter <150) by IChTJ variant of sol-gel processes by water extraction from drops of emulsion sols in 2-ethylhexanol-1 by this solvent. Uranium dioxide was obtained by a reduction of gels with hydrogen at temperatures >700 deg. C, while thorium dioxide by a simple calcination in the air atmosphere. (authors)

Monolithic lithium-based aerogels via dispersed inorganic sol-gel method

International Nuclear Information System (INIS)

Xiao Shufang; Zhou Bin; Du Ai; Xu Xiang; Yang Xiaoyun; Shen Jun; Wu Guangming; Zhang Zhihua; Wan Huijun

2008-01-01

Monolithic lithium-based aerogels were prepared by poly acrylic acid (PAA) and propylene oxide (PO) via the dispersed inorganic sol-gel method and drying with CO 2 supercritical fluid dry process. The density of the prepared sample is about 150 g/m 3 . The microstructure of the lithium-based aerogels was characterized by TEM, IR, XPS and BET. The results show that the material mainly contains Li, C and O element s. BET surface area is up to 18.9 m 2 /g. (authors)

Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: bonding to titanium and scanning electron microscopy.

Science.gov (United States)

Tredwin, Christopher J; Georgiou, George; Kim, Hae-Won; Knowles, Jonathan C

2013-05-01

Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) production has been characterised and optimised by the sol-gel method and the dissolution and biological properties of these materials were investigated. It was the objective of this study to investigate the potential bond strength and interaction of these materials with titanium. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the FHA and FA sol-gels. Using a spin coating technique the sol-gels were coated onto commercially pure titanium disks and crystallised at various temperatures. Using scanning electron microscopy (SEM) and elemental analysis, the surface characteristics, coating thickness and interaction of the Ti substrate and coating were investigated. The bond strengths of the coating to the Ti were investigated using an Instron Universal Load Testing Machine. Statistical analysis was performed with a two-way analysis of variance and post hoc testing with a Bonferroni correction. (1) Coating speed inversely influenced the coating thickness. (2) Increasing fluoride ion substitution and heating temperature significantly increased bond strength and (3) increasing fluoride ion substitution increased the coating thickness. FHA and FA synthesised using the sol-gel technique may offer a superior alternative to coating titanium implants with HA and plasma spraying. HA, FHA and FA materials synthesised by the sol-gel method may also have a use as bone grafting materials. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

Science.gov (United States)

Chu, Chung-tse; Zheng, Haixing

1996-01-01

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.

Characterisation of a new alkoxide sol-gel hydroxyapatite

International Nuclear Information System (INIS)

Green, D.D.; Kannangara, G.S.K.; Milev, A.; Ben-Nissan, B.

1999-01-01

Hydroxyapatite (HAp) coatings have been used to promote bone growth and fixation towards implant surfaces to encourage faster recovery times for the recipient. Current coating processing techniques, capable of producing thin HAp layers are pulsed-laser deposition and sputtering (high-temperature processing). Other technologies are in vitro methods, electrodeposition and sol-gel, due to the fact that these techniques utilise lower processing temperatures they avoid structural instabilities of HAp at elevated temperatures. The term sol-gel encompasses any process of producing ceramic materials (single and mixed oxides, as well as non-oxides e.g. nitrides) from solutions. The sol-gel process was first identified by Ebelman, and has been used to produce ceramic powders, coatings, and bulk materials including glasses. The implementation of a sol-gel methodology enables increased stoichiometry and homogeneity, while having the ability to coat complex shapes. Sol-gel hydroxyapatite reported by Chai et al. employed tri ethyl phosphite [ P(OEt) 3 ] as the staring phosphorus alkoxide precursor, whereby it was established that in order to obtain monophasic hydroxyapatite upon firing there must be a 24 hour ripening period. The ripening period was determined to be an equilibrium step whereby the equilibrium intermediate phase lied in favour of a diethyl phosphite arrangement (species) within the sol. Therefore, the work here under taken was to produce hydroxyapatite using diethyl phosphite [HOP(OEt) 2 ] as a starting alkoxide precursor with a final aim to reduce or eliminate the ageing period as observed by Chai et al in P(OEt) 3 solutions

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

Science.gov (United States)

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

2013-02-01

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.

Mechanical compatibility of sol-gel annealing with titanium for orthopaedic prostheses.

Science.gov (United States)

Greer, Andrew I M; Lim, Teoh S; Brydone, Alistair S; Gadegaard, Nikolaj

2016-01-01

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.

Fast Processing of Sol-Gel TCO

NARCIS (Netherlands)

Deelen, J. van; Rem, M.; Arfsten, N.; Buskens, P.P.

2016-01-01

TCOs are usually deposited using sputtering or chemical vapor deposition, which have a yield of typically 50-75%. The sol gel method does not need low pressure and can be done with a high precursor yield in the range of 90 – 100%. Sol gel enables also the TCO function as a planarization or

Surface Behavior of Rhodamin and Tartrazine on Silica-Cellulose Sol-Gel Surfaces by Thin Layer Elution

Directory of Open Access Journals (Sweden)

Surjani Wonorahardjo

2016-05-01

Full Text Available Physical and chemical interactions are the principles for different types of separation systems as the equillibrium dynamics on surface plays a key-role. Surface modification is a way for selective separation at interfaces. Moreover, synthesis of gel silica by a sol-gel method is preferred due to the homogeneity and surface feature easily controlled. Cellulose can be added in situ to modified the silica features during the process. Further application for to study interaction of rhodamin and tartrazine in its surface and their solubilities in mobile phase explains the possibility for their separation. This paper devoted to evaluate the surface behavior in term of adsorption and desorption of tartrazine and rhodamin on silica-cellulose thin layer in different mobile phase. Some carrier liquids applied such as methanol, acetone, n-hexane and chloroform. The result proves tartrazine and rhodamin is separated and have different behavior in different mobile phase. The retardation factors (Rf of the mixtures suggest complexity behavior on silica-cellulose surface.

Preparation and characterization of ZnO transparent semiconductor thin films by sol-gel method

International Nuclear Information System (INIS)

Tsay, Chien-Yie; Fan, Kai-Shiung; Chen, Sih-Han; Tsai, Chia-Hao

2010-01-01

Transparent semiconductor thin films of zinc oxide (ZnO) were deposited onto alkali-free glass substrates by the sol-gel method and spin-coating technique. In this study, authors investigate the influence of the heating rate of the preheating process (4 or 10 o C/min) on the crystallization, surface morphology, and optical properties of sol-gel derived ZnO thin films. The ZnO sol was synthesized by dissolving zinc acetate dehydrate in ethanol, and then adding monoethanolamine. The as-coated films were preheated at 300 o C for 10 min and annealed at 500 o C for 1 h in air ambiance. Experimental results indicate that the heating rate of the preheating process strongly affected the surface morphology and transparency of ZnO thin film. Specifically, a heating rate of 10 o C/min for the preheating process produces a preferred orientation along the (0 0 2) plane and a high transmittance of 92% at a wavelength of 550 nm. Furthermore, this study reports the fabrication of thin-film transistors (TFTs) with a transparent ZnO active channel layer and evaluates their electrical performance.

Reversible sol-gel-sol medium for enzymatic optical biosensors

NARCIS (Netherlands)

Safaryan, S.; Yakovlev, A.; Pidko, E.A.; Vinogradov, A.; Vinogradov, V.

2017-01-01

In this paper we for the first time report a reversible sol-gel-sol approach to obtain optical enzymatic biosensors with improved enzyme stability and good sensitivity by using desktop inkjet printing. The developed technique is based on the bio-inorganic inks allowing for a sol-gel-sol transition

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.

Science.gov (United States)

Seyyal, Emre; Malik, Abdul

2017-04-29

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-C 12 ) and phenethyl (PhE) ligands. Here, the ability of the PF-C 12 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-C 12 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

Synthesis of nanoparticles of magnetite by sol-gel and precipitation methods: study of chemical composition and structure

International Nuclear Information System (INIS)

Picasso, Gino; Vega, Jaime; Uzuriaga, Rosario; Ruiz, Gean Pieer

2012-01-01

In this work, nanoparticles based on magnetite have been prepared by sol-gel and precipitation methods. In the first case two variants have been applied: by growing of sol starting from nitrate precursor and ethylene glycol as solvent and to control the reduction process and force hydrolysis and steric control prepared from ferrum sulfate precursor and sodium citrate. In the second case the starting material was sulfate precursor, ammonium hydroxide as precipitaing agent and ethylene glycol as surfactant. The samples have been characterized by X-ray diffraction technique (XRD), adsorption-desorption of N 2 (BET equation model) and Moessbauer spectroscopy. XRD patterns of all samples showed typical peaks of magnetite which were detected in the following positions: 30,06 o , 35,42 o , 62,55 o . Average specific surface quantified by BET method was ranging from 40 to 50 m 2 /g with isotherm type IV corresponding to mesoporous surface. Moessbauer spectra of sample prepared from sol-gel (gel growing) carried out at home temperature detected the presence of 2 sextets consisting in 2 type of sites: first one due to octahedral positions (Fe 2+ , Fe 3+ ) and the second one due to tetrahedral positions (Fe 3+ ). Grain size of magnetite samples, evaluated by Scherrer equation and specific surface area, was ranging from 2 to 20 nm. (author).

Sol-gel technology for biomedical engineering

International Nuclear Information System (INIS)

Podbielska, H.; Ulatowska-Jarza, A.

2005-01-01

Sol-gel derived silica possess many promising features, including low-temperature preparation procedure, porosity, chemical and physical stability. Applications exploiting porous materials to encapsulate sensor molecules, enzymes and many other compounds, are developing rapidly. In this paper some potential applications, with emphasis on biomedical and environmental ones, are reviewed. The material preparation procedure is described and practical remarks on silica-based sol-gels are included. It is reported that sol-gels with entrapped various molecules may be used in construction of implants and coatings with bioactive properties. It is shown how to exploit the sol-gel production route for construction of sol-gel coated fiberoptic applicators for laser therapy. The applications of bioactive materials are discussed, as well. It is demonstrated that it is possible to immobilize photosensitive compounds in sol-gel matrix without loosing their photoactivity. Some examples of sol-gel based biosensors are demonstrated, as well, showing their potential for detecting various gases, toxic substances, acidity, humidity, enzymes and biologically active agents. (authors)

SAXS study of silica sols, gels and glasses obtained by the sol gel process

International Nuclear Information System (INIS)

Santos, D.I. dos; Aegerter, M.A.

1988-01-01

Systematic SAXS studies have been performed at the LURE Synchrotron, Orsay, using an intense beam of point like cross-section to obtain information about the sol -> humid gel -> dried gel -> silica glass transformation. The intensity curves have been analysed in term of power law in log-log plots, whose exponent is related to mass and surface fractal dimensions of the structure. It was found that almost all phases present fractal structures and for the case of basic gels, is of hierarchical nature. The aerogels are formed by a dense matrix, with a smooth surface and exhibit a very narrow auto-similarity range that gives a mass fractal dimension. (author) [pt

Photocatalytic Activity in CH3CN Related to the Surface Properties of TiO2 Powders Prepared by Sol-Gel Method

OpenAIRE

Bettoni, Marta; Candori, Pietro; Marmottini, Fabio; Perenze, Nicoletta; Rol, Cesare; Sebastiani, Giovanni V.; Vecchiocattivi, Franco

2009-01-01

Some TiO2 powders, prepared from titanium(IV)tetraisopropoxide by the sol-gel method and thermally treated between 100 and 1000∘C, have been characterized by X-ray powder diffraction and by nitrogen adsorption and desorption at 77 K to calculate the BET-specific surface area, from which the micropore volume and the external surface area can be derived. The photocatalytic activity (ka) of the above powders has been evaluated considering the TiO2-sensitized photo-oxidation of 4-methoxybenzyl al...

Tantala-based sol-gel coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

Science.gov (United States)

Tran, MinhPhuong; Turner, Erica B; Segro, Scott S; Fang, Li; Seyyal, Emre; Malik, Abdul

2017-11-03

A sol-gel organic-inorganic hybrid sorbent, consisting of chemically integrated tantalum (V) ethoxide (TaEO) and polypropylene glycol methacrylate (PPGM), was developed for capillary microextraction (CME). The sol-gel sorbent was synthesized within a fused silica capillary through hydrolytic polycondensation of TaEO and chemical incorporation of PPGM into the evolving sol-gel tantala network. A part of the organic-inorganic hybrid sol-gel network evolving in the vicinity of the capillary walls had favorable conditions to get chemically bonded to the silanol groups on the capillary surface forming a surface-bonded coating. The newly developed sol-gel sorbent was employed to isolate and enrich a variety of analytes from aqueous samples for on-line analysis by high-performance liquid chromatography (HPLC) equipped with a UV detector. CME was performed on aqueous samples containing trace concentrations of analytes representing polycyclic aromatic hydrocarbons, ketones, alcohols, amines, nucleosides, and nucleotides. This sol-gel hybrid coating provided efficient extraction with CME-HPLC detection limits ranging from 4.41pM to 28.19 pM. Due to direct chemical bonding between the sol-gel sorbent coating and the fused silica capillary inner surface, this sol-gel sorbent exhibited enhanced solvent stability. The sol-gel tantala-based sorbent also exhibited excellent pH stability over a wide pH range (pH 0-pH 14). Furthermore, it displayed great performance reproducibility in CME-HPLC providing run-to-run HPLC peak area relative standard deviation (RSD) values between 0.23% and 3.83%. The capillary-to-capillary RSD (n=3), characterizing capillary preparation method reproducibility, ranged from 0.24% to 4.11%. The results show great performance consistency and application potential for the sol-gel tantala-PPGM sorbent in various fields including biomedical, pharmaceutical, and environmental areas. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2014-02-18

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

Ultrasound-assisted sol-gel synthesis of ZrO2.

Science.gov (United States)

Guel, Marlene Lariza Andrade; Jiménez, Lourdes Díaz; Hernández, Dora Alicia Cortés

2017-03-01

Synthesis of tetragonal ZrO 2 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 ZrO 2 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. Copyright © 2016 Elsevier B.V. All rights reserved.

Nanocrystal/sol-gel nanocomposites

Science.gov (United States)

Petruska, Melissa A [Los Alamos, NM; Klimov, Victor L [Los Alamos, NM

2007-06-05

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.

Synthesis of yttrium silicate luminescent materials by sol-gel method

International Nuclear Information System (INIS)

Arkhipov, D.V.; Vasina, O.Yu.; Popovich, N.V.; Galaktionov, S.S.; Soshchin, N.P.

1996-01-01

Several yttrium-silicate composition with Y 2 O 3 content within 44-56% have been synthesized. it is ascertained that employment of sol-gel technique permits preparation of luminescent materials on yttrium silicate basis, which compare favourably with bath-produced specimens. The influence of phase composition of sol-gel phosphors on basic performance indices: intensity and luminescence spectrum, has been analyzed

Bioactive materials for biomedical applications using sol-gel technology

International Nuclear Information System (INIS)

Gupta, Radha; Kumar, Ashok

2008-01-01

This review paper focuses on the sol-gel technology that has been applied in many of the potential research areas and highlights the importance of sol-gel technology for preparing bioactive materials for biomedical applications. The versatility of sol-gel chemistry enables us to manipulate the characteristics of material required for particular applications. Sol-gel derived materials have proved to be good biomaterials for coating films and for the construction of super-paramagnetic nanoparticles, bioactive glasses and fiberoptic applicators for various biomedical applications. The introduction of the sol-gel route in a conventional method of preparing implants improves the mechanical strength, biocompatibility and bioactivity of scaffolds and prevents corrosion of metallic implants. The use of organically modified silanes (ORMOSILS) yields flexible and bioactive materials for soft and hard tissue replacement. A novel approach of nitric-oxide-releasing sol-gels as antibacterial coatings for reducing the infection around orthopedic implants has also been discussed

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

Directory of Open Access Journals (Sweden)

Rita B. Figueira

2015-04-01

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

Production of continuous mullite fiber via sol-gel processing

Science.gov (United States)

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

1990-01-01

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.

Effect of Precursor Concentration of MgO nanostructure by using Sol-Gel Method

Directory of Open Access Journals (Sweden)

V.T. Srisuvetha

2017-04-01

Full Text Available MgO thin flims have been prepared on substrates by a novel and simple sol-gel method using magnesium nitrate and collusion as starting material.The MgO nano catalyst with good sensor crystallization were obtained after annealing at 100°C Magnesium oxide was prepared by sol-gel method. The method involves the hydrolysis of magnesium alkoxide in the presence of acid or basic catalysts followed by a Oxalic acid reaction. The synthesized solids were characterized by IR spectroscopy X-ray diffraction electron microscopy. Ultraviolet visible absorbance measurement photoluminescence and Raman scattering spectra. X-ray diffraction (XRD characterization showed the formation of smaller particles after sol gel irradiation the structure and morphology of the MgO particles were analyzed byXRD. These articles were used for FTIR spectroscopic measurement and spectra were collected. In EDS we calculated the peak intensity the SEM the images of metal oxide.UV (Ultra Violet refers to adsorption spectroscopy optical properties of assorption, band gap energy.This means if use light in the visible and adjacent ranges.

Preparation and characterization of bismuth ruthenate pyrochlore via solid state reaction and sol-gel methods

Directory of Open Access Journals (Sweden)

Mayuree Sansernnivet

2010-01-01

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-07-01

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)

Structural Evolution and Stability of Sol-Gel Biocatalysts

International Nuclear Information System (INIS)

Rodgers, L.E.; Foster, L.J.R.; Holden, P.J.; Knott, R.B.; Bartlett, J.B.

2005-01-01

Full text: Immobilisation strategies for catalytic enzymes are important as they allow reuse of the biocatalysts. Sol-gel materials have been used to immobilise Candida antarctica lipase B (CALB), a commonly used industrial enzyme with a known crystal structure. The sol-gel bioencapsulate is produced through the condensation of suitable metal alkoxides in the presence of CALB, yielding materials with controlled pore sizes, volume and surface chemistry. Sol-gel matrices have been shown to 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 analysis techniques applied to date. Small angle neutron scattering (SANS) allows such multicomponent 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 percent. 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. The SANS protocol developed here may be applied more generally to bioencapsulates. (authors)

Ionogel Electrolytes through Sol-Gel Processing

Science.gov (United States)

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

Sol-gel matrices for direct colorimetric detection of analytes

Science.gov (United States)

Charych, Deborah H.; Sasaki, Darryl; Yamanaka, Stacey

2000-01-01

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.

Spatially resolved speckle-correlometry of sol-gel transition

Science.gov (United States)

Isaeva, A. A.; Isaeva, E. A.; Pantyukov, A. V.; Zimnyakov, D. A.

2018-04-01

Sol-gel transition was studied using the speckle correlometry method with a localized light source and spatial filtering of backscattered radiation. Water solutions of technical or food gelatin with added TiO2 nanoparticles were used as studied objects. Structural transformation of "sol-gel" system was studied at various temperatures from 25°C to 50°C using analysis of the correlation and structure functions of speckle intensity fluctuations. The characteristic temperatures of "sol - gel" transition were evaluated for studied systems. Obtained results can be used for various applications in biomedicine and food industry.

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

Directory of Open Access Journals (Sweden)

Ting Ke Tseng

2010-05-01

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.

Preparation and characterization of conductive and transparent ruthenium dioxide sol-gel films.

Science.gov (United States)

Allhusen, John S; Conboy, John C

2013-11-27

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.

THERMALLY STABLE NANOCRYSTALLINE TIO2 PHOTOCATALYSTS SYNTHESIZED VIA SOL-GEL METHODS MODIFIED WITH IONIC LIQUID AND SURFACTANT MOLECULES

Science.gov (United States)

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...

Sol-gel growth of vanadium dioxide

International Nuclear Information System (INIS)

Speck, K.R.

1990-01-01

This thesis examines the chemical reactivity of vanadium (IV) tetrakis(t-butoxide) as a precursor for the sol-gel synthesis of vanadium dioxide. Hydrolysis and condensation of the alkoxide was studied by FTIR spectroscopy. Chemical modification of the vanadium tetraalkoxide by alcohol interchange was studied using 51 V NMR and FTIR. Vanadium dioxide thin films and powders were made from vanadium tetrakis(t-butoxide) by standard sol-gel techniques. Post-deposition heating under nitrogen was necessary to transform amorphous gels into vanadium dioxide. Crystallization of films and powders was studied by FTIR, DSC, TGA, and XRD. Gel-derived vanadium dioxide films undergo a reversible semiconductor-to-metal phase transition near 68C, exhibiting characteristic resistive and spectral changes. The electrical resistance decreased by two to three orders of magnitude and the infrared transmission sharply dropped as the material was cycled through this thermally induced phase transition. The sol-gel method was also used to make doped vanadium dioxide films. Films were doped with tungsten and molybdenum ions to effectively lower the temperature at which the transition occurs

Agar/gelatin bilayer gel matrix fabricated by simple thermo-responsive sol-gel transition method.

Science.gov (United States)

Wang, Yifeng; Dong, Meng; Guo, Mengmeng; Wang, Xia; Zhou, Jing; Lei, Jian; Guo, Chuanhang; Qin, Chaoran

2017-08-01

We present a simple and environmentally-friendly method to generate an agar/gelatin bilayer gel matrix for further biomedical applications. In this method, the thermally responsive sol-gel transitions of agar and gelatin combined with the different transition temperatures are exquisitely employed to fabricate the agar/gelatin bilayer gel matrix and achieve separate loading for various materials (e.g., drugs, fluorescent materials, and nanoparticles). Importantly, the resulting bilayer gel matrix provides two different biopolymer environments (a polysaccharide environment vs a protein environment) with a well-defined border, which allows the loaded materials in different layers to retain their original properties (e.g., magnetism and fluorescence) and reduce mutual interference. In addition, the loaded materials in the bilayer gel matrix exhibit an interesting release behavior under the control of thermal stimuli. Consequently, the resulting agar/gelatin bilayer gel matrix is a promising candidate for biomedical applications in drug delivery, controlled release, fluorescence labeling, and bio-imaging. Copyright © 2017 Elsevier B.V. All rights reserved.

Sol-gel materials for optofluidics - process and applications

DEFF Research Database (Denmark)

Mikkelsen, Morten Bo Lindholm

2011-01-01

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...

Controlled release of vancomycin from thin sol-gel films on implant surfaces successfully controls osteomyelitis.

Science.gov (United States)

Adams, Christopher S; Antoci, Valentin; Harrison, Gerald; Patal, Payal; Freeman, Terry A; Shapiro, Irving M; Parvizi, Javad; Hickok, Noreen J; Radin, Shula; Ducheyne, Paul

2009-06-01

Peri-prosthetic infection remains a serious complication of joint replacement surgery. Herein, we demonstrate that a vancomycin-containing sol-gel film on Ti alloy rods can successfully treat bacterial infections in an animal model. The vancomycin-containing sol-gel films exhibited predictable release kinetics, while significantly inhibiting S. aureus adhesion. When evaluated in a rat osteomyelitis model, microbiological analysis indicated that the vancomycin-containing sol-gel film caused a profound decrease in S. aureus number. Radiologically, while the control side showed extensive bone degradation, including abscesses and an extensive periosteal reaction, rods coated with the vancomycin-containing sol-gel film resulted in minimal signs of infection. MicroCT analysis confirmed the radiological results, while demonstrating that the vancomycin-containing sol-gel film significantly protected dense bone from resorption and minimized remodeling. These results clearly demonstrate that this novel thin sol-gel technology can be used for the targeted delivery of antibiotics for the treatment of periprosthetic as well as other bone infections. Copyright 2008 Orthopaedic Research Society

Preparation of oxide glasses from metal alkoxides by sol-gel method

Science.gov (United States)

Kamiya, K.; Yoko, T.; Sakka, S.

1987-01-01

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.

Neutron detector based on lithiated sol-gel glass

CERN Document Server

Wallace, S; Miller, L F; Dai, S

2002-01-01

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.

Sol-Gel Chemistry for Carbon Dots.

Science.gov (United States)

Malfatti, Luca; Innocenzi, Plinio

2018-03-14

Carbon dots are an emerging class of carbon-based nanostructures produced by low-cost raw materials which exhibit a widely-tunable photoluminescence and a high quantum yield. The potential of these nanomaterials as a substitute of semiconductor quantum dots in optoelectronics and biomedicine is very high, however they need a customized chemistry to be integrated in host-guest systems or functionalized in core-shell structures. This review is focused on recent advances of the sol-gel chemistry applied to the C-dots technology. The surface modification, the fine tailoring of the chemical composition and the embedding into a complex nanostructured material are the main targets of combining sol-gel processing with C-dots chemistry. In addition, the synergistic effect of the sol-gel precursor combined with the C-dots contribute to modify the intrinsic chemo-physical properties of the dots, empowering the emission efficiency or enabling the tuning of the photoluminescence over a wide range of the visible spectrum. © 2018 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sol-gel bonding of silicon wafers

International Nuclear Information System (INIS)

Barbe, C.J.; Cassidy, D.J.; Triani, G.; Latella, B.A.; Mitchell, D.R.G.; Finnie, K.S.; Short, K.; Bartlett, J.R.; Woolfrey, J.L.; Collins, G.A.

2005-01-01

Sol-gel bonds have been produced between smooth, clean silicon substrates by spin-coating solutions containing partially hydrolysed silicon alkoxides. The two coated substrates were assembled and the resulting sandwich fired at temperatures ranging from 60 to 600 deg. C. The sol-gel coatings were characterised using attenuated total reflectance Fourier transform infrared spectroscopy, ellipsometry, and atomic force microscopy, while the corresponding bonded specimens were investigated using scanning electron microscopy and cross-sectional transmission electron microscopy. Mechanical properties were characterised using both microindentation and tensile testing. Bonding of silicon wafers has been successfully achieved at temperatures as low as 60 deg. C. At 300 deg. C, the interfacial fracture energy was 1.55 J/m 2 . At 600 deg. C, sol-gel bonding provided superior interfacial fracture energy over classical hydrophilic bonding (3.4 J/m 2 vs. 1.5 J/m 2 ). The increase in the interfacial fracture energy is related to the increase in film density due to the sintering of the sol-gel interface with increasing temperature. The superior interfacial fracture energy obtained by sol-gel bonding at low temperature is due to the formation of an interfacial layer, which chemically bonds the two sol-gel coatings on each wafer. Application of a tensile stress on the resulting bond leads to fracture of the samples at the silicon/sol-gel interface

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

Science.gov (United States)

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

2002-01-01

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.

Investigation of sol-gel transition by rheological methods. Part II. Results and discussion.

Directory of Open Access Journals (Sweden)

KUDRYAVTSEV Pavel Gennadievich

2017-10-01

Full Text Available In this work rheological studies of the gelling process were carried out. We have developed a measuring system for studying the rheology of the gelation process. It consisted of several measuring cells of the Weiler-Rebinder type, system for automatic regulation of the composition of the medium and thermostabilization system. This complex is designed to measure the dependence of the value of the ultimate shear stress as a function of time, from the start of the sol-gel transition to the complete conversion of the sol to the gel. The developed device has a wide range of measured values of critical shear stresses τ0 = (0,05÷50000 Dyne/cm2. Using the developed instrument, it was possible to establish the shape of the initial section of the curve τ0 = f(t and develop a methodology for more accurate determination of gelation time. The developed method proved that the classical method for determining the start time of the sol-gel transition using the point of intersection of the tangent to the linear part of the rheological curve τ0 = f(t, gives significantly distorted results. A new phenomenon has been discovered: the kinetic curves in the coordinates of the Avrami-Erofeev-Bogolyubov equation have an inflection point which separates the kinetic curve into two parts, the initial and the final. It was found that the constant k in the Avrami–Erofeev–Bogolyubov equation does not depend on the temperature and is the same for both the initial and final parts of the kinetic curve. It depends only on the chemical nature of the reacting system. It was found that for the initial section of the kinetic curves, the value of the parameter n in the Avrami-Erofeev-Bogolyubov equation was n = 23,4±2,8 and, unlike the final section of the rheological curve, does not depend on temperature. A large value of this parameter can be interpreted as the average number of directions of growth of a fractal aggregate during its growth. The value of this parameter

Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

Energy Technology Data Exchange (ETDEWEB)

Abdullah, M. A. R., E-mail: ameerridhwan89@gmail.com; Mamat, M. H., E-mail: hafiz-030@yahoo.com; Ismail, A. S., E-mail: kyrin-samaxi@yahoo.com [NANO-ElecTronic Centre (NET), Faculty of Electrical Engineering, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor (Malaysia); Malek, M. F., E-mail: firz-solarzelle@yahoo.com [NANO-SciTech Centre (NST), Institute of Science (IOS), Universiti Teknologi MARA - UiTM, 40450 Shah Alam, Selangor (Malaysia); Alrokayan, Salman A. H., E-mail: dr.salman@alrokayan.com; Khan, Haseeb A., E-mail: khan-haseeb@yahoo.com [Chair of Targeting and Treatment of Cancer Using Nanoparticles, Deanship of Scientific Research, King Saud University (KSU), Riyadh 11451 (Saudi Arabia); Rusop, M., E-mail: rusop@salam.uitm.my [NANO-ElecTronic Centre (NET), Faculty of Electrical Engineering, Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor (Malaysia); NANO-SciTech Centre (NST), Institute of Science (IOS), Universiti Teknologi MARA - UiTM, 40450 Shah Alam, Selangor (Malaysia)

2016-07-06

Preparation of NiO thin films at different annealing temperature by sol-gel method was conducted to synthesize the quality of the surface thin films. The effects of annealing temperature on the surface topology were systematically investigated. Our studies confirmed that the surface roughness of the thin films was increased whenever annealing temperature was increase. NiO thin films morphology structure analysis was confirmed by field emission scanning electron microscope. Surface roughness of the thin films was investigated by atomic force microscopy.

Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

International Nuclear Information System (INIS)

Abdullah, M. A. R.; Mamat, M. H.; Ismail, A. S.; Malek, M. F.; Alrokayan, Salman A. H.; Khan, Haseeb A.; Rusop, M.

2016-01-01

Preparation of NiO thin films at different annealing temperature by sol-gel method was conducted to synthesize the quality of the surface thin films. The effects of annealing temperature on the surface topology were systematically investigated. Our studies confirmed that the surface roughness of the thin films was increased whenever annealing temperature was increase. NiO thin films morphology structure analysis was confirmed by field emission scanning electron microscope. Surface roughness of the thin films was investigated by atomic force microscopy.

Fabrication of mesoporous silica nanoparticles by sol gel method followed various hydrothermal temperature

Science.gov (United States)

Purwaningsih, Hariyati; Pratiwi, Vania Mitha; Purwana, Siti Annisa Bani; Nurdiansyah, Haniffudin; Rahmawati, Yenny; Susanti, Diah

2018-04-01

Rice husk is an agricultural waste that is potentially used as natural silica resources. Natural silica claimed to be safe in handling, cheap and can be generate from cheap resource. In this study mesoporous silica was synthesized using sodium silicate extracted from rice husk ash. This research's aim are to study the optimization of silica extraction from rice husk, characterizing mesoporous silica from sol-gel method and surfactant templating from rice husk and the effect of hydrothermal temperature on mesoporous silica nanoparticle (MSNp) formation. In this research, rice husk was extracted with sol-gel method and was followed by hydrothermal treatment; several of hydrothermal temperatures were 85°C, 100°C, 115°C, 130°C and 145° for 24 hours. X-ray diffraction analysis was identified of α-SiO2 phase and NaCl compound impurities. Scherer's analysis method for crystallite size have resulted 6.27-40.3 nm. FTIR results of silica from extraction and MSNp indicated Si-O-Si bonds on the sample. SEM result showed the morphology of the sample that has spherical shape and smooth surface. TEM result showed particle size ranged between 69,69-84,42 nm. BET showed that the pore size classified as mesoporous with pore diameter size is 19,29 nm.

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

Science.gov (United States)

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

2009-09-01

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.

Sol-gel additive for systems with inorganic binders

International Nuclear Information System (INIS)

Akstinat, M.; Antenen, D.; Suter, W.

1996-01-01

A sol-gel additive for inorganic binder systems and sol-gel process for producing air-placed concrete and mortar by using such sol-gel additives are disclosed. Sol-gel additives for gel-derived inorganic binder systems (for example plaster, cement, lime, special slags, etc.) marked improve the consistency of such binder systems during processing or allow their consistency to be regulated. In addition, these sol-gel additives regulate setting times and substantially improve durability (chemical resistance, reduced permeability) and the mechanical properties of the set binder system. (author)

Sol-Gel Production; Proceedings of the First International Conference on Application and Commercialization of Sol-Gel Processing Held in Saarbruecken, Germany on 24-25 May 1993

National Research Council Canada - National Science Library

Schmidt, Helmut

1998-01-01

...; Sol-Gel Coatings on Large Glass Substrates for Multilayer Interference Systems; A SiO2-ZrO2 Gel Film doped with Organic Pigments Made by the Sol-Gel Method for Contrast Enhancement of Color Picture Tubes...

Sol-gel open tubular ODS columns with reversed electroosmotic flow for capillary electrochromatography.

Science.gov (United States)

Hayes, J D; Malik, A

2001-03-01

Sol-gel chemistry was successfully used for the fabrication of open tubular columns with surface-bonded octadecylsilane (ODS) stationary-phase coating for capillary electrochromatography (OT-CEC). Following column preparations, a series of experiments were performed to investigate the performance of the sol-gel coated ODS columns in OT-CEC. The incorporation of N-octadecyldimethyl[3-(trimethoxysilyl)propyl]ammonium chloride as one of the sol-gel precursors played an important role in the electrochromatographic performance of the prepared columns. This chemical reagent possesses a chromatographically favorable, bonded ODS moiety, in conjunction with three methoxy groups allowing for sol-gel reactivity. In addition, a positively charged nitrogen atom is present in the molecular structure of this reagent and provides a positively charged capillary surface responsible for the reversed electroosmotic flow (EOF) in the columns during CEC operation. Comparative studies involving the EOF within such sol-gel ODS coated and uncoated capillaries were performed using acetonitrile and methanol as the organic modifiers in the mobile phase. The use of a deactivating reagent, phenyldimethylsilane, in the sol-gel solution was evaluated. Efficiency values of over 400,000 theoretical plates per meter were achieved in CEC on a 64 cm x 25 microm i.d. sol-gel ODS open tubular column. Test mixtures of polycyclic aromatic hydrocarbons, benzene derivatives, and aromatic aldehydes and ketones were used to evaluate the CEC performances of both nondeactivated and deactivated open tubular sol-gel columns. The effects of mobile-phase organic modifier contents and pH on EOF in such columns were evaluated. The prepared sol-gel ODS columns are characterized by switchable electroosmotic flow. A pH value of approximately 8.5 was found correspond to the isoelectric point for the prepared sol-gel ODS coatings.

Low Concentration Fe-Doped Alumina Catalysts Using Sol-Gel and Impregnation Methods: The Synthesis, Characterization and Catalytic Performance during the Combustion of Trichloroethylene

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Carolina Solis Maldonado

2014-03-01

Full Text Available The role of iron in two modes of integration into alumina catalysts was studied at 0.39 wt% Fe and tested in trichloroethylene combustion. One modified alumina was synthesized using the sol-gel method with Fe added in situ during hydrolysis; another modification was performed using calcined alumina, prepared using the sol-gel method and impregnated with Fe. Several characterization techniques were used to study the level of Fe modification in the γ-Al2O3 phase formed and to correlate the catalytic properties during trichloroethylene (TCE combustion. The introduction of Fe in situ during the sol-gel process influenced the crystallite size, and three iron species were generated, namely, magnetite, maghemite and hematite. The impregnated Fe-alumina formed hematite and maghemite, which were highly dispersed on the γ-Al2O3 surface. The X-ray photoelectron spectra (XPS, FT-IR and Mössbauer spectroscopy analyses revealed how Fe interacted with the γ-Al2O3 lattice in both catalysts. The impregnated Fe-catalyst showed the best catalytic performance compared to the catalyst that was Fe-doped in situ by the sol-gel method; both had better catalytic activity than pure alumina. This difference in activity was correlated with the accessibility of the reactants to the hematite iron species on the surface. The chlorine poisoning for all three catalysts was less than 1.8%.

Low Concentration Fe-Doped Alumina Catalysts Using Sol-Gel and Impregnation Methods: The Synthesis, Characterization and Catalytic Performance during the Combustion of Trichloroethylene.

Science.gov (United States)

Maldonado, Carolina Solis; De la Rosa, Javier Rivera; Lucio-Ortiz, Carlos J; Hernández-Ramírez, Aracely; Barraza, Felipe F Castillón; Valente, Jaime S

2014-03-12

The role of iron in two modes of integration into alumina catalysts was studied at 0.39 wt% Fe and tested in trichloroethylene combustion. One modified alumina was synthesized using the sol-gel method with Fe added in situ during hydrolysis; another modification was performed using calcined alumina, prepared using the sol-gel method and impregnated with Fe. Several characterization techniques were used to study the level of Fe modification in the γ-Al₂O₃ phase formed and to correlate the catalytic properties during trichloroethylene (TCE) combustion. The introduction of Fe in situ during the sol-gel process influenced the crystallite size, and three iron species were generated, namely, magnetite, maghemite and hematite. The impregnated Fe-alumina formed hematite and maghemite, which were highly dispersed on the γ-Al₂O 3 surface. The X-ray photoelectron spectra (XPS), FT-IR and Mössbauer spectroscopy analyses revealed how Fe interacted with the γ-Al₂O₃ lattice in both catalysts. The impregnated Fe-catalyst showed the best catalytic performance compared to the catalyst that was Fe-doped in situ by the sol-gel method; both had better catalytic activity than pure alumina. This difference in activity was correlated with the accessibility of the reactants to the hematite iron species on the surface. The chlorine poisoning for all three catalysts was less than 1.8%.

Structural and physicochemical properties of nickel manganite NiMn{sub 2}O{sub 4-δ}synthesized by sol-gel and ultra sound assisted methods

Energy Technology Data Exchange (ETDEWEB)

Alburquenque, D. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Metallurgy Department, USACH, Ave Ecuador 3469, Santiago 9170124 (Chile); Troncoso, L.; Denardin, J.C. [Physics Department, USACH, Ave. Ecuador 3493, Santiago 9170124 (Chile); Butera, A. [Atomic Center, CNEA, Ito. Balseiro, Bariloche Rio Negro 84000 (Argentina); Padmasree, K.D. [Cinvestav, U.Saltillo, Monterrey Km 13.5, Saltillo CP 25900 (Mexico); Ortiz, J.; Herrera, F. [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile); Marco, J.F. [Institute of Physical Chemistry “Rocasolano”, CSIC, Serrano 119, Madrid 28006 (Spain); Gautier, J.L., E-mail: juan.gautier@usach.cl [Materials Chemistry Department, USACH, Ave L.B.O' Higgins 3363, Santiago 9170022 (Chile)

2016-07-05

In this work we present the structural, magnetic and surface characterization of the ceramic nickel manganite oxide NiMn{sub 2}O{sub 4-δ} synthesized by two methods: sol-gel and ultrasound-assisted sol-gel using nitrate salts as precursors. We have characterized the non-stoichiometric samples NiMn{sub 2}O{sub 4-δ} using different physicochemical analyses. X-ray diffraction and Rietveld refinement of the X-ray data indicated that the samples crystallize in the Fd3m space group characteristic of cubic spinel-related oxides. The specific surface area of the oxides was 1.3 m{sup 2}/g (SG) and 16.3 m{sup 2}/g (UASG). SEM results showed particle agglomerates of 1.05 μm (SG) and 0.85 μm (UASG). Temperature dependence magnetization measurements were performed and a ferrimagnetic transition was identified at 103 K and 105 K depending on the preparation method (SG and UASG, respectively). The observed Curie constant was found to vary from 7.4 to 7.7 cm{sup 3} K mol{sup −1} and hysteretic magnetization vs. applied field curves at different temperatures were obtained. XPS studies of these oxides reveal the presence of Ni{sup 2+}, Mn{sup 2+}, Mn{sup 3+} and Mn{sup 4+} ions at the surface. A probable ionic distribution as a function of the synthesis method is proposed. - Highlights: • Nickel manganite was synthesized by sol gel synthesis and a novel ultrasound-assisted sol gel method. . • Bulk and surface cation distributions are proposed. • Physicochemical properties, including magnetic and surface area measurements, were studied for both types of samples.

Enhancement of the electrochemical performance in LiFePO4 cathode materials synthesized by using the sol-gel method

Directory of Open Access Journals (Sweden)

Kyong-Soo Hong

2010-11-01

Full Text Available LiFePO4 powders were synthesized by using the sol-gel and the solid-state reaction methods. The chemical states of Fe ions were studied by using XPS, and their electrochemical properties according to the oxidation states of Fe ions were compared. The average oxidation state of Fe ions in LiFePO4 powders synthesized by using the solid-state reaction method was found to be Fe3+, on the other hand, that of Fe ions synthesized by using the sol-gel method was found to be Fe2+. The obtained discharge capacities were 50 mAh/g and 120 mAh/g at a rate 0.1 C in LiFePO4 synthesized by using the solid-state reaction and sol-gel methods, respectively. Relatively a good cycling stability was observed in sol-gel prepared powder.

Neutron detector using sol-gel absorber

Science.gov (United States)

Hiller, John M.; Wallace, Steven A.; Dai, Sheng

1999-01-01

An neutron detector composed of fissionable material having ions of lithium, uranium, thorium, plutonium, or neptunium, contained within a glass film fabricated using a sol-gel method combined with a particle detector is disclosed. When the glass film is bombarded with neutrons, the fissionable material emits fission particles and electrons. Prompt emitting activated elements yielding a high energy electron contained within a sol-gel glass film in combination with a particle detector is also disclosed. The emissions resulting from neutron bombardment can then be detected using standard UV and particle detection methods well known in the art, such as microchannel plates, channeltrons, and silicon avalanche photodiodes.

A Sol-gel Integrated Dual-readout Microarray Platform for Quantification and Identification of Prostate-specific Antigen.

Science.gov (United States)

Lee, SangWook; Lee, Jong Hyun; Kwon, Hyuck Gi; Laurell, Thomas; Jeong, Ok Chan; Kim, Soyoun

2018-01-01

Here, we report a sol-gel integrated affinity microarray for on-chip matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) that enables capture and identification of prostate?specific antigen (PSA) in samples. An anti-PSA antibody (H117) was mixed with a sol?gel, and the mixture was spotted onto a porous silicon (pSi) surface without additional surface modifications. The antibody easily penetrates the sol-gel macropore fluidic network structure, making possible high affinities. To assess the capture affinity of the platform, we performed a direct assay using fluorescein isothiocyanate-labeled PSA. Pure PSA was subjected to on-chip MALDI-TOF-MS analysis, yielding three clear mass peptide peaks (m/z = 1272, 1407, and 1872). The sol-gel microarray platform enables dual readout of PSA both fluorometric and MALDI-TOF MS analysis in biological samples. Here we report a useful method for a means for discovery of biomarkers in complex body fluids.

Nanostructured Mesoporous Titanium Dioxide Thin Film Prepared by Sol-Gel Method for Dye-Sensitized Solar Cell

Directory of Open Access Journals (Sweden)

Yu-Chang Liu

2011-01-01

Full Text Available Titanium dioxide (TiO2 paste was prepared by sol-gel and hydrothermal method with various precursors. Nanostructured mesoporous TiO2 thin-film back electrode was fabricated from the nanoparticle colloidal paste, and its performance was compared with that made of commercial P25 TiO2. The best performance was demonstrated by the DSSC having a 16 μm-thick TTIP-TiO2 back electrode, which gave a solar energy conversion efficiency of 6.03%. The ability of stong adhesion on ITO conducting glass substrate and the high surface area are considered important characteristics of TiO2 thin film. The results show that a thin film with good adhesion can be made from the prepared colloidal paste as a result of alleviating the possibility of electron transfer loss. One can control the colloidal particle size from sol-gel method. Therefore, by optimizing the preparation conditions, TiO2 paste with nanoparticle and narrow diameter distribution was obtained.

Fabrication of YBa2Cu3O7-δ superconducting fibers by the sol-gel method

International Nuclear Information System (INIS)

Umeda, Tetsu; Kozuka, Hiromitsu; Sakka, Sumio

1988-01-01

High-T c superconducting oxide fibers were fabricated by the sol-gel method. An aqueous solution of metal acetates was concentrated to form a viscous sol, from which gel fibers were spun. The gel fibers, 5 to 1,000 μm in diameter, were converted to ceramic fibers by heating to 900 degree C. The fired fibers (T c (onset) of 94 K and T c (end) of 62.2 K) were rough and had porous microstructures

Dip coating of sol-gels

Science.gov (United States)

Schunk, P. R.; Hurd, A. J.; Brinker, C. J.

Dip coating is the primary means of depositing sol-gel films for precision optical coatings. Sols are typically multicomponent systems consisting of an inorganic phase dispersed in a solvent mixture, with each component differing in volatility and surface tension. This, together with slow coating speeds (less than 1cm/s), makes analysis of the coating process complicated; unlike most high-speed coating methods, solvent evaporation, evolving rheology, and surface tension gradients alter significantly the fluid mechanics of the deposition stage. These phenomena were studied with computer-aided predictions of the flow and species transport fields. The underlying theory involves mass, momentum, and species transport on a domain of unknown shape, with models and constitutive equations for vapor-liquid equilibria and surface tension. Due accounting is made for the unknown position of the free surface, which locates according to the capillary hydrodynamic forces and solvent loss by evaporation. Predictions of the effects of mass transfer, hydrodynamics, and surface tension gradients on final film thickness are compared with ellipsometry measurements of film thickness on a laboratory pilot coater. Although quantitative agreement is still lacking, both experiment and theory reveal that the film profile near the drying line takes on a parabolic shape.

Functional coatings: the sol-gel approach

International Nuclear Information System (INIS)

Belleville, Ph.

2010-01-01

CEA's sol-gel laboratory is specialized in the development of innovative sol-gel optical coatings and has extended its application field to membrane materials and coatings for energy conversion, to electric coatings for microelectronics devices and to thin films for gas sensing. This article describes, by way of examples, the laboratory's research on sol-gel functional coatings, including nano-material synthesis, organic-inorganic hybrid-based solution preparation as well as deposition process development and prototyping. (author)

Hybrid sol-gel optical materials

Science.gov (United States)

Zeigler, John M.

1992-01-01

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.

Thermal properties and water repellency of cotton fabric prepared through sol-gel method

Directory of Open Access Journals (Sweden)

Gu Jia-Li

2016-01-01

Full Text Available Cotton fabrics were treated by one-step sol-gel method. The pure silica hydrosol and phosphorus-doped hydrosol were prepared with the addition of a hydrophobic hexadecyltrimethoxysilane to decrease the surface energy of cotton fabric. The thermal properties and water repellency of treated cotton fabric were characterized by thermo-gravimetric analysis, micro combustion, limiting oxygen index, and contact angle measurement. The results showed that cotton fabric treated by phosphorus-doped silica hydrosol had excellent flame retardance, and the water repellence was apparently improved with the addition of hexadecyltrimethoxysilane.

Synthesis of Silica Nanoparticles by Sol-Gel: Size-Dependent Properties, Surface Modification, and Applications in Silica-Polymer Nano composites-A Review

International Nuclear Information System (INIS)

Ismail, A.R.; Vejayakumaran, P.

2012-01-01

Application of silica nanoparticles as fillers in the preparation of nano composite of polymers has drawn much attention, due to the increased demand for new materials with improved thermal, mechanical, physical, and chemical properties. Recent developments in the synthesis of monodispersed, narrow-size distribution of nanoparticles by sol-gel method provide significant boost to development of silica-polymer nano composites. This paper is written by emphasizing on the synthesis of silica nanoparticles, characterization on size-dependent properties, and surface modification for the preparation of homogeneous nano composites, generally by sol-gel technique. The effect of nano silica on the properties of various types of silica-polymer composites is also summarized.

Fabrication of optical chemical ammonia sensors using anodized alumina supports and sol-gel method.

Science.gov (United States)

Markovics, Akos; Kovács, Barna

2013-05-15

In this comparative study, the fabrication and the sensing properties of various reflectometric optical ammonia gas sensors are described. In the first set of experiments the role of the support material was investigated on four different sensor membranes. Two of them were prepared by the adsorption of bromocresol green indicator on anodized aluminum plates. The applied anodizing voltages were 12 V and 24 V, which resulted in different dynamic ranges and response times for gaseous ammonia. The sol-gel method was used for the preparation of the other batch of sensors. These layers were coated on anodized aluminum plates (24 V) and on standard microscope cover glasses. In spite of the identical sensing chemistry, slightly different response times were measured merely because of the aluminum surface porosity. Gas molecules can remain entrapped in the pores, which results in delayed recovery time. On the other hand, the porous oxide film provides excellent adhesion, making the anodized aluminum an attractive support for the sol-gel layer. Copyright © 2013 Elsevier B.V. All rights reserved.

Sol-gel-state of hydrated zirconium dioxide

International Nuclear Information System (INIS)

Karakchiev, L.G.; Lyakhov, N.Z.

1995-01-01

The change in viscosity and density of a system in the course of sol-gel-xerogel has been traced. The size and molecular mass of particles in sol have been determined. Initial sol is practically a monodisperse system. Gel is a spatial net of similar particles. Reversible character of sol-gel transition with a change in water content in the system suggests instability of the bond between the particles in the structure of the solid state body formed. 11 refs.; 4 figs

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

Science.gov (United States)

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

2016-03-04

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.

Fabrication of superhydrophobic sol-gel composite films using hydrophobically modified colloidal zinc hydroxide.

Science.gov (United States)

Lakshmi, R V; Basu, Bharathibai J

2009-11-15

A superhydrophobic sol-gel composite film was fabricated by incorporating hydrophobically modified colloidal zinc hydroxide (CZH) in sol-gel matrix. CZH was prepared by controlled precipitation and modified by treatment with stearic acid. The concentration of stearic acid and stirring time were optimized to obtain modified CZH with very high water contact angle (WCA) of 165 degrees and sliding angle (SA)superhydrophobic surfaces. FTIR spectrum also confirmed the presence of zinc stearate in the composite film. The method is simple and cost-effective and does not involve any expensive chemicals or equipments.

Preparation, microstructure and properties of yttrium aluminum garnet fibers prepared by sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Li Chengshun [Key Laboratory for Liquid Structure and Heredity of Materials of Ministry of Education, Shandong University, Jinan 250061 (China); Zhang Yujun [Key Laboratory for Liquid Structure and Heredity of Materials of Ministry of Education, Shandong University, Jinan 250061 (China)], E-mail: yujunzhangcn@sdu.edu.cn; Gong Hongyu; Zhang Jingde; Nie Lifang [Key Laboratory for Liquid Structure and Heredity of Materials of Ministry of Education, Shandong University, Jinan 250061 (China)

2009-01-15

Yttrium aluminum garnet (YAG) fiber was prepared by sol-gel method using water as the solvent. The spinnable YAG sol was synthesized using Al powder, Y(CH{sub 3}COOH){sub 3}.4H{sub 2}O and HCl as precursors, polyethylene oxide as viscosity adjusting agent. Gel fibers with diameter of 5-10 {mu}m were prepared from the YAG sol by using centrifugal spinning technique. YAG crystalline fibers were obtained by drying gel fibers and heat-treating at selected temperature. TG/DTA analysis showed an exotherm at 906 deg. C attributed to formation of YAG phase and weight loss of 45% at 1000 deg. C. XRD and FT-IR analysis showed that phase-pure YAG can be formed at 900 deg. C, and no other intermediate was observed. The grain size of YAG fibers increased from 25 to 220 nm and tensile strength decreased rapidly from 970 to 380 MPa when the sintering temperature increased from 900 to 1550 deg. C.

Hydrogen permeation through sol-gel-coated iron during galvanostatic charging

International Nuclear Information System (INIS)

Zakorchemna, I.; Carmona, N.; Zakroczymski, T.

2008-01-01

One-layer sol-gel silica-zirconia and two-layer silica-zirconia and zirconia coatings were deposited on one side of iron membranes by spin-coating, densified in air and annealed up to 800 deg. C in vacuum. Hydrogen permeation through the membranes, coated and uncoated, polarised cathodically under galvanostatic control in 0.1 M NaOH solution was studied using the electrochemical permeation technique. During the initial period, the effect of the sol-gel coatings was insignificant. However, the coatings quite efficiently prevented the iron surface become more active to hydrogen entry during a long-lasting cathodic polarisation. In addition, the electrochemical-corrosion behaviour of the coated iron and the effect of the sol-gel coatings on the effective diffusivity of hydrogen in the coated membranes were studied. On the basis of the polarisation curves and the hydrogen permeation data it was proved that the sol-gel coatings blocked the iron surface for the hydrogen evolution reaction and, consequently, for the hydrogen entry into iron. The effective coating coverage was determined by comparison of the hydrogen fluxes permeating the coated and uncoated membranes. Finally the real concentration of hydrogen beneath the uncoated iron sites and the amount of hydrogen stored in a membrane were evaluated

Dissolution testing of intermediary products in uranium dioxide production by the sol-gel method

International Nuclear Information System (INIS)

Melichar, F.; Landspersky, H.; Urbanek, V.

1979-01-01

A method was developed of dissolving polyuranates and uranium dioxides in sulphuric acid and in carbonate solutions for testing intermediate products in the sol-gel process preparation of uranium dioxide. A detailed granulometric analysis of spherical particle dispersion was included as part of the tests. Two different production methods were used for the two types of studied materials. The test results show that the test method is suitable for determining temperature sensitivity of the materials to dissolution reaction. The geometrical distribution of impurities in the spherical particles can be determined from the dissolution kinetics. The method allows the determination of the effect of carbon from impurities on the process of uranium dioxide leaching and is thus applicable for testing materials prepared by the sol-gel method. (Z.M.)

Sol-gel process for thermal reactor fuel fabrication

International Nuclear Information System (INIS)

Mukerjee, S.K.

2008-01-01

Full text: Sol-gel processes have revolutionized conventional ceramic technology by providing extremely fine and uniform powders for the fabrication of ceramics. The use of this technology for nuclear fuel fabrication has also been explored in many countries. Unlike the conventional sol-gel process, sol-gel process for nuclear fuels tries to eliminate the preparation of powders in view of the toxic nature of the powders particularly those of plutonium and 233 U. The elimination of powder handling thus makes this process more readily amenable for use in glove boxes or for remote handling. In this process, the first step is the preparation of microspheres of the fuel material from a solution which is then followed by vibro-compaction of these microspheres of different sizes to obtain the required smear density of fuel inside a pin. The maximum achievable packing density of 92 % makes it suitable for fast reactors only. With a view to extend the applicability of sol-gel process for thermal reactor fuel fabrication the concept of converting the gel microspheres derived from sol-gel process, to the pellets, has been under investigation for several years. The unique feature of this process is that it combines the advantages of sol-gel process for the preparation of fuel oxide gel microspheres of reproducible quality with proven irradiation behavior of the pellet fuel. One of the important pre-requisite for the success of this process is the preparation of soft oxide gel microspheres suitable for conversion to dense pellets free from berry structure. Studies on the internal gelation process, one of the many variants of sol-gel process, for obtaining soft oxide gel microspheres suitable for gel pelletisation is now under investigation at BARC. Some of the recent findings related to Sol-Gel Microsphere Pelletisation (SGMP) in urania-plutonia and thoria-urania systems will be presented

Analysis on the factors affecting the preparation of TIO2-ADUN composite sol by sol-gel method

International Nuclear Information System (INIS)

Wang Hui; Yin Rongcai; Liu Jinhong

2010-01-01

With C 2 H 2 O 5 and water as solvent and TBT as precursor and HNO 3 as the activator and valorize, the process for preparing TiO 2 -ADUN composite Sol method was studied. The influence of different reaction conditions on Sol-Gel time was analyzed in this study. The optimal reaction condition are: reaction temperature 20-25 degree C; pH value of reaction mixture 2-5; HNO 3 value of reaction mixture 0.3-0.5 ml; molar rations of alcohol to TBT 10, of water to TBT 2-3, respectively. A concentrated ADUN solution with Ti Sol , urea, water as additive is dispersed into uniform which are prepared by external mlii. (authors)

Synthesis of phthalocyanine doped sol-gel materials

Science.gov (United States)

Dunn, Bruce

1993-01-01

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

Separation of oligopeptides, nucleobases, nucleosides and nucleotides using capillary electrophoresis/electrochromatography with sol-gel modified inner capillary wall.

Science.gov (United States)

Svobodová, Jana; Kofroňová, Olga; Benada, Oldřich; Král, Vladimír; Mikšík, Ivan

2017-09-29

The aim of this article is to study the modification of an inner capillary wall with sol-gel coating (pure silica sol-gel or silica sol-gel containing porphyrin-brucine conjugate) and determine its influence on the separation process using capillary electrophoresis/electrochromatography method. After modification of the inner capillary surface the separation of analytes was performed using two different phosphate buffers (pH 2.5 and 9.0) and finally the changes in electrophoretic mobilities of various samples were calculated. To confirm that the modification of the inner capillary surface was successful, the parts of the inner surfaces of capillaries were observed using scanning electron microscopy. The analytes used as testing samples were oligopeptides, nucleosides, nucleobases and finally nucleotides. Copyright © 2017 Elsevier B.V. All rights reserved.

Silica-Based Sol-Gel Coating on Magnesium Alloy with Green Inhibitors

Directory of Open Access Journals (Sweden)

Vinod Upadhyay

2017-06-01

Full Text Available In this work, the performances of several natural organic inhibitors were investigated in a sol-gel system (applied on the magnesium alloy Mg AZ31B substrate. The inhibitors were quinaldic acid (QDA, betaine (BET, dopamine hydrochloride (DOP, and diazolidinyl urea (DZU. Thin, uniform, and defect-free sol-gel coatings were prepared with and without organic inhibitors, and applied on the Mg AZ31B substrate. SEM and EDX were performed to analyze the coating surface properties, the adhesion to the substrate, and the thickness. Electrochemical measurements, including electrochemical impedance spectroscopy (EIS and anodic potentiodynamic polarization scan (PDS, were performed on the coated samples to characterize the coatings’ protective properties. Also, hydrogen evolution measurement—an easy method to measure magnesium corrosion—was performed in order to characterize the efficiency of coating protection on the magnesium substrate. Moreover, scanning vibrating electrode technique (SVET measurements were performed to examine the efficiency of the coatings loaded with inhibitors in preventing and containing corrosion events in defect areas. From the testing results it was observed that the formulated sol-gel coatings provided a good barrier to the substrate, affording some protection even without the presence of inhibitors. Finally, when the inhibitors’ performances were compared, the QDA-doped sol-gel was able to contain the corrosion event at the defect.

Photocatalytic Activity in CH3CN Related to the Surface Properties of TiO2 Powders Prepared by Sol-Gel Method

Directory of Open Access Journals (Sweden)

Marta Bettoni

2009-01-01

Full Text Available Some TiO2 powders, prepared from titanium(IVtetraisopropoxide by the sol-gel method and thermally treated between 100 and 1000∘C, have been characterized by X-ray powder diffraction and by nitrogen adsorption and desorption at 77 K to calculate the BET-specific surface area, from which the micropore volume and the external surface area can be derived. The photocatalytic activity (ka of the above powders has been evaluated considering the TiO2-sensitized photo-oxidation of 4-methoxybenzyl alcohol in CH3CN as the test reaction. The decrease of ka have been related to the decrease of the BET surface area, the micropore volume, and the external surface area of the TiO2 powders, but a satisfactory linear correlation is observed only for the last superficial parameter.

Influence of silane on the structure of polystyrene prepared by sol-gel coatings via UV curing

Directory of Open Access Journals (Sweden)

Balbay Senay

2017-01-01

Full Text Available Light, heat, oxygen, moisture, ozone, atmospheric pollution and biological effects are the most important effectives wreak to chemical degradation in the polymer structure. In result of chemical degradation on the polymer consist of problems such as discoloration, brittleness, surface cracks, perspiration, crumbling, smell, surface acidity. In this work, it is aimed to improve the problem of the polystyrene (PS material against chemical degradation. For this reason, PS is coated with silica sol-gel hybrid coating. Silica sol-gel was synthesized by using vinyltrimethoxysilane (VTMS as a cross-linker and tetraethylorthosilicate (TEOS as a silica source. Firstly, four different pre-treatment technique (oven, vacuum oven, lyophilizer and freezing was studied to determine the most suitable pre-treatment technique for coating on PS substrate of sol-gel prepared with initial formulation (S1. A freezing technique gave the best results for coating sample. The change of surface colour of coated PS was measured by CIE L*a*b* methods. Secondly, the most suitable curing agent (Irgacure 184, Irgacure 819, Darocur 1173 and TiO2 as crystalline anatase phase was determined to coat the sol-gel on PS. It was determined to the lowest yellowing of PS surface hybrid coated as UV curing of TEOS sol modified by VTMS and TiO2 as photo-initiators. Finally, the chemical and morphological structure of the coated PS samples was determined by FT-IR and SEM instruments, respectively.

Sol-Gel Derived Hafnia Coatings

Science.gov (United States)

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

2002-01-01

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.

Photocatalytic degradation of methylene blue dye by zinc oxide nanoparticles obtained from precipitation and sol-gel methods.

Science.gov (United States)

Balcha, Abebe; Yadav, Om Prakash; Dey, Tania

2016-12-01

Zinc oxide (ZnO) nanoparticles were synthesized by precipitation and sol-gel methods. The aim of this study was to understand how different synthetic methods can affect the photocatalytic activity of ZnO nanoparticles. As-synthesized ZnO nanoparticles were characterized by X-ray diffraction (XRD) and UV-Visible spectroscopic techniques. XRD patterns of ZnO powders synthesized by precipitation and sol-gel methods revealed their hexagonal wurtzite structure with crystallite sizes of 30 and 28 nm, respectively. Their photocatalytic activities were evaluated by photocatalytic degradation of methylene blue, a common water pollutant, under UV radiation. The effects of operational parameters such as photocatalyst load and initial concentration of the dye on photocatalytic degradation of methylene blue were investigated. While the degradation of dye decreased over the studied dye concentration range of 20 to 100 mg/L, an optimum photocatalyst load of 250 mg/L was needed to achieve dye degradation as high as 81 and 92.5 % for ZnO prepared by precipitation and sol-gel methods, respectively. Assuming pseudo first-order reaction kinetics, this corresponded to rate constants of 8.4 × 10 -3 and 12.4 × 10 -3  min -1 , respectively. Hence, sol-gel method is preferred over precipitation method in order to achieve higher photocatalytic activity of ZnO nanostructures. Photocatalytic activity is further augmented by better choice of capping ligand for colloidal stabilization, starch being more effective than polyethylene glycol (PEG).

Sol-gel process for the manufacture of high power switches

Science.gov (United States)

Landingham, Richard L.; Satcher, Jr, Joe; Reibold, Robert

2016-09-27

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.

Formulation and evaluation of antimicrobial activity of Morus alba sol-gel against periodontal pathogens

Directory of Open Access Journals (Sweden)

Shilpa Gunjal

2015-01-01

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.

Sol-gel synthesis of hydroxyapatite

International Nuclear Information System (INIS)

Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P.

2010-01-01

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)

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

Science.gov (United States)

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

2015-01-01

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.

Synthesis and characterization of high surface area nanosilica from rice husk ash by surfactant-free sol-gel method

Czech Academy of Sciences Publication Activity Database

Hassan, A F.; Abdelghny, A.M.; Elhadidy, Hassan; Youssef, A.M.

2014-01-01

Roč. 69, č. 3 (2014), 465-472 ISSN 0928-0707 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0068; GA MŠk(CZ) EE2.3.20.0214 Institutional support: RVO:68081723 Keywords : Nanosilica * Rice husk * Sol-gel method * N-2 adsorption Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 1.532, year: 2014

Superconductive ceramics obtained with sol gel method

International Nuclear Information System (INIS)

Arcangeli, A.; Mosci, A.; Nardi, A.; Vatteroni, R.; Zondini, C.

1988-01-01

Several sol gel routes have been considered, studied and developed to produce large quantities of granulates which can be processed to obtain ceramics having good superconducting characteristics. In the considered process a mixture of commercial nitrates is atomized, at room temperature, in a solution 1:1 of Primene JMT and Benzene and a pale blue gel of the starting elements is suddently formed. The granulates obtained are free flowing, very reactive and well suited for pressing. For their intrinsic characteristics they could be very good precursors for the production of large quantities of superconductive ceramics in different forms. The precipitated gel is dried, calcinated, pressed in the form of cylindrical pellets which are sintered up to 960 degrees C. No griding or different thermal treatments are needed. The sintered material has low electric resistence, shows a clear Meissner effect and has a transition temperature of between 91 and 95 K

Sol-gel applications for ceramic membrane preparation

Science.gov (United States)

Erdem, I.

2017-02-01

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.

Fabrication of carbon microcapsules containing silicon nanoparticles-carbon nanotubes nanocomposite by sol-gel method for anode in lithium ion battery

International Nuclear Information System (INIS)

Bae, Joonwon

2011-01-01

Carbon microcapsules containing silicon nanoparticles (Si NPs)-carbon nanotubes (CNTs) nanocomposite (Si-CNT-C) have been fabricated by a surfactant mediated sol-gel method followed by a carbonization process. Silicon nanoparticles-carbon nanotubes (Si-CNT) nanohybrids were produced by a wet-type beadsmill method. To obtain Si-CNT nanocomposites with spherical morphologies, a silica precursor (tetraethylorthosilicate, TEOS) and polymer (PMMA) mixture was employed as a structure-directing medium. Thus the Si-CNT/Silica-Polymer microspheres were prepared by an acid catalyzed sol-gel method. Then a carbon precursor such as polypyrrole (PPy) was incorporated onto the surfaces of pre-existing Si-CNT/silica-polymer to generate Si-CNT/Silica-Polymer-PPy microspheres. Subsequent thermal treatment of the precursor followed by wet etching of silica produced Si-CNT-C microcapsules. The intermediate silica/polymer must disappear during the carbonization and etching process resulting in the formation of an internal free space. The carbon precursor polymer should transform to carbon shell to encapsulate remaining Si-CNT nanocomposites. Therefore, hollow carbon microcapsules containing Si-CNT nanocomposites could be obtained (Si-CNT-C). The successful fabrication was confirmed by scanning electron microscopy (SEM) and X-ray diffraction (XRD). These final materials were employed for anode performance improvement in lithium ion battery. The cyclic performances of these Si-CNT-C microcapsules were measured with a lithium battery half cell tests. - Graphical Abstract: Carbon microcapsules containing silicon nanoparticles (Si NPs)-carbon nanotubes (CNTs) nanocomposite (Si-CNT-C) have been fabricated by a surfactant mediated sol-gel method. Highlights: → Polymeric microcapsules containing Si-CNT transformed to carbon microcapsules. → Accommodate volume changes of Si NPs during Li ion charge/discharge. → Sizes of microcapsules were controlled by experimental parameters. �

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

Science.gov (United States)

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

2015-01-01

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. PMID:26322304

Production of Monodisperse Cerium Oxide Microspheres with Diameters near 100 µm by Internal Gelation Sol-Gel Methods

Energy Technology Data Exchange (ETDEWEB)

Katalenich, Jeffrey A.; Kitchen, Brian B.; Pierson, Bruce

2018-05-01

Internal gelation sol-gel methods have used a variety of sphere forming methods in the past to produce metal oxide microspheres, but typically with poor control over the size uniformity at diameters near 100 µm. This work describes efforts to make and measure internal gelation, sol-gel microspheres with very uniform diameters in the 100 – 200 µm size range using a two-fluid nozzle. A custom apparatus was used to form aqueous droplets of sol-gel feed solutions in silicone oil and heat them to cause gelation of the spheres. Gelled spheres were washed, dried, and sintered prior to mounting on glass slides for optical imaging and analysis. Microsphere diameters and shape factors were determined as a function of silicone oil flow rate in a two-fluid nozzle and the size of a needle dispensing the aqueous sol-gel solution. Nine batches of microspheres were analyzed and had diameters ranging from 65.5 ± 2.4 µm for the smallest needle and fastest silicone oil flow rate to 211 ± 4.7 µm for the largest needle and slowest silicone oil flow rate. Standard deviations for measured diameters were less than 8% for all samples and most were less than 4%. Microspheres had excellent circularity with measured shape factors of 0.9 – 1. However, processing of optical images was complicated by shadow effects in the photoresist layer on glass slides and by overlapping microspheres. Based on calculated flow parameters, microspheres were produced in a simple dripping mode in the two-fluid nozzle. Using flow rates consistent with a simple dripping mode in a two-fluid nozzle configuration allows for very uniform oxide microspheres to be produced using the internal-gelation sol-gel method.

Sol-Gel Derived, Nanostructured Oxide Lubricant Coatings

National Research Council Canada - National Science Library

Taylor, Douglas

2000-01-01

In this program, we deposited oxide coatings of titanium and nickel by wet-chemical deposition methods, also referred to as sol-gel, which showed excellent tribological properties in previous investigations...

Optical Studies on Sol-Gel Derived Lead Chloride Crystals

OpenAIRE

Rejeena, I; Lillibai, B; Nithyaja, B; Nampoori, P.N V; Radhakrishnan, P

2013-01-01

Optical characterization of lead chloride crystals prepared by sol-gel method is reported. The relevant sol-gel technique is used for the preparation of PbCl2 samples with five different types. In this paper, we report the absorption and fluorescence behaviour of pure, UV& IR irradiated and electric & magnetic field applied lead chloride crystal samples in solution phase at two different concentrations. Optical bandgap and emission studies of these crystals are also done.

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

Science.gov (United States)

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

2015-02-01

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. Copyright © 2014 Elsevier B.V. All rights reserved.

Hydrogen permeation through steel coated with erbium oxide by sol-gel method

International Nuclear Information System (INIS)

Yao Zhenyu; Suzuki, Akihiro; Levchuk, Denis; Chikada, Takumi; Tanaka, Teruya; Muroga, Takeo; Terai, Takayuki

2009-01-01

Er 2 O 3 coating is formed on austenitic stainless steel 316ss by sol-gel method. The results showed good crystallization of coating by baking in high purity flowing-argon at 973 K, and indicated that a little oxygen in baking atmosphere is necessary to crystallization of coating. The best baking temperature could be thought as 973 K, to get good crystallization of coating and avoid strong oxidation of steel substrate. The deuterium permeation test was performed for coated and bare 316ss, to evaluate the property of Er 2 O 3 sol-gel coating as a potential tritium permeation barrier. In this study, the deuterium permeability of coated 316ss is about 1-2 orders of magnitude lower than that of bare 316ss, and is about 2-3 orders of magnitude than the referred data of bare Eurofer97 and F82H martensitic steel.

Optical characterization of Er-implanted ZnO films formed by sol-gel method

International Nuclear Information System (INIS)

Fukudome, T.; Kaminaka, A.; Isshiki, H.; Saito, R.; Yugo, S.; Kimura, T.

2003-01-01

In this paper, we report on the 1.54 μm photoluminescence (PL) of Er-implanted ZnO thin films formed by a sol-gel method on Si substrates. In spite of the polycrystalline structure of the sol-gel ZnO thin films, they showed strong PL emissions due to the near band edge recombination at 375 nm as well as the Er-related luminescence at 1.54 μm. The Er-related luminescence showed no decrease (quench) in the intensity up to the Er concentration of 1.5 x 10 21 cm -3 . The PL intensity of Er-implanted ZnO at 1.54 μm was found to be as strong as Er-doped PS (porous Si) at 20 K, and the intensity reduced to 1/3 at room temperature

Sol-gel-based biosensing applied to medicinal science.

Science.gov (United States)

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

2015-01-01

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.

Urea functionalized surface-bonded sol-gel coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

Science.gov (United States)

Jillani, Shehzada Muhammad Sajid; Alhooshani, Khalid

2018-03-30

Sol-gel urea functionalized-[bis(hydroxyethyl)amine] terminated polydimethylsiloxane coating was developed for capillary microextraction-high performance liquid chromatographic analysis from aqueous samples. A fused silica capillary is coated from the inside with surface bonded coating material and is created through in-situ sol-gel reaction. The urea-functionalized coating was immobilized to the inner surface of the capillary by the condensation reaction of silanol groups of capillary and sol-solution. The characterization of the coating material was successfully done by using X-ray photoelectron spectroscopy, thermogravimetric analysis, field emission scanning electron microscope, and energy dispersive X-ray spectrometer. To make a setup of online capillary microextraction-high performance liquid chromatography, the urea functionalized capillary was installed in the HPLC manual injection port. The analytes of interest were pre-concentrated in the coated sampling loop, desorbed by the mobile phase, chromatographically separated on C-18 column, and analyzed by UV detector. Sol-gel coated capillaries were used for online extraction and high-performance liquid chromatographic analysis of phenols, ketones, aldehydes, and polyaromatic hydrocarbons. This newly developed coating showed excellent extraction for a variety of analytes ranging from highly polar to non-polar in nature. The analysis using sol-gel coating showed excellent overall sensitivity in terms of lower detection limits (S/N = 3) for the analytes (0.10 ng mL -1 -14.29 ng mL -1 ) with acceptable reproducibility that is less than 12.0%RSD (n = 3). Moreover, the capillary to capillary reproducibility of the analysis was also tested by changing the capillary of the same size. This provided excellent%RSD of less than 10.0% (n = 3). Copyright © 2018 Elsevier B.V. All rights reserved.

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

International Nuclear Information System (INIS)

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

2016-01-01

A coating with self-cleaning characteristics has been developed using a TiO_2/SiO_2 hybrid sol-gel, TiO_2 nanoparticles and organosilicate nanoparticles (OSNP). A patented technology of the hybrid sol-gel and OSNP was combined with TiO_2 nanoparticles to create the surface chemistry for self-cleaning. Two synthesis methods have been developed to prepare TiO_2 nanoparticles (NPs), resulting in the enhancement of local paint by the addition of anatase and rutile TiO_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_2 NPs in combination with irradiation show a great enhancement of RhB degradation (1%) wt. with a decrease in contact angle and improved washability.

Synthesis and studies of Y-Ba-Cu-O high temperature superconductor prepared by sol-gel method

International Nuclear Information System (INIS)

Grigoryan, S.G.; Manukyan, A.L.; Hayrapetyan, A.G.; Arzumanyan, A.M.; Rashidyan, L.H.; Mkrtichyan, N.Y.; Mkrtchyan, A.A.; Kurginyan, K.A.; Trozyan, A.H.; Vardanyan, R.S.

2004-01-01

The method of preparation of Y-Ba-Cu-O high temperature superconducting materials by sol-gel processing technique both for powders and thin films are described. All these methods are based on using yttrium alkoxides as precursors, which are not ready available reagents, besides the majority of these methods use copper alkoxides, which show low solubility in organic solvents, moreover they are very sensitive to hydrolysis in air. The new method of preparation of Y-Ba-Cu-O ceramic materials by sol-gel processing technique based on new and convenient precursors stable in air, having high compatibility with each other is offered. Basic scientific and technological issues related to the synthesis of bulk materials, their structure and electrical conductivity are discussed

Nanocrystalline Ni-Zn ferrites prepared by sol-gel method

Czech Academy of Sciences Publication Activity Database

Popovici, M.; Savii, C.; Nižňanský, Daniel; Šubrt, Jan; Boháček, Jaroslav; Becherescu, D.; Caizer, C.; Enache, C.; Ionescu, C.

2003-01-01

Roč. 5, č. 1 (2003), s. 251-256 ISSN 1454-4164 R&D Projects: GA MŠk LN00A028 Institutional research plan: CEZ:AV0Z4032918 Keywords : nanostructures * sol-gel processing * XRD Subject RIV: CA - Inorganic Chemistry Impact factor: 0.996, year: 2003

Sol-gel optical coatings for lasers: Part 1

International Nuclear Information System (INIS)

Floch, H.G.; Belleville, P.F.; Priotton, J.J.

1995-01-01

Many manufacturers and users claim that optical coatings are best prepared by physical vapor deposition technology. Others believe that sol-gel technology is an effective and competitive alternative. This article, the first of three, emphasizes sol-gel thin-film history and relates it to high-power laser technology, chemistry of the sol-gel process, production of optical coatings and deposition techniques. The second and third articles describe the preparation and performance of antireflective and highly reflective sol-gel optical coatings, respectively, that have been developed for the 1.8-MJ/500-TW (351-nm) pulsed neodymium-glass laser. This powerful laser is to be used in France's Inertial Confinement Fusion (ICF) program. It will demonstrate, at the laboratory scale, ignition of deuterium-tritium fusion fuel

Self-Healing Corrosion Protective Sol-Gel Coatings

NARCIS (Netherlands)

Abdolah Zadeh, M.

2016-01-01

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

Screen-printable sol-gel enzyme-containing carbon inks.

Science.gov (United States)

Wang, J; Pamidi, P V; Park, D S

1996-08-01

Enzymes usually cannot withstand the high-temperature curing associated with the thick-film fabrication process and require a separate immobilization step in connection with the production of single-use biosensors. We report on the development of sol-gel-derived enzyme-containing carbon inks that display compatibility with the screen-printing process. Such coupling of sol-gel and thick-film technologies offers a one-step fabrication of disposable enzyme electrodes, as it obviates the need for thermal curing. The enzyme-containing sol-gel carbon ink, prepared by dispersing the biocatalyst, along with the graphite powder and a binder, within the sol-gel precursors, is cured very rapidly (10 min) at low temperature (4 °C). The influence of the ink preparation conditions is explored, and the sensor performance is evaluated in connection with the incorporation of glucose oxidase or horseradish peroxidase. The resulting strips are stable for at least 3 months. Such sol-gel-derived carbon inks should serve as hosts for other heat-sensitive biomaterials in connection with the microfabrication of various thick-film biosensors.

Preparation and Optoelectrical Properties of p-CuO/n-Si Heterojunction by a Simple Sol-Gel Method

Science.gov (United States)

He, Bo; Xu, Jing; Ning, Huanpo; Zhao, Lei; Xing, Huaizhong; Chang, Chien-Cheng; Qin, Yuming; Zhang, Lei

The Cuprous oxide (CuO) thin film was prepared on texturized Si wafer by a simple sol-gel method to fabricate p-CuO/n-Si heterojunction photoelectric device. The novel sol-gel method is very cheap and convenient. The structural, optical and electrical properties of the CuO film were studied by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), X-ray photoelectron spectroscopy (XPS), UV-Vis spectrophotometer and Hall effect measurement. A good nonlinear rectifying behavior is obtained for the p-CuO/n-Si heterojunction. Under reverse bias, good photoelectric behavior is obtained.

Low-Temperature Sol-Gel Synthesis of Nitrogen-Doped Anatase/Brookite Biphasic Nanoparticles with High Surface Area and Visible-Light Performance

Directory of Open Access Journals (Sweden)

Liang Jiang

2017-12-01

Full Text Available Nitrogen doping in combination with the brookite phase or a mixture of TiO2 polymorphs nanomaterials can enhance photocatalytic activity under visible light. Generally, nitrogen-dopedanatase/brookite mixed phases TiO2 nanoparticles obtained by hydrothermal or solvothermal method need to be at high temperature and with long time heating treatment. Furthermore, the surface areas of them are low (<125 m2/g. There is hardly a report on the simple and direct preparation of N-doped anatase/brookite mixed phase TiO2 nanostructures using sol-gel method at low heating temperature. In this paper, the nitrogen-doped anatase/brookite biphasic nanoparticles with large surface area (240 m2/g were successfully prepared using sol-gel method at low temperature (165 °C, and with short heating time (4 h under autogenous pressure. The obtained sample without subsequent annealing at elevated temperatures showed enhanced photocatalytic efficiency for the degradation of methyl orange (MO with 4.2-, 9.6-, and 7.5-fold visible light activities compared to P25 and the amorphous samples heated in muffle furnace with air or in tube furnace with a flow of nitrogen at 165 °C, respectively. This result was attributed to the synergistic effects of nitrogen doping, mixed crystalline phases, and high surface area.

Effect of cobalt sources on properties of co-b catalysts synthesized by sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Figen, Aysel Kantürk; Co ú kuner, Bilge; Özdemir, Özgül Dere [Department of Chemical Engineering, Yildiz Technical University Istanbul (Turkey); Burçin Pi ú kin, Mehmet [Department of Bioengineering, Y Õ ld Õ z Technical University, Istanbul (Turkey)

2013-07-01

In this studying, Co-B catalysts were prepared by sol-gel method via kinds of cobalt source for clarifying the effect of these for characteristic properties of Co-B catalysts. Co sources, cobalt(II)chloride (CoCl{sub 2} .6H{sub 2}O), cobalt(II)sulfate (CoSO{sub 4} .7H{sub 2}O) and cobalt(II)nitrate (Co(NO{sub 3}){sub 2} .6H{sub 2}O), were used as a metal source with boron oxide (B{sub 2}O{sub 3} ) while citric acid (C{sub 6}H{sub 8}O{sub 7} ) used as organic ligand to forming sol-gel structure. The crystalline structures of Co-B catalysts were determined by X-ray diffraction. The N{sub 2} sorption technique was used for analyzing catalysts surface area. The variety of Co-B catalysts morphological properties were investigated via scanning electron microscope. By the effect of cobalt sources the Co-B catalyst’s properties were altered that clarified from analysis results. The amorphous Co-B catalyst produced from CoCl{sub 2}.6H{sub 2} O as metal source had the largest porous surface area with 122.7 m 2 .g -1 . Investigation of hydrolysis were performed under variety of temperatures (22, 40 and 60 o C), NaOH concentrations (1-15 wt. %) and NaBH 4 /Co-B catalyst ratio (2-40 wt./wt.) ratios in order to investigate the activation of Co-B catalyst. The maximum hydrogen generation rate 0.84L H 2 .min -1 .g -1 was obtained under 40 °C, 10 wt. % NaOH and 9.52wt./wt. NaBH{sub 4}/Co-B catalyst ratio. Yet the kinetic investigations, the reaction order was found that zero order with 0.9954 coefficient of correlation and 51.83 kJ/mol activation energy. Key words: Sol-gel, Co-B Catalyst, Boron.

Persistent superhydrophilicity of sol-gel derived nanoporous silica thin films

International Nuclear Information System (INIS)

Ganjoo, S; Azimirad, R; Akhavan, O; Moshfegh, A Z

2009-01-01

In this investigation, sol-gel synthesized nanoporous silica thin films, annealed at different temperatures, with long time superhydrophilic property have been studied. Two kinds of sol-gel silica thin films were fabricated by dip-coating of glass substrates in two different solutions; with low and high water. The transparent coated films were dried at 100 deg. C and then annealed in a temperature range of 200-500 deg. C. The average water contact angle of the silica films prepared with low water content and annealed at 300 deg. C measured about 5 deg. for a long time (6 months) without any UV irradiation. Instead, adding water into the sol resulted in silica films with an average water contact angle greater than 60 deg. Atomic force microscopic analysis revealed that the silica films prepared with low water had a rough surface (∼30 nm), while the films prepared with high water had a smoother surface (∼2 nm). Using x-ray photoelectron spectroscopy, we have shown that with a decrease in the surface water on the film, its hydrophilicity increases logarithmically.

Characterizations of maghemite thin films prepared by a sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Lau, L. N., E-mail: lau7798@gmail.com; Ibrahim, N. B., E-mail: baayah@ukm.edu.my [School of Applied Physics, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor. Malaysia (Malaysia)

2015-09-25

Iron is one of the abundant elements of Mother Nature and its compound, iron oxide is an interesting material to study since its discovery in the form of magnetite. It can exist in many phases such as hematite and maghemite, this unique nature has put it as a potential candidate in various applications. The aim of this work is to study the influence of different precursor concentrations on the microstructural and magnetic properties of iron oxide thin film. All samples were prepared via the sol-gel method followed by a spin coating technique on quartz substrates. Iron oxide films were confirmed as maghemite phase from X-ray diffraction patterns. The film morphology was examined by a field emission scanning electron microscope and it showed non-systematic value of average grain size and film thickness throughout the study. Hysteresis loop further confirmed that maghemite is a magnetic material when it was characterized by a vibrating sample magnetometer. The coercivity did not show any correlation with molarity. Nevertheless, it increased as the precursor concentration of the film increased due to the domain behaviour. In conclusion, maghemite thin films were successfully synthesized by the sol-gel method with different precursor concentrations in this work.

Silica Sol-Gel Entrapment of the Enzyme Chloro peroxidase

International Nuclear Information System (INIS)

Le, T.; Chan, S.; Ebaid, B.; Sommerhalter, M.

2015-01-01

The enzyme chloro peroxidase (CPO) was immobilized in silica sol-gel beads prepared from tetramethoxysilane. The average pore diameter of the silica host structure (∼3 nm) was smaller than the globular CPO diameter (∼6 nm) and the enzyme remained entrapped after sol-gel maturation. The catalytic performance of the entrapped enzyme was assessed via the pyrogallol peroxidation reaction. Sol-gel beads loaded with 4 μg CPO per mL sol solution reached 9-12% relative activity compared to free CPO in solution. Enzyme kinetic analysis revealed a decrease in K_cat but no changes in K_M or K_I . Product release or enzyme damage might thus limit catalytic performance. Yet circular dichroism and visible absorption spectra of transparent CPO sol-gel sheets did not indicate enzyme damage. Activity decline due to methanol exposure was shown to be reversible in solution. To improve catalytic performance the sol-gel protocol was modified. The incorporation of 5, 20, or 40% methyltrimethoxysilane resulted in more brittle sol-gel beads but the catalytic performance increased to 14% relative to free CPO in solution. The use of more acidic casting buffers (ph 4.5 or 5.5 instead of 6.5) resulted in a more porous silica host reaching up to 18% relative activity

Radiation hardening in sol-gel derived Er3+-doped silica glasses

International Nuclear Information System (INIS)

Hari Babu, B.; León Pichel, Mónica; Ollier, Nadège; El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed; Poumellec, Bertrand; Lancry, Matthieu; Ibarra, Angel

2015-01-01

The aim of the present paper is to report the effect of radiation on the Er 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 3+ -doped sol-gel silica is found to increase with erbium content. Electron paramagnetic resonance studies reveal the presence of E′ 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 3+ to Er 2+ ions. This process occurs in association with the formation of aluminum oxygen hole centers and different intrinsic point defects

Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

Science.gov (United States)

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

2010-01-01

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…

Patterned transparent zinc oxide films produced by sol-gel embossing

Energy Technology Data Exchange (ETDEWEB)

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.

2008-08-15

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.)

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

Energy Technology Data Exchange (ETDEWEB)

Catauro, M., E-mail: michelina.catauro@unina2.it [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)

2016-08-01

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.

Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process.

Science.gov (United States)

Li, Fa-Liang; Zhang, Hai-Jun

2017-08-25

The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined.

Analyses of laser and furnace treated sol-gel coatings

NARCIS (Netherlands)

De Hosson, JT; De Haas, M; Sudarshan, TS; Jeandin, M; Khor, KA

1998-01-01

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.

Characterization of selenium doped silica glasses synthesized by sol-gel method

International Nuclear Information System (INIS)

Kobayashi, R.A.; Toffoli, S.M.

2012-01-01

Selenium is a rare element in nature. It is used in the food, pharmaceutical, and glass industries. In commercial glasses, selenium is the element responsible for most of the pink or light red color, but its effect is primarily dependent on the oxidation state of the element in the glassy matrix. Besides, selenium is highly volatile, and as high as 80 wt% may be lost in the furnace during the industrial glass elaboration. The sol– gel method yields synthesized materials of high purity and homogeneity, and uses low processing temperatures. Samples of silica glass were obtained by sol-gel method, incorporating precursors of selenium, with the main objective of reducing selenium losses during its heating. The results of optical absorption, XRD and thermal analysis (TGA, DSC) of the glasses are presented and discussed. (author)

SOL-GEL SILICA-BASED Ag–Ca–P COATINGS WITH AGRESSIVE PRETREATMENT OF TITANIUM SUBSTRATE

Directory of Open Access Journals (Sweden)

ELENA BORSHCHEVA

2011-12-01

Full Text Available 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 dip-coating process the samples were dried and fired. The adhesion of fired coatings was measured by tape test according to ASTM procedure and the bioactivity of the coatings was tested using in vitro test. The surfaces of the samples after firing, tape test and in vitro test were observed with the optical and electron microscopes. The firing results showed that silica-silver coatings did not change, brushite sol-gel coatings have cracked and the monetite sol-gel coatings have cracked also, but less than brushite ones. In spite of coating´s crackings, the square’s frames made on the surfaces were without any breakdowns after tape tests and the adhesion of all coatings was very good, classified by the highest grade 5. The results of in vitro tests showed that all coatings interacted with simulated body fluid (SBF. After exposition in SBF the new layer formed on substrates. In case of 7 days aged coatings containing brushite the new layer was uniform and compact. In case of 7 days aged coatings containing monetite the new layer was formed by crystals aggregated tightly together. The monetite and brushite coatings prepared from 14 days aged sol were the same as previous ones, but they were thicker. X-ray analyses after in vitro test confirmed dellaite, titanate and hydroxyapatite phases.

Making MgO/SiO2 Glasses By The Sol-Gel Process

Science.gov (United States)

Bansal, Narottam P.

1989-01-01

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.

Electrical stability of Al-doped ZnO transparent electrode prepared by sol-gel method

International Nuclear Information System (INIS)

Tabassum, Samia; Yamasue, Eiji; Okumura, Hideyuki; Ishihara, Keiichi N.

2016-01-01

Highlights: • Al-doped ZnO thin film was deposited by sol-gel method in different annealing temperature and duration. • We examined the environmental stability in ambient and damp heat condition. • We investigated chemical state of thin film. • Better stability was observed in the film annealed at high temperature (600 °C) along with longer duration (120 min). • An ultrathin aluminum oxide layer formation was predicted by XPS measurement which protects further oxidation and improves stability. - Abstract: Al-doped zinc oxide (AZO) thin films have been considered as a promising alternative to tin doped indium oxide (ITO), which is currently used in various optoelectronic applications. However, the environmental stability of AZO film is not satisfactory, in that the resistivity is significantly increases in air. Here, we investigate the resistivity stability of AZO thin films prepared by sol-gel method using various annealing temperatures and durations. The degradation of resistivity property was observed for AZO films stored in ambient or damp heat environment, where the degradation rate was influenced by annealing temperature. A significant improvement of electrical stability was attained in AZO films that were prepared at high annealing temperature. The films, which showed the highest and the lowest increasing rate of resistivity, were further characterized in detail to shed light on the possible mechanisms explaining the improved stability through crystallinity, surface morphology and elemental state of the thin film.

Electrical stability of Al-doped ZnO transparent electrode prepared by sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Tabassum, Samia, E-mail: shawon14@gmail.com; Yamasue, Eiji; Okumura, Hideyuki; Ishihara, Keiichi N.

2016-07-30

Highlights: • Al-doped ZnO thin film was deposited by sol-gel method in different annealing temperature and duration. • We examined the environmental stability in ambient and damp heat condition. • We investigated chemical state of thin film. • Better stability was observed in the film annealed at high temperature (600 °C) along with longer duration (120 min). • An ultrathin aluminum oxide layer formation was predicted by XPS measurement which protects further oxidation and improves stability. - Abstract: Al-doped zinc oxide (AZO) thin films have been considered as a promising alternative to tin doped indium oxide (ITO), which is currently used in various optoelectronic applications. However, the environmental stability of AZO film is not satisfactory, in that the resistivity is significantly increases in air. Here, we investigate the resistivity stability of AZO thin films prepared by sol-gel method using various annealing temperatures and durations. The degradation of resistivity property was observed for AZO films stored in ambient or damp heat environment, where the degradation rate was influenced by annealing temperature. A significant improvement of electrical stability was attained in AZO films that were prepared at high annealing temperature. The films, which showed the highest and the lowest increasing rate of resistivity, were further characterized in detail to shed light on the possible mechanisms explaining the improved stability through crystallinity, surface morphology and elemental state of the thin film.

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

Science.gov (United States)

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

2016-08-01

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. Copyright © 2016 Elsevier B.V. All rights reserved.

ARSENIC REMOVAL USING SOL-GEL SYNTHESIZED TITANIUM DIOXIDE NANOPARTICLES

Science.gov (United States)

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...

Analyses of desorbed H2O with temperature programmed desorption technique in sol-gel derived HfO2 thin films

International Nuclear Information System (INIS)

Shimizu, H.; Nemoto, D.; Ikeda, M.; Nishide, T.

2009-01-01

Hafnium oxide (HfO 2 ) is a promising material for the gate insulator in highly miniaturized silicon (Si) ultra-large-scale-integration (ULSI) devices (32 nm and beyond). In the field chemistry, a sol-gel processing has been used to fabricate HfO 2 thin film with the advantages of low cost, relative simplicity, and easy control of the composition of the layers formed. Temperature-programmed desorption (TPD) has been used not only for analyzing adsorbed gases on the surfaces of bulk sol-gel-derived HfO 2 of sol-gel-derived HfO 2 thin film fired at 350, 450, 550 and 700 deg C in sol-gel derived HfO 2 films in air is investigated using TPD, and also the material characterization of HfO 2 thin films is evaluated by X-ray diffraction (XRD) method. The dielectric constant of the films was also estimated using the capacitance-voltage (C-V) method. TPD is essentially a method of analyzing desorped gases from samples heated by infra-red light as a function of temperature under vacuum conditions using a detector of quadruple mass spectroscopy (QMS). Sol-gel-derived HfO 2 films were fabricated on 76-mm-diameter Si(100) wafers as follows. Hafnia sol solutions were prepared by dissolving HfCl 4 in NH 4 OH solution, followed by the of HCOOH. (author)

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

International Nuclear Information System (INIS)

Kim, Dae-Sung; Ryu, Bong-ki

2017-01-01

In this study, quaternary phosphate-based sol-gel derived glasses were synthesized from a P 2 O 5 -CaO-Na 2 O-TiO 2 system with a high TiO 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 2 enters the network as (TiO 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 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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-04-15

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.

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

Energy Technology Data Exchange (ETDEWEB)

Jameel, Zainab N., E-mail: zeinb76-alrekbe@yahoo.com; Haider, Adawiya J., E-mail: adawiyahaider@yahoo.com [Nanotechnology and Advanced Materials Research Center, The University of Technology, Baghdad (Iraq); Taha, Samar Y., E-mail: samarjam2002@yahoo.com [College of Science for Women, University of Baghdad, Baghdad (Iraq); Gangopadhyay, Shubhra, E-mail: gangopadhyays@missouri.edu; Bok, Sangho, E-mail: BokSa@missouri.edu [Department of Electrical and Computer, University of Missouri, Engineering, Building West, Columbia, Missouri 65211 (United States)

2016-07-25

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.

Anion embedded sol-gel films on Al for corrosion protection

International Nuclear Information System (INIS)

Sheffer, Mari; Groysman, Alec; Starosvetsky, David; Savchenko, Natali; Mandler, Daniel

2004-01-01

We report here on the successful incorporation of organic anions into a sol-gel film on Al as a means of enhancing the protection against corrosion. Following our previous study where we showed that hydrophobic sol-gel films provided pronounced corrosion inhibition, we studied the corrosion inhibition that phenylphosphonic acid (PPA) has when embedded inside a thin sol-gel coating on Al. The anion of this organic anion tends to stay inside a phenyltrimethoxysilane (PTMOS) based sol-gel film due to π-interactions. Our findings, which are derived primarily from potentiodynamic polarization measurements, electrochemical noise, scanning electron microscopy measurements and Auger electron spectroscopy (AES), clearly show that the organic phosphonate adds to the protection efficiency of the sol-gel film

Preparation of sol-gel TiO2/purified Na-bentonite composites and their photovoltaic application for natural dye-sensitized solar cells

International Nuclear Information System (INIS)

Saelim, Ni-on; Magaraphan, Rathanawan; Sreethawong, Thammanoon

2011-01-01

Highlights: → Natural dye from red cabbage was successfully employed in DSSC. → A fast sol-gel method to produce TiO 2 /clay thin film was proposed. → The sol-gel-prepared TiO 2 /clay was applied as the scattering layer on top of TiO 2 electrode. → Thicker sol-gel-prepared TiO 2 /clay electrode showed higher DSSC efficiency. - Abstract: The sol-gel TiO 2 /purified natural clay electrodes having Ti:Si molar ratios of 95:5 and 90:10 were initially prepared, sensitized with natural red cabbage dye, and compared to the sol-gel TiO 2 electrode in terms of physicochemical characteristics and solar cell efficiency. The results showed that the increase in purified Na-bentonite content greatly increased the specific surface area and total pore volume of the prepared sol-gel TiO 2 /purified Na-bentonite composites because the clay platelets prevented TiO 2 particle agglomeration. The sol-gel TiO 2 /5 mol% Si purified Na-bentonite and sol-gel TiO 2 /10 mol% Si purified Na-bentonite composites could increase the film thickness of solar cells without cracking when they were coated as a scattering layer on the TiO 2 semiconductor-based film, leading to increasing the efficiency of the natural dye-sensitized solar cells in this work.

Preparation of silica by sol-gel method using formamide

Directory of Open Access Journals (Sweden)

R.F.S. Lenza

2001-07-01

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.

A novel tantalum-based sol-gel packed microextraction syringe for highly specific enrichment of phosphopeptides in MALDI-MS applications.

Science.gov (United States)

Çelikbıçak, Ömür; Atakay, Mehmet; Güler, Ülkü; Salih, Bekir

2013-08-07

A new tantalum-based sol-gel material was synthesized using a unique sol-gel synthesis pathway by PEG incorporation into the sol-gel structure without performing a calcination step. This improved its chemical and physical properties for the high capacity and selective enrichment of phosphopeptides from protein digests in complex biological media. The specificity of the tantalum-based sol-gel material for phosphopeptides was evaluated and compared with tantalum(V) oxide (Ta2O5) in different phosphopeptide enrichment applications. The tantalum-based sol-gel and tantalum(V) oxide were characterized in detail using FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM), and also using a surface area and pore size analyzer. In the characterization studies, the surface morphology, pore volume, crystallinity of the materials and PEG incorporation into the sol-gel structure to produce a more hydrophilic material were successfully demonstrated. The X-ray diffractograms of the two different materials were compared and it was noted that the broad signals of the tantalum-based sol-gel clearly represented the amorphous structure of the sol-gel material, which was more likely to create enough surface area and to provide more accessible tantalum atoms for phosphopeptides to be easily adsorbed when compared with the neat and more crystalline structure of Ta2O5. Therefore, the phosphopeptide enrichment performance of the tantalum-based sol-gels was found to be remarkably higher than the more crystalline Ta2O5 in our studies. Phosphopeptides at femtomole levels could be selectively enriched using the tantalum-based sol-gel and detected with a higher signal-to-noise ratio by matrix-assisted laser desorption/ionization-mass spectrometer (MALDI-MS). Moreover, phosphopeptides in a tryptic digest of non-fat bovine milk as a complex real-world biological sample were retained with higher yield using a tantalum-based sol-gel. Additionally, the sol-gel material

New insights into uranium (VI) sol-gel processing

International Nuclear Information System (INIS)

King, C.M.; Thompson, M.C.; Buchanan, B.R.; King, R.B.; Garber, A.R.

1990-01-01

Nuclear Magnetic Resonance (NMR) investigations on the Oak Ridge National Laboratory process for sol-gel synthesis of microspherical nuclear fuel (UO 2 ), has been extremely useful in sorting out the chemical mechanism in the sol-gel steps. 13 C, 15 N, and 1 H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C 6 H 12 N 4 ) has revealed near quantitative stability of this adamantane-like compound in the sol-gel process, contrary to its historical role as an ammonia source for gelation from the worldwide technical literature. 17 O NMR of uranyl (UO 2 ++ ) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, [(UO 2 ) 3 (μ 3 -O)(μ 2 -OH) 3 ] + , induced by basic hydrolysis with the HMTA gelation agent. Spectroscopic results will be presented to illustrate that trimer condensation occurs during sol-gel processing leading to layered polyanionic hydrous uranium oxides in which HMTAH + is occluded as an ''intercalation'' cation. Subsequent sol-gel processing of microspheres by ammonia washing results in in-situ exchange and formation of a layered hydrous ammonium uranate with a proposed structural formula of (NH 4 ) 2 [(UO 2 ) 8 O 4 (OH) 10 ] · 8H 2 O. This compound is the precursor to sintered UO 2 ceramic fuel. 23 refs., 10 figs

Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

Science.gov (United States)

Gąsiorek, Jolanta; Babiarczuk, Bartosz; Kaleta, Jerzy; Jones, Walis; Krzak, Justyna

2018-01-01

Corrosion is constantly a major problem of the world economy in the field of metal products, metal processing and other areas that utilise metals. Previously used compounds utilizing hexavalent chromium were amongst the most effective materials for corrosion protection but regulations have been recently introduced that forbid their use. Consequently, there is a huge drive by engineers, technologists and scientists from different disciplines focused on searching a new, more effective and environmentally-friendly means of corrosion protection. One novel group of materials with the potential to solve metal protection problems are sol-gel thin films, which are increasingly interesting as mitigation corrosion barriers. These environmentally-friendly and easy-to-obtain coatings have the promise to be an effective alternative to hexavalent chromium compounds using for anti-corrosion industrial coatings. In this review the authors present a range of different solutions for slow down the corrosion processes of metallic substrates by using the oxides and doped oxides obtained by the sol-gel method. Examples of techniques used to the sol-gel coating examinations, in terms of anti-corrosion protection, are also presented. PMID:29373540

Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation.

Science.gov (United States)

Gąsiorek, Jolanta; Szczurek, Anna; Babiarczuk, Bartosz; Kaleta, Jerzy; Jones, Walis; Krzak, Justyna

2018-01-26

Corrosion is constantly a major problem of the world economy in the field of metal products, metal processing and other areas that utilise metals. Previously used compounds utilizing hexavalent chromium were amongst the most effective materials for corrosion protection but regulations have been recently introduced that forbid their use. Consequently, there is a huge drive by engineers, technologists and scientists from different disciplines focused on searching a new, more effective and environmentally-friendly means of corrosion protection. One novel group of materials with the potential to solve metal protection problems are sol-gel thin films, which are increasingly interesting as mitigation corrosion barriers. These environmentally-friendly and easy-to-obtain coatings have the promise to be an effective alternative to hexavalent chromium compounds using for anti-corrosion industrial coatings. In this review the authors present a range of different solutions for slow down the corrosion processes of metallic substrates by using the oxides and doped oxides obtained by the sol-gel method. Examples of techniques used to the sol-gel coating examinations, in terms of anti-corrosion protection, are also presented.

Development of novel biocompatible hybrid nanocomposites based on polyurethane-silica prepared by sol gel process

Energy Technology Data Exchange (ETDEWEB)

Rashti, Ali [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Yahyaei, Hossein [Department of Polymer Engineering and Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Firoozi, Saman [Department of Tissue Engineering & Regenerative Medicine, Faculty of Advanced Technologies in Medicine, Iran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Ramezani, Sara [Department of Neuroscience, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Rahiminejad, Ali [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Karimi, Roya [Department of Tissue Engineering and Applied Cell Science, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Farzaneh, Khadijeh [Tehran Heart Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Mohseni, Mohsen [Department of Polymer Engineering and Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Ghanbari, Hossein, E-mail: hghanbari@tums.ac.ir [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Tehran Heart Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Medical Biomaterials Research Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of)

2016-12-01

Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants. - Highlights: • Nanocomposites based on polyurethane and nanosilica prepared by sol-gel method fabricated • Addition of inorganic phase improved mechanical properties. • Nanosilica prepared by sol-gel method increased hydrophilicity. • By adding nanosilica to polyurethane biocompatibility increased significantly.

Enhancement of Ce/Cr Codopant Solubility and Chemical Homogeneity in TiO2 Nanoparticles through Sol-Gel versus Pechini Syntheses.

Science.gov (United States)

Chen, Wen-Fan; Mofarah, Sajjad S; Hanaor, Dorian Amir Henry; Koshy, Pramod; Chen, Hsin-Kai; Jiang, Yue; Sorrell, Charles Christopher

2018-06-18

Ce/Cr codoped TiO 2 nanoparticles were synthesized using sol-gel and Pechini methods with heat treatment at 400 °C for 4 h. A conventional sol-gel process produced well-crystallized anatase, while Pechini synthesis yielded less-ordered mixed-phase anatase + rutile; this suggests that the latter method enhances Ce solubility and increases chemical homogeneity but destabilizes the TiO 2 lattice. Greater structural disruption from the decomposition of the Pechini precursor formed more open agglomerated morphologies, while the lower levels of structural disruption from pyrolysis of the dried sol-gel precursor resulted in denser agglomerates of lower surface areas. Codoping and associated destabilization of the lattice reduced the binding energies in both powders. Cr 4+ formation in sol-gel powders and Cr 6+ formation in Pechini powders suggest that these valence changes derive from synergistic electron exchange from intervalence and/or multivalence charge transfer. Since Ce is too large to allow either substitutional or interstitial solid solubility, the concept of integrated solubility is introduced, in which the Ti site and an adjacent interstice are occupied by the large Ce ion. The photocatalytic performance data show that codoping was detrimental owing to the effects of reduced crystallinity from lattice destabilization and surface area. Two regimes of mechanistic behavior are seen, which are attributed to the unsaturated solid solutions at lower codopant levels and supersaturated solid solutions at higher levels. The present work demonstrates that the Pechini method offers a processing technique that is superior to sol-gel because the former facilitates solid solubility and consequent chemical homogeneity.

Special Advanced Studies for Pollution Prevention. Delivery Order 0017: Sol-Gel Surface Preparation for Carbon Steel and Stainless Steel Bonding

National Research Council Canada - National Science Library

Zheng, Haixing

1997-01-01

The objective of this program is to study the feasibility of using sol-gel active alumina coatings for the surface preparation of carbon steel and stainless steel for adhesive bonding, and to optimize...

Synthesis and characterization of the Pt/SiO2 nanocomposite by the sol-gel method

Directory of Open Access Journals (Sweden)

A. Salabat

2011-01-01

Full Text Available The silica supported platinum nanoparticles was synthesized by using the sol-gel method. The possibility of using diamminedinitro platinum (II as Pt precursor and effect of metal precursor concentration on the final Pt nanoparticle size was investigated. A stable silica sol was prepared via hydrolysis of tetraethyl orthosilicate (TEOS as a metal alcoxide and condensation reaction. Subsequently, diamminedinitro platinum (II was added to sol to form the Pt/silica sol. After drying and calcination of the sol, the Pt/SiO2 nanocpmposite has been obtained. Crystallographic information and crystalline size of the synthesized Pt/SiO2 were determined by X-ray diffraction (XRD method. Morphology of the nanoparticles and hydrogen-bonding interaction between silanol groups and amine ligands were characterized by SEM and Fourier transform infrared (FTIR spectra, respectively. Transmission Electron Microscopy (TEM was employed in evaluating the distribution and size of the platinum nanoparticles in the silica.

Synthesis of hybrid chitosan/calcium aluminosilicate using a sol-gel method for optical applications

Energy Technology Data Exchange (ETDEWEB)

Elnahrawy, Amany Mohamed [Department of Solid State, Physics Division, National Research Center (NRC), Giza 12622, Cairo (Egypt); Kim, Yong Soo, E-mail: yskim2@ulsan.ac.kr [Department of Physics and Energy Harvest-Storage Research Center (EHSRC), University of Ulsan, Ulsan 44610 (Korea, Republic of); Ali, Ahmed I., E-mail: Ahmed_ali_2010@helwan.edu.eg [Department of Physics and Energy Harvest-Storage Research Center (EHSRC), University of Ulsan, Ulsan 44610 (Korea, Republic of); Basic Science Department, Faculty of Industrial Education & Technology, Helwan University, Cairo 11281 (Egypt)

2016-08-15

Hybrid chitosan (CS)/calcium aluminosilicate nanocomposites thin films and membranes were prepared using a sol–gel method with three different concentrations of Al{sub 2}O{sub 3} (5, 7 and 10 mol. %). The prepared nanocomposites were characterized by transmission electron microscopy, X-ray diffraction and Fourier Transform Infrared spectroscopy. The optical properties of the prepared samples were analyzed by UV/Vis spectrophotometry and photoluminescence (PL) spectroscopy. The optical parameters revealed an increase in both the refractive index and band gap of the nanocomposites with increasing Al concentration. In addition, the PL spectra revealed a blue shift that was consistent with an increase in the optical band gap. These results suggest that CS/calcium aluminosilicate in two different forms can be a good candidate for optical sensors applications. - Highlights: • We show a large specific surface area of hybrid CS/calcium aluminosilicate thin films and membranes using sol-gel method. • Inorganic SiO{sub 2}-based phase are perfectly embedded onto chitosan matrix has a reliable stability. • CS/calcium aluminosilicate could be usable for optical sensors, planar waveguide, and bio-sensing.

Microcontroller based instrumentation for the fuel pin preparation facility by sol-gel method

International Nuclear Information System (INIS)

Suhasini, B.; Prabhakar Rao, J.; Srinivas, K.C.

2009-01-01

The fuel pin preparation facility by Sol-Gel route has been set up at Chemistry Group at Indira Gandhi Centre for Atomic Research, Kalpakkam. Sol-Gel, a solution-gelation process involves conversion of solutions of nitrates of uranium-plutonium (at 0 deg C) into gel microspheres. To measure the exact quantities of the above solutions and to ensure their temperatures, a variety of sensors have been used at various stages in the plant. To monitor and acquire the data of process parameters used in the production and for an automated operation of the plant, a PC (master)-microcontroller (slave) based instrumentation has been developed along with acquisition software and a GU interface developed in Visual Basic. (author)

Methylene blue degradation by NaTaO3 sol-gel doped with Sm and La

International Nuclear Information System (INIS)

Torres-Martinez, Leticia M.; Cruz-Lopez, Arquimedes; Juarez-Ramirez, Isaias; Meza-de la Rosa, Ma. Elena

2009-01-01

In this work, NaTaO 3 compounds doped with 1 M% of La and Sm, were prepared by the sol-gel (SG) method and solid state (SS) reaction; and tested as photocatalysts on the degradation of methylene blue (MB) under UV light. The structural characterization by X-ray powder diffraction revealed that the crystallization of the NaTaO 3 phase prepared by the sol-gel method started at 600 deg. C, reaching maximum crystallization at 800 deg. C. It was determined that the presence of Sm and La retard the crystallization of the NaTaO 3 phase. On the other hand, the compounds synthesized in this work showed particle sizes in the nanometric scale, as it was observed by scanning electron microscopy (SEM). The specific surface area of the compounds synthesized by the sol-gel method, showed values 4 times higher than those obtained by the solid state reaction, favoring their functional and photocatalytic performance in the methylene blue degradation. In addition, the best photocatalytic performance was shown by the NaTaO 3 doped with Sm and heated at 600 deg. C, having a half-life time of 65 min.

Recubrimientos de hidroxiapatita preparados mediante un proceso sol-gel

Directory of Open Access Journals (Sweden)

Peón, E.

2005-12-01

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

Synthesis and photocatalytic properties of porous TiO2 films prepared by ODA/sol-gel method

International Nuclear Information System (INIS)

Zhang Wenjie; Bai Jiawei

2012-01-01

Porous TiO 2 films were deposited on SiO 2 pre-coated glass-slides by sol-gel method using octadecylamine (ODA) as template. The amount of ODA in the sol played an important role on the physicochemical properties and photocatalytic performance of the TiO 2 films. The films prepared at different conditions were all composed of anatase titanium dioxide crystals, and TiO 2 crystalline size got larger with increasing ODA amount. The maximum specific surface area of 41.5 m 2 /g was obtained for TiO 2 powders prepared from titanium sol containing 2.0 g ODA. Methyl orange degradation rate was enhanced along with increasing ODA amount and reached the maximal value at 2.0 g addition of ODA. After 40 min of UV-light irradiation, methyl orange degradation rate reached 30.5% on the porous film, which was about 10% higher than that on the smooth film. Porous TiO 2 film showed almost constant activity with slight decrease from 30.5% to 28.5% after 4 times of recycles.

Fluorescence metrology of silica sol-gels

Indian Academy of Sciences (India)

We have developed a new method for measuring in-situ the growth of the nanometre-size silica particles which lead to the formation of sol-gel glasses. This technique is based on the decay of fluorescence polarisation anisotropy due to Brownian rotation of dye molecules bound to the particles. Results to date give near ...

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

Science.gov (United States)

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

2016-10-14

Nonhydrolytic sol-gel (NHSG) route was used for the creation of novel zirconia-polypropylene oxide (ZrO 2 -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 ZrCl 4 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 ZrO 2 -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. Copyright © 2016 Elsevier B.V. All rights reserved.

Sol-Gel Thin Films for Plasmonic Gas Sensors

Science.gov (United States)

Della Gaspera, Enrico; Martucci, Alessandro

2015-01-01

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. PMID:26184216

Determination of hexamethylene tetramine in the process solution of sol-gel method for nuclear fuel fabrication

International Nuclear Information System (INIS)

Ganatra, V.R.; Sawant, R.M.; Chaudhuri, N.K.; Vaidya, V.N.

1998-01-01

Hexamethylene tetramine (HMTA) was determined in the presence of large quantities of urea, formaldehyde and ammonium hydroxide by potentiometric titration with perchloric acid solution using an autotitrator coupled to a personal computer. This analysis is required for the process control of the sol-gel method in the production of ceramic metal oxide (e.g., oxides and mixed oxides of Th, U and Pu) microspheres using the internal gelation route. Feed solution used for preparation of microspheres contains large quantities of urea. The washings of gel microspheres produced after the internal gelation process contain urea, formaldehyde, urea-formaldehyde complex and ammonium hydroxide. The presence of these constituents in the feed solution and washings seriously interfere in the commonly used methods for the determination of HMTA. Using this method the relative standard deviation was found to be 0.27% in eleven determinations of a typical feed solution (3.0M HMTA) when the aliquots contained 75 to 125 mg of HMTA. Time required for each titration was 5-7 minutes. Feed and effluent solutions of sol-gel process were analysed. (author)

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

International Nuclear Information System (INIS)

Dubuisson, E; Monnier, V; Sanz-Menez, N; Ibanez, A; Boury, B; Usson, Y; Pansu, R B

2009-01-01

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.

A sol-gel-modified poly(methyl methacrylate) electrophoresis microchip with a hydrophilic channel wall.

Science.gov (United States)

Chen, Gang; Xu, Xuejiao; Lin, Yuehe; Wang, Joseph

2007-01-01

A sol-gel method was employed to fabricate a poly(methyl methacrylate) (PMMA) electrophoresis microchip that contains a hydrophilic channel wall. To fabricate such a device, tetraethoxysilane (TEOS) was injected into the PMMA channel and was allowed to diffuse into the surface layer for 24 h. After removing the excess TEOS, the channel was filled with an acidic solution for 3 h. Subsequently, the channel was flushed with water and was pretreated in an oven to obtain a sol-gel-modified PMMA microchip. The water contact angle for the sol-gel-modified PMMA was approximately 27.4 degrees compared with approximately 66.3 degrees for the pure PMMA. In addition, the electro-osmotic flow increased from 2.13x10(-4) cm2 V(-1) s(-1) for the native-PMMA channel to 4.86x10(-4) cm2 V(-1) s(-1) for the modified one. The analytical performance of the sol-gel-modified PMMA microchip was demonstrated for the electrophoretic separation of several purines, coupled with amperometric detection. The separation efficiency of uric acid increased to 74,882.3 m(-1) compared with 14,730.5 m(-1) for native-PMMA microchips. The result of this simple modification is a significant improvement in the performance of PMMA for microchip electrophoresis and microfluidic applications.

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

Science.gov (United States)

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

2013-07-01

A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sol-gel based oxidation catalyst and coating system using same

Science.gov (United States)

Watkins, Anthony N. (Inventor); Leighty, Bradley D. (Inventor); Oglesby, Donald M. (Inventor); Patry, JoAnne L. (Inventor); Schryer, Jacqueline L. (Inventor)

2010-01-01

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.

Innovative Sol-Gel Routes for the Bottom-up Preparation of Heterogeneous Catalysts.

Science.gov (United States)

Debecker, Damien P

2017-12-11

Heterogeneous catalysts can be prepared by different methods offering various levels of control on the final properties of the solid. In this account, we exemplify bottom-up preparation routes that are based on the sol-gel chemistry and allow to tailor some decisive properties of solid catalysts. First, an emulsion templating strategy is shown to lead to macrocellular self-standing monoliths with a macroscopic 3D structure. The latter can be used as catalyst or catalyst supports in flow chemistry, without requiring any subsequent shaping step. Second, the aerosol-assisted sol-gel process allows for the one-step and continuous production of porous mixed oxides. Tailored textural properties can be obtained together with an excellent control on composition and homogeneity. Third, the application of non-hydrolytic sol-gel routes, in the absence of water, leads to mixed oxides with outstanding textural properties and with peculiar surface chemistry. In all cases, the resulting catalytic performance can be correlated with the specificities of the preparation routes presented. This is exemplified in catalytic reactions in the fields of biomass conversion, petro chemistry, enantioselective organic synthesis, and air pollution mitigation. © 2017 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Doped indium nitride thin film by sol-gel spin coating method

Science.gov (United States)

Lee, Hui San; Ng, Sha Shiong; Yam, Fong Kwong

2017-12-01

In this study, magnesium doped indium nitride (InN:Mg) thin films grown on silicon (100) substrate were prepared via sol-gel spin coating method followed by nitridation process. A custom-made tube furnace was used to perform the nitridation process. Through this method, the low dissociation temperature issue of InN:Mg thin films can be solved. The deposited InN:Mg thin films were investigated using various techniques. The X-rays diffraction results revealed that two intense diffraction peaks correspond to wurtzite structure InN (100), and InN (101) were observed at 29° and 33.1° respectively. Field emission scanning electron microscopy images showed that the surface of the films exhibits densely packed grains. The elemental composition of the deposited thin films was analyzed using energy dispersive X-rays spectroscopy. The detected atomic percentages for In, N, and Mg were 43.22 %, 3.28 %, and 0.61 % respectively. The Raman spectra showed two Raman- and infrared-active modes of E2 (High) and A1 (LO) of the wurtzite InN. The band gap obtained from the Tauc plot showed around 1.74 eV. Lastly, the average surface roughness measured by AFM was around 0.133 µm.

Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

Directory of Open Access Journals (Sweden)

Jolanta Gąsiorek

2018-01-01

Full Text Available Corrosion is constantly a major problem of the world economy in the field of metal products, metal processing and other areas that utilise metals. Previously used compounds utilizing hexavalent chromium were amongst the most effective materials for corrosion protection but regulations have been recently introduced that forbid their use. Consequently, there is a huge drive by engineers, technologists and scientists from different disciplines focused on searching a new, more effective and environmentally-friendly means of corrosion protection. One novel group of materials with the potential to solve metal protection problems are sol-gel thin films, which are increasingly interesting as mitigation corrosion barriers. These environmentally-friendly and easy-to-obtain coatings have the promise to be an effective alternative to hexavalent chromium compounds using for anti-corrosion industrial coatings. In this review the authors present a range of different solutions for slow down the corrosion processes of metallic substrates by using the oxides and doped oxides obtained by the sol-gel method. Examples of techniques used to the sol-gel coating examinations, in terms of anti-corrosion protection, are also presented.

Effect of UV-irradiation on sol-gel optical films

International Nuclear Information System (INIS)

Yang Fan; Shen Jun; Zhou Bin; Wu Guangming; Luo Aiyun; Sun Qi

2005-01-01

Sol-gel optical films were deposited on K9 glass and silicon wafer substrates by spin-coating method and a high-pressure mercury lamp was used to perform ultraviolet treating to solidify these films and improve their performance. SEM, AFM, IR and ellipsometer were used to characterize the structure and optical properties of the films. Mechanical property of films was measured by pencil hardness-testing device. Laser damage threshold of films was measured by a Q-switched Nd:YAG high power laser with the wave length of 1064 nm and the pulse width of 15 ns. The results show that UV-irradiation can improve the mechanical property and increase the refractive index of the films. Besides, the nodules on the surface of the films can be changed into pits by UV-irradiation process, so the laser damage threshold of sol-gel thin films will be increased. After UV-irradiation the laser damage threshold of single-layer ZrO 2 film reached 50.6 J/cm 2 (1064 nm, 1 ns). It is found that UV-irradiation is an effective method to avoid the infiltrating between the layers, and the degree of homogeneity of the multilayer films can be improved by this way. (authors)

The development and characterization of sol-gel substrates for chemical and optical applications

Science.gov (United States)

Powers, Kevin William

1998-12-01

The sol gel process can be used to make monolithic porous glass for various scientific and engineering uses. The porosity of the material imparts a large surface area which is advantageous in applications such as catalyst supports or in the study of surface mediated chemical reactions. The chemical stability and transparency of the porous glass also make it suitable for use in the emerging field of optical sensors. In this study fluoride catalysis is used to produce sol gel monoliths with pore radii of up to 400 Angstroms, four times larger than any previously reported using conventional drying techniques. Gel monoliths with pore radii of 200 Angstroms were found to have the best combination of surface area, pore volume and optical transparency. Typical monoliths have surface areas of 150 m2/g and pore volumes of 1.60 cm3/g with good transparency. The monoliths are chemically stable, have good mechanical strength and can be easily rehydrated without cracking. The substrates are also suitable for sintering into dense high purity silica glass with little tendency towards foaming. An in-depth study of the catalytic effect of fluoride on the sol gel process is also included. It has been theorized that fluoride serves to expand the coordination sphere of the silicon center making it more subject to nucleophilic attack. In this work an ion-specific fluoride electrode is used to monitor free fluoride concentrations in HF catalyzed sols while silicic acid is added in the form of tetramethoxysilane (TMOS). It is found that fluoride is rapidly bound by the silicic acid in a ratio of four to one, indicating the formation of silicon tetrafluoride. A concurrent decrease in pH suggests that a pentacoordinate species is formed that is more stable than previously thought. A polymerization mechanism is proposed that explains the hydrophobicity of fluoride catalyzed gels and the difficulty in retaining structural fluoride in fluoride catalyzed sol gel glasses. Finally, several

Slow Release of Plant Volatiles Using Sol-Gel Dispensers.

Science.gov (United States)

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

2014-12-01

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. © 2014 Entomological Society of America.

Sol-gel encapsulation for controlled drug release and biosensing

Science.gov (United States)

Fang, Jonathan

The main focus of this dissertation is to investigate the use of sol-gel encapsulation of biomolecules for controlled drug release and biosensing. Controlled drug release has advantages over conventional therapies in that it maintains a constant, therapeutic drug level in the body for prolonged periods of time. The anti-hypertensive drug Captopril was encapsulated in sol-gel materials of various forms, such as silica xerogels and nanoparticles. The primary objective was to show that sol-gel silica materials are promising drug carriers for controlled release by releasing Captopril at a release rate that is within a therapeutic range. We were able to demonstrate desired release for over a week from Captopril-doped silica xerogels and overall release from Captopril-doped silica nanoparticles. As an aside, the antibiotic Vancomycin was also encapsulated in these porous silica nanoparticles and desired release was obtained for several days in-vitro. The second part of the dissertation focuses on immobilizing antibodies and proteins in sol-gel to detect various analytes, such as hormones and amino acids. Sol-gel competitive immunoassays on antibody-doped silica xerogels were used for hormone detection. Calibration for insulin and C-peptide in standard solutions was obtained in the nM range. In addition, NASA-Ames is also interested in developing a reagentless biosensor using bacterial periplasmic binding proteins (bPBPs) to detect specific biomarkers, such as amino acids and phosphate. These bPBPs were doubly labeled with two different fluorophores and encapsulated in silica xerogels. Ligand-binding experiments were performed on the bPBPs in solution and in sol-gel. Ligand-binding was monitored by fluorescence resonance energy transfer (FRET) between the two fluorophores on the bPBP. Titration data show that one bPBP has retained its ligand-binding properties in sol-gel.

Optimization of Catalytic Ozonation Process for Formaldehyde Mineralization from Synthetic Wastewater by Fe/MgO Nanoparticles Synthesis by Sol-Gel Method by Response Surface Model

Directory of Open Access Journals (Sweden)

Ghorban Asgari

2014-09-01

Full Text Available Background: Design experiment stages of formalin mineralization process by center composition design (CCD cause ease of work, reducing the number of samples, increasing the accuracy of optimized conditions and the interaction parameters determined during the process. The aim of this study was optimization of catalytic ozonation process for formaldehyde mineralization from synthetic wastewater by Fe/MgO nanoparticles synthesis by sol-gel method by response surface model. Methods: This experimental study was conducted in a semi-batch reactor, using a RSM by taking 3 factors in the final stage of pH (7-9, reaction time (10-20 min and catalyst dose (1.1-1.3 g/L was investigated. Synthesis of nanoparticles was done by sol-gel method. The results were analyzed by Design Expert 7.0.1 software. Results: The results showed that the process was dependent on the parameters studied and changing each parameter, affected the process efficiency and other parameters. The optimum conditions predicted for the process was 86.51% of mineralization efficiency. Optimum condition included pH=8.82, reaction time of 20 minute and catalyst dose of 1.3 g/L. The correlation coefficient for the process was determined 0.91. Conclusion: Using a statistical model could reduce the number of experiments, the accuracy and the prediction process. The catalytic ozonation process has the ability to remove formaldehyde with high efficiency and the process was environmental friendly.

Processing of non-oxide ceramics from sol-gel methods

Science.gov (United States)

Landingham, Richard; Reibold, Robert A.; Satcher, Joe

2014-12-12

A general procedure applied to a variety of sol-gel precursors and solvent systems for preparing and controlling homogeneous dispersions of very small particles within each other. Fine homogenous dispersions processed at elevated temperatures and controlled atmospheres make a ceramic powder to be consolidated into a component by standard commercial means: sinter, hot press, hot isostatic pressing (HIP), hot/cold extrusion, spark plasma sinter (SPS), etc.

Holographic sol-gel monoliths: optical properties and application for humidity sensing

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Ilatovskii, Daniil A.; Milichko, Valentin; Vinogradov, Alexander V.; Vinogradov, Vladimir V.

2018-05-01

Sol-gel monoliths based on SiO2, TiO2 and ZrO2 with holographic colourful diffraction on their surfaces were obtained via a sol-gel synthesis and soft lithography combined method. The production was carried out without any additional equipment at near room temperature and atmospheric pressure. The accurately replicated wavy structure with nanoscale size of material particles yields holographic effect and its visibility strongly depends on refractive index (RI) of materials. Addition of multi-walled carbon nanotubes (MWCNTs) in systems increases their RI and lends absorbing properties due to extremely high light absorption constant. Further prospective and intriguing applications based on the most successful samples, MWCNTs-doped titania, were investigated as reversible optical humidity sensor. Owing to such property as reversible resuspension of TiO2 nanoparticles while interacting with water, it was proved that holographic xerogels can repeatedly act as humidity sensors. Materials which can be applied as humidity sensors in dependence on holographic response were discovered for the first time.

Vanadium dioxide formed by the sol-gel process

International Nuclear Information System (INIS)

Potember, R.S.; Speck, K.R.; Hu, H.S.

1990-01-01

This patent describes a process for the deposition of a crystalline vanadium dioxide thin film. It comprises: providing a solution comprising a vanadium tetraalkoxide and solvent; allowing hydrolysis and condensation reactions to progressively form a homogeneous sol from the solution, applying a coating of the sol to the substrate; allowing a gel to form from the sol on the substrate by evaporating the solvent; dehydrating the gel by heat treatment under an inert atmosphere to form the crystalline vanadium dioxide film

Strength of interactions between immobilized dye molecules and sol-gel matrices.

Science.gov (United States)

Ismail, Fanya; Schoenleber, Monika; Mansour, Rolan; Bastani, Behnam; Fielden, Peter; Goddard, Nicholas J

2011-02-21

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.

Surface functionalization of carbon nanofibers by sol-gel coating of zinc oxide

Energy Technology Data Exchange (ETDEWEB)

Shao Dongfeng [Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi 214122 (China); Changzhou Textile Garment Institute, Changzhou 213164 (China); Wei Qufu [Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi 214122 (China)], E-mail: qfwei@jiangnan.edu.cn; Zhang Liwei; Cai Yibing; Jiang Shudong [Key Laboratory of Eco-textiles, Ministry of Education, Jiangnan University, Wuxi 214122 (China)

2008-08-15

In this paper the functional carbon nanofibers were prepared by the carbonization of ZnO coated PAN nanofibers to expand the potential applications of carbon nanofibers. Polyacrylonitrile (PAN) nanofibers were obtained by electrospinning. The electrospun PAN nanofibers were then used as substrates for depositing the functional layer of zinc oxide (ZnO) on the PAN nanofiber surfaces by sol-gel technique. The effects of coating, pre-oxidation and carbonization on the surface morphology and structures of the nanofibers were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM), respectively. The results of SEM showed a significant increase of the size of ZnO nanograins on the surface of nanofibers after the treatments of coating, pre-oxidation and carbonization. The observations by SEM also revealed that ZnO nanoclusters were firmly and clearly distributed on the surface of the carbon nanofibers. FTIR examination also confirmed the deposition of ZnO on the surface of carbon nanofibers. The XRD analysis indicated that the crystal structure of ZnO nanograins on the surface of carbon nanofibers.

Effect of concentrations of plasticizers on the sol-gel properties developed from alkoxides precursors

Energy Technology Data Exchange (ETDEWEB)

Kunst, Sandra Raquel; Longhi, Marielen; Zini, Lucas Pandolphi [Universidade de Caxias do Sul (CCET/UCS), Caxias do Sul, RS (Brazil). Centro de Ciências Exatas e Tecnologia; Beltrami, Lilian Vanessa Rossa; Boniatti, Rosiana; Cardoso, Henrique Ribeiro Piaggio; Vega, Maria Rita Ortega; Malfatti, Célia de Fraga, E-mail: lvrossa@yahoo.com.br [Universidade Federal do Rio Grande do Sul (LAPEC/UFRGS), Porto Alegre, RS (Brazil). Laboratorio de Pesquisa em Corrosão

2017-07-01

Coatings developed through sol-gel method is presented as an interesting replacement to chromium coating. Sol-gel method present advantages as high purity and excellent distribution of the components. The objective of this work is to synthesize and characterize a film obtained by sol-gel route. The film was prepared with 3-(trimethoxysilylpropyl) methacrylate (TMSPMA), tetraethoxysilane (TEOS) and cerium nitrate, using water and ethanol as solvents. Polyethyleneglycol (PEG) plasticizer was added at four different concentrations. The sol was characterized by techniques of viscosity, thermogravimetric analysis (TGA), X-ray diffraction (XRD) nuclear magnetic resonance spectroscopy (NMR) and Fourier transform infrared spectroscopy (FT-IR). The results showed that tetrafunctional alkoxides condensation was retarded by the plasticizer, forming a compact film. The film with 20 g.L-1 of PEG showed the best electrochemical behavior. (author)

Deposition of tin oxide doped with fluorine produced by sol-gel method and deposited by spray-pyrolysis

International Nuclear Information System (INIS)

Maia, Paulo Herbert Franca; Lima, Francisco Marcone; Sena, Aline Cosmo de; Silva, Alvaro Neuton; Almeida, Ana Fabiola Leite de; Freire, Francisco Nivaldo Aguiar

2014-01-01

Solar energy is one of the most important sources of renewable energy today, but its production is based on silicon cells, expensive and difficult to produce, so the research seek new materials to replace them. This work aims to deposit tin oxide doped with fluorine on the glass substrate using the sol-gel method to provide a working solution and spray pyrolysis technique to perform the deposition. F-SnO2 (FTO) were synthesized by sol-gel method, employing NH_4F and SnCl_2 precursor in an ethanol solution. Before the formation of the gel phase, the entire solution was sprayed, with the aid of a pistol aerographic substrate under heated at 600 °C divided by 50 applications and cooled in the furnace. The substrates had resistances between 10 and 30 S.cm. The energy dispersive x-ray (EDS) revealed the presence of fluorine in the SnO_2 network. (author)

Antimicrobial activity of thin solid films of silver doped hydroxyapatite prepared by sol-gel method.

Science.gov (United States)

Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

2014-01-01

In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x(Ag) = 0.5 are effective against E. coli and S. aureus after 24 h.

Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

Directory of Open Access Journals (Sweden)

Simona Liliana Iconaru

2014-01-01

Full Text Available In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM with energy Dispersive X-ray attachment (X-EDS, Fourier transform infrared spectroscopy (FT-IR, and glow discharge optical emission spectroscopy (GDOES. These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with xAg=0.5 are effective against E. coli and S. aureus after 24 h.

Antimicrobial Activity of Thin Solid Films of Silver Doped Hydroxyapatite Prepared by Sol-Gel Method

Science.gov (United States)

Iconaru, Simona Liliana; Chapon, Patrick; Le Coustumer, Philippe; Predoi, Daniela

2014-01-01

In this work, the preparation and characterization of silver doped hydroxyapatite thin films were reported and their antimicrobial activity was characterized. Silver doped hydroxyapatite (Ag:HAp) thin films coatings substrate was prepared on commercially pure Si disks by sol-gel method. The silver doped hydroxyapatite thin films were characterized by various techniques such as Scanning electron microscopy (SEM) with energy Dispersive X-ray attachment (X-EDS), Fourier transform infrared spectroscopy (FT-IR), and glow discharge optical emission spectroscopy (GDOES). These techniques have permitted the structural and chemical characterisation of the silver doped hydroxyapatite thin films. The antimicrobial effect of the Ag:HAp thin films on Escherichia coli and Staphylococcus aureus bacteria was then investigated. This is the first study on the antimicrobial effect of Ag:HAp thin films obtained by sol-gel method. The results of this study have shown that the Ag:HAp thin films with x Ag = 0.5 are effective against E. coli and S. aureus after 24 h. PMID:24523630

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

Energy Technology Data Exchange (ETDEWEB)

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: n.carmona@fis.ucm.es [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain)

2012-06-01

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.

Effects of parameters of sol-gel process on the phase evolution of sol-gel-derived hydroxyapatite

International Nuclear Information System (INIS)

Eshtiagh-Hosseini, Hossein; Housaindokht, Mohammad Reza; Chahkandi, Mohammad

2007-01-01

It has been established that hydroxyapatite powders can be produced using an alkoxide-based sol-gel technique. Nanocrystalline powders of hydroxyapatite (HA) were prepared from Ca(NO 3 ) 2 .4H 2 O and PO(OC 2 H 5 ) 3 as calcium and phosphorus precursors, respectively, using a sol-gel route. For a number of samples, sol of phosphorus was first hydrolyzed for 24 h with distilled water. The sol temperature, aging time and heat treatment temperature on apatite formation were systematically studied. Increasing the aging time affected the reducing of CaO. Also, increasing the mixed sol solution temperature up to 80 deg. C had a positive effect on the disappearance of impurity phases. With the increase of the calcination temperature >600 deg. C, calcium phosphate impurity phases disappeared. Structural evolution during the synthesis of hydroxyapatite is investigated by using infrared (IR) analysis, X-ray diffraction (XRD), thermal behavior (DTA), and elemental analysis of electron microscopy examination (SEM). X-ray diffraction with the aid of Scherrer and Williamson-Hall equations has been used to characterize the distributions of crystallite size and micro-strain of HA powders .The results indicated that mean crystallite size increased and micro-strain decreased significantly with the rise in firing temperature

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

Energy Technology Data Exchange (ETDEWEB)

Shiquan Tao

2006-12-31

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

Mullite fibres preparation by aqueous sol-gel process and activation energy of mullitization

International Nuclear Information System (INIS)

Tan Hongbin; Ding Yaping; Yang Jianfeng

2010-01-01

Mullite fibres were prepared by sol-gel process using aluminum carboxylates (ACs) and silica sol. ACs was synthesized from dissolving aluminum powder in a mixture of formic acid and oxalic acid using aluminum chloride hexahydrate as catalyst. A molar ratio of 1:2:1 for aluminum, formic acid and oxalic acid was optimized to obtain clear solution and viscous ACs sol for fibres synthesis. Thermogravimetry-differential scanning calorimetry (TG-DSC), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM) analysis were used to characterize the properties of the gel and ceramic fibres. The gel fibres completely transformed to mullite at 1200 o C, with a smooth surface and uniform diameter. The activation energy for mullite formation in precursor gel fibres was determined by means of differential thermal analysis. The value obtained, E a = 741.4 kJ/mol, was lower than most data reported in the literatures, which was attributed to the silica-alumina micro-phase separation when organic acids decomposed during gel fibres heating.

Optical Sensors for Biomolecules Using Nanoporous Sol-Gel Materials

Science.gov (United States)

Fang, Jonathan; Zhou, Jing C.; Lan, Esther H.; Dunn, Bruce; Gillman, Patricia L.; Smith, Scott M.

2004-01-01

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

Investigation of the visible light photocatalytic activity of BiVO4 prepared by sol gel method assisted by ultrasonication.

Science.gov (United States)

Deebasree, J P; Maheskumar, V; Vidhya, B

2018-07-01

Visible light induced photocatalyst BiVO 4 with monoclinic scheelite structure has been synthesised via sol gel method assisted by ultrasonication. The prepared samples were characterised using X-ray diffraction (XRD), scanning electron microscope (SEM), UV-Vis diffused reflectance spectroscopy (DRS) techniques. The photocatalytic efficiency was evaluated by decolourisation of MB under visible light irradiation. The effect of ultrasound output power on the properties of BiVO 4 during and after preparation by sol-gel method has been compared with normal agitated sample (As prepared). The power of ultrasonic vibration has been varied and an ideal output power which yields better catalytic efficiency is determined. BiVO 4 sonicated with 80 W during preparation 80 W (D) exhibited relatively high surface area, better surface morphology and better catalytic efficiency compared to other samples which were sonicated with 100, 160 and 200 W. The results signify that the photodegradation rate of BiVO 4 80 W (D) sample is high up to 96% in 90 min compared to other samples. Change in morphology leading to better catalytic efficiency was obtained just by exposing the sample to ultrasonic radiation without addition of any surfactant. The recovery test showed that the sample was stable for four consecutive cycles. Using radical test, a reasonable mechanism for photodegradation has been proposed. Copyright © 2018 Elsevier B.V. All rights reserved.

Catalytic activity of acid and base with different concentration on sol-gel kinetics of silica by ultrasonic method.

Science.gov (United States)

Das, R K; Das, M

2015-09-01

The effects of both acid (acetic acid) and base (ammonia) catalysts in varying on the sol-gel synthesis of SiO2 nanoparticles using tetra ethyl ortho silicate (TEOS) as a precursor was determined by ultrasonic method. The ultrasonic velocity was received by pulsar receiver. The ultrasonic velocity in the sol and the parameter ΔT (time difference between the original pulse and first back wall echo of the sol) was varied with time of gelation. The graphs of ln[ln1/ΔT] vs ln(t), indicate two region - nonlinear region and a linear region. The time corresponds to the point at which the non-linear region change to linear region is considered as gel time for the respective solutions. Gelation time is found to be dependent on the concentration and types of catalyst and is found from the graphs based on Avrami equation. The rate of condensation is found to be faster for base catalyst. The gelation process was also characterized by viscosity measurement. Normal sol-gel process was also carried out along with the ultrasonic one to compare the effectiveness of ultrasonic. The silica gel was calcined and the powdered sample was characterized with scanning electron microscopy, energy dispersive spectra, X-ray diffractogram, and FTIR spectroscopy. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

Kayili, H Mehmet; Salih, Bekir

2016-08-01

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. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrophoretic deposition of sol-gel-derived ceramic coatings

International Nuclear Information System (INIS)

Zhang, Y.; Crooks, R.M.

1992-01-01

In this paper the physical, optical, and chemical characteristics of electrophoretically and dip-coated sol-gel ceramic films are compared. The results indicate that electrophoresis may allow a higher level of control over the chemistry and structure of ceramic coatings than dip-coating techniques. For example, controlled-thickness sol-gel coatings can be prepared by adjusting the deposition time or voltage. Additionally, electrophoretic coatings can be prepared in a four-component alumino-borosilicate sol display interesting optical characteristics. For example, the ellipsometrically-measured refractive indices of electrophoretic coatings are higher than the refractive indices of dip-coated films cast from identical sols, and they are also higher than any of the individual sol components. This result suggests that there are physical and/or chemical differences between films prepared by dip-coating and electrophoresis

Optical sensing of HCl with phenol red doped sol-gels

International Nuclear Information System (INIS)

Wang Enju; Chow, Kwok-Fan; Wang Wenqun; Wong, Crystal; Yee, Cynthia; Persad, Alvin; Mann, Jonathan; Bocarsly, Andrew

2005-01-01

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

Optical sensing of HCl with phenol red doped sol-gels

Energy Technology Data Exchange (ETDEWEB)

Wang Enju [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States)]. E-mail: wange@stjohns.edu; 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)

2005-04-08

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.

Evolution of heterogeneity accompanying sol-gel transitions in a supramolecular hydrogel.

Science.gov (United States)

Matsumoto, Yuji; Shundo, Atsuomi; Ohno, Masashi; Tsuruzoe, Nobutomo; Goto, Masahiro; Tanaka, Keiji

2017-10-18

When a peptide amphiphile is dispersed in water, it self-assembles into a fibrous network, leading to a supramolecular hydrogel. When the gel is physically disrupted by shaking, it transforms into a sol state. After aging at room temperature for a while, it spontaneously returns to the gel state, called sol-gel transition. However, repeating the sol-gel transition often causes a change in the rheological properties of the gel. To gain a better understanding of the sol-gel transition and its reversibility, we herein examined the thermal motion of probe particles at different locations in a supramolecular hydrogel. The sol obtained by shaking the gel was heterogeneous in terms of the rheological properties and the extent decreased with increasing aging time. This time course of heterogeneity, or homogeneity, which corresponded to the sol-to-gel transition, was observed for the 1st cycle. However, this was not the case for the 2nd and 3rd cycles; the heterogeneity was preserved even after aging. Fourier-transform infrared spectroscopy, small-angle X-ray scattering, and atomic force and confocal laser scanning microscopies revealed that, although the molecular aggregation states of amphiphiles both in the gel and sol remained unchanged with the cycles, the fibril density diversified to high and low density regions even after aging. The tracking of particles with different sizes indicated that the partial mesh size in the high density region and the characteristic length scale of the density fluctuation were smaller than 50 nm and 6 μm, respectively.

Structural study of some gadolinium glass ceramics obtained by sol-gel method

International Nuclear Information System (INIS)

Coroiu, Ilioara; Simiti, Vida I.; Bratu, I.; Borodi, Gh.; Darabont, Al.

2004-01-01

Increased interest in silicate systems containing different rare earth oxides has resulted from their important applications in various fields of technology including laser, optical fiber and optical waveguides in telecommunication applications, microelectronics and catalysis. Glass-ceramics of 0.95 SiO 2 -0.05 Na 2 O composition containing up to 15% molar Gd 2 O 3 were obtained by the sol-gel method. We chose the sol-gel method because this offers the advantage of a good chemical homogeneity and a better control of physical and chemical properties in comparison with traditional methods used to obtain glasses and ceramics. The obtained samples were pressed at 200 kgf/cm 2 as disks with a diameter of Φ=22 mm and a thickness of around 1 mm. Then, they were heat-treated at 250 deg C, 500 deg C and 1000 deg C for about 48 hours. The structural study was made using X-ray diffraction, scanning electron microscopy (SEM) and IR spectroscopy. The X-ray diffraction patterns show that addition of Gd 2 O 3 exerts an important influence on the crystallization process of the studied samples. The crystalline phase decreases with increasing the Gd 2 O 3 concentration. SEM data support this assertion. IR spectra point out also that the increasing of the gadolinium oxide content and the thermal treatment temperature produce the strengthening of the glass ceramic network. Thus, the gadolinium ions play the role of network modifier of the glass ceramic structure. (authors)

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

International Nuclear Information System (INIS)

Crespo, M.A. Dominguez; Murillo, A. Garcia; Torres-Huerta, A.M.; Yanez-Zamora, C.; Carrillo-Romo, F. de J

2009-01-01

Chromate conversion coatings have been widely applied for the corrosion of different metallic substrates. However, the waste containing Cr 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 2 O 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 2 O 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.

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

Energy Technology Data Exchange (ETDEWEB)

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)

2009-08-26

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.

Effect of concentrations of plasticizers on the sol-gel properties developed from alkoxides precursors

Directory of Open Access Journals (Sweden)

Sandra Raquel Kunst

Full Text Available Abstract Coatings developed through sol-gel method is presented as an interesting replacement to chromium coating. Sol-gel method present advantages as high purity and excellent distribution of the components. The objective of this work is to synthesize and characterize a film obtained by sol-gel route. The film was prepared with 3-(trimethoxysilylpropyl methacrylate (TMSPMA, tetraethoxysilane (TEOS and cerium nitrate, using water and ethanol as solvents. Polyethyleneglycol (PEG plasticizer was added at four different concentrations. The sol was characterized by techniques of viscosity, thermogravimetric analysis (TGA, X-ray diffraction (XRD nuclear magnetic resonance spectroscopy (NMR and Fourier transform infrared spectroscopy (FT-IR. The results showed that tetrafunctional alkoxides condensation was retarded by the plasticizer, forming a compact film. The film with 20 g.L-1 of PEG showed the best electrochemical behavior.

Methods for and products of processing nanostructure nitride, carbonitride and oxycarbonitride electrode power materials by utilizing sol gel technology for supercapacitor applications

Science.gov (United States)

Huang, Yuhong; Wei, Oiang; Chu, Chung-tse; Zheng, Haixing

2001-01-01

Metal nitride, carbonitride, and oxycarbonitride powder with high surface area (up to 150 m.sup.2 /g) is prepared by using sol-gel process. The metal organic precursor, alkoxides or amides, is synthesized firstly. The metal organic precursor is modified by using unhydrolyzable organic ligands or templates. A wet gel is formed then by hydrolysis and condensation process. The solvent in the wet gel is then be removed supercritically to form porous amorphous hydroxide. This porous hydroxide materials is sintered to 725.degree. C. under the ammonia flow and porous nitride powder is formed. The other way to obtain high surface area nitride, carbonitride, and oxycarbonitride powder is to pyrolyze polymerized templated metal amides aerogel in an inert atmosphere. The electrochemical capacitors are prepared by using sol-gel prepared nitride, carbonitride, and oxycarbonitride powder. Two methods are used to assemble the capacitors. Electrode is formed either by pressing the mixture of nitride powder and binder to a foil, or by depositing electrode coating onto metal current collector. The binder or coating is converted into a continuous network of electrode material after thermal treatment to provide enhanced energy and power density. Liquid electrolyte is soaked into porous electrode. The electrochemical capacitor assembly further has a porous separator layer between two electrodes/electrolyte and forming a unit cell.

Superhydrophobic properties induced by sol-gel routes on copper surfaces

Science.gov (United States)

Raimondo, M.; Veronesi, F.; Boveri, G.; Guarini, G.; Motta, A.; Zanoni, R.

2017-11-01

Superhydrophobic surfaces are attracting increasing attention in different fields such as energy, transportation, building industry and electronics, as they exhibit many interesting properties such as high water repellence, anti-fogging, anti-corrosion, anti-fouling and self-cleaning abilities. Here, superhydrophobic nanostructured hybrid materials obtained by depositing alumina nanoparticles on copper surfaces via dip coating in Al2O3 sol are presented. Two different preparation routes were explored, based on either an alcoholic or an aqueous Al2O3 sol, and the resulting wetting properties were compared. Wettability measurements showed that when the alcoholic sol is used superhydrophobicity is attained, with values of water contact angle very close to the upper limit of 180°, while highly hydrophobic coatings are obtained with the aqueous sol. These findings were further supported by electron microscopy and X-ray photoelectron spectroscopy, which revealed that the surface layer deposited on Cu is more homogenous and richer in alumina nanoparticles when the alcoholic sol was used. Durability of the superhydrophobic coating was assessed by performing ageing tests in chemically aggressive environments. A remarkable resistance is displayed by the superhydrophobic coating in acid environment, while alkaline conditions severely affect its properties. Such behaviors were investigated by XPS and FE-SEM measurements, which disclosed the nature of the surface reactions under the different conditions tested. The present results underline that a thorough investigation of surface morphology, chemical composition and wetting properties reveals their strongly connection and helps optimizing the combination of substrate nanostructuring and suitable chemical coating for an improved durability in different aggressive environments.

Preparation and characterization of strontium-fluorapatite nanopowders by sol-gel method

Science.gov (United States)

Kamaei, Maryam; Fathi, Mohammad Hossein

2018-01-01

Biomaterials based on calcium orthophosphate are especially attractive for use in medicine, for bone and teeth implants due to their biological properties, such as biocompatibility and bioactivity. Among them, hydroxyapatite (HAP; Ca10(PO4)6(OH)2) is used particularly because of its similarities to the inorganic component of bone. Hydroxyapatite has been widely used for biomedical applications. Despite desirable properties such as bioactivity, biocompatibility, solubility and adsorption, synthetic HA is limited in application due to poor thermostability and poor mechanical properties. Properties of HA can be tailored over a wide range by incorporating different ions into HA lattice. Use of the sol-gel technique is technically simple, cost effective and beneficial for fabrication biomaterials. This research aimed to prepare and characterize Sr-doped FA nanopowders (Sr-FA). Sr-FA with different Sr contents was prepared by sol-gel method. The designated degree of substitution of Ca by Sr in the mixture was determined by the x value in the general formula of (Ca10-x Srx(PO4)6F2), where x=0,0.5,1. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques were utilized to characterize the obtained nano powders. Results showed that Sr ions entered into the fluorapatite lattice and occupied Ca sites. The incorporation of Sr ions into the fluorapatite resulted in the increase of the lattice parameters.

Fabrication of silica ceramic membrane via sol-gel dip-coating method at different nitric acid amount

Science.gov (United States)

Kahlib, N. A. Z.; Daud, F. D. M.; Mel, M.; Hairin, A. L. N.; Azhar, A. Z. A.; Hassan, N. A.

2018-01-01

Fabrication of silica ceramics via the sol-gel method has offered more advantages over other methods in the fabrication of ceramic membrane, such as simple operation, high purity homogeneous, well defined-structure and complex shapes of end products. This work presents the fabrication of silica ceramic membrane via sol-gel dip-coating methods by varying nitric acid amount. The nitric acid plays an important role as catalyst in fabrication reaction which involved hydrolysis and condensation process. The tubular ceramic support, used as the substrate, was dipped into the sol of Tetrethylorthosilicate (TEOS), distilled water and ethanol with the addition of nitric acid. The fabricated silica membrane was then characterized by (Field Emission Scanning Electron Microscope) FESEM and (Fourier transform infrared spectroscopy) FTIR to determine structural and chemical properties at different amount of acids. From the XRD analysis, the fabricated silica ceramic membrane showed the existence of silicate hydrate in the final product. FESEM images indicated that the silica ceramic membrane has been deposited on the tubular ceramic support as a substrate and penetrate into the pore walls. The intensity peak of FTIR decreased with increasing of amount of acids. Hence, the 8 ml of acid has demonstrated the appropriate amount of catalyst in fabricating good physical and chemical characteristic of silica ceramic membrane.

The Influence of Microgravity on Silica Sol-Gel Formation

Science.gov (United States)

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)

2000-01-01

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.

Sol-gel bonding of silicon wafers

International Nuclear Information System (INIS)

Barbe, C.J.; Cassidy, D.J.; Triani, G.; Latella, B.A.; Mitchell, D.R.G.; Finnie, K.S.; Bartlett, J.R.; Woolfrey, J.L.; Collins, G.A.

2005-01-01

Low temperature bonding of silicon wafers was achieved using sol-gel technology. The initial sol-gel chemistry of the coating solution was found to influence the mechanical properties of the resulting bonds. More precisely, the influence of parameters such as the alkoxide concentration, water-to-alkoxide molar ratio, pH, and solution aging on the final bond morphologies and interfacial fracture energy was studied. The thickness and density of the sol-gel coating were characterised using ellipsometry. The corresponding bonded specimens were investigated using attenuated total reflectance Fourier transformed infrared spectroscopy to monitor their chemical composition, infrared imaging to control bond integrity, and cross-sectional transmission electron microscopy to study their microstructure. Their interfacial fracture energy was measured using microindentation. An optimum water-to-alkoxide molar ratio of 10 and hydrolysis water at pH = 2 were found. Such conditions led to relatively dense films (> 90%), resulting in bonds with a fracture energy of 3.5 J/m 2 , significantly higher than those obtained using classical hydrophilic bonding (typically 1.5-2.5 J/m 2 ). Ageing of the coating solution was found to decrease the bond strength

Direct synthesis of La9.33Si6O26 ultrafine powder via sol-gel self-combustion method

International Nuclear Information System (INIS)

Tian Changan; Liu Junliang; Cai Jun; Zeng Yanwei

2008-01-01

Single phase La 9.33 Si 6 O 26 ultrafine powder, as a kind of highly activated precursor to prepare medium-to-low temperature electrolyte for solid oxide fuel cells (SOFCs), has been successfully synthesized via a non-aqueous sol-gel and self-combustion approach from the starting materials: lanthanum nitrate (La(NO 3 ) 3 .6H 2 O), citric acid, ethylene glycol (EG), tetraethyl orthosilicate (TEOS) and ammonium nitrate. The details of gel's self-combustion were investigated by DTA-TG and the structural characterization of as-synthesized powder from self-combustion was performed by XRD and SEM. The results show that La 9.33 Si 6 O 26 single phase of apatite-type crystal structure can be directly synthesized by sol-gel self-combustion method without further calcinations on the condition that the molar ratio (R) of NO 3 - to citric acid and ethylene glycol being 6:1. Such powders composed of well-dispersed particles with an average size of 200 nm and a specific surface area of 5.54 m 2 /g. It can be sintered to 90% of its theoretical density at 1500 deg. C for 10 h, about 200 deg. C lower than the sintering temperature for the powder derived from traditional solid reactions. The sintered material has a thermal expansion coefficient of 9.2 x 10 -6 K -1 between room temperature and 800 deg. C

Deposition of sol-gel sensor spots by nanoimprint lithography and hemi-wicking

DEFF Research Database (Denmark)

Mikkelsen, Morten Bo Lindholm; Marie, Rodolphe; Hansen, Jan H.

2011-01-01

We present a method for homogeneous deposition of sol-gel sensor materials, which enable fabrication of sensor spots for optical pH and oxygen measurements inside plastic containers. A periodic pattern of posts is imprinted into a polycarbonate substrate and, using the principle of hemi-wicking, ......We present a method for homogeneous deposition of sol-gel sensor materials, which enable fabrication of sensor spots for optical pH and oxygen measurements inside plastic containers. A periodic pattern of posts is imprinted into a polycarbonate substrate and, using the principle of hemi...

Bactericidal micron-thin sol-gel films prevent pin tract and periprosthetic infection.

Science.gov (United States)

Qu, Haibo; Knabe, Christine; Burke, Megan; Radin, Shula; Garino, Jonathan; Schaer, Thomas; Ducheyne, Paul

2014-08-01

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. Reprint & Copyright © 2014 Association of Military Surgeons of the U.S.

Influence of p H on optical properties of nano structure sol-gel-derived silica films

International Nuclear Information System (INIS)

Heshmatpuor, F.; Adelkhani, H.; Nahavandi, M.; Noorbakhsh Shourabadi, M.

2006-01-01

Sol-gel derived silica films were fabricated by dip-coating onto glass microscope substrates. Film properties such as transmission and surface morphology were monitored as function of dip speed and sol p H. Film transmission was increased with increasing of p H in visible range. The surface morphology of films were investigated with scanning electron microscopy.

Sol-gel coatings on carbon/carbon composites

International Nuclear Information System (INIS)

Sim, S.M.; Krabill, R.M.; Dalzell, W.J. Jr.; Chu, P.Y.; Clark, D.E.

1986-01-01

The need for structural materials that can withstand severe environments up to 4000 0 F has promulgated the investigation of sol-gel derived ceramic and composite coatings on carbon/carbon composite materials. Alumina and zirconia sols have been deposited via thermophoresis on carbon/carbon substrates

Safe and Environmentally Acceptable Sol-Gel-Derived Pyrophoric Pyrotechnics

National Research Council Canada - National Science Library

Simpson, Randall L; Hubble, William; Stevenson, Bradley; Gash, Alexander; Satcher, Joe; Metcalf, Patricia

2004-01-01

...% H2 in Ar, N2, CO2, 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...

Administration of a Sol-Gel Formulation of Phenylephrine Using Low-Temperature Hollow Microneedle for Treatment of Intermittent Fecal Incontinence.

Science.gov (United States)

Lee, Hyunji; Park, Jung-Hwan; Park, Jung Ho

2017-12-01

A low temperature hollow microneedle system was devised to deliver sol-gel transition formulation near the surface of the skin for extended release and local delivery of drug by a non-invasive method. This new system can improve treatment of intermittent fecal incontinence. The low-temperature system was integrated with a hollow microneedle to maintain the low temperature of the sol formulation. Various sol-gel formulations using Pluronic F-127 (PF-127) and Hydroxy-propyl-methyl-cellulose (HPMC) were prepared, and their gelation temperature, flow property, and diffusion retardation were observed. Resting anal sphincter pressure in response to a phenylephrine (PE) sol-gel formulation was measured using an air-charged catheter. The biocompatibility of the sol-gel PE formulation was evaluated by observing the immunological response. When the PF-127 25%, HPMC 1% and PE formulation (PF25-HPMC1-PE) was injected through the peri-anal skin of the rat in vivo, the highest pressure on the anal sphincter muscle occurred at 6-8 h and anal pressure increased and lasted twice as long as with the phosphate-buffered saline (PBS)-PE formulation. There was no significant difference in the number of mast cells after administration into the rat in vivo between the PF25-HPMC1-PE formulation and the PBS-PE formulation. The combination of a low-pain hollow microneedle system and an injectable sol-gel formulation improved the efficacy of treatment of intermittent fecal incontinence. A low-temperature hollow microneedle system using a sol-gel formulation has many applications in medical treatments that require depot effect, local targeting, and pain control.

Tunable Optical Properties of Metal Nanoparticle Sol-Gel Composites

Science.gov (United States)

Smith, David D.; Snow, Lanee A.; Sibille, Laurent; Ignont, Erica

2001-01-01

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.

Study and fabrication of ZnNb2O6 thin films by sol-gel method

International Nuclear Information System (INIS)

Hsu, Cheng-Hsing; Yang, Pai-Chuan; Yang, Hsi-Wen; Yan, Shu-Fong; Tung, Hsin-Han

2011-01-01

Zinc niobium oxide (ZnNb 2 O 6 ) thin films were grown on ITO/glass substrate by sol-gel process. Microstructure and surface morphology of the ZnNb 2 O 6 thin films have been studied by X-ray diffraction and scanning electron microscopy. Optical properties of the ZnNb 2 O 6 thin films were obtained by UV-visible recording spectrophotometer. The dependence of the microstructure, optical transmittance spectra, optical band gap on annealing temperature was also investigated.

Bioactivity of sol-gel-derived TiO2 coating on polyetheretherketone: In vitro and in vivo studies.

Science.gov (United States)

Shimizu, Takayoshi; Fujibayashi, Shunsuke; Yamaguchi, Seiji; Yamamoto, Koji; Otsuki, Bungo; Takemoto, Mitsuru; Tsukanaka, Masako; Kizuki, Takashi; Matsushita, Tomiharu; Kokubo, Tadashi; Matsuda, Shuichi

2016-04-15

A polyetheretherketone (PEEK) surface was modified using a sol-gel-derived TiO2 coating in order to confer bone-bonding ability. To enhance the bonding strength of the coating layer, pretreatment with either O2 plasma or sandblasting was performed prior to sol-gel coating. Additionally, post-treatment with acid was carried out to confer apatite (calcium phosphate)-forming ability to the surface. Biomechanical and histological analyses performed using an in vivo rabbit tibia model showed that PEEK surfaces modified with sol-gel-derived TiO2 and acid post-treatment had better bone-bonding properties than uncoated PEEK surfaces. These modified surfaces also performed well in terms of their in vitro cell responses due to their modified surface chemistries and topographies. Although O2 plasma or sandblasting treatment were, for the most part, equivocal in terms of performance, we conclude that sol-gel-derived TiO2 coating followed by acid post-treatment significantly improves the bone bonding ability of PEEK surfaces, thus rendering them optimal for their use in surgical implants. The role of polyetheretherketone (PEEK) as an alternative biomaterial to conventional metallic implant materials has become increasingly important. However, its low bone bonding ability is yet to be resolved. This in vivo and in vitro investigation on the functionalization of PEEK surfaces highlights the utility of this material in clinical interventions that require implants, and may extend range of applications of PEEK. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Sol-gel based sensor for selective formaldehyde determination

Energy Technology Data Exchange (ETDEWEB)

Bunkoed, Opas [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Davis, Frank [Cranfield Health, Cranfield University, Bedford MK43 0AL (United Kingdom); Kanatharana, Proespichaya, E-mail: proespichaya.K@psu.ac.th [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Thavarungkul, Panote [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Physics, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Higson, Seamus P.J., E-mail: s.p.j.higson@cranfield.ac.uk [Cranfield Health, Cranfield University, Bedford MK43 0AL (United Kingdom)

2010-02-05

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.

Sol-gel based sensor for selective formaldehyde determination

International Nuclear Information System (INIS)

Bunkoed, Opas; Davis, Frank; Kanatharana, Proespichaya; Thavarungkul, Panote; Higson, Seamus P.J.

2010-01-01

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 β-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.

SOL-Gel microspheres and nanospheres for controlled release applications

International Nuclear Information System (INIS)

Barbe, C.; Beyer, R.; Kong, L.; Blackford, M.; Trautman, R.; Bartlett, J.

2002-01-01

one hour. The particles thus produced were washed with cyclohexane and carefully dried. Release Kinetics. The release of the encapsulated species from the particles was monitored by placing a fixed quantity of the sample in water or physiological saline, and monitoring the concentration of the released species using UV/Vis spectroscopy. The fraction released was normalised to the total mass initially encapsulated. The influence of the emulsion chemistry on the size of the microspheres obtained at pH 2 is illustrated in Figure 1 for microspheres containing encapsulated Orange II Using essentially identical sol-gel chemistries, particles with dimensions ranging from 50 nm to 50 μm can be readily obtained. The size of the particles is controlled by the size of the emulsion droplets, which act as micro-reactors for the sol-gel reactions. In turn, the size of the droplets is determined predominantly by the hydrophile/lipophile balance of the surfactant/ solvent couple and by processing parameters such as the water to surfactant ratio and the concentration of surfactant. The effect of sol-gel processing parameters on the morphology and associated release kinetics is illustrated in Figure 2. Although both samples have essentially identical particle sizes (not shown), their morphologies are significantly different. Processing under acidic conditions leads to the formation of nanosized linear silicate 'building block' which are woven tightly together in the final gel matrix, to produce a microporous material (pore diameters 2 nm). The different morphologies are clearly reflected in the release rate of the encapsulated species from the respective matrices; rapid release kinetics are evident for the mesoporous material (high pH), while significantly slower release rates are obtained for the microporous material (low pH). A combined sol-gel/emulsion processing method has been developed to produce inorganic matrices with tailored nanostructures containing encapsulated organic and

Positron annihilation lifetime studies of sol-gel transition of carrageenan gels

International Nuclear Information System (INIS)

Wakabayashi, Y.; Ito, K.; Li, H.L.; Ujihara, Y.

1996-01-01

Positron annihilation lifetime measurement was applied to study the sol-gel transition of anionic polysaccharide aqueous solutions in terms of free-volume parameters the size, intensity, and size distribution of free volumes of the gelation of K-form κ-carrageenan solutions as a function of temperature. Slight variations of free volume size and intensity against temperature were observed near 295 K. The correlation of free-volume data with other physical properties vibrational spectra (IR and Raman), conductivity, SAXS, elastic measurement, differential scanning calorimetry were investigated to understand the mechanism of sol-gel transition of carrageenan. (author)

The influence of precursor addition order on the porosity of sol-gel bioactive glasses.

Science.gov (United States)

Fernando, Delihta; Colon, Pierre; Cresswell, Mark; Journet, Catherine; Pradelle-Plasse, Nelly; Jackson, Phil; Grosgogeat, Brigitte; Attik, Nina

2018-06-16

The superior textural properties of sol-gel derived bioactive glasses compared to conventional melt quench glasses accounts for their accelerated bioactivity in vitro. Several studies have explored ways to improve the surface properties of sol-gel glasses in order to maximise their efficiency for bone and tooth regeneration. In this study, we investigated the effect of order of network modifying precursor addition on the textural properties of sol-gel derived bioactive glasses. The effect of precursor addition order on the glass characteristics was assessed by switching the order of network modifying precursor (calcium acetate monohydrate and sodium acetate anhydrous) addition for a fixed composition of bioactive glass (75SiO 2 :5CaO:10Na 2 O:10P 2 O 5 ). The results of this study showed that the order of precursor addition does influence the porosity of these glasses. For the glasses of a fixed composition and preparation conditions we achieved a doubling of surface area, a 1.5 times increase in pore volume and a 1.2 times decrease in pore size just by the mixing the network modifying precursors and adding them together in the sol-gel preparation. This simple and straightforward route adaptation to the preparation of bioactive glasses would allow us to enhance the textural properties of existing and novel composition of bioactive glasses and thus accelerate their bioactivity. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

Sol-gel-cum-hydrothermal synthesis of mesoporous Co-Fe@Al2O3 ...

Indian Academy of Sciences (India)

Oxides; sol-gel; adsorption; surface properties; composite materials. 1. Introduction. Industrial dyes ... acid green 25, Congo red, N719), phenolic compounds. (bromophenol blue .... microscopy (TEM) images were obtained using Philips CM.

Study of Different Sol-Gel Coatings to Enhance the Lifetime of PDMS Devices: Evaluation of Their Biocompatibility.

Science.gov (United States)

Aymerich, María; Gómez-Varela, Ana I; Álvarez, Ezequiel; Flores-Arias, María T

2016-08-25

A study of PDMS (polydimethylsiloxane) sol-gel-coated channels fabricated using soft lithography and a laser direct writing technique is presented. PDMS is a biocompatible material that presents a high versatility to reproduce several structures. It is widely employed in the fabrication of preclinical devices due to its advantages but it presents a rapid chemical deterioration to organic solvents. The use of sol-gel layers to cover the PDMS overcomes this problem since it provides the robustness of glass for the structures made with PDMS, decreasing its deterioration and changing the biocompatibility of the surface. In this work, PDMS channels are coated with three different kinds of sol-gel compositions (60MTES/40TEOS, 70MTES/30TISP and 80MTES/20TISP). The endothelial cell adhesion to the different coated devices is evaluated in order to determine the most suitable sol-gel preparation conditions to enhance cellular adhesion.

Preparation and characterization of Mn-doped Li{sub 0.06}(Na{sub 0.5}K{sub 0.5}){sub 0.94}NbO{sub 3} lead-free piezoelectric ceramics with surface sol-gel coatings

Energy Technology Data Exchange (ETDEWEB)

Yoo, Ae Ri; Lee, Seong Eui; Lee, Hee Chul [Korea Polytechnic University, Shiheung (Korea, Republic of)

2014-08-15

This study investigated the effects of Mn doping and sol-gel surface coating on the structural and the electrical properties of lead-free Li{sub 0.06}(K{sub 0.5}Na{sub 0.5}){sub 0.94}NbO{sub 3}(LNKN) ceramics in disc form for use as eco-friendly piezoelectric devices. The 1-mol% Mn-doped LNKN ceramic showed a relatively high piezoelectric constant owing to its high density in the case of its being annealed at a temperature of 1010 .deg. C. A Mn-doped LNKN sol-gel solution with the same composition as that of the ceramics was spin-coated and sintered on both sides of the ceramic surfaces to acquire improved electrical properties. The sol-gel surface coating could play a decisive role in filling the pores, resulting in flat and stable interfaces between the electrodes and the piezoelectric elements. As a result, the highest piezoelectric constant, d{sub 33}, of 173 pC/N could be obtained for the Mn-doped LNKN ceramics with 420-nm-thick sol-gel surface coatings.

Ceramic protective coatings applied by sol-gel or electrophoresis

International Nuclear Information System (INIS)

Stoch, A.

1993-01-01

Sol-gel and electrophoresis are the complementary techniques which may be used for obtaining the ceramic coatings. The composition of such a coatings depends on the composition of electrophoresis bath or sol solution. Thermal treatment is used for densifying the coating and promoting the adherence of coating to the substrate. In presented work silica, silica-alumina or alumina coatings are applied by sol-gel dip coating procedure on steel, aluminium or ceramic substrates. Electrophoresis is employed for obtaining zirconia, alumina or hydroxyapatite coatings on stainless steel. (author). 7 refs

Preparation and characterization of sol-gel derived TiO2 films

International Nuclear Information System (INIS)

Hong, Y.J.; Brungs, M.P.; Chaplin, R.P.; Sizgek, E.

2001-01-01

Crack-free transparent titania films have been prepared through a new sol-gel process combined with hydrogen peroxide treatment. Hydrogen peroxide and HCl were used to dissolve amorphous titania powder which is obtained by drying common sol-gel titania sol. The peroxo-titania sol produced a thicker film than the common sol-gel titania sol due to a higher degree of condensation. Film thickness could be further increased by controlled drying conditions of the amorphous titania powder or 'aging' the sol. Polyethylene glycol (PEG) and chemical additives were effective in controlling condensation rate by preventing rapid condensation during curing of the film. When these two components were incorporated, it was possible to create a 0.5μm transparent film and PEG could also control the porosity of the film. The cured film was analysed by XRD and Raman spectroscopy. In order to measure the reflective index and thickness of the titania film, an ellipsometer was used. Copyright (2001) The Australian Ceramic Society

Stoichiometric hydroxyapatite obtained by precipitation and sol gel processes

Energy Technology Data Exchange (ETDEWEB)

Guzman V, C.; Pina B, C.; Munguia, N. [IIM-UNAM, A.P. 70-360, 04510 Mexico D.F. (Mexico)]. e-mail: caroguz@servidor.unam.mx

2005-07-01

Three methods for obtaining hydroxyapatite (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 alkoxides. The products were characterized and compared. The observed differences are important for practical applications. (Author)

Electroluminescence of zinc oxide thin-films prepared via polymeric precursor and via sol-gel methods

International Nuclear Information System (INIS)

Lima, S.A.M.; Cremona, M.; Davolos, M.R.; Legnani, C.; Quirino, W.G.

2007-01-01

Zinc oxide (ZnO) is an electroluminescent (EL) material that can emit light in different regions of electromagnetic spectrum when electrically excited. Since ZnO is chemically stable, inexpensive and environmentally friendly material, its EL property can be useful to construct solid-state lamps for illumination or as UV emitter. We present here two wet chemical methods to prepare ZnO thin-films: the Pechini method and the sol-gel method, with both methods resulting in crystalline and transparent films with transmittance >85% at 550 nm. These films were used to make thin-film electroluminescent devices (TFELD) using two different insulator layers: lithium fluoride (LiF) or silica (SiO 2 ). All the devices exhibit at least two wide emission bands in the visible range centered at 420 nm and at 380 nm attributed to the electronic defects in the ZnO optical band gap. Besides these two bands, the device using SiO 2 and ZnO film obtained via sol-gel exhibits an additional band in the UV range centered at 350 nm which can be attributed to excitonic emission. These emission bands of ZnO can transfer their energy when a proper dopant is present. For the devices produced the voltage-current characteristics were measured in a specific range of applied voltage

Effect of sol concentration on the properties of ZnO thin films prepared by sol-gel technique

International Nuclear Information System (INIS)

Dutta, M.; Mridha, S.; Basak, D.

2008-01-01

ZnO thin films are deposited on the glass substrates by sol-gel drain coating technique by varying the concentration of the sol. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis were used to investigate the effect of sol concentration on the crystallinity and surface morphology of the films. The results show that with increase in sol concentration, the value of full width at half maximum (FWHM) of (0 0 2) peak decreases while the strain first increases and then decreases. The sol with higher concentration results in the increase in the grain size. The studies on the optical properties show that the band gap value increases from 3.27 to 3.3 eV when the sol concentration changes from 0.03 to 0.1 M. The photoconductivity studies reveal that the film for 0.05 M sol shows the maximum photoresponse for ultraviolet (UV) wavelength (<400 nm) which is co-related with the deep-level defects. The growth and decay of the photocurrent is found to be slowest for the same film

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

DEFF Research Database (Denmark)

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

2011-01-01

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...

Synthesis and characterization of nanosized MgxMn1−xFe2O4 ferrites by both sol-gel and thermal decomposition methods

International Nuclear Information System (INIS)

De-León-Prado, Laura Elena; Cortés-Hernández, Dora Alicia; Almanza-Robles, José Manuel; Escobedo-Bocardo, José Concepción; Sánchez, Javier; Reyes-Rdz, Pamela Yajaira; Jasso-Terán, Rosario Argentina; Hurtado-López, Gilberto Francisco

2017-01-01

This work reports the synthesis of Mg x Mn 1−x Fe 2 O 4 (x=0–1) nanoparticles by both sol-gel and thermal decomposition methods. In order to determine the effect of synthesis conditions on the crystal structure and magnetic properties of the ferrites, the synthesis was carried out varying some parameters, including composition. By both methods it was possible to obtain ferrites having a single crystalline phase with cubic inverse spinel structure and a behavior near to that of superparamagnetic materials. Saturation magnetization values were higher for materials synthesized by sol-gel. Furthermore, in both cases particles have a spherical-like morphology and nanometric sizes (11–15 nm). Therefore, these materials can be used as thermoseeds for the treatment of cancer by magnetic hyperthermia. - Highlights: • Mg–Mn ferrites were synthesized by sol-gel and thermal decomposition methods. • Materials showed a single cubic inverse spinel crystalline structure. • Ferrites have a soft ferrimagnetic behavior close to superparamagnetic materials.

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

Directory of Open Access Journals (Sweden)

Antonio A. S. Alfaya

2002-09-01

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.

Synthesis of Alkylpoly glucoside from Dextrose-Decanol in the Presence of Silicotungstic Acid Sol-Gel Catalyst

International Nuclear Information System (INIS)

Izazi Azzahidah Amin; Mohd Ambar Yarmo; Nik Idris Nik Yusoff

2013-01-01

The purpose of this study is to synthesis alkylpoly glucoside via condensation of decanol with dextrose in the presence of heterogenous catalyst. In this study, silicotungstic acid sol-gel (STSG) prepared using sol-gel was used as solid acid catalyst. The catalyst was characterized using BET surface area measurement, X-ray Diffraction (XRD) and X-ray Photoelectron Spectroscopy (XPS) surface analysis. The final product was easy to be separated from catalyst without the need of a further neutralization. Silicotungstic acid sol-gel has been found efficient to be solid catalyst for synthesis alkylpoly glucosides. Condensation reaction was carried out 8 hours at 110-120 degree Celsius under vacuum condition at 10 mmHg. The determination of decyl glucoside has been achieved by LC/ ESI-MS/ MS (ToF) giving a mass peak at m/z = 343.2 correspond to the m/z of [M+Na] + . Alkylpoly glucoside produced was analysed by FTIR, 1 H and 13 C NMR spectrometric technique. (author)

Spectroscopic and electrochemical characterization of cytochrome c encapsulated in a bio sol-gel matrix.

Science.gov (United States)

Deriu, Daniela; Pagnotta, Sara Emanuela; Santucci, Roberto; Rosato, Nicola

2008-08-01

Sol-gel technique represents a remarkably versatile method for protein encapsulation. To enhance sol-gel biocompatibility, systems envisaging the presence of calcium and phosphates in the sol-gel composition were recently prepared and investigated. Unfortunately, the low pH at which solutions were prepared (pH proteins, because the acidic environment induces protein denaturation. In this paper we apply a new protocol based on the introduction of calcium nitrate to the inorganic phase, with formation of a binary bioactive system. In this case protein encapsulation results versatile and secure, being achieved at a pH close to neutrality (pH 6.0); also, the presence of calcium is expected to enhance system biocompatibility. To determine the properties of the salt-doped sol-gel and the influence exerted on entrapped biosystems, the structural and functional properties of embedded cytochrome c have been investigated. Data obtained indicate that the salt-doped sol-gel induces no significant change in the structure and the redox properties of the embedded protein; also, the matrix increases protein stability. Interestingly, the presence of calcium nitrate appears determinant for refolding of the acid-denatured protein. This is of interest in the perspective of future applications in biosensoristic area.

Mechanical and thermal expansion properties of β-eucryptite prepared by sol-gel methods and hot pressing

International Nuclear Information System (INIS)

Xia, L.; Wen, G.W.; Qin, C.L.; Wang, X.Y.; Song, L.

2011-01-01

Research highlights: → Dense LAS glass-ceramics were fabricated by sol-gel and hot pressing technique. → The LAS glass-ceramics have relative good mechanical properties. → The negative thermal expansion behavior of LAS glass-ceramics was investigated. -- Abstract: The microstructures, mechanical properties and thermal expansion behavior of monolithic lithium aluminosilicate glass-ceramics, prepared by sol-gel method and hot pressing, were investigated by using X-ray diffraction, scanning and transmission electron microscopies, three-point bend tests and dilatometry. β-eucryptite appeared as main phase in the monolithic lithium aluminosilicate glass-ceramics. The glass ceramics exhibited high relative densities and the average flexural strength and fracture toughness values were 154 MPa and 2.46 MPa m 1/2 , respectively. The lithium aluminosilicate glass-ceramics hot pressed 1300 and 1350 o C demonstrated negative coefficient of thermal expansion, which was affected by amount and type of crystalline phases.

Water-based sol-gel synthesis of hydroxyapatite: process development.

Science.gov (United States)

Liu, D M; Troczynski, T; Tseng, W J

2001-07-01

Hydroxyapatite (HA) ceramics were synthesized using a sol-gel route with triethyl phosphite and calcium nitrate as phosphorus and calcium precursors, respectively. Two solvents, water and anhydrous ethanol, were used as diluting media for HA sol preparation. The sols were stable and no gelling occurred in ambient environment for over 5 days. The sols became a white gel only after removal of the solvents at 60 degrees C. X-ray diffraction showed that apatitic structure first appeared at a temperature as low as 350 degrees C. The crystal size and the HA content in both gels increase with increasing calcination temperature. The type of initial diluting media (i.e., water vs. anhydrous ethanol) did not affect the microstructural evolution and crystallinity of the resulting HA ceramic. The ethanol-based sol dip-coated onto a Ti substrate, followed by calcination at 450 degrees C, was found to be porous with pore size ranging from 0.3 to 1 microm. This morphology is beneficial to the circulation of physiological fluid when the coating is used for biomedical applications. The satisfactory adhesion between the coating and substrate suggests its suitability for load-bearing uses.

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

Science.gov (United States)

Shalev, Moran; Miriam, Altstein

2011-01-01

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-hydroxyethyl)orthosilicate (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. PMID:28880001

Extraction of Silica from Cassava Periderm using Modified Sol-Gel ...

African Journals Online (AJOL)

Akorede

6School of Chemical and Metallurgical Engineering, Faculty of Engineering and the Built ... glycol as capping agent in modified sol-gel method for ..... Effect of Organic Acid Treatment on the Properties of ... Journal of Analytical and Applied.

Sol-gel antireflective coating on plastics

Science.gov (United States)

Ashley, Carol S.; Reed, Scott T.

1990-01-01

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.

Salt-assisted and salt-suppressed sol-gel transitions of methylcellulose in water.

Science.gov (United States)

Xu, Y; Wang, C; Tam, K C; Li, L

2004-02-03

The effects of various salts on the sol-gel transition of aqueous methylcellulose (MC) solutions have been studied systematically by means of a micro differential scanning calorimeter. It was found that the heating process was endothermic while the cooling process was exothermic for both MC solutions with and without salts. The addition of salts did not change the patterns of gelation and degelation of MC. However, the salts could shift the sol-gel transition and the gel-sol transition to lower or higher temperatures from a pure MC solution, depending on the salt type. These opposite effects were termed the salt-assisted and salt-suppressed sol-gel transitions. Either the salt-assisted transition or the salt-suppressed sol-gel transition was a function of salt concentration. In addition, each salt was found to have its own concentration limit for producing a stable aqueous solution of MC at a given concentration of MC, which was related to the anionic charge density of the salt. Cations were proved to have weaker effects than anions. The "salt-out strength", defined as the salt effect per mole of anion, was obtained for each anion studied. The thermodynamic mechanisms involved in the salt-assisted and salt-suppressed sol-gel transitions are discussed.

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

Science.gov (United States)

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

2016-10-07

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.

Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

International Nuclear Information System (INIS)

Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve; Berthier, Serge

2008-01-01

An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C

Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

Energy Technology Data Exchange (ETDEWEB)

Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve [Unite mixte CNRS/Saint Gobain Saint Gobain Recherche, BP135, 93303 Aubervilliers (France); Berthier, Serge [Institut des Nanosciences de Paris, UMR 7588, CNRS, Universite Pierre et Marie Curie-Paris 6, 140 rue Lourmel, 75015 Paris (France)], E-mail: cperoz@lbl.gov

2008-12-01

An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C.

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

Directory of Open Access Journals (Sweden)

Muhammad Aqeel eAshraf

2015-08-01

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.

Coating of the orthopaedic titanium alloys with sol-gel derived hydroxyapatite

International Nuclear Information System (INIS)

Milev, A.; Green, D.; Chai, C.S.; Ben-Nissan, B.

1999-01-01

Hydroxyapatite (HAp) is known to be both biocompatible and bioactive material, however, due to its poor mechanical properties and design limitations is not suitable for applying as a load bearing implant. This could be overcome by using appropriate metallic substrates covered with HAp, derived via different techniques. These coatings allow improved adhesion strength of the load bearing substrate to the bone, resulting in shorter healing periods as well as predictable behaviour of the implant for longer periods of time. There are different techniques of producing HAp appropriate for coating purposes. Due to the small particle size of the grains derived, sol-gel route is preferable where lower sintering temperatures are of primary importance. For better adhesion between substrate and hydroxyapatite coating, the surface of titanium substrate, in this study, was converted to titanium nitride and/or oxynitride. Sintering temperatures of 900 deg C have been used for producing crystalline HAp coatings. The control of sol-gel solutions and the analysis of the coatings were carried out using XRD, SEM and DTA techniques. Results obtained indicate high quality HAp coatings can be produced on titanium substrates especially with complex shapes that benefits over the other coating methods

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

Science.gov (United States)

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

2017-11-01

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 (TiO 2 ) coating, zirconia with sol-gel derived zirconia (ZrO 2 ) 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 TiO 2 coated and ZrO 2 coated groups (5.7 and 5.4, respectively) were lower than the control (8.0). Specimens coated with ZrO 2 showed significantly lower fibroblast proliferation compared to other groups (p sol-gel derived coatings have no influence on the flexural strength of zirconia. ZrO 2 coated specimens showed significantly lower cell proliferation after 12 days than TiO 2 coated or non-coated control. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 2401-2407, 2017. © 2016 Wiley Periodicals, Inc.

Structural and electrical characteristics of ZrO2-TiO2 thin films by sol-gel method

International Nuclear Information System (INIS)

Hsu, Cheng-Hsing; Tseng, Ching-Fang; Lai, Chun-Hung; Tung, Hsin-Han; Lin, Shih-Yao

2010-01-01

In this paper, we investigated electrical properties and microstructures of ZrTiO 4 (ZrO 2 -TiO 2 ) thin films prepared by the sol-gel method on ITO substrates at different annealing temperatures. All films exhibited ZrTiO 4 (1 1 1) and (1 0 1) orientations perpendicular to the substrate surface, and the grain size increased with increase in the annealing temperature. A low leakage current density of 2.06 x 10 -6 A/cm 2 was obtained for the prepared films. Considering the primary memory switching behavior of ZrTiO 4 , ReRAM based on ZrTiO 4 shows promise for future nonvolatile memory applications.

Amoeba-like self-oscillating polymeric fluids with autonomous sol-gel transition.

Science.gov (United States)

Onoda, Michika; Ueki, Takeshi; Tamate, Ryota; Shibayama, Mitsuhiro; Yoshida, Ryo

2017-07-13

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.

Electrochemical impedimetric sensor based on molecularly imprinted polymers/sol-gel chemistry for methidathion organophosphorous insecticide recognition.

Science.gov (United States)

Bakas, Idriss; Hayat, Akhtar; Piletsky, Sergey; Piletska, Elena; Chehimi, Mohamed M; Noguer, Thierry; Rouillon, Régis

2014-12-01

We report here a novel method to detect methidathion organophosphorous insecticides. The sensing platform was architected by the combination of molecularly imprinted polymers and sol-gel technique on inexpensive, portable and disposable screen printed carbon electrodes. Electrochemical impedimetric detection technique was employed to perform the label free detection of the target analyte on the designed MIP/sol-gel integrated platform. The selection of the target specific monomer by electrochemical impedimetric methods was consistent with the results obtained by the computational modelling method. The prepared electrochemical MIP/sol-gel based sensor exhibited a high recognition capability toward methidathion, as well as a broad linear range and a low detection limit under the optimized conditions. Satisfactory results were also obtained for the methidathion determination in waste water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication of carbon microcapsules containing silicon nanoparticles-carbon nanotubes nanocomposite by sol-gel method for anode in lithium ion battery

Science.gov (United States)

Bae, Joonwon

2011-07-01

Carbon microcapsules containing silicon nanoparticles (Si NPs)-carbon nanotubes (CNTs) nanocomposite (Si-CNT@C) have been fabricated by a surfactant mediated sol-gel method followed by a carbonization process. Silicon nanoparticles-carbon nanotubes (Si-CNT) nanohybrids were produced by a wet-type beadsmill method. To obtain Si-CNT nanocomposites with spherical morphologies, a silica precursor (tetraethylorthosilicate, TEOS) and polymer (PMMA) mixture was employed as a structure-directing medium. Thus the Si-CNT/Silica-Polymer microspheres were prepared by an acid catalyzed sol-gel method. Then a carbon precursor such as polypyrrole (PPy) was incorporated onto the surfaces of pre-existing Si-CNT/silica-polymer to generate Si-CNT/Silica-Polymer@PPy microspheres. Subsequent thermal treatment of the precursor followed by wet etching of silica produced Si-CNT@C microcapsules. The intermediate silica/polymer must disappear during the carbonization and etching process resulting in the formation of an internal free space. The carbon precursor polymer should transform to carbon shell to encapsulate remaining Si-CNT nanocomposites. Therefore, hollow carbon microcapsules containing Si-CNT nanocomposites could be obtained (Si-CNT@C). The successful fabrication was confirmed by scanning electron microscopy (SEM) and X-ray diffraction (XRD). These final materials were employed for anode performance improvement in lithium ion battery. The cyclic performances of these Si-CNT@C microcapsules were measured with a lithium battery half cell tests.

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

Directory of Open Access Journals (Sweden)

YASSUKO IAMAMOTO

2000-03-01

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.

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

Science.gov (United States)

Iamamoto; Sacco; Biazzotto; Ciuffi; Serra

2000-01-01

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.

Adjustable rheology of fumed silica dispersion in urethane prepolymers: Composition-dependent sol and gel behaviors and energy-mediated shear responses

Energy Technology Data Exchange (ETDEWEB)

Zheng, Zhong, E-mail: 11329038@zju.edu.cn; Song, Yihu, E-mail: s-yh0411@zju.edu.cn; Wang, Xiang, E-mail: 11229036@zju.edu.cn; Zheng, Qiang, E-mail: zhengqiang@zju.edu.cn [MOE Key Laboratory of Macromolecule Synthesis and Functionalization, Department of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027 (China)

2015-07-15

Variation of colloidal and interfacial interactions leads to a microstructural diversity in fumed silica dispersions exhibiting absolutely different sol- or gel-like rheological responses. In this study, fumed silicas with different surface areas (200–400 m{sup 2}/g) and surface characteristics (hydrophilic or hydrophobic) are dispersed into moisture-cured polyurethane. The microstructures investigated using transmission electron microscope are associated perfectly with three different rheological behaviors: (i) Sols with well-dispersed silica aggregates, (ii) weak gels with agglomerate-linked networks, and (iii) strong gels with concentrated networks of large agglomerates. Though sols and gels are well distinguished by shear thickening or sustained thinning response through steady shear flow test, it is interesting that the sols and weak gels exhibit a uniform modulus plateau-softening-hardening-softening response with increasing dynamic strain at frequency 10 rad s{sup −1} while the strong gels show a sustained softening beyond the linear regime. Furthermore, the onset of softening and hardening can be normalized: The two softening are isoenergetic at mechanical energies of 0.3 J m{sup −3} and 10 kJ m{sup −3}. On the other hand, the hardening is initiated by a critical strain of 60%. The mechanisms involved in the generation of the sol- and the gel-like dispersions and their structural evolutions during shear are thoroughly clarified in relation to the polyols, the characteristic and content of silica and the curing catalysts.

Uniform Thin Films of CdSe and CdSe(ZnS) Core(shell) Quantum Dots by Sol-Gel Assembly: Enabling Photoelectrochemical Characterization and Electronic Applications

Science.gov (United States)

Korala, Lasantha; Wang, Zhijie; Liu, Yi; Maldonado, Stephen; Brock, Stephanie L.

2013-01-01

Optoelectronic properties of quantum dot (QD) films are limited by (1) poor interfacial chemistry and (2) non-radiative recombination due to surface traps. To address these performance issues, sol-gel methods are applied to fabricate thin films of CdSe and core(shell) CdSe(ZnS) QDs. High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) imaging with chemical analysis confirms that the surface of the QDs in the sol-gel thin films are chalcogen-rich, consistent with an oxidative-induced gelation mechanism in which connectivity is achieved by formation of dichalcogenide covalent linkages between particles. The ligand removal and assembly process is probed by thermogravimetric, spectroscopic and microscopic studies. Further enhancement of inter-particle coupling via mild thermal annealing, which removes residual ligands and reinforces QD connectivity, results in QD sol-gel thin films with superior charge transport properties, as shown by a dramatic enhancement of electrochemical photocurrent under white light illumination relative to thin films composed of ligand-capped QDs. A more than 2-fold enhancement in photocurrent, and a further increase in photovoltage can be achieved by passivation of surface defects via overcoating with a thin ZnS shell. The ability to tune interfacial and surface characteristics for the optimization of photophysical properties suggests that the sol-gel approach may enable formation of QD thin films suitable for a range of optoelectronic applications. PMID:23350924

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

Science.gov (United States)

Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan

2014-12-01

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.

Waveguide fabrication in UV-photocurable sol-gel materials: Influence of the photoinitiating system

International Nuclear Information System (INIS)

Versace, D.L.; Oubaha, M.; Copperwhite, R.; Croutxe-Barghorn, C.; MacCraith, B.D.

2008-01-01

In this paper we identify and explain the different chemical interactions involved between a sol-gel matrix and photoinitiators used in the fabrication of optical waveguides. A well-established sol-gel matrix composed of 3-methacryloxypropyltrimethoxysilane, zirconium n-propoxide and methacrylic acid was developed, and two different photoinitiators (Irgacure (registered) 819 and 1800) were added to the host matrix. Optical microscopy was used to characterise the structure of the waveguides as a function of the photoinitiator nature and concentration, and aging of the hybrid sol-gel material. It is clearly demonstrated that the width of the waveguides is strongly influenced by the sol aging. Furthermore, it is shown that degradation of photoinitiators occurs during the sol-gel process. Oxidation of the phosphonyl groups by the zirconium complex accounts for this results

Low temperature synthesis of CaO-SiO2 glasses having stable liquid-liquid immiscibility by sol-gel process

Science.gov (United States)

Bansal, Narottam P.

1990-01-01

Calcium silicate glass compositions lying within the liquid-liquid immiscibility dome of the phase diagram, which could not have been prepared by the conventional melting method, were synthesized by the sol-gel process. Hydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) solutions containing up to 20 mol percent calcium nitrate resulted in the formation of clear and transparent gels. The gel formation time decreased with increase in water:TEOS mole ratio, calcium content, and the reaction temperature. Smaller values of gel times in the presence of calcium nitrate are probably caused by lowering of the ionic charge on the sol particles by the salt present. The gelation activation energy, E(sub gel), was evaluated from temperature dependence of the gel time. Presence of Ca(2+) ions or the water:TEOS mole ratio did not have an appreciable effect on the value of E(sub gel). Presence of glycerol in the solution helped in the formation of crack-free monolithic gel specimens. Chemical and structural changes occurring in the gels, as a function of the heat treatments, have been monitored using DTA, TGA, IR-spectroscopy, x ray diffraction, surface area and pore size distribution measurements.

Determination of Insulator-to-Semiconductor Transition in Sol-Gel Oxide Semiconductors Using Derivative Spectroscopy.

Science.gov (United States)

Lee, Woobin; Choi, Seungbeom; Kim, Kyung Tae; Kang, Jingu; Park, Sung Kyu; Kim, Yong-Hoon

2015-12-23

We report a derivative spectroscopic method for determining insulator-to-semiconductor transition during sol-gel metal-oxide semiconductor formation. When an as-spun sol-gel precursor film is photochemically activated and changes to semiconducting state, the light absorption characteristics of the metal-oxide film is considerable changed particularly in the ultraviolet region. As a result, a peak is generated in the first-order derivatives of light absorption ( A' ) vs. wavelength (λ) plots, and by tracing the peak center shift and peak intensity, transition from insulating-to-semiconducting state of the film can be monitored. The peak generation and peak center shift are described based on photon-energy-dependent absorption coefficient of metal-oxide films. We discuss detailed analysis method for metal-oxide semiconductor films and its application in thin-film transistor fabrication. We believe this derivative spectroscopy based determination can be beneficial for a non-destructive and a rapid monitoring of the insulator-to-semiconductor transition in sol-gel oxide semiconductor formation.

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

Energy Technology Data Exchange (ETDEWEB)

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: frrcarrillo@yahoo.com.mx [University of Texas at San Antonio, Department of Physics and Astronomy, San Antonio TX 78249 (United States)

2015-07-01

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)

Novel hybrid sol-gel coatings for corrosion protection of AZ31B magnesium alloy

International Nuclear Information System (INIS)

Lamaka, S.V.; Montemor, M.F.; Galio, A.F.; Zheludkevich, M.L.; Trindade, C.; Dick, L.F.; Ferreira, M.G.S.

2008-01-01

This work aims to develop and study new anticorrosion films for AZ31B magnesium alloy based on the sol-gel coating approach. Hybrid organic-inorganic sols were synthesized by copolymerization of epoxy-siloxane and titanium or zirconium alkoxides. Tris(trimethylsilyl) phosphate was also used as additive to confer additional corrosion protection to magnesium-based alloy. A sol-gel coating, about 5-μm thick, shows good adhesion to the metal substrate and prevents corrosion attack in 0.005 M NaCl solution for 2 weeks. The sol-gel coating system doped with tris(trimethylsilyl)-phosphate revealed improved corrosion protection of the magnesium alloy due to formation of hydrolytically stable Mg-O-P chemical bonds. The structure and the thickness of the sol-gel film were characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The corrosion behaviour of AZ31B substrates pre-treated with the sol-gel derived hybrid coatings was tested by electrochemical impedance spectroscopy (EIS). The chemical composition of the silylphosphate-containing sol-gel film at different depths was investigated by X-ray photoelectron spectroscopy (XPS) with depth profiling

High-power microcavity lasers based on highly erbium-doped sol-gel aluminosilicate glasses

International Nuclear Information System (INIS)

Le Ngoc Chung; Chu Thi Thu Ha; Nguyen Thu Trang; Pham Thu Nga; Pham Van Hoi; Bui Van Thien

2006-01-01

High-power whispering-gallery-mode (WGM) lasing from highly erbium-doped sol-gel aluminosilicate microsphere cavity coupled to a half-tapered optical fiber is presented. The lasing output power as high as 0.45 mW (-3.5 dBm) was obtained from sol-gel glass microsphere cavity with diameters in the range of 40-150 μm. The sol-gel method for making highly concentration Er-doped aluminosilicate glasses with Er-ion concentrations from 0.125 to 0.65 mol% of Er 3+ is described. Controlling collected lasing wavelength at each WGM is possible by adjusting the distance between the half-taper fiber and the microcavity and by diameter of the waist of half-taper fiber. Using the analytic formulas we calculated the TE and TM lasing modes and it is shown that the experimental results are in good agreement with the calculation prediction

Sol-Gel Synthesis Of Aluminoborosilicate Powders

Science.gov (United States)

Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna

1992-01-01

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.

Foldable and Cytocompatible Sol-gel TiO2 Photonics.

Science.gov (United States)

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

2015-09-07

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.

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

Science.gov (United States)

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

2000-01-01

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.

Preparation and studies of Co(II) and Co(III)-substituted barium ferrite prepared by sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Teh, Geok Bee [Department of Bioscience and Chemistry, Faculty of Engineering and Science, Universiti Tunku Abdul Rahman, 53300 Kuala Lumpur (Malaysia)]. E-mail: tehgb@mail.utar.edu.my; Nagalingam, Saravanan [Department of Bioscience and Chemistry, Faculty of Engineering and Science, Universiti Tunku Abdul Rahman, 53300 Kuala Lumpur (Malaysia); Jefferson, David A. [Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW (United Kingdom)

2007-01-15

The sol-gel preparative method was employed to synthesise Co(II) and Co(III)-substituted barium ferrite. This method was attempted to achieve higher homogeneity of the final product. Samples of substituted ferrites were characterised by various experimental techniques including high resolution transmission electron microscopy, X-ray diffraction analysis, magnetometry and thermal gravimetric analysis. The microstructural changes induced by such substitution are also discussed.

Preparation and studies of Co(II) and Co(III)-substituted barium ferrite prepared by sol-gel method

International Nuclear Information System (INIS)

Teh, Geok Bee; Nagalingam, Saravanan; Jefferson, David A.

2007-01-01

The sol-gel preparative method was employed to synthesise Co(II) and Co(III)-substituted barium ferrite. This method was attempted to achieve higher homogeneity of the final product. Samples of substituted ferrites were characterised by various experimental techniques including high resolution transmission electron microscopy, X-ray diffraction analysis, magnetometry and thermal gravimetric analysis. The microstructural changes induced by such substitution are also discussed

Formation of Mg(OH)2 nanowhiskers on LTA zeolite surfaces using a sol–gel method

KAUST Repository

Liu, Junqiang

2011-09-20

A facile three step sol-gel-precipitation process is used to synthesize Mg(OH)2 nanowhiskers on micron-sized zeolite 5A particle surfaces at room temperature. The putative amorphous gelation product, Mg(OH) n(OR)2-n, forms first by a controlled hydrolysis and condensation reaction involving magnesium isopropoxide and water, ultimately leading to precipitation to form Mg(OH)2 structures on the zeolite surface. The optimum conditions for one dimensional Mg(OH)2 whisker formation are found to be six times the stoichiometric amount of water using 1 M HCl as the catalyst for the sol-gel reaction. The one-dimensional Mg(OH) 2 whiskers have an average diameter of 5-10 nm and length of 50-100 nm. The zeolite micropores are not affected by the Mg(OH)2 whiskers formed on the surface. The surface roughened zeolite 5A, with a Mg(OH) 2 content of about 9 wt%, showed improved adhesion between the zeolite and the polymer in a mixed-matrix composite membrane. © 2011 Springer Science+Business Media, LLC.

Effect of Sol Concentration, Aging and Drying Process on Cerium Stabilization Zirconium Gel Produced by External Gelation

Science.gov (United States)

Sukarsono, R.; Rachmawati, M.; Susilowati, S. R.; Husnurrofiq, D.; Nurwidyaningrum, K.; Dewi, A. K.

2018-02-01

Cerium Stabilized Zirconium gel has been prepared using external gelation process. As the raw materials was used ZrO(NO3)2 and Ce(NO3)4 nitrate salt which was dissolved with water into Zr-Ce nitrate mixture. The concentration of the nitrate salt mixture in the sol solution was varied by varying the concentration of zirconium and cerium nitrate in the sol solution and the addition of PVA and THFA to produce a sol with a viscosity of 40-60 cP. The viscosity range of 40-60cP is the viscosity of the sol solution that was easy to produce a good gel in the gelation apparatus. Sol solution was casted in a gelation column equipped with following tools: a 1 mm diameter drip nozzle which was vibrated to adjust the best frequency and amplitude of vibration, a flow meter to measure the flow rate of sol, flowing of NH3 gas to presolidification process. Gelation column was contained NH4OH solution as gelation medium and gel container to collect gel product. Gel obtained from the gelation process than processed with ageing, washing, drying and calcinations to get round gel and not broken at calcinations up to 500°C. The parameters observed in this research are variation of Zr nitrate concentration, Ce nitrate concentration, ratio of Zr and Ce in the sol and ageing and drying process method which was appropriate to get a good gel. From the gelation processes that has been done, it can be seen that with the presolidification process can be obtained a round gel and without presolidification process, produce not round gel. In the process of ageing to get not broken gel, ageing was done on the rotary flask so that during the ageing, gels rotate in gelation media. Gels, then be washed by dilute ammonium nitrate, demireralized water and iso prophyl alcohol. The washed gel was then dried by vacuum drying to form pores on the gel which become the path for the gases resulting from decomposition of the gel to exit the gel. Vacuum drying can prevent cracking because the pores allow the gel

α Fe2O3 films grown by the spin-on sol-gel deposition method

International Nuclear Information System (INIS)

Avila G, A.; Carbajal F, G.; Tiburcio S, A.; Barrera C, E.; Andrade I, E.

2003-01-01

α-Fe 2 O 3 polycrystalline films with grains larger than 31 nm were grown by the spin-on sol-gel deposition method. The particular sol used was prepared starting from two distinct precursor reagents. Both precursors leaded to similar films. Order within the films was altered by adding tin to the samples. Transmittance measurements confirmed that the hematite phase is obtained by annealing the samples above 400 C and yielded an optical gap of about 2.2 eV, but additional transitions at 2.7 eV were also observed. From RBS measurements it was found that tin inclusion decreases iron content as expected, but also increases oxygen concentration within the films. This last observation was associated to the disorder rise when introducing tin atoms. (Author)

Formation of Mg(OH)2 nanowhiskers on LTA zeolite surfaces using a sol–gel method

KAUST Repository

Liu, Junqiang; Bae, Tae-Hyun; Esekhile, Omoyemen; Nair, Sankar; Jones, Christopher W.; Koros, William J.

2011-01-01

A facile three step sol-gel-precipitation process is used to synthesize Mg(OH)2 nanowhiskers on micron-sized zeolite 5A particle surfaces at room temperature. The putative amorphous gelation product, Mg(OH) n(OR)2-n, forms first by a controlled

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

Science.gov (United States)

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

2016-04-01

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. Copyright © 2015 Elsevier Ltd. All rights reserved.

ITO/Poly(Aniline/Sol-Gel Glass: An Optically Transparent, pH-Responsive Substrate for Supported Lipid Bilayers

Directory of Open Access Journals (Sweden)

Ahmed Al-Obeidi

2013-01-01

Full Text Available Described here is fabrication of a pH-sensitive, optically transparent transducer composed of a planar indium-tin oxide (ITO electrode overcoated with a poly(aniline (PANI thin film and a porous sol-gel layer. Adsorption of the PANI film renders the ITO electrode sensitive to pH, whereas the sol-gel spin-coated layer makes the upper surface compatible with fusion of phospholipid vesicles to form a planar supported lipid bilayer (PSLB. The response to changes in the pH of the buffer contacting the sol-gel/PANI/ITO electrode is pseudo-Nernstian with a slope of 52 mV/pH over a pH range of 4–9. Vesicle fusion forms a laterally continuous PSLB on the upper sol-gel surface that is fluid with a lateral lipid diffusion coefficient of 2.2 μm2/s measured by fluorescence recovery after photobleaching. Due to its lateral continuity and lack of defects, the PSLB blocks the pH response of the underlying electrode to changes in the pH of the overlying buffer. This architecture is simpler to fabricate than previously reported ITO electrodes derivatized for PSLB formation and should be useful for optical monitoring of proton transport across supported membranes derivatized with ionophores and ion channels.

Effect of hydrothermal process for inorganic alumina sol on crystal structure of alumina gel

Directory of Open Access Journals (Sweden)

K. Yamamura

2016-09-01

Full Text Available This paper reports the effect of a hydrothermal process for alumina sol on the crystal structure of alumina gel derived from hydrothermally treated alumina sol to help push forward the development of low temperature synthesis of α-Al2O3. White precipitate of aluminum hydroxide was prepared with a homogeneous precipitation method using aluminum nitrate and urea in aqueous solution. The obtained aluminum hydroxide precipitate was peptized by using acetic acid at room temperature, which resulted in the production of a transparent alumina sol. The alumina sol was treated with a hydrothermal process and transformed into an alumina gel film by drying at room temperature. Crystallization of the alumina gel to α-Al2O3 with 900 °C annealing was dominant for a hydrothermal temperature of 100 °C and a hydrothermal time of 60 min, as production of diaspore-like species was promoted with the hydrothermal temperature and time. Excess treatments with hydrothermal processes at higher hydrothermal temperature for longer hydrothermal time prevented the alumina gel from being crystallized to α-Al2O3 because the excess hydrothermal treatments promoted production of boehmite.

Processing, adhesion and electrical properties of silicon steel having non-oriented grains coated with silica and alumina sol-gel

International Nuclear Information System (INIS)

Vasconcelos, D.C.L.; Orefice, R.L.; Vasconcelos, W.L.

2007-01-01

Silicon steels having non-oriented grains are usually coated with a series of inorganic or organic films to be used in electrical applications. However, the commercially available coatings have several disadvantages that include poor adhesion to the substrates, low values of electrical resistance and degradation at higher temperatures. In this work, silica and alumina sol-gel films were deposited onto silicon steel in order to evaluate the possibility of replacing the commercially available coatings by these sol-gel derived materials. Silica and alumina sol-gel coatings were prepared by dipping silicon steel samples into hydrolyzed silicon or aluminum alkoxides. Samples coated with sol-gel films were studied by scanning electron microscopy, energy dispersive spectroscopy and infrared spectroscopy. Adhesion between silicon steel and sol-gel films was measured by using several standard adhesion tests. Electrical properties were evaluated by the Franklin method. Results showed that homogeneous sol-gel films can be deposited onto silicon steel. Thicknesses of the films could be easily managed by altering the speed of deposition. The structure of the films could also be tailored by introducing additives, such as nitric acid and N,N-dimethyl formamide. Adhesion tests revealed a high level of adhesion between coatings and metal. The Franklin test showed that sol-gel films can produce coated samples with electrical resistances suitable for electrical applications. Electrical properties of the coated samples could also be manipulated by altering the structure of the sol-gel films or by changing the thickness of them

Use of CdSe/ZnS luminescent quantum dots incorporated within sol-gel matrix for urea detection

International Nuclear Information System (INIS)

Duong, Hong Dinh; Rhee, Jong Il

2008-01-01

In this work, urea detection techniques based on the pH sensitivity of CdSe/ZnS QDs were developed using three types of sol-gel membranes: a QD-entrapped membrane, urease-immobilized membrane and double layer consisting of a QD-entrapped membrane and urease-immobilized membrane. The surface morphology of the sol-gel membranes deposited on the wells in a 24-well microtiter plate was investigated. The linear detection range of urea was in the range of 0-10 mM with the three types of sol-gel membranes. The urea detection technique based on the double layer consisting of the QD-entrapped membrane and urease-immobilized membrane resulted in the highest sensitivity to urea due to the Michaelis-Menten kinetic parameters. That is, the Michaelis-Menten constant (K m =2.0745 mM) of the free urease in the QD-entrapped membrane was about 4-fold higher than that (K m =0.549 mM) of the immobilized urease in the urease-immobilized membrane and about 12-fold higher than that (K m =0.1698 mM) of the immobilized urease in the double layer. The good stability of the three sol-gel membranes for urea sensing over 2 months showed that the use of sol-gel membranes immobilized with QDs or an enzyme is suitable for biomedical and environmental applications

Use of CdSe/ZnS luminescent quantum dots incorporated within sol-gel matrix for urea detection.

Science.gov (United States)

Duong, Hong Dinh; Rhee, Jong Il

2008-09-19

In this work, urea detection techniques based on the pH sensitivity of CdSe/ZnS QDs were developed using three types of sol-gel membranes: a QD-entrapped membrane, urease-immobilized membrane and double layer consisting of a QD-entrapped membrane and urease-immobilized membrane. The surface morphology of the sol-gel membranes deposited on the wells in a 24-well microtiter plate was investigated. The linear detection range of urea was in the range of 0-10mM with the three types of sol-gel membranes. The urea detection technique based on the double layer consisting of the QD-entrapped membrane and urease-immobilized membrane resulted in the highest sensitivity to urea due to the Michaelis-Menten kinetic parameters. That is, the Michaelis-Menten constant (K(m)=2.0745mM) of the free urease in the QD-entrapped membrane was about 4-fold higher than that (K(m)=0.549mM) of the immobilized urease in the urease-immobilized membrane and about 12-fold higher than that (K(m)=0.1698mM) of the immobilized urease in the double layer. The good stability of the three sol-gel membranes for urea sensing over 2 months showed that the use of sol-gel membranes immobilized with QDs or an enzyme is suitable for biomedical and environmental applications.

Electrochemical corrosion behavior of composite MAO/sol-gel coatings on magnesium alloy AZ91D using combined micro-arc oxidation and sol-gel technique

International Nuclear Information System (INIS)

Shang Wei; Chen Baizhen; Shi Xichang; Chen Ya; Xiao Xiang

2009-01-01

Protective composite coatings were obtained on a magnesium alloy by micro-arc oxidation (MAO) and sol-gel technique. The coatings consisted of a MAO layer and a sol-gel layer. The microstructure and composition of the MAO coating and the composite coatings were analyzed by scanning electron microscopy (SEM) and energy dispersive X-rays (EDX). Potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and total immersion tests were used to evaluate the corrosion behavior of these coatings in a 3.5 wt.% NaCl solution. The results show that the sol-gel layer provides corrosion protection by physically sealing the pores in the MAO coating and acting as a barrier. The composite coatings can suppress the corrosion process by preventing the corrosive ions from transferring or diffusing to the magnesium alloy substrate. This enhances the corrosion resistance of the magnesium alloy AZ91D significantly

Effect of Sn-doped on microstructural and optical properties of ZnO thin films deposited by sol-gel method

International Nuclear Information System (INIS)

Tsay, C.-Y.; Cheng, H.-C.; Tung, Y.-T.; Tuan, W.-H.; Lin, C.-K.

2008-01-01

In this study, transparent thin films of Sn-doped ZnO (ZnO:Sn) were deposited onto alkali-free glass substrates by a sol-gel method; the effect of Sn doping on crystallinity, microstructural and optical properties was investigated. The atomic percentages of dopant in ZnO-based sols were Sn/Zn = 0, 1, 2, 3, and 5 at.%. The as-deposited films were pre-heated at 300 deg. C for 10 min and then annealed in air at 500 deg. C for 1 h. The results show that Sn-doped ZnO thin films demonstrate obviously improved surface roughness, enhanced transmittance in the 400-600 nm wavelength range and reduced average crystallite size. Among all of the annealed ZnO-based films in this study, films doped with 2 at.% Sn concentration exhibited the best properties, namely an average transmittance of 90%, an RMS roughness value of 1.92 nm and a resistivity of 9.3 x 10 2 Ω-cm

Sol-Gel Process for Making Pt-Ru Fuel-Cell Catalysts

Science.gov (United States)

Narayanan, Sekharipuram; Valdez, Thomas; Kumta, Prashant; Kim, Y.

2005-01-01

A sol-gel process has been developed as a superior alternative to a prior process for making platinum-ruthenium alloy catalysts for electro-oxidation of methanol in fuel cells. The starting materials in the prior process are chloride salts of platinum and ruthenium. The process involves multiple steps, is time-consuming, and yields a Pt-Ru product that has relatively low specific surface area and contains some chloride residue. Low specific surface area translates to incomplete utilization of the catalytic activity that might otherwise be available, while chloride residue further reduces catalytic activity ("poisons" the catalyst). In contrast, the sol-gel process involves fewer steps and less time, does not leave chloride residue, and yields a product of greater specific area and, hence, greater catalytic activity. In this sol-gel process (see figure), the starting materials are platinum(II) acetylacetonate [Pt(C5H7O2)2, also denoted Pt-acac] and ruthenium(III) acetylacetonate [Ru(C5H7O2)3, also denoted Ru-acac]. First, Pt-acac and Ru-acac are dissolved in acetone at the desired concentrations (typically, 0.00338 moles of each salt per 100 mL of acetone) at a temperature of 50 C. A solution of 25 percent tetramethylammonium hydroxide [(CH3)4NOH, also denoted TMAH] in methanol is added to the Pt-acac/Ruacac/ acetone solution to act as a high-molecular-weight hydrolyzing agent. The addition of the TMAH counteracts the undesired tendency of Pt-acac and Ru-acac to precipitate as separate phases during the subsequent evaporation of the solvent, thereby helping to yield a desired homogeneous amorphous gel. The solution is stirred for 10 minutes, then the solvent is evaporated until the solution becomes viscous, eventually transforming into a gel. The viscous gel is dried in air at a temperature of 170 C for about 10 hours. The dried gel is crushed to make a powder that is the immediate precursor of the final catalytic product. The precursor powder is converted to the

Study of the Effect of Sol pH and Nanoclay Incorporation on the Corrosion Protection Performance of a Silane Sol-Gel Coating

Directory of Open Access Journals (Sweden)

Najmeh Asadi

2014-06-01

Full Text Available This work is aimed to evaluate the role of nanoclay in the protective performance of an eco-friendly silane sol-gel layer applied on mild steel substrate in 0.1M sodium chloride solution. At the first step, the effect of pH of the silane solution, consisting of a mixture of γ-glycidoxypropiltrimethoxysilane and methyltriethoxysilane and tetraethoxysilane, on the coating performance was evaluated through electrochemical noise measurements. The values of characteristic charge as a parameter extracted from shot noise theory revealed that the sol pH determining the rate of hydrolysis can play an important role in the corrosion protection behavior of silane coatings. Then, the influence of clay nanoparticles on the corrosion protective performance of the hybrid silane film was studied through taking advantage of electrochemical techniques, including electrochemical impedance spectroscopy and polarization curves, as well as surface analysis methods. The obtained electrochemical data including the values of charge transfer resistance, coating resistance, low frequency impedance and corrosion current density showed that the silane sol gel film in the presence of clay nanoparticles can present an improved corrosion protection. The behavior was connected to an enhancement in the coating barrier properties. Moreover, FESEM and water contact angle confirmed the higher reticulation in case of the coating incorporating nanoclay.

Sol-gel processing of bioactive glass nanoparticles: A review.

Science.gov (United States)

Zheng, Kai; Boccaccini, Aldo R

2017-11-01

Silicate-based bioactive glass nanoparticles (BGN) are gaining increasing attention in various biomedical applications due to their unique properties. Controlled synthesis of BGN is critical to their effective use in biomedical applications since BGN characteristics, such as morphology and composition, determining the properties of BGN, are highly related to the synthesis process. In the last decade, numerous investigations focusing on BGN synthesis have been reported. BGN can mainly be produced through the conventional melt-quench approach or by sol-gel methods. The latter approaches are drawing widespread attention, considering the convenience and versatility they offer to tune the properties of BGN. In this paper, we review the strategies of sol-gel processing of BGN, including those adopting different catalysts for initiating the hydrolysis and condensation of silicate precursors as well as those combining sol-gel chemistry with other techniques. The processes and mechanism of different synthesis approaches are introduced and discussed in detail. Considering the importance of the BGN morphology and composition to their biomedical applications, strategies put forward to control the size, shape, pore structure and composition of BGN are discussed. BGN are particularly interesting biomaterials for bone-related applications, however, they also have potential for other biomedical applications, e.g. in soft tissue regeneration/repair. Therefore, in the last part of this review, recently reported applications of BGN in soft tissue repair and wound healing are presented. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

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

2006-01-15

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.

Preparation of Nd-doped gadolinium-gallium garnet laser ceramic powder by sol-gel method

Institute of Scientific and Technical Information of China (English)

YAO Yan-ping; LIU Jing-he

2006-01-01

Preparation of Nd3+:Gd3Ga5O12 polycrystalline material by sol-gel method was preparated in this paper.The structure and the pattern of the sample were analyzed by thermogravimetric analysis and differential thermal analysis(TG-DTA),Infrared spectrum,XRD,TEM and electron spectrum,which indicated that the powder with good characteristics of 70-100 nm can be obtained by sintering at 1 000℃.It was shown that the chemical composition of the sample was agreed with experimental requirements by electron spectrum analysis.

Functionalization of sol-gel zirconia composites with europium complexes

International Nuclear Information System (INIS)

Danchova, Nina; Gutzov, Stoyan

2014-01-01

Different sol-gel strategies based on functionalization of ZrO 2 :Eu microparticles with 1,10-phenanthroline (phen) and incorporation of colloidal Eu(phen) 2 (NO 3 ) 3 into zirconia have been used to obtain hybrid sol-gel composites with controlled optical properties. The process leads to materials with quantum yields of about 48 % monitoring the 615 nm emission line at 350 nm excitation. Excitation/luminescence spectroscopy, diffuse reflectance spectroscopy and X-ray diffraction have been used to characterize the hybrid zirconia composites. (orig.)

Efficacy of a new tan doped sol-gel sorbent for uptake of zinc

International Nuclear Information System (INIS)

Khan, A.; Ahmed, S.; Riaz, M.; Mahmood, F.; Younas Khokhar, M.

2003-01-01

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.)

Characterization and hydrogen gas sensing properties of TiO{sub 2} thin films prepared by sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Haidry, Azhar Ali [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Bratislava (Slovakia); Puskelova, Jarmila [Department of Inorganic Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia); Plecenik, Tomas; Durina, Pavol; Gregus, Jan; Truchly, Martin; Roch, Tomas; Zahoran, Miroslav [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Bratislava (Slovakia); Vargova, Melinda [Department of Inorganic Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia); Kus, Peter; Plecenik, Andrej [Department of Experimental Physics, Faculty of Mathematics, Physics and Informatics, Comenius University, Bratislava (Slovakia); Plesch, Gustav, E-mail: plesch@fns.uniba.sk [Department of Inorganic Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia)

2012-10-15

Highlights: Black-Right-Pointing-Pointer Preparation and characterization of hydrogen sensing TiO{sub 2} thin films by sol-gel method. Black-Right-Pointing-Pointer The annealing effect on the structure, electrical, optical and sensing properties was studied. Black-Right-Pointing-Pointer The best sensitivity show the films composed of rutile with grain size of {approx}100 nm. - Abstract: Thin films of titanium dioxide with thickness of about 150 nm were deposited by spin coating method on a sapphire substrate from a sol-gel and annealed at various temperatures (from 600 Degree-Sign C to 1000 Degree-Sign C). Structural, optical and hydrogen gas sensing properties of the films were investigated. The annealing temperatures from 600 to 800 Degree-Sign C led to anatase phase with grain size in the range of 14-28 nm. Further increase of the annealing temperature resulted in transformation to rutile phase with larger grain size of about 100-120 nm. The optical band gap tended to decrease with increasing annealing temperature. The estimated values of activation energy for charge transport were in the range of 0.6-1.0 eV for films annealed at temperatures from 600 Degree-Sign C to 800 Degree-Sign C and 0.37-0.38 eV for films annealed at 900 Degree-Sign C and 1000 Degree-Sign C. The films annealed at 900 Degree-Sign C and 1000 Degree-Sign C showed better hydrogen sensitivity, what can be at least partially caused by their higher surface roughness.

Low temperature synthesis of CaO-SiO2 glasses having stable liquid-liquid immiscibility by the sol-gel process

Science.gov (United States)

Bansal, N. P.

1992-01-01

Calcium silicate glass compositions lying within the liquid-liquid immiscibility dome of the phase diagram, which could not have been prepared by the conventional melting method, were synthesized by the sol-gel process. Hydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) solutions containing up to 20 mol percent calcium nitrate resulted in the formation of clear and transparent gels. The gel formation time decreased with increase in water: TEOS mole ratio, calcium content, and the reaction temperature. Smaller values of gel times in the presence of calcium nitrate are probably caused by lowering of the ionic charge on the sol particles by the salt present. The gelation activation energy, E(sub gel), was evaluated from temperature dependence of the gel time. Presence of Ca(2+) ions or the water:TEOS mole ratio did not have an appreciable effect on the value of E(sub gel). Presence of glycerol in the solution helped in the formation of crack-free monolithic gel specimens. Chemical and structural changes occurring in the gels, as a function of the heat treatments, have been monitored using DTA, TGA, IR-spectroscopy, X-ray diffraction, surface area and pore size distribution measurements.

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

International Nuclear Information System (INIS)

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

2016-01-01

A pH-responsive surface molecularly imprinted poly(ionic liquids) (MIPILs) was prepared on the surface of multiwall carbon nanotubes (MWCNTs) by a sol-gel technique. The material was synthesized using a 3-aminopropyl triethoxysilane modified multiwall carbon nanotube (MWCNT-APTES) as the substrate, bovine serum albumin (BSA) as the template molecule, an alkoxy-functionalized IL 1-(3-trimethoxysilyl propyl)-3-methyl imidazolium chloride ([TMSPMIM]Cl) as both the functional monomer and the sol-gel catalyst, and tetraethoxysilane (TEOS) as the crosslinking agent. The molecular interaction between BSA and [TMSPMIM]Cl was quantitatively evaluated by UV–vis spectroscopy prior to polymerization so as to identify an optimal template/monomer ratio and the most suitable pH value for the preparation of the MWCNTs@BSA-MIPILs. This strategy was found to be effective to overcome the problems of trial-and-error protocol in molecular imprinting. The optimum synthesis conditions were as follows: template/monomer ratio 7:20, crosslinking agent content 2.0–2.5 mL, temperature 4 °C and pH 8.9 Tris–HCl buffer. The influence of incubation pH on adsorption was also studied. The result showed that the imprinting effect and selectivity improved significantly with increasing incubation pH from 7.7 to 9.9. This is mainly because the non-specific binding from electrostatic and hydrogen bonding interactions decreased greatly with the increase of pH value, which made the specific binding affinity from shape selectivity strengthened instead. The polymers synthesized under the optimal conditions were then characterized by BET surface area measurement, FTIR, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The adsorption capacity, imprinting effect, selective recognition and reusability were also evaluated. The as-prepared MWCNTs@BSA-MIPILs were also found to have a number of advantages including high surface area (134.2 m"2 g"−"1), high adsorption capacity (55

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-08-17

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

Double-Layer Surface Modification of Polyamide Denture Base Material by Functionalized Sol-Gel Based Silica for Adhesion Improvement.

Science.gov (United States)

Hafezeqoran, Ali; Koodaryan, Roodabeh

2017-09-21

Limited surface treatments have been proposed to improve the bond strength between autopolymerizing resin and polyamide denture base materials. Still, the bond strength of autopolymerizing resins to nylon polymer is not strong enough to repair the fractured denture effectively. This study aimed to introduce a novel method to improve the adhesion of autopolymerizing resin to polyamide polymer by a double layer deposition of sol-gel silica and N-2-(aminoethyl)-3-aminopropyltrimethoxysilane (AE-APTMS). The silica sol was synthesized by acid-catalyzed hydrolysis of tetraethylorthosilicate (TEOS) as silica precursors. Polyamide specimens were dipped in TEOS-derived sol (TS group, n = 28), and exposed to ultraviolet (UV) light under O 2 flow for 30 minutes. UV-treated specimens were immersed in AE-APTMS solution and left for 24 hours at room temperature. The other specimens were either immersed in AE-APTMS solution (AP group, n = 28) or left untreated (NT group, n = 28). Surface characterization was investigated by fourier transform infrared spectroscopy (FTIR) and atomic force microscopy (AFM). Two autopolymerizing resins (subgroups G and T, n = 14) were bonded to the specimens, thermocycled, and then tested for shear bond strength with a universal testing machine. Data were analyzed with one-way ANOVA followed by Tukey's HSD (α = 0.05). FTIR spectra of treated surfaces confirmed the chemical modification and appearance of functional groups on the polymer. One-way ANOVA revealed significant differences in shear bond strength among the study groups. Tukey's HSD showed that TS T and TS G groups had significantly higher shear bond strength than control groups (p = 0.001 and p < 0.001, respectively). Moreover, bond strength values of AP T were statistically significant compared to controls (p = 0.017). Amino functionalized TEOS-derived silica coating is a simple and cost-effective method for improving the bond strength between the autopolymerizing resin and polyamide

Performance of the sol-gel method for the preparation of optical fibers

Czech Academy of Sciences Publication Activity Database

Matějec, Vlastimil; Hayer, Miloš; Mrázek, Jan; Kašík, Ivan; Podrazký, Ondřej; Pospíšilová, Marie

2007-01-01

Roč. 52, č. 10 (2007), s. 991-998 ISSN 0035-3930. [Physical Chemistry Conference ROMPHYSCHEM /12./. Bucharest, 06.09.2006-08.09.2006] R&D Projects: GA ČR GA102/05/0956 Institutional research plan: CEZ:AV0Z20670512 Keywords : sol-gel processing * optical fibres * chemical sensors Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 0.262, year: 2007

Topography and surface energy dependent calcium phosphate formation on Sol-Gel derived TiO2 coatings.

Science.gov (United States)

Järn, Mikael; Areva, Sami; Pore, Viljami; Peltonen, Jouko; Linden, Mika

2006-09-12

Heterogeneous nucleation and growth of calcium phosphate (CaP) on sol-gel derived TiO(2) coatings was investigated in terms of surface topography and surface energy. The topography of the coatings was derived from AFM measurements, while the surface energy was determined with contact angle measurements. The degree of precipitation was examined with scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The precipitation of CaP was found to be dependent on both topography and surface energy. A high roughness value when combining the RMS roughness parameter S(q) with the number of local maxima per unit area parameter S(ds) enhances CaP formation. The hydrophilicity of the coating was also found to be of importance for CaP formation. We suggest that the water contact angle, which is a direct measure of the hydrophilicity of the surface, may be used to evaluate the surface energy dependent precipitation kinetics rather than using the often applied Lewis base parameter.

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-08-15

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)

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

Energy Technology Data Exchange (ETDEWEB)

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)

2012-06-29

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.

Minimally Adhesive, Advanced Non-toxic Coatings of Dendrimeric Catalysts in Sol-Gel Matrices

Science.gov (United States)

2015-10-19

Catalysts in Sol -Gel Matrices 5a. CONTRACT NUMBER 5b. GRANT NUMBER N00014-09-1-0217 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Detty, Michael R. 5d...Technical Report for ONR N00014-09-1-0217 Minimally Adhesive, Advanced Non-toxic Coatings of Dendrimeric Catalysts in Sol -Gel Matrices Michael R. Detty, PI...Environmentally benign sol -gel antifouling and foul-releasing coatings. Ace. Chem. Res. 2014, 47, 678-687. 11) Alberto, E. E.; Müller, L. M

Sol-gel precursors and products thereof

Science.gov (United States)

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

2017-02-14

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##

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

Science.gov (United States)

Miyawaki, Osato; Omote, Chiaki; Matsuhira, Keiko

2015-12-01

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. © 2015 Wiley Periodicals, Inc.

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

International Nuclear Information System (INIS)

Paganini, Paula P.; Felinto, Maria Claudia F.C.; Brito, Hermi F.

2011-01-01

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)

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-07-01

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)

Fundamental electrochemiluminescence characteristics of fluorine-doped tin oxides synthesized by sol-gel combustion.

Science.gov (United States)

Moon, B H; Chaoumead, A; Sung, Y M

2013-10-01

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.

Magnetic resonance as a structural probe of a uranium (VI) sol-gel process

International Nuclear Information System (INIS)

King, C.M.; Thompson, M.C.; Buchanan, B.R.; King, R.B.; Garber, A.R.

1989-01-01

NMR investigations on the ORNL process for sol-gel synthesis of microspherical nuclear fuel (UO 2 ), has been useful in sorting out the chemical mechanism in the sol-gel steps. 13 C, 15 N, and 1 H NMR studies on the HMTA gelation agent (Hexamethylene tetramine, C 6 H l2 N 4 ) has revealed near quantitative stability of this adamantane-like compound in the sol-Gel process, contrary to its historical role as an ammonia source for gelation from the worldwide technical literature. 17 0 NMR of uranyl (UO 2 ++ ) hydrolysis fragments produced in colloidal sols has revealed the selective formation of a uranyl trimer, [(UO 2 ) 3 (μ 3 -O)(μ 2 -OH) 3 ] + , induced by basic hydrolysis with the HMTA gelation agent. Spectroscopic results show that trimer condensation occurs during sol-gel processing leading to layered polyanionic hydrous uranium oxides in which HMTAH + is occluded as an ''intercalation'' cation. Subsequent sol-gel processing of microspheres by ammonia washing results in in-situ ion exchange and formation of a layered hydrous ammonium uranate with a proposed structural formula of (NH 4 ) 2 [(UO 2 ) 8 O 4 (OH) 10 ] · 8H 2 0. This compound is the precursor to sintered U0 2 ceramic fuel

Sol-gel auto-combustion synthesis of hydroxyapatite nanotubes array in porous alumina template

International Nuclear Information System (INIS)

Yuan Yuan; Liu Changsheng; Zhang Yuan; Shan Xiaoqian

2008-01-01

In this paper, an array of highly ordered hydroxyapatite (HAP) nanotubes was synthesized by sol-gel auto-combustion method with porous anodic aluminum oxide (AAO) template for the first time. Based on thermogravimetry (DTA/TG), Fourier transform infrared (FTIR) and X-ray diffraction (XRD), the dried gel, derived from the sol solution with Ca(NO 3 ) 2 .4H 2 O and PO(CH 3 O) 3 as precursors and ethylene glycol as the polymeric matrix, exhibited a typical self-propagating combustion behavior at low temperature, directly resulting in hexagonal crystalline HAP materials. The resultant HAP arrays fabricated from the above sol-gel in the AAO template were uniformly distributed, highly ordered nanotubes with uniform length and diameter according to the observations of scanning electron microscopy (SEM) and transmission electron microscope (TEM). The electron diffraction (ED), XRD and X-ray photoelectron spectroscopy (XPS) survey proved the formation of HAP phase with polycrystalline structure in the AAO template. Based on these results, a potential mechanism of 'an auto-combustion from dried gel to nanoparticles and a subsequent in situ reaction from nanoparticles to nanotubes' was proposed

Composite Biomaterials Based on Sol-Gel Mesoporous Silicate Glasses: A Review

Science.gov (United States)

Baino, Francesco; Fiorilli, Sonia; Vitale-Brovarone, Chiara

2017-01-01

Bioactive glasses are able to bond to bone and stimulate the growth of new tissue while dissolving over time, which makes them ideal materials for regenerative medicine. The advent of mesoporous glasses, which are typically synthesized via sol-gel routes, allowed researchers to develop a broad and versatile class of novel biomaterials that combine superior bone regenerative potential (compared to traditional melt-derived glasses) with the ability of incorporating drugs and various biomolecules for targeted therapy in situ. Mesoporous glass particles can be directly embedded as a bioactive phase within a non-porous (e.g., microspheres), porous (3D scaffolds) or injectable matrix, or be processed to manufacture a surface coating on inorganic or organic (macro)porous substrates, thereby obtaining hierarchical structures with multiscale porosity. This review provides a picture of composite systems and coatings based on mesoporous glasses and highlights the challenges for the future, including the great potential of inorganic–organic hybrid sol-gel biomaterials. PMID:28952496

Sol-gel/hydrothermal synthesis of mixed metal oxide of Titanium and ...

African Journals Online (AJOL)

Mixed metal oxides of titanium and zinc nanocomposites were prepared through sol-gel method under hydrothermal condition using titanium oxy-(1, 2 - pentadione) and zinc acetate without hazardous additives. The resulting composites were characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscope ...

Amperometric biosensor for hydrogen peroxide based on hemoglobin entrapped in titania sol-gel film

International Nuclear Information System (INIS)

Yu Jiuhong; Ju Huangxian

2003-01-01

Hemoglobin (Hb) was entrapped in a titania sol-gel matrix and used as a mimetic peroxidase to construct a novel amperometric biosensor for hydrogen peroxide. The Hb entrapped titania sol-gel film was obtained with a vapor deposition method, which simplified the traditional sol-gel process for protein immobilization. The morphologies of both titania sol-gel and the Hb films were characterized using scanning electron microscopy (SEM) and proved to be chemically clean, porous, homogeneous. This matrix provided a biocompatible microenvironment for retaining the native structure and activity of the entrapped Hb and a very low mass transport barrier to the substrates. H 2 O 2 could be reduced by the catalysis of the entrapped hemoglobin at -300 mV without any mediator. The reagentless H 2 O 2 sensor exhibited a fast response (less than 5 s) and sensitivity as high as 1.29 mA mM -1 cm -2 . The linear range for H 2 O 2 determination was from 5.0x10 -7 to 5.4x10 -5 M with a detection limit of 1.2x10 -7 M. The apparent Michaelis-Menten constant of the encapsulated hemoglobin was calculated to be 0.18±0.02 mM. The stability of the biosensor was also evaluated

Sol-gel transition accelerated by the co-assembly of two components in supramolecular hydrogels.

Science.gov (United States)

Matsumoto, Keigo; Shundo, Atsuomi; Ohno, Masashi; Saruhashi, Kowichiro; Miyachi, Nobuhide; Tsuruzoe, Nobutomo; Tanaka, Keiji

2015-10-28

N-Palmitoyl-Gly-His (PalGH) and glycerol 1-monopalmitate (GMP) in water co-assembled into fibrils with twisted ribbon structures and formed a homogeneous network, resulting in gel formation. Shaking the gel easily broke the fibril network leading to a sol in which high and low fibril density regions exist. After a period at room temperature, the higher density regions became interconnected. The spontaneous sol-gel transition did not take place for a gel made from only PalGH. Also, during the transition, the aggregation state of the co-assembly remained unchanged at a molecular level, unlike the fibril network. Thus, it can be claimed that the sol-gel transition is not associated with the assembled molecular configuration, but with the change in the fibril network. This knowledge might be useful for understanding and controlling sol-gel transition, thereby leading to the design and functionalization of hydrogels.

Sol-Gel SiO2-CaO-P2O5 biofilm with surface engineered for medical application

Directory of Open Access Journals (Sweden)

Sonia Regina Federman

2007-06-01

Full Text Available Sol-gel film in the SiO2-CaO-P2O5 system was prepared from TEOS, TEP, alcohol and hydrated calcium nitrate in an acidic medium. The coatings were deposited on stainless steel using the dip-coating technique. After deposition, the composite was submitted to heat treatment, at different temperatures and exposure times to investigate the influence of such parameters on the surface morphology of the composite. The coated surfaces were characterized by AFM, SEM and FTIR. The present study showed that the formation of different textures (an important parameter in implant fixation could be controlled by temperature and time of heat treatment.

Nanostructured sol-gel coatings doped with cerium nitrate as pre-treatments for AA2024-T3

International Nuclear Information System (INIS)

Zheludkevich, M.L.; Serra, R.; Montemor, M.F.; Yasakau, K.A.; Salvado, I.M. Miranda; Ferreira, M.G.S.

2005-01-01

Nanostructured hybrid sol-gel coatings doped with cerium ions were investigated in the present work as pre-treatments for the AA2024-T3 alloy. The sol-gel films have been synthesized from tetraethylorthosilicate (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTMS) precursors. Additionally the hybrid sol was doped with zirconia nanoparticles prepared from hydrolyzed tetra-n-propoxyzirconium (TPOZ). Cerium nitrate, as corrosion inhibitor, was added into the hybrid matrix or into the oxide nanoparticles. The chemical composition and the structure of the hybrid sol-gel films were studied by XPS (X-ray photoelectron spectroscopy) and AFM (atomic force microscopy), respectively. The evolution of the corrosion protection properties of the sol-gel films was studied by EIS (electrochemical impedance spectroscopy), which can provide quantitative information on the role of the different pre-treatments. Different equivalent circuits, for different stages of the corrosion processes, were used in order to model the coating degradation. The models were supported by SEM (scanning electron microscopy) measurements. The results show that the sol-gel films containing zirconia nanoparticles present improved barrier properties. Doping the hybrid nanostructured sol-gel coatings with cerium nitrate leads to additional improvement of the corrosion protection. The zirconia particles present in the sol-gel matrix seem to act as nanoreservoirs providing a prolonged release of cerium ions. The nanostructured sol-gel films doped with cerium nitrate can be proposed as a potential candidate for substitution of the chromate pre-treatments for AA2024-T3

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

Science.gov (United States)

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

2015-04-01

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

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

Science.gov (United States)

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

2016-09-20

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.

Structural studies on iron-tellurite glasses prepared by sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Rada, S., E-mail: Simona.Rada@phys.utcluj.r [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Dehelean, A. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Stan, M. [Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Chelcea, R. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania); Nat. Inst. for R and D of Isotopic and Molec. Technologies, Cluj-Napoca (Romania); Culea, E. [Department of Physics, Technical University of Cluj-Napoca, Bibliotecii, No. 10, 400020 Cluj-Napoca (Romania)

2011-01-05

Research highlights: {yields} Iron-tellurite glasses obtained using the sol-gel synthesis. - Abstract: In this study, we report structural properties of the iron-tellurite glasses obtained using the sol-gel synthesis. The samples were characterized by X-ray diffraction, FTIR, UV-vis and EPR spectroscopy. Our results indicate dominant presence of iron ions in the trivalent state and the existence some Fe{sup 2+} ions. The analysis of the IR spectra indicates a gradual transformation of iron ions from tetrahedral into octahedral sites when the concentration of Fe(NO{sub 3}){sub 3} is increased beyond 0.64 mol%. EPR studies show that the increase of Fe(NO{sub 3}){sub 3} content in the host matrix induces the growth of the number of effective g values. This can be explained considering that the orbitals of O{sup 2-} ion with a large spin-orbit interaction constant will interact with the 3d orbital of Fe{sup 3+} ion bonded to this O{sup 2-} ion, thus leading to appearance of an orbital angular momentum which contributes to the magnetic moment of Fe{sup 3+} ion. A strong dipolar interaction, which is more predominant in a glass with higher content of Fe(NO{sub 3}){sub 3}, causing a localized magnetic field along the site of the Fe{sup 3+} ions and the increase the effective g values.

Photodegradation of indigo carmine and methylene blue dyes in aqueous solution by SiC-TiO{sub 2} catalysts prepared by sol-gel

Energy Technology Data Exchange (ETDEWEB)

Gomez-Solis, Christian [Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, San Luis Potosi Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); Juarez-Ramirez, Isaias, E-mail: isajua13@yahoo.com [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Moctezuma, Edgar [Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, San Luis Potosi Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); Torres-Martinez, Leticia M. [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico)

2012-05-30

Highlights: Black-Right-Pointing-Pointer Photodegradation of organic dyes is possible using sol-gel SiC-TiO{sub 2} catalysts. Black-Right-Pointing-Pointer SiC-TiO{sub 2} makes a synergy effect that enhances its catalytic activity. Black-Right-Pointing-Pointer Sol-gel allows good dispersion and attachment of TiO{sub 2} particles on SiC surface. Black-Right-Pointing-Pointer SiC-TiO{sub 2} exhibits better activity than TiO{sub 2} (P25) on organic dyes degradation. Black-Right-Pointing-Pointer SiC-TiO{sub 2} catalysts are settled down and easily separated after photocatalysis. - Abstract: Indigo carmine and methylene blue dyes in aqueous solution were photodegraded using SiC-TiO{sub 2} catalysts prepared by sol-gel method. After thermal treatment at 450 Degree-Sign C, SiC-TiO{sub 2} catalysts prepared in this work showed the presence of SiC and TiO{sub 2} anatase phase. Those compounds showed specific surface area values around 22-25 m{sup 2} g{sup -1}, and energy band gap values close to 3.05 eV. In comparison with TiO{sub 2} (P25), SiC-TiO{sub 2} catalysts showed the highest activity for indigo carmine and methylene blue degradation, but this activity cannot be attributed to the properties above mentioned. Therefore, photocatalytic performance is due to the synergy effect between SiC and TiO{sub 2} particles caused by the sol-gel method used to prepare the SiC-TiO{sub 2} catalysts. TiO{sub 2} nanoparticles are well dispersed onto SiC surface allowing the transfer of electronic charges between SiC and TiO{sub 2} semiconductors, which avoid the fast recombination of the electron-hole pair during the photocatalytic process.

Template-directed formation of functional complex metal-oxide nanostructures by combination of sol-gel processing and spin coating

International Nuclear Information System (INIS)

Choi, Y.C.; Kim, J.; Bu, S.D.

2006-01-01

We report the template-based formation of functional complex metal-oxide nanostructures by a combination of sol-gel processing and spin coating. This method employs the spin-coating of a sol-gel solution into an anodic aluminum oxide membrane (SSAM). Various metal-oxide nanowires and nanotubes with a high aspect-ratio were prepared. The aspect-ratios of the PbO 2 nanowires and Pb(Zr 0.52 Ti 0.48 )O 3 nanowires were about 300 and 400, respectively, and their diameters were about 50 nm. The fabricated PbTiO 3 nanotubes have a relatively constant wall thickness of about 20 nm with an outer diameter of about 60 nm. The deposition time for all of the fabricated metal-oxide nanowires and nanotubes is less than 120 s, which is far shorter than those required in both the sol-gel dipping and sol-gel electrophoretic methods. These results indicate that the SSAM method can be a versatile pathway to prepare functional complex metal-oxide nanowires and nanotubes with a high aspect-ratio. The possible formation process for the one-dimensional nanostructures by SSAM is discussed

Development of vapor deposited silica sol-gel particles for use as a bioactive materials system.

Science.gov (United States)

Snyder, Katherine L; Holmes, Hallie R; VanWagner, Michael J; Hartman, Natalie J; Rajachar, Rupak M

2013-06-01

Silica-based sol-gel and bioglass materials are used in a variety of biomedical applications including the surface modification of orthopedic implants and tissue engineering scaffolds. In this work, a simple system for vapor depositing silica sol-gel nano- and micro-particles onto substrates using nebulizer technology has been developed and characterized. Particle morphology, size distribution, and degradation can easily be controlled through key formulation and manufacturing parameters including water:alkoxide molar ratio, pH, deposition time, and substrate character. These particles can be used as a means to rapidly modify substrate surface properties, including surface hydrophobicity (contact angle changes >15°) and roughness (RMS roughness changes of up to 300 nm), creating unique surface topography. Ions (calcium and phosphate) were successfully incorporated into particles, and induced apatitie-like mineral formation upon exposure to simulated body fluid Preosteoblasts (MC3T3) cultured with these particles showed up to twice the adhesivity within 48 h when compared to controls, potentially indicating an increase in cell proliferation, with the effect likely due to both the modified substrate properties as well as the release of silica ions. This novel method has the potential to be used with implants and tissue engineering materials to influence cell behavior including attachment, proliferation, and differentiation via cell-material interactions to promote osteogenesis. Copyright © 2012 Wiley Periodicals, Inc.

The influence of the matrix structure on the oxidation of aniline in a silica sol-gel composite

International Nuclear Information System (INIS)

Widera, J.; Kijak, A.M.; Ca, D.V.; Pacey, G.E.; Taylor, R.T.; Perfect, H.; Cox, J.A.

2005-01-01

Mesoporous and microporous silica matrices were formed on indium tin oxide electrodes for liquid-phase voltammetry and as monoliths for solid-state voltammetry of aniline. The pore structure, which was verified by scanning probe microscopy and by surface area measurement, was directed by either control of pH during sol-gel processing or by inclusion of a templating agent. Whether aniline was included as a dopant in the sol-gel or as a component of the contacting liquid, the pore size influenced the coupling of the product of its electrochemical oxidation. With microporous silica, the dominant products were dimers and related short-chain products whereas with mesoporous silica, polymerization was suggested. As a step toward the formation of polyaniline (PANI) that is covalently anchored to the sol-gel, the electrochemistry of aniline was investigated using composites prepared from sols comprising tetraethyl orthosilicate (TEOS), 3-aminophenyl-[3-triethoxylsilyl)-propyl] urea (ormosil), and aniline in various ratios. Combinatorial chemistry identified that the optimum combination of silica precursors in terms of obtaining PANI was a 1:12 mole ratio of ormosil:TEOS

Porous MnO2 prepared by sol-gel method for electrochemical supercapacitor

Science.gov (United States)

Bazzi, K.; Kumar, A.; Jayakumar, O. D.; Nazri, G. A.; Naik, V. M.; Naik, R.

2015-03-01

MnO2 has attracted great attention as material for electrochemical pseudocapacitor due to its high theoretical specific faradic capacitance (~ 1370 F .g-1) , environmental friendliness and wide potential window in both aqueous and nonaqueous electrolytes. However, the MnO2 has a low surface area which depresses its electrochemical performance. The amorphous α-MnO2 composite was synthesized by sol gel method in the presence of the tri-block copolymer P123. Our aim is to investigate the role of P123 on the electrochemical performance of MnO2. The samples with and without P123 were prepared and characterized by x-ray diffraction (XRD), SEM, TEM and Brunauer-Emmett-Teller (BET) method. The electrochemical performances of the amorphous MnO2 composites as the electrode materials for supercapacitors were evaluated by cyclic voltammetry and AC impedance measurements in a 1M Na2SO4 solution. The results show that the sample prepared without P123 exhibited a relatively low specific capacitance of 28F .g-1, whereas the porous MnO2 prepared with P123 exhibited 117 F .g-1at 5 mV/s. The results of crystalline MnO2 composites will also be presented. The authors acknowledge the support from the Richard J. Barber Foundation for Interdisciplinary Research.

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

Directory of Open Access Journals (Sweden)

E. P. Avés

2008-12-01

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.

Sol-Gel Material-Enabled Electro-Optic Polymer Modulators

Science.gov (United States)

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

2015-01-01

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. PMID:26225971

Sol-gel synthesis of lanthanum-gallate-based ceramic coatings

International Nuclear Information System (INIS)

Golubko, N.V.; Kaleva, G.M.; Roginskaya, Yu.E.; Politova, E.D.

2007-01-01

Phase-pure (La 0.9 Sr 0.1 )(Ga 0.7 Fe 0.3 )O 3-y and (Sr 1.8 La 0.2 )(GaFe)O 5.1 solid solutions with the perovskite and brownmillerite structures have been prepared from salt solutions by sol-gel processing at temperatures from 570 to 870 K. Ceramic coatings up to 100 μm in thickness have been produced by applying suspensions of the sol-gel powders to various substrates. The structure and microstructure of the ceramic coatings have been studied by X-ray diffraction and scanning electron microscopy [ru

Fabrication and application of mesoporous TiO{sub 2} film coated on Al wire by sol-gel method with EISA

Energy Technology Data Exchange (ETDEWEB)

Zhao, Linkang; Lu, Jianjun, E-mail: lujianjunktz@tyut.edu.cn

2017-04-30

Highlights: • Successfully fabricated mesoporous TiO{sub 2} thin film on Al wire by sol-gel method with EISA. • Ni supported on this film and exhibits good methanation performance. • Investigate the decomposition temperature of template agent F127 in TiO{sub 2} precursor system. - Abstract: Mesoporous TiO{sub 2} film on Al wire was fabricated by sol-gel method with evaporation induced self assembly (EISA) process using F127 as templating agent in the mixed solution of ethanol and Tetra-n-butyl Titanate. The Ni/TiO{sub 2} film catalyst supported on Al wire was prepared by impregnation and the catalytic performance on methanation was carried out in a titanium alloy micro-reactor tube. It was shown that anatase mesoporous TiO{sub 2} film was prepared in this conditions (1 g F127,calcined at 400 °C and aged for 24 h), which has specific surface area of 127 m{sup 2} g{sup −1} and narrow pore size distribution of 5.3 nm. Low calcined temperature (300 °C) cannot transfer film to anatase and decompose F127 completely. Ni/TiO{sub 2} film on Al wire catalyst was proved to be active in CO methanation reaction. And the CO conversion reaches 99% and CH{sub 4} selectivity close is to 80% when the reaction temperature is higher 360 °C.

The application of silicon sol-gel technology to forensic blood substitute development: Mimicking aspects of whole human blood rheology.

Science.gov (United States)

Stotesbury, Theresa; Illes, Mike; Wilson, Paul; Vreugdenhil, Andrew J

2017-01-01

Solution-gelation chemistry has promising applications in forensic synthetic blood substitute development. This research offers a silicon-based sol-gel approach to creating stable materials that share similar rheological properties to that of whole human blood samples. Room temperature, high water content, silicon sol-gels were created using the organosilane precursors 3-glycidoxypropyltrimethoxysilane and tetraethylorthosilicate along with various concentrations of filler and pigment. Shear-thinning non-Newtonian properties were observed within most formulations of the presented materials. The effects of colloidal concentration, temperature, age and filler addition on the viscosity of the sol-gels were investigated. SEM-EDS analysis was used to identify the behavior of the fillers within the film and support their inclusion for basic bloodstain pattern simulation. A final proposed candidate sol-gel was assessed using a previously reported passive drip simulation test on a hard, dry surface and passed. This works represents encouraging development in providing safe material alternatives to using whole human blood for forensic training and research. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Monolayer nanoparticle-covered liquid marbles derived from a sol-gel coating

Science.gov (United States)

Li, Xiaoguang; Wang, Yiqi; Huang, Junchao; Yang, Yao; Wang, Renxian; Geng, Xingguo; Zang, Duyang

2017-12-01

A sol-gel coating consisting of hydrophobic SiO2 nanoparticles (NPs) was used to produce monolayer NP-covered (mNPc) liquid marbles. The simplest approach was rolling a droplet on this coating, and an identifiable signet allowed determination of the coverage ratio of the resulting liquid marble. Alternatively, the particles were squeezed onto a droplet surface with two such coatings, generating surface buckling from interfacial NP jamming, and then a liquid marble was produced via a jamming-relief process in which water was added into the buckled droplet. This process revealed an ˜7% reduction in particle distance after interfacial jamming. The mNPc liquid marbles obtained by the two methods were transparent with smooth profiles, as naked droplets, and could be advantageously used in fundamental and applied researches for their unique functions.

A concetration-dependent model for silver colloids in nanostructured sol-gel materials

Science.gov (United States)

Garcia-Macedo, Jorge A.; Franco, Alfredo; Renteria, Victor; Valverde-Aguilar, Guadalupe

2005-08-01

We report on the physical modelling of the photoconductive response of nanostructured sol-gel films in function of the silver nitrate concentration (ions and colloids). This model considers several factors as the silver nitrate concentration and the transport parameters obtained. The model is compared with others commonly used. 2d-hexagonal nanostructured sol-gel thin films were prepared by dip-coating method using a non-ionic diblock copolymer Brij58 (surfactant) to produce channels into the film. Silver colloids (metallic Ag0 nanoparticles ) were obtained by spontaneous reduction process of Ag+ ions to Ag0. These nanoparticles were deposited into the channels formed by the surfactant. The structure was identified by X-ray diffraction and TEM. An absorption band located at 430 nm was detected by optical absorption; it corresponds to the plasmon surface. Fit to this band with modified Gans theory is presented. Photoconductivity studies were performed on films with silver ions and films with silver colloids to characterized their mechanisms of charge transport in the darkness and under illumination at 420, 633 nm wavelengths. Transport parameters were calculated. The films with silver colloids exhibit a photovoltaic effect stronger than the films with silver ions. While, the last ones possesses a photoconductivity behaviour.

A sol-gel method for preparing ZnO quantum dots with strong blue emission

International Nuclear Information System (INIS)

Chen Zhong; Li Xiaoxia; Du Guoping; Chen Nan; Suen, Andy Y.M.

2011-01-01

ZnO quantum dots (QDs) with strong blue emission have been successfully synthesized by sol-gel method, and their crystal structures, sizes, and photoluminescence properties were characterized by X-ray diffractometer, scanning electron microscope, and ultraviolet-visible spectroscopy. It has been found that ZnO QDs had a hexagonal wurtzite crystal structure, and their average diameter was about 16.0-32.2 nm. Both the reaction time and temperature were found to have a strong influence on the average size and photoluminescence properties of ZnO QDs. Longer reaction time and higher reaction temperature resulted in larger average size for ZnO QDs. It has been shown that at reaction temperature 60 deg. C the emission intensity for ZnO QDs increased first with reaction time before 7 h and then decreased after 7 h. For the same reaction time 7 h, ZnO QDs synthesized at 60 deg. C showed the strongest emission intensity. It was found that annealing in nitrogen, vacuum, and air all resulted in an increase of the size of ZnO QDs and a reduction in their photoluminescence. The dependence of the size and properties of ZnO QDs on the reaction parameters as well as the annealing conditions has been discussed. - Highlights: → ZnO quantum dots (QDs) with strong blue emission were prepared by sol-gel method. → ZnO QDs had a pure spectral blue with the chromaticity coordinates (0.166, 0.215). → Optimal reaction time and temperature were 7 h and 60 deg. C, respectively.

Fabrication of Meso-Porous Gamma-Alumina Films by Sol-Gel and Gel Casting Processes for Making Moisture Sensors

Directory of Open Access Journals (Sweden)

Kalyan Kumar Mistry

2007-04-01

Full Text Available Meso-porous g-Al2O3 film may be used as a highly sensitive trace moisture sensor. The crack-free alumina film was developed using a combination of sol-gel and tape casting processes, which produce high porosity, high surface area and small pore dimensions in the range of few nano-meter at uniform distribution. Sol-gel processes are well known in nano-technology and nano-material preparation, but it is difficult to make crack-free thick or thin films using this method. Tape cast methods are used for the fabrication of flexible crack-free thick ceramic sheets. Our objective was to develop nano-structured, crack-free, transparent Al2O3 film a few microns thick, has a highly porous and stable crystallographic nature. A metallic paste was printed by screen printing on both side of the film surface for electrodes to form a sensitive element. A silver wire (dia j=0.1mm lead was connected to a grid structure electrode using a silver paste spot for fine joining. Alumina is absorbs moisture molecules into its meso-porous layer and changes its electrical characteristics according to the moisture content, its dielectric constant increase as moisture increase. Moisture molecules can be conceived of as dipoles in random state before the application of an electric field. When the dipole orientation was changed from random to an equilibrium state under the application of external field, a large change in dielectric constant was observed. The number of water molecules absorbed determines the electrical impedance of the capacitor, which in turn is proportional to water vapor pressure.

Sol-gel Derived Warfarin - Silica Composites for Controlled Drug Release.

Science.gov (United States)

Dolinina, Ekaterina S; Parfenyuk, Elena V

2017-01-01

Warfarin, commonly used anticoagulant in clinic, has serious shortcomings due to its unsatisfactory pharmacodynamics. One of the efficient ways for the improvement of pharmacological and consumer properties of drugs is the development of optimal drug delivery systems. The aim of this work is to synthesize novel warfarin - silica composites and to study in vitro the drug release kinetics to obtain the composites with controlled release. The composites of warfarin with unmodified (UMS) and mercaptopropyl modified silica (MPMS) were synthesized by sol-gel method. The composite formation was confirmed by FTIR spectra. The concentrations of warfarin released to media with pH 1.6, 6.8 and 7.4 were measured using UV spectroscopy. The drug release profiles from the solid composites were described by a series of kinetic models which includes zero order kinetics, first order kinetics, the modified Korsmeyer-Peppas model and Hixson-Crowell model. The synthesized sol-gel composites have different kinetic behavior in the studied media. In contrast to the warfarin composite with unmodified silica, the drug release from the composite with mercaptopropyl modified silica follows zero order kinetics for 24 h irrespective to the release medium pH due to mixed mechanism (duffusion + degradation and/or disintegration of silica matrix). The obtained results showed that warfarin - silica sol-gel composites have a potential application for the development of novel oral formulation of the drug with controlled delivery. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Luminescent hybrid porphyrinosilica obtained by sol gel chemistry

Directory of Open Access Journals (Sweden)

Neri Cláudio Roberto

2003-01-01

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.

Syntheses of rare-earth metal oxide nanotubes by the sol-gel method assisted with porous anodic aluminum oxide templates

International Nuclear Information System (INIS)

Kuang Qin; Lin Zhiwei; Lian Wei; Jiang Zhiyuan; Xie Zhaoxiong; Huang Rongbin; Zheng Lansun

2007-01-01

In this paper, we report a versatile synthetic method of ordered rare-earth metal (RE) oxide nanotubes. RE (RE=Y, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb) oxide nanotubes were successfully prepared from corresponding RE nitrate solution via the sol-gel method assisted with porous anodic aluminum oxide (AAO) templates. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM, and X-ray diffraction (XRD) have been employed to characterize the morphology and composition of the as-prepared nanotubes. It is found that as-prepared RE oxides evolve into bamboo-like nanotubes and entirely hollow nanotubes. A new possible formation mechanism of RE oxide nanotubes in the AAO channels is proposed. These high-quantity RE oxide nanotubes are expected to have promising applications in many areas such as luminescent materials, catalysts, magnets, etc. - Graphical abstract: A versatile synthetic method for the preparation of ordered rare-earth (RE) oxide nanotubes is reported, by which RE (RE=Y, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb) oxide nanotubes were successfully prepared from corresponding RE nitrate solution via the sol-gel method assisted with porous anodic aluminum oxide (AAO) templates

Synthesis of cadmium tungstate films via sol-gel processing

Energy Technology Data Exchange (ETDEWEB)

Lennstrom, Kirk; Limmer, Steven J.; Cao Guozhong

2003-06-23

Cadmium tungstate is a scintillator material with excellent intrinsic photoluminescent properties. It is highly resistant to gamma radiation, has an almost non-existent afterglow and is highly efficient. Cadmium tungstate is also non-hydroscopic, unlike the more prevalent thallium-doped alkali halide scintillators. In order to create thin films of cadmium tungstate with precise stoichiometric control, a sol-gel processing technique has been applied to produce this material for the first time. In addition to lower processing temperatures, sol-gel-derived cadmium tungstate is cheaper and easier than other technologies, particularly for thin films. Furthermore, it has the potential to produce nanostructured materials with good optical quality. X-Ray diffraction results of sol-gel-derived materials fired at various temperatures imply crystallization of cadmium tungstate without the intermediate formation of either tungsten oxide or cadmium oxide. Scanning electron microscopy analysis shows the formation of nano-sized particles prior to heat treatment, which form meso-sized particles after the heat treatment. Photoluminesce analysis indicates emission of derived films at 480 nm, which agrees with other published data. Finally, the efficiency of derived films was approximately 6%{+-}1.8%.

Sol-gel processes. January 1970-September 1989 (Citations from the NTIS data base). Report for January 1970-September 1989

International Nuclear Information System (INIS)

1989-09-01

This bibliography contains citations concerning the development and utilization of sol-gel processes and techniques. Topics include antireflective coatings, studies of sol-gel transitions, sol-gel synthesis and polymerization, sol-gel derived thin films and glasses, and sol-gel production of microspheres. Applications in nuclear waste management, nuclear-fuel manufacturing, glass optical waveguide development, and solar-energy collection are presented. (This updated bibliography contains 179 citations, 39 of which are new entries to the previous edition.)

Preparation of Natural Rubber (NR) Based Nano-Sized Materials Using Sol-Gel Technique

International Nuclear Information System (INIS)

Dahlan Mohd; Mahathir Mohamed

2011-01-01

The objectives of this project are to prepare nano-sized natural rubber-based hybrid coating material by sol-gel technique; to explore the possibility of producing ENR-Si (epoxidized natural rubber-silica) cramer with toughening effects; and to use it in radiation curing of surface coating. Since early 1960s Malaysia has introduced various forms of value-added natural rubber such as Standard Malaysian Rubber (SMR), methylmethacrylate-grafted natural rubber (MG rubber), followed by liquid natural rubber and epoxidized natural rubber (ENR). Products such as liquid epoxidized natural rubber acrylate (LENRA) and thermoplastic natural rubber (TPNR) are still on-going research projects in Nuclear Malaysia. The former has strong possibility to be used as radiation-sensitive comparabilities in TPNR blends, besides its original purpose for example in radiation curing of surface coating. But earlier findings indicated that, to make it (as for surface coating) more effective, reinforcement system is needed to be introduced. Strong candidate is silica by sol-gel technique, since common reinforcement filler for example carbon black has drawbacks in this particular case. This technique was introduced in late 1960s to produce metal oxides such as silica and titanium oxides in solution. (author)

Gel stabilization in chelate sol-gel preparation of Bi-2223 superconductors

Czech Academy of Sciences Publication Activity Database

Rubešová, K.; Jakeš, V.; Hlásek, T.; Vašek, Petr; Matějka, P.

2012-01-01

Roč. 73, č. 3 (2012), s. 448-453 ISSN 0022-3697 Institutional research plan: CEZ:AV0Z10100521 Keywords : superconductors * sol-gel growth * infrared spectroscopy * thermogravimetric analysis (TGA) * X-ray diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.527, year: 2012

rhEGF-containing thermosensitive and mucoadhesive polymeric sol-gel for endoscopic treatment of gastric ulcer and bleeding.

Science.gov (United States)

Maeng, Jin Hee; So, Jung Won; Kim, Jungju; Kim, In Ae; Jung, Ji Hoon; Min, Kyunghyun; Lee, Don Haeng; Yang, Su-Geun

2014-03-01

Gastrointestinal endoscopy is a standard diagnostic tool for gastrointestinal ulcers and cancer. In this study, we have developed recombinant human epidermal growth factor-containing ulcer-coating polymeric sol-gel for endoscopic application. Chitosan and pluronic F127 were employed for their thermoresponsive and bioadhesive properties. At temperatures below 21, polymeric sol-gel remains liquid during endoscopic application and transforms to gel at body temperature after application on ulcers. In an in vitro cellular wounding assay, recombinant human epidermal growth factor sol-gel significantly enhanced the cell migration and decreased the wounding area (68%) compared to nontreated, recombinant human epidermal growth factor solution, and sol-gel without recombinant human epidermal growth factor (42, 49, and 32 % decreased at day 1). The in vivo ulcer-healing study was performed in an acetic acid-induced gastric ulcer rat model and proved that our recombinant human epidermal growth factor endoscopic sol-gel facilitated the ulcer-healing process more efficiently than the other treatments. Ulcer sizes in the recombinant human epidermal growth factor sol-gel group were decreased 2.9- and 2.1-fold compared with those in the nontreated group on days 1 and 3 after ulceration, respectively. The mucosal thickness in the recombinant human epidermal growth factor sol-gel group was significantly increased compared to that in the nontreated group (3.2- and 6.9-fold on days 1 and 3 after ulceration, respectively). In a gastric retention study, recombinant human epidermal growth factor sol-gel stayed on the gastric mucosa more than 2 h after application. The present study suggests that recombinant human epidermal growth factor sol-gel is a prospective candidate for treating gastric ulcers via endoscopic application.

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

Energy Technology Data Exchange (ETDEWEB)

Granado, S.R.; Silva, D.W.; Lopes, S.A.; Cavalheiro, A.A., E-mail: sandrogranado02@gmail.com [Universidade Estadual de Mato Grosso do Sul (CPTREN/UEMS), Navirai, MS (Brazil). Centro de Pesquisas Tecnologicas em Recursos Naturais

2011-07-01

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)

Modified silica sol coatings for surface enhancement of leather.

Science.gov (United States)

Mahltig, Boris; Vossebein, Lutz; Ehrmann, Andrea; Cheval, Nicolas; Fahmi, Amir

2012-06-01

The presented study reports on differently modified silica sols for coating applications on leather. Silica sols are prepared by acidic hydrolysis of tetraethoxysilane and modified by silane compounds with fluorinated and non-fluorinated alkylgroups. In contrast to many earlier investigations regarding sol-gel applications on leather, no acrylic resin is used together with the silica sols when applying on leather. The modified silica particles are supposed to aggregate after application, forming thus a modified silica coating on the leather substrate. Scanning electron microscopy investigation shows that the applied silica coatings do not fill up or close the pores of the leather substrate. However, even if the pores of the leather are not sealed by this sol-gel coating, an improvement of the water repellent and oil repellent properties of the leather substrates are observed. These improved properties of leather by application of modified silica sols can provide the opportunity to develop sol-gel products for leather materials present in daily life.

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

Science.gov (United States)

Kojarunchitt, Thunjiradasiree; Baldursdottir, Stefania; Dong, Yao-Da; Boyd, Ben J; Rades, Thomas; Hook, Sarah

2015-01-01

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 A and monophosphoryl lipid A), were free-flowing liquids at room temperature and formed stable gels at physiological temperatures. Rheological results showed that both systems meet the criteria of being thermoresponsive gels. The P407-25R4 sol-gels did not significantly sustain the release of antigen in vivo while 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 synchronous vaccine release and may in fact retard release, reducing efficacy in some cases. From these results, chitosan-MC sol-gels show potential as sustained release vaccine delivery systems, as compared to the P407-25R4 system that had a limited ability to sustain antigen release. Copyright © 2014 Elsevier B.V. All rights reserved.

Atomic force microscopy study of TiO2 sol-gel films thermally treated under NH3 atmosphere

International Nuclear Information System (INIS)

Trapalis, C.; Todorova, N.; Anastasescu, M.; Anastasescu, C.; Stoica, M.; Gartner, M.; Zaharescu, M.; Stoica, T.

2009-01-01

Multilayered TiO 2 films were obtained by sol-gel and dipping deposition on quartz substrate followed by thermal treatment under NH 3 atmosphere. In an attempt to understand the close relationship between microstructural characteristics and the synthesis parameters, a systematic research of the structure and the morphology of NH 3 modified TiO 2 sol-gel films by XRD and Atomic Force Microscopy is reported. The surface morphology has been evaluated in terms of grains size, fractal dimension and surface roughness. For each surface, it was found a self-similar behavior (with mean fractal dimension in the range of 2.67-3.00) related to an optimum morphology favorable to maintain a nano-size distribution of the grains. The root mean square (RMS) roughness of the samples was found to be in the range of 0.72-6.02 nm.

Morphology evolution of ZrB2 nanoparticles synthesized by sol-gel method

International Nuclear Information System (INIS)

Zhang Yun; Li Ruixing; Jiang Yanshan; Zhao Bin; Duan Huiping; Li Junping; Feng Zhihai

2011-01-01

Zirconium diboride (ZrB 2 ) nanoparticles were synthesized by sol-gel method using zirconium n-propoxide (Zr(OPr) 4 ), boric acid (H 3 BO 3 ), sucrose (C 12 H 22 O 11 ), and acetic acid (AcOH). Clearly, it was a non-aqueous solution system at the very beginning of the reactions. Here, AcOH was used as both chemical modifier and solvent to control Zr(OPr) 4 hydrolysis. Actually, AcOH could dominate the hydrolysis by self-produced water of the chemical propulsion, rather than the help of outer water. C 12 H 22 O 11 was selected, since it can be completely decomposed to carbon. Thus, carbon might be accounted precisely for the carbothermal reduction reaction. Furthermore, we investigated the influence of the gelation temperature on the morphology of ZrB 2 particles. Increasing the gelation temperature, the particle shapes changed from sphere-like particles at 65 deg. C to a particle chain at 75 deg. C, and then form rod-like particles at 85 deg. C. An in-depth HRTEM observation revealed that the nanoparticles of ZrB 2 were gradually fused together to evolve into a particle chain, finally into a rod-like shape. These crystalline nature of ZrB 2 related to the gelation temperature obeyed the 'oriented attachment mechanism' of crystallography. - Graphical Abstract: Increasing the gelation temperature, the particle shapes changed from sphere-like particles at 65 deg. C to a particle chain at 75 deg. C, and then form rod-like particles at 85 deg. C. Highlights: → ZrB 2 nanoparticles were synthesized by sol-gel method in an non-aqueous solution system. → AcOH was used as both chemical modifier and solvent to control Zr(OPr) 4 hydrolysis. → C 12 H 22 O 11 was selected since it can be completely decomposed to carbon. → Increasing the gelation temperature, the particles changed from sphere-like to rod-like ones. → Crystalline nature of ZrB 2 obeyed the 'oriented attachment mechanism' of crystallography.

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

International Nuclear Information System (INIS)

Sharma, Mamta; Mehra, R.M.

2010-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Sharma, Mamta [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India); Mehra, R.M., E-mail: rammehra2003@yahoo.co [Department of Electronic Science, University of Delhi South Campus, Benito Juarez Road, New Delhi 110 021 (India)

2010-05-03

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

Reflection Enhancement Using TiO2/SiO2 Bilayer Films Prepared by Cost-Effective Sol-gel Method

Directory of Open Access Journals (Sweden)

R. Ajay Kumar

2017-04-01

Full Text Available Multilayer dielectric thin film structure has been demanded for its application in optoelectronic devices such as optical waveguides, vertical cavity surface-emitting devices, biosensors etc. In this paper, we present the fabrication and characterization of bilayer thin films of TiO2/SiO2 using sol-gel spin coating method. Ellipsometer measurement showed refractive index values 1.46, 2.1 corresponding to the SiO2 and TiO2 films respectively. The FTIR transmittance peaks observed at ~970 cm-1, ~1100 cm-1 and ~1400 cm-1 are attributed to the Ti-O-Si, Si-O-Si and Ti-O-Ti bonds respectively. Maximum reflectance is observed from two bilayer film structure which can be further optimized to get the high reflection to a broad wavelength range.

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

Science.gov (United States)

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

2014-11-11

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. Copyright © 2014 Elsevier B.V. All rights reserved.

Short communication: Evaluation of a sol-gel-based stainless steel surface modification to reduce fouling and biofilm formation during pasteurization of milk.

Science.gov (United States)

Liu, Dylan Zhe; Jindal, Shivali; Amamcharla, Jayendra; Anand, Sanjeev; Metzger, Lloyd

2017-04-01

Milk fouling and biofilms are common problems in the dairy industry across many types of processing equipment. One way to reduce milk fouling and biofilms is to modify the characteristics of milk contact surfaces. This study examines the viability of using Thermolon (Porcelain Industries Inc., Dickson, TN), a sol-gel-based surface modification of stainless steel, during thermal processing of milk. We used stainless steel 316L (control) and sol-gel-modified coupons in this study to evaluate fouling behavior and bacterial adhesion. The surface roughness as measured by an optical profiler indicated that the control coupons had a slightly smoother finish. Contact angle measurements showed that the modified surface led to a higher water contact angle, suggesting a more hydrophobic surface. The modified surface also had a lower surface energy (32.4 ± 1.4 mN/m) than the control surface (41.36 ± 2.7 mN/m). We evaluated the susceptibility of control and modified stainless steel coupons to fouling in a benchtop plate heat exchanger. We observed a significant reduction in the amount of fouled layer on modified surfaces. We found an average fouling weight of 19.21 mg/cm 2 and 0.37 mg/cm 2 on the control and modified stainless steel coupons, respectively. We also examined the adhesion of Bacillus and biofilm formation, and observed that the modified stainless steel surface offered greater resistance to biofilm formation. Overall, the Thermolon-modified surface showed potential in the thermal processing of milk, offering significantly lower fouling and bacterial attachment than the control surface. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Evaluation of sol-gel based magnetic 45S5 bioglass and bioglass-ceramics containing iron oxide.

Science.gov (United States)

Shankhwar, Nisha; Srinivasan, A

2016-05-01

Multicomponent oxide powders with nominal compositions of (45-x)·SiO2·24.5CaO·24.5Na2O·6P2O5xFe2O3 (in wt.%) were prepared by a modified sol-gel procedure. X-ray diffraction (XRD) patterns and high resolution transmission electron microscope images of the sol-gel products show fully amorphous structure for Fe2O3 substitutions up to 2 wt.%. Sol-gel derived 43SiO2·24.5CaO·24.5Na2O·6P2O5·2Fe2O3 glass (or bioglass 45S5 with SiO2 substituted with 2 wt.% Fe2O3), exhibited magnetic behavior with a coercive field of 21 Oe, hysteresis loop area of 33.25 erg/g and saturation magnetization of 0.66 emu/g at an applied field of 15 kOe at room temperature. XRD pattern of this glass annealed at 850 °C for 1h revealed the formation of a glass-ceramic containing sodium calcium silicate and magnetite phases in nanocrystalline form. Temperature dependent magnetization and room temperature electron spin resonance data have been used to obtain information on the magnetic phase and distribution of iron ions in the sol-gel glass and glass-ceramic samples. Sol-gel derived glass and glass-ceramic exhibit in-vitro bioactivity by forming a hydroxyapatite surface layer under simulated physiological conditions and their bio-response is superior to their melt quenched bulk counterparts. This new form of magnetic bioglass and bioglass ceramics opens up new and more effective biomedical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

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

DEFF Research Database (Denmark)

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

2015-01-01

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...

The Influence of Poly Vinil Alcohol Amount and Temperatures of the SolProcess on the Formation of (NH4)2U2O7 Gel

International Nuclear Information System (INIS)

Indra-Suryawan; Bangun-Wasito; Damunir; Hidayati; Setyo-Sulardi; Bambang-Siswanto; Ari-Handayani

2000-01-01

Research on the influence of poly vinil alcohol and temperatures on theresulted sol solutions. The sols were fed into gelation process using ammoniamedium and resulted were (NH 4 ) 2 U 2 O 7 gels spherical. The PVA variablesaddition on the sol process were 10; 15; 20; 25 and 30 g/1l uranyl nitrates.The temperature variables on the sol process were 75, 80, 85, 90 and 95 o C.The sol which successfully resulted (NH 4 ) 2 U 2 O 7 gel the gelation processwas on the PVA amount of 15 g and 90 o C. The resulted gel was then washed,dried and calcinate. The characterization of shape and surface of gel havebeen carried out using SEM photography. The density of gels were measured.For the 15 g PVA addition, the density was 8.3710 g/ml. While for process at90 o C, the density was 7.8871 g/ml. (author)

Morphology, structure and optical properties of sol-gel ITO thin films

Energy Technology Data Exchange (ETDEWEB)

Stoica, T.F.; Teodorescu, V.S.; Blanchin, M.G.; Stoica, T.A.; Gartner, M.; Losurdo, M.; Zaharescu, M

2003-08-15

The alkoxidic route and the spinning deposition were used to prepare monolayer sol-gel indium tin oxide (ITO) films. The morphology and crystalline structure were investigated by cross-section transmission electron microscopy (XTEM) and atomic force microscopy (AFM). The ITO sol-gel mono-layer contains three regions of different porosities. The basic crystalline structure is that of the In{sub 2}O{sub 3} lattice. The optical properties have been studied by optical transmission and spectroscopic ellipsometry.

Melting Behavior of Organic Nanocrystals Grown in Sol-gel Matrices

International Nuclear Information System (INIS)

Sanz, N.; Boudet, A.; Ibanez, A.

2002-01-01

We have characterized the thermal stability of organic nanocrystals grown in the pores of sol-gel matrices. The structure has been measured with transmission electron microscopy (TEM) analysis. Depending on the nature of organic molecules and sol-gel matrices, we have modified the dye-matrix interactions and the interfacial structure between nanocrystals and gel-glasses. When the dye-matrix interactions are weak (Van der Waals' bonds), the corresponding interfacial structure observed by TEM is sharp and the nanocrystals melt below the bulk melting point. On the other hand, when the dye-matrix interactions are strong (hydrogen bonds), the interfacial structure is fuzzy and a great superheating of organic nanocrystals is observed in comparison to the bulk melting point of the dye

Exploring encapsulation mechanism of DNA and mononucleotides in sol-gel derived silica.

Science.gov (United States)

Kapusuz, Derya; Durucan, Caner

2017-07-01

The encapsulation mechanism of DNA in sol-gel derived silica has been explored in order to elucidate the effect of DNA conformation on encapsulation and to identify the nature of chemical/physical interaction of DNA with silica during and after sol-gel transition. In this respect, double stranded DNA and dAMP (2'-deoxyadenosine 5'-monophosphate) were encapsulated in silica using an alkoxide-based sol-gel route. Biomolecule-encapsulating gels have been characterized using UV-Vis, 29 Si NMR, FTIR spectroscopy and gas adsorption (BET) to investigate chemical interactions of biomolecules with the porous silica network and to examine the extent of sol-gel reactions upon encapsulation. Ethidium bromide intercalation and leach out tests showed that helix conformation of DNA was preserved after encapsulation. For both biomolecules, high water-to-alkoxide ratio promoted water-producing condensation and prevented alcoholic denaturation. NMR and FTIR analyses confirmed high hydraulic reactivity (water adsorption) for more silanol groups-containing DNA and dAMP encapsulated gels than plain silica gel. No chemical binding/interaction occurred between biomolecules and silica network. DNA and dAMP encapsulated silica gelled faster than plain silica due to basic nature of DNA or dAMP containing buffer solutions. DNA was not released from silica gels to aqueous environment up to 9 days. The chemical association between DNA/dAMP and silica host was through phosphate groups and molecular water attached to silanols, acting as a barrier around biomolecules. The helix morphology was found not to be essential for such interaction. BET analyses showed that interconnected, inkbottle-shaped mesoporous silica network was condensed around DNA and dAMP molecules.

The Preparation of TiO₂ Film by the Sol-Gel Method and Evaluation of Its Self-Cleaning Property.

Science.gov (United States)

Liang, Yu; Sun, Sijia; Deng, Tongrong; Ding, Hao; Chen, Wanting; Chen, Ying

2018-03-19

TiO₂ sol was produced by the sol-gel method through the hydrolysis and the aging of tetrabutyl titanate and the TiO₂ film was obtained by dipping and uniform lifting of the acid-treated and ultrasound-treated clean glass slides into the TiO₂ sol followed by aging, drying, and calcination. The effect of the hydrolysis control agents to the formed sol was researched and the crystalline state, the morphology, and the photocatalytic properties of the products after calcination were characterized. The structural morphology, the contact angles before and after illumination, and the self-cleaning properties of the TiO₂ film were characterized as well. The results showed that by using acetylacetone as the hydrolysis control agent, the formed TiO₂ sol had relatively high stability. The product after the calcination of the TiO₂ sol was of single anatase type with crystalline size of 18-20 nm and it could degrade nearly 100% of methylene blue after 90 min illumination. The formed TiO₂ film is compact, continuous, smooth, and had the properties of super-hydrophilicity (after 30 min illumination due to its contact angle decreasing from 21° to nearly 0°) and anti-fogging capability, which indicated its excellent self-cleaning property.

Processing and Characterization of Sol-Gel Cerium Oxide Microspheres

Energy Technology Data Exchange (ETDEWEB)

McClure, Zachary D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Padilla Cintron, Cristina [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

2016-09-27

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.

Sol-gel derived antireflective coatings for silicon

Energy Technology Data Exchange (ETDEWEB)

Brinker, C J; Harrington, M S

1981-08-01

The preparation of TiO2-SiO2 AR coatings, containing from 30 to 95 mol % TiO2, from alkoxide precursor solutions (titanium tetraethoxide and silicon tetraethoxide) by a sol-gel process is presented. The preparation of the solutions is described, which involves the separate partial hydrolysis of one or both alkoxides prior to their mixing (Yoldas, 1980). The solutions are applied to polished, circular (1 and 2 in. diameter) silicon wafers by a spinning process. The coated wafers are successively heated in air at each of the following temperatures: 200, 300, 350, 400, and 450 C, and optical measurements are performed on them after each heat treatment. The durability of 90 and 95% TiO2 coatings is evaluated in both acidic and basic environments, and reflectivity, film thickness, and refractive index are measured as a function of exposure time. It is shown that sol-gel films applied at 400 C reveal broad regions of antireflectance compared to other titanium-based films.

Comparative analysis of synthesis and characterization of La_0_,_9Sr_0_,_1O_3 via sol-gel and combustion reaction

International Nuclear Information System (INIS)

Tarrago, D.P.; Haeser, G.S.; Malfatti, C.F.; Sousa, V.C.

2011-01-01

Strontium doped lanthanum manganites (LSM) are potential materials for cathode application in solid oxide fuel cells (SOFC) due to their properties and compatibility with yttria stabilized zirconia. In this work a LSM powder obtained by the sol-gel process is compared others previously obtained combustion synthesis using urea or sucrose as fuel. For the synthesis of LSM the nitrates of lanthanum, strontium and manganese were dissolved in citric acid and ethylene glycol forming a gel that was calcinated at 800 deg C. Both methods allowed the synthesis of a single phase powder, according to the X-ray diffraction patterns. Through gas adsorption it was found a specific surface area of 17m²/g, an intermediary value among the combustion synthesized powders. Scanning electron microscopy (SEM) revealed more compact agglomerates in the sol-gel powder, however, the transmission electron microscope (TEM) showed smaller and more uniform particles in this powder. (author)

New Functionalized Sol-Gel Hybrid Sorbent Coating for Stir Bar Sorptive Extraction of Selected Non-Steroidal Anti Inflammatory Drugs in Human Urine Samples

International Nuclear Information System (INIS)

Mashkurah Abd Rahim; Wan Aini Wan Ibrahim; Zainab Ramli; Mohd Marsin Sanagi

2015-01-01

A new sol-gel hybrid material, methyltrimethoxysilane-cyanopropyltriethoxysilane (MTMOS-CNPrTEOS) was successfully synthesized and used as a coating material in stir bar sorptive extraction (SBSE) of selected non-steroidal anti-inflammatory drugs (NSAIDs) in urine samples. The MTMOS-CNPrTEOS hybrid was synthesized by hydrolysis and condensation of MTMOS and CNPrTEOS in the presence of trifluoroacetic acid as catalyst via sol-gel method. Several factors influencing the synthesized sol-gel hybrid MTMOS-CNPrTEOS process such as mole ratio of MTMOS-CNPrTEOS, NaOH concentrations as etching solution, etching time, coating time and water content were investigated and optimized in this study. The optimum synthesis conditions obtained were 1:1 mol ratio of MTMOS-CNPrTEOS, 1 M NaOH as etching solution, 60 min etching time, 2 h coating time and 6 mmol water. The sol-gel hybrid MTMOS-CNPrTEOS synthesized under the optimum conditions was used to determine selected NSAIDs in human urine samples using normal stacking mode capillary electrophoresis with ultraviolet detection. MTMOS-CNPrTEOS SBSE method demonstrated good linearity (60 to 20,000 μg L -1 ) with excellent coefficient of determination (r 2 > 0.9990). The sol-gel hybrid MTMOS-CNPrTEOS SBSE method showed low limit of detection (35 - 41 μg L -1 ) with good precision (RSD < 6 %, n = 3) and excellent extraction recoveries (83.5 - 98.9 %) for the selected NSAIDs. The sol-gel hybrid MTMOS-CNPrTEOS SBSE method demonstrated good potential as an alternative sorbent in SBSE method for NSAIDs. (author)

Effect of vanadium on the obtaining of the titanium dioxide by Sol-Gel Method

International Nuclear Information System (INIS)

Granado, S.R.; Silva, D.W.; Lopes, S.A.; Cavalheiro, A.A.

2011-01-01

The obtaining of transition metal modified titanium dioxide (TiO 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)

Micro- and nanostructured sol-gel-based materials for optical chemical sensing (2005–2015)

International Nuclear Information System (INIS)

Barczak, Mariusz; McDonagh, Colette; Wencel, Dorota

2016-01-01

This review (with 172 references) highlights the progress made in the past 10 years in silica sol-gel-based materials for use in optical chemical sensing. Following an introduction, the processes leading to the sol-gel-based and ormosil materials, their printability and methods for characterisation are discussed. Then various classes of optical sensors, with a focus on sensors for pH values, oxygen, carbon dioxide, ammonia (also in dissolved form), and heavy metal ions are described. A further section covers nanoparticle-based optical sensors mainly for use in intracellular sensing of the above species. Recent developments in this area are also emphasised and future trends discussed. (author)

Size control of nanocrystals in InGaZnO4 thin films fabricated by using the sol-gel method

International Nuclear Information System (INIS)

Seo, S. J.; Cho, J. H.; Jang, Y. H.; Kim, C. H.

2012-01-01

We report the structural properties of InGaZnO 4 (IGZO) thin films prepared by using the sol-gel method. The structural properties of IGZO thin films were controlled by using the film thickness and thermal annealing temperature. In this study, the crystallization temperature of amorphous IGZO thin films was observed to be about 700 .deg. C. Also, we observed that the crystal size of IGZO thin films increased as the thickness and the annealing temperature were increased. In addition, we could observe that the atomic ratio of In, Ga and Zn of the IGZO thin film was slightly different from the molar ratio of a previous IGZO sol-gel solution (In:Ga:Zn = 1:1:1) post-annealed at 900 .deg. C because In and Zn are more volatile than Ga. The study of the crystallization of amorphous IGZO thin films provides an understanding of the growth mechanisms and thermal annealing effects for IGZO nanocrystals.

The role of crosslinkers in epoxy-amine crosslinked silicon sol-gel barrier protection coatings

International Nuclear Information System (INIS)

Vreugdenhil, A.J.; Gelling, V.J.; Woods, M.E.; Schmelz, J.R.; Enderson, B.P.

2008-01-01

The search for chromate replacements in corrosion prevention materials has identified the use of hybrid sol-gel coatings as one, very promising approach. Appropriately functionalized hybrid sol-gel materials can be crosslinked to enhance their chemical durability and mechanical strength. In this work, we evaluate three crosslinkers used in a tetramethoxysilane-glycidoxypropyltrimethoxysilane binary sol-gel system in order to identify the role of the crosslinkers in corrosion protection. The crosslinkers examined were ethylenediamine, N-aminethylepiperazine, and diethylenetriamine. The sol-gel coatings were examined by contact angle, atomic force microscopy, and electrochemical impedance spectroscopy (EIS). Circuit modeling of the EIS results yielded valuable insights into the significant differences between the durabilities of the variously crosslinked coatings. Crosslinker hydrophobicity was identified as not playing a significant role whereas the number of reactive sites per crosslinker and the resulting morphology of the material may be an important parameter

Synthesis and sintering of nanocrystalline hydroxyapatite powders by citric acid sol-gel combustion method

International Nuclear Information System (INIS)

Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

2004-01-01

The citric acid sol-gel combustion method has been used for the synthesis of nanocrystalline hydroxyapatite (HAP) powder from calcium nitrate, diammonium hydrogen phosphate and citric acid. The phase composition of HAP powder was characterized by X-ray powder diffraction analysis (XRD). The morphology of HAP powder was observed by transmission electron microscope (TEM). The HAP powder has been sintered into microporous ceramic in air at 1200 deg. C with 3 h soaking time. The microstructure and phase composition of the resulting HAP ceramic were characterized by scanning electron microscope (SEM) and XRD, respectively. The physical characterization of open porosity and flexural strength have also been carried out

Comparison of the redox activities of sol-gel and conventionally prepared Bi-Mo-Ti mixed oxides

Energy Technology Data Exchange (ETDEWEB)

Wildberger, M.; Grundwaldt, J.D.; Mallat, T.; Baiker, A. [Lab. of Technical Chemistry, Swiss Federal Inst. of Technology, ETH-Zentrum, Zuerich (Switzerland)

1998-12-31

Novel sol-gel Bi-Mo-Ti oxides have been prepared and characterized by XRD, XPS, FT-Raman and HRTEM. The surface Bi{sup 3+} and Mo{sup 6+} species of some xerogels and an aerogel could be reduced and oxidized at room temperature, whereas the conventionally prepared reference materials were not reduced by H{sub 2} below 300 C. The unusual redox properties, under very mild conditions, are likely due to the unique morphology of Bi-Mo-oxides stabilized by titania. During butadiene oxidation to furan at above 400 C to sol-gel mixed oxides restructured considerably and their performance was barely better than that of titania-supported Bi-Mo oxides. (orig.)

Sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) electrogenerated chemiluminescence sensor for high-performance liquid chromatography

International Nuclear Information System (INIS)

Choi, Han Nim; Cho, Sung-Hee; Park, Yu-Jin; Lee, Dai Woon; Lee, Won-Yong

2005-01-01

The sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy) 3 2+ ] electrogenerated chemiluminescence (ECL) sensor was applied to the reversed-phase high-performance liquid chromatography (HPLC) determination of phenothiazine derivatives (promazine, chlorpromazine, triflupromazine, thioridazine, and trifluoperazine) and erythromycin in human urine samples. In this method, Ru(bpy) 3 2+ was immobilized in sol-gel-derived titania (TiO 2 )-Nafion nanocomposite films coated on a dual platinum electrode. This method eliminates an extra pump needed for the delivery of Ru(bpy) 3 2+ reagent into a reaction/observation zone in front of photomultiplier tube because the immobilized-Ru(bpy) 3 2+ is recycled on the electrode surface by an applied potential at +1.3 V versus Ag/AgCl (3 M NaCl) reference electrode. The resulting analytical performances such as detection limit, working range, sensitivity, and measurement precision were slightly worse than those obtained with the conventional post-column Ru(bpy) 3 2+ addition approach. The lack of significant interferences and the low detection limits for phenothiazine derivatives and erythromycin indicate that the proposed HPLC-Ru(bpy) 3 2+ ECL detection method is suitable for the determination of those compounds in biological fluids

Electrophoretic Porosimetry of Sol-Gels

Science.gov (United States)

Snow, L. A.; Smith, D. D.; Sibille, L.; Hunt, A. J.; Ng, J.; Rose, M. Franklin (Technical Monitor)

2000-01-01

It has been hypothesized that gravity has an effect on the formation and resulting microstructure of sol-gels. In order to more clearly resolve the effect of gravity, pores may be non-destructively analyzed in the wet gel, circumventing the shrinkage and coarsening associated with the drying procedure. We discuss the development of an electrophoretic technique, analogous to affinity chromatography, for the determination of pore size distribution and its application to silica gels. Specifically a monodisperse charged dye is monitored by an optical densitometer as it moves through the wet gel under the influence of an electric field. The transmittance data (output) represents the convolution of the dye concentration profile at the beginning of the run (input) with the pore size distribution (transfer function), i.e. linear systems theory applies. Because of the practical difficulty in producing a delta function input dye profile we prefer instead to use a step function. Average pore size is then related to the velocity of this dye front, while the pore size distribution is related to the spreading of the front. Preliminary results of this electrophoretic porosimetry and its application to ground and space-grown samples will be discussed.

Effect of annealing temperature on structural, morphological and electrical properties of nanoparticles TiO{sub 2} thin films by sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Muaz, A. K. M.; Hashim, U., E-mail: uda@unimap.edu.my; Arshad, M. K. Md.; Ruslinda, A. R.; Ayub, R. M.; Gopinath, Subash C. B.; Voon, C. H.; Liu, Wei-Wen; Foo, K. L. [Institute of Nano Electronic Engineering, Univerisiti Malaysia Perlis, 01000 Kangar, Perlis (Malaysia)

2016-07-06

In this paper, the sol-gel method is used to prepare nanoparticles titanium dioxide (TiO{sub 2}) thin films at different annealing temperature. The prepared sol was deposited on the p-SiO{sub 2} substrates by spin coating technique under room temperature. The nanoparticles TiO{sub 2} solution was synthesized using Ti{OCH(CH_3)_2}{sub 4} as a precursor with an methanol solution at a molar ratio 1:10. The prepared TiO{sub 2} sols will further validate through structural, morphological and electrical properties. From the X-ray diffraction (XRD) analysis, as-deposited films was found to be amorphous in nature and tend to transform into tetragonal anatase and rutile phase as the films annealed at 573 and 773 K, respectively. The diversification of the surface roughness was characterized by atomic force microscopy (AFM) indicated the roughness and thickness very dependent on the annealing temperature. The two-point probe electrical resistance and conductance of nanoparticles TiO{sub 2} thin films were determined by the DC current-voltage (IV) analysis. From the I-V measurement, the electrical conductance increased as the films annealed at higher temperature.

Electrochemically deposited sol-gel-derived silicate films as a viable alternative in thin-film design.

Science.gov (United States)

Deepa, P N; Kanungo, Mandakini; Claycomb, Greg; Sherwood, Peter M A; Collinson, Maryanne M

2003-10-15

Sol-gel-derived silicate films were electrochemically deposited on conducting surfaces from a sol consisting of tetramethoxysilane (TMOS). In this method, a sufficiently negative potential is applied to the electrode surface to reduce oxygen to hydroxyl ions, which serves as the catalyst for the hydrolysis and condensation of TMOS. The electrodeposition process was followed by the electrochemical quartz crystal microbalance and cyclic voltammetry. The electrodeposited films were characterized for their surface morphology, porosity, and film thickness using atomic force microscopy, electrochemical probe techniques, surface area and pore size analysis, and profilometry. The electrodeposited films were found to have a completely different surface structure and to be significantly rougher relative to spin-coated films. This is likely due in part to the separation of the gelation and evaporation stages of film formation. The electrodeposited films were found to be permeable to simple redox molecules, such as ruthenium(III) hexaammine and ferrocene methanol. Film thickness can be easily varied from 15 microm by varying the electrode potential from -600 mV to more than -1000 mV, respectively. The electrodeposition process was further applied for the electroencapsulation of redox molecules and organic dyes within the silicate network. Cyclic voltammograms for the gel-entrapped ferrocene methanol (FcCH2OH) and ruthenium(II) tris(bipyridine) (Ru(bpy)3(2+)) exhibited the characteristic redox behavior of the molecules. The electroencapsulation of organic dyes in their "native" form proved to be more difficult because these species typically contain reducible functionalities that change the structure of the dye.

Synthesis, Structural and Optical Properties of Co Doped TiO2 Nanocrystals by Sol-Gel Method

OpenAIRE

Sridevi , D.V ,; Ramesh , V; Sakthivel , T; Geetha , K ,; Ratchagar , V ,; Jagannathan , K ,; Rajarajan , K ,; Ramachadran , K ,

2017-01-01

International audience; A TiO2 nanoparticle doped with cobalt was synthesized by sol-gel technique employed at room temperature with appropriate reactants. In the present case, we used titanium tetra isoprotoxide (TTIP) and 2–propanol as a common starting material and the obtained products were calcined at 450˚C450˚450˚C. From the Powder XRD data the particle size was calculated by Scherrer method. The FE-SEM analysis shows the morphology of cobalt doped TiO2 nanoparticles. The various functi...

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

Science.gov (United States)

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

2016-03-31

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

Synthesis of hydroxyapatite nanoparticles from egg shells by sol-gel method

Science.gov (United States)

Azis, Y.; Adrian, M.; Alfarisi, C. D.; Khairat; Sri, R. M.

2018-04-01

Hydroxyapatite, [Ca10(PO4)6(OH)2, (HAp)] is widely used in medical fields especially as a bone and teeth substitute. Hydroxyapatite nanoparticles have been succesfully synthesized from egg shells as a source of calcium by using sol-gel method. The egg shells were calcined, hydrated (slaking) and undergone carbonation to form Precipitated Calcium Carbonate (PCC).Then the PCC was added (NH4)2HPO4 to form HAp with variation the mole ratio Ca and P (1.57; 1.67 and 1.77), aging time (24, 48, and 72 hr) and under basic condition pH (9, 10 and 11). The formation of hydroxyapatite biomaterial was characterized using XRD, FTIR, SEM-EDX. The XRD patterns showed that the products were hydroxyapatite crystals. The best result was obtained at 24 hr aging time, pH 9 with hexagonal structure of hydroxyapatite. Particle size of HAp was 35-54 nm and the morphology of hydroxyapatite observed using SEM, it showed that the uniformity crystal of hydroxyapatite.

Modelling of erosion of bentonite gel by gel/sol flow

Energy Technology Data Exchange (ETDEWEB)

Moreno, Luis; Neretnieks, Ivars; Longcheng Liu (Chemical Engineering and Technology, School of Chemical Science and Engineering, Royal Institute of Technology, Stockholm (Sweden))

2010-11-15

Bentonite intrusion into a fracture intersecting the canister deposition hole is modelled. The model describes the expansion of the bentonite within the fracture. It accounts for the repulsive electrostatic double-layer forces, the attractive van der Waals forces and friction forces between the particles and the water. The model also takes into account the diffusion of the colloid particles in the smectite sol. Diffusion of a counterion, sodium, is accounted for as this strongly influences the double layer force and the viscosity of the gel/sol. The gel/sol is considered to be a fluid with a varying viscosity that is strongly dependent on the bentonite volume fraction in the gel and the sodium concentration in the water. Two different geometries were modelled; a rectangular and a cylindrical. The rectangular geometry was used to gain experience with the processes and mechanisms and how they interact since the cylindrical geometry was somewhat less stable numerically and more time consuming. In the rectangular geometry a fracture 1 metre long in the flow direction was modelled. In both geometries the fracture size was selected sufficiently large to ensure that the water velocity, near the distant border was nearly the same as the approaching water velocity and that the smectite concentration there was vanishingly small. It was found that the velocity of the fluid drops considerably where the bentonite volume fraction is larger than 1-2%. This is due to the strong increase in viscosity with increasing bentonite volume fraction. The loss of smectite by the slowly flowing fluid was found to be proportional to the square root of the seeping water velocity for the rectangular geometry. For the cylindrical geometry, the dependence is somewhat lower (exponent about 0.4) since the length of the gel/water interface decreases with increasing water flow rate. The penetration depth of the gel/water interface decreases with increasing water flow rate. For water velocity of the

Modelling of erosion of bentonite gel by gel/sol flow

International Nuclear Information System (INIS)

Moreno, Luis; Neretnieks, Ivars; Longcheng Liu

2010-11-01

Bentonite intrusion into a fracture intersecting the canister deposition hole is modelled. The model describes the expansion of the bentonite within the fracture. It accounts for the repulsive electrostatic double-layer forces, the attractive van der Waals forces and friction forces between the particles and the water. The model also takes into account the diffusion of the colloid particles in the smectite sol. Diffusion of a counterion, sodium, is accounted for as this strongly influences the double layer force and the viscosity of the gel/sol. The gel/sol is considered to be a fluid with a varying viscosity that is strongly dependent on the bentonite volume fraction in the gel and the sodium concentration in the water. Two different geometries were modelled; a rectangular and a cylindrical. The rectangular geometry was used to gain experience with the processes and mechanisms and how they interact since the cylindrical geometry was somewhat less stable numerically and more time consuming. In the rectangular geometry a fracture 1 metre long in the flow direction was modelled. In both geometries the fracture size was selected sufficiently large to ensure that the water velocity, near the distant border was nearly the same as the approaching water velocity and that the smectite concentration there was vanishingly small. It was found that the velocity of the fluid drops considerably where the bentonite volume fraction is larger than 1-2%. This is due to the strong increase in viscosity with increasing bentonite volume fraction. The loss of smectite by the slowly flowing fluid was found to be proportional to the square root of the seeping water velocity for the rectangular geometry. For the cylindrical geometry, the dependence is somewhat lower (exponent about 0.4) since the length of the gel/water interface decreases with increasing water flow rate. The penetration depth of the gel/water interface decreases with increasing water flow rate. For water velocity of the

Fluorescent silica hybrid materials containing benzimidazole dyes obtained by sol-gel method and high pressure processing

International Nuclear Information System (INIS)

Hoffmann, Helena Sofia; Stefani, Valter; Benvenutti, Edilson Valmir; Costa, Tania Maria Haas; Gallas, Marcia Russman

2011-01-01

Research highlights: → Sol-gel technique was used to obtain silica based hybrid materials containing benzimidazole dyes. → The sol-gel catalysts, HF and NaF, produce xerogels with different optical and textural characteristics. → High pressure technique (6.0 GPa) was used to produce fluorescent and transparent silica compacts with the dyes entrapped in closed pores, maintaining their optical properties. → The excited state intramolecular proton transfer (ESIPT) mechanism of benzimidazole dyes was studied by steady-state fluorescence spectroscopy for the monoliths, powders, and compacts. - Abstract: New silica hybrid materials were obtained by incorporation of two benzimidazole dyes in the silica network by sol-gel technique, using tetraethylorthosilicate (TEOS) as inorganic precursor. Several syntheses were performed with two catalysts (HF and NaF) producing powders and monoliths with different characteristics. The dye 2-(2'-hydroxy-5'-aminophenyl)benzimidazole was dispersed and physically adsorbed in the matrix, and the dye 2'(5'-N-(3-triethoxysilyl)propylurea-2'-hydroxyphenyl)benzimidazole was silylated, becoming chemically bonded to the silica network. High pressure technique was used to produce fluorescent and transparent silica compacts with the silylated and incorporated dye, at 6.0 GPa and room temperature. The excited state intramolecular proton transfer (ESIPT) mechanism of benzimidazole dyes was studied by steady-state fluorescence spectroscopy for the monoliths, powders, and compacts. The influence of the syntheses conditions was investigated by textural analysis using nitrogen adsorption isotherms.

Sol-gel synthesis and optical properties of titanium dioxide thin film

Science.gov (United States)

Ullah, Irfan; Khattak, Shaukat Ali; Ahmad, Tanveer; Saman; Ludhi, Nayab Ali

2018-03-01

The titanium dioxide (TiO2) is synthesized by sol-gel method using titanium-tetra-iso-propoxide (TTIP) as a starting material, and deposited on the pre-cleaned glass substrate using spin coating technique at optimized parameters. Energy dispersive X-ray (EDX) spectroscopy confirms successful TiO2 growth. The optical properties concerning the transmission and absorption spectra show 85% transparency and 3.28 eV wide optical band gap for indirect transition, calculated from absorbance. The exponential behavior of absorption edge is observed and attributed to the localized states electronic transitions, curtailed in the indirect band gap of the thin film. The film reveals decreasing refractive index with increasing wavelength. The photoluminescence (PL) study ascertains that luminescent properties are due to the surface defects.

Photo catalytic Degradation of Organic Dye by Sol-Gel-Derived Gallium-Doped Anatase Titanium Oxide Nanoparticles for Environmental Remediation

International Nuclear Information System (INIS)

Arghya, N.B.; Sang, W.J.; Bong-Ki, M.

2012-01-01

Photo catalytic degradation of toxic organic chemicals is considered to be the most efficient green method for surface water treatment. We have reported the sol-gel synthesis of Gadoped anatase TiO 2 nanoparticles and the photo catalytic oxidation of organic dye into nontoxic inorganic products under UV irradiation. Photodegradation experiments show very good photo catalytic activity of Ga-doped TiO 2 nanoparticles with almost 90% degradation efficiency within 3 hrs of UV irradiation, which is faster than the undoped samples. Doping levels created within the bandgap of TiO 2 act as trapping centers to suppress the photo generated electron-hole recombination for proper and timely utilization of charge carriers for the generation of strong oxidizing radicals to degrade the organic dye. Photo catalytic degradation is found to follow the pseudo-first-order kinetics with the apparent 1 st-order rate constant around 1.3 x 10 -2 min -1 . The cost-effective, sol-gel-derived TiO 2 : Ga nanoparticles can be used efficiently for light-assisted oxidation of toxic organic molecules in the surface water for environmental remediation.

ZnO-SiO{sub 2} based nanocomposites prepared by a modified sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Grigorie, Alexandra Carmen [Politehnica University Timisoara, Faculty of Industrial Chemistry and Environmental Engineering, 6 V. Parvan Blv., RO-300223, Timisoara (Romania); Muntean, Cornelia, E-mail: cornelia.muntean@upt.ro [Politehnica University Timisoara, Faculty of Industrial Chemistry and Environmental Engineering, 6 V. Parvan Blv., RO-300223, Timisoara (Romania); Politehnica University Timisoara, Research Institute for Renewable Energy, 2 Piata Victoriei, RO-300006, Timisoara (Romania); Vlase, Titus [West University of Timisoara, 4 V. Parvan Blv., RO-300223, Timisoara (Romania); Locovei, Cosmin [Politehnica University Timisoara, Research Institute for Renewable Energy, 2 Piata Victoriei, RO-300006, Timisoara (Romania); Politehnica University Timisoara, Faculty of Mechanical Engineering, 1 Mihai Viteazul Blv., RO-300222, Timisoara (Romania); Stefanescu, Mircea [Politehnica University Timisoara, Faculty of Industrial Chemistry and Environmental Engineering, 6 V. Parvan Blv., RO-300223, Timisoara (Romania)

2017-01-15

This paper presents a study on nanocomposites formation in ZnO-SiO{sub 2} systems with different ZnO:SiO{sub 2} molar ratios (1:4, 1:1, and 4:1), prepared employing a sol-gel method modified by an original procedure. The evolution of ZnO-SiO{sub 2} systems depending on the composition and temperature was studied by thermal analysis, Fourier transform infrared spectroscopy, X-ray diffractometry and transmission electron microscopy. Zn(II) carboxylate was synthesized in situ in hybrid silica gels by redox reaction between zinc nitrate and 1,3-propanediol. Its thermal decomposition at low temperatures led to ZnO dispersed in the pores of silica matrix. Only for the 4:1 system, at 400 and 600 °C, ZnO nanocrystallites (average size ∼9 nm) embedded in the amorphous silica matrix were obtained, the other systems being amorphous. Whatever the mixture composition is, above 600 °C, ZnO reacts with SiO{sub 2} to form zinc silicate. At 800 °C, for both 1:4 and 1:1 systems, poor crystallized β-Zn{sub 2}SiO{sub 4} and α-Zn{sub 2}SiO{sub 4} phases embedded in silica matrix were formed. Increasing the temperature, at 1000 °C, only for 1:1 system, β-Zn{sub 2}SiO{sub 4} phase turned into single phase α-Zn{sub 2}SiO{sub 4} (average crystallites size 28.3 nm). For 4:1 composition, at 800 and 1000 °C, systems consisting of ZnO and α-Zn{sub 2}SiO{sub 4} nanocrystallites dispersed in silica were obtained. - Highlights: • By modified sol-gel method, ZnO/SiO{sub 2} and Zn{sub 2}SiO{sub 4}/SiO{sub 2} nanocomposites were obtained. • ZnO dispersed in silica matrix results from zinc carboxylate thermal decomposition. • Zinc carboxylate was synthesized in situ in hybrid silica gels via redox reaction. • Evolution of ZnO in SiO{sub 2} matrix depends on temperature and system composition.

Iron-based soft magnetic composites with Mn-Zn ferrite nanoparticles coating obtained by sol-gel method

Science.gov (United States)

Wu, Shen; Sun, Aizhi; Xu, Wenhuan; Zhang, Qian; Zhai, Fuqiang; Logan, Philip; Volinsky, Alex A.

2012-11-01

This paper focuses on iron-based soft magnetic composites which were synthesized by utilizing Mn-Zn ferrite nanoparticles to coat iron powder. The nanocrystalline iron powders, with an average particle diameter of 20 nm, were obtained via the sol-gel method. Scanning electron microscopy, energy dispersive X-ray spectroscopy and distribution maps show that the iron particle surface is covered with a thin layer of Mn-Zn ferrites. Mn-Zn ferrite uniformly coated the surface of the powder particles, resulting in a reduced imaginary permeability, increased electrical resistivity and a higher operating frequency of the synthesized magnets. Mn-Zn ferrite coated samples have higher permeability and lower magnetic loss when compared with the non-magnetic epoxy resin coated compacts. The real part of permeability increases by 33.5% when compared with the epoxy resin coated samples at 10 kHz. The effects of heat treatment temperature on crystalline phase formation and on the magnetic properties of the Mn-Zn ferrite were investigated via X-ray diffraction and a vibrating sample magnetometer. Ferrites decomposed to FeO and MnO after annealing above 400 °C in nitrogen; thus it is the optimum annealing temperature to attain the desired permeability.

Variables of synthesis in obtaining nanosilicas with sol-gel

International Nuclear Information System (INIS)

Elia, A; Martin-Aispuro, P; Musante, L; Martin-Martinez, J.M; Vazquez, P

2008-01-01

Amorphous silica materials and polycrystalline are now being developed for different applications as optic components, superconductors, nano-particles used as charges in adhesives and paints, among others. Some methods of obtaining these materials involve complex techniques and high costs. Generally, the materials constituents are fused, for example, using the pyrogenic silica technique, widely used industrially. Meanwhile, the sol-gel meted is based on a mixture of liquid reagents at the molecular level, to easily obtain amorphous and polycrystalline materials, even at room temperature. Therefore, the sol-gel way is a promising option for producing new materials, due to its cost advantages compared to the traditional methods. The sol-gel technique consists of the simultaneous reaction of the hydrolysis and the condensation. In this process the precursor solution, the TEOS in our case, becomes a polymeric gel network polymer. The partial hydrolysis of the orthosilicate takes place when it is mixed with water and ethanol (EtOH), the reaction that occurs is: S i(OEt) 4 + H 2 O S i(OEt) 3 (OH) + EtOH. The condensation takes place between two OH groups or between an OH group and an ethoxy to form an oxygen bridge plus water or ethanol. S i(OEt) 4 + H 2 O + S i(OEt) 3 (OH)(EtO) 3 Si-O-Si(OEt) 3 (OH) + H 2 O S i-OH + HO-Si S i-O-Si + H 2 O. The addition of a base or of an acid catalyzes the process and changes the pH of the solution influencing the condensation process and size of the final particle. This work focuses on finding different conditions by varying the pH, using HCI, with and without agitation during the addition of the HCI, and washing the solid obtained with ethanol in order to study its effect. The nanosilicas were characterized by TEM-EDX, DTA-TGA, S BET , FT-IR, DRX, DRS, SEM and pH measurements. The morphology of the nanosilicas was characterized with SEM and TEM. Using these techniques a partial conclusion showed that the samples synthesized with HCI

{alpha} Fe{sub 2}O{sub 3} films grown by the spin-on sol-gel deposition method

Energy Technology Data Exchange (ETDEWEB)

Avila G, A.; Carbajal F, G. [Seccion de Electronica del Estado Solido, Departamento de Ingenieria Electrica, CINVESTAV del l.P.N., Av. I.P.N. No. 2508, Apartado Postal 14-740, Mexico 07360, D.F (Mexico); Tiburcio S, A. [Division Posg, lnstituto Tecnologico de Toluca-SEP, P.O. Box 890, 50000 Toluca, Edo. Mex. (Mexico); Barrera C, E. [Departamento de IPH, Area de Ingenieria en Recursos Energeticos, Universidad Autonoma Metropolitana-lztapalapa, Apartado Postal 55-5340, Mexico, D.F. (Mexico); Andrade I, E. [Instituto de Fsica, Universidad Nacional Autononca de Mexico, Apartado Postal 20-364, Mexico 01000, D. F (Mexico)

2003-07-01

{alpha}-Fe{sub 2}O{sub 3} polycrystalline films with grains larger than 31 nm were grown by the spin-on sol-gel deposition method. The particular sol used was prepared starting from two distinct precursor reagents. Both precursors leaded to similar films. Order within the films was altered by adding tin to the samples. Transmittance measurements confirmed that the hematite phase is obtained by annealing the samples above 400 C and yielded an optical gap of about 2.2 eV, but additional transitions at 2.7 eV were also observed. From RBS measurements it was found that tin inclusion decreases iron content as expected, but also increases oxygen concentration within the films. This last observation was associated to the disorder rise when introducing tin atoms. (Author)

Fabrication of highly conductive graphene/ITO transparent bi-film through CVD and organic additives-free sol-gel techniques.

Science.gov (United States)

Hemasiri, Bastian Waduge Naveen Harindu; Kim, Jae-Kwan; Lee, Ji-Myon

2017-12-19

Indium tin oxide (ITO) still remains as the main candidate for high-performance optoelectronic devices, but there is a vital requirement in the development of sol-gel based synthesizing techniques with regards to green environment and higher conductivity. Graphene/ITO transparent bi-film was synthesized by a two-step process: 10 wt. % tin-doped ITO thin films were produced by an environmentally friendly aqueous sol-gel spin coating technique with economical salts of In(NO 3 ) 3 .H 2 O and SnCl 4 , without using organic additives, on surface free energy enhanced (from 53.826 to 97.698 mJm -2 ) glass substrate by oxygen plasma treatment, which facilitated void-free continuous ITO film due to high surface wetting. The chemical vapor deposited monolayer graphene was transferred onto the synthesized ITO to enhance its electrical properties and it was capable of reducing sheet resistance over 12% while preserving the bi-film surface smoother. The ITO films contain the In 2 O 3 phase only and exhibit the polycrystalline nature of cubic structure with 14.35 ± 0.5 nm crystallite size. The graphene/ITO bi-film exhibits reproducible optical transparency with 88.66% transmittance at 550 nm wavelength, and electrical conductivity with sheet resistance of 117 Ω/sq which is much lower than that of individual sol-gel derived ITO film.

Active corrosion protection of AA2024 by sol-gel coatings with corrosion inhibitors =

Science.gov (United States)

Yasakau, Kiryl

A industria aeronautica utiliza ligas de aluminio de alta resistencia para o fabrico dos elementos estruturais dos avioes. As ligas usadas possuem excelentes propriedades mecanicas mas apresentam simultaneamente uma grande tendencia para a corrosao. Por esta razao essas ligas necessitam de proteccao anticorrosiva eficaz para poderem ser utilizadas com seguranca. Ate a data, os sistemas anticorrosivos mais eficazes para ligas de aluminio contem cromio hexavalente na sua composicao, sejam pre-tratamentos, camadas de conversao ou pigmentos anticorrosivos. O reconhecimento dos efeitos carcinogenicos do cromio hexavalente levou ao aparecimento de legislacao banindo o uso desta forma de cromio pela industria. Esta decisao trouxe a necessidade de encontrar alternativas ambientalmente inocuas mas igualmente eficazes. O principal objectivo do presente trabalho e o desenvolvimento de pretratamentos anticorrosivos activos para a liga de aluminio 2024, baseados em revestimentos hibridos produzidos pelo metodo sol-gel. Estes revestimentos deverao possuir boa aderencia ao substrato metalico, boas propriedades barreira e capacidade anticorrosiva activa. A proteccao activa pode ser alcancada atraves da incorporacao de inibidores anticorrosivos no pretratamento. O objectivo foi atingido atraves de uma sucessao de etapas. Primeiro investigou-se em detalhe a corrosao localizada (por picada) da liga de aluminio 2024. Os resultados obtidos permitiram uma melhor compreensao da susceptibilidade desta liga a processos de corrosao localizada. Estudaram-se tambem varios possiveis inibidores de corrosao usando tecnicas electroquimicas e microestruturais. Numa segunda etapa desenvolveram-se revestimentos anticorrosivos hibridos organico-inorganico baseados no metodo sol-gel. Compostos derivados de titania e zirconia foram combinados com siloxanos organofuncionais a fim de obter-se boa aderencia entre o revestimento e o substrato metalico assim como boas propriedades barreira. Testes

Synthesis and characterization of nanosized Mg{sub x}Mn{sub 1−x}Fe{sub 2}O{sub 4} ferrites by both sol-gel and thermal decomposition methods

Energy Technology Data Exchange (ETDEWEB)

De-León-Prado, Laura Elena, E-mail: laura.elena.prado@gmail.com [Cinvestav-Unidad Saltillo, Av. Industria Metalúrgica #1062, Parque Industrial Saltillo-Ramos Arizpe, CP 25900, Ramos Arizpe, Coahuila, México (Mexico); Cortés-Hernández, Dora Alicia; Almanza-Robles, José Manuel; Escobedo-Bocardo, José Concepción; Sánchez, Javier; Reyes-Rdz, Pamela Yajaira; Jasso-Terán, Rosario Argentina [Cinvestav-Unidad Saltillo, Av. Industria Metalúrgica #1062, Parque Industrial Saltillo-Ramos Arizpe, CP 25900, Ramos Arizpe, Coahuila, México (Mexico); Hurtado-López, Gilberto Francisco [Centro de Investigación en Química Aplicada, Blvd. Enrique Reyna Hermosillo #140, CP 25294, Saltillo, Coahuila, México (Mexico)

2017-04-01

This work reports the synthesis of Mg{sub x}Mn{sub 1−x}Fe{sub 2}O{sub 4} (x=0–1) nanoparticles by both sol-gel and thermal decomposition methods. In order to determine the effect of synthesis conditions on the crystal structure and magnetic properties of the ferrites, the synthesis was carried out varying some parameters, including composition. By both methods it was possible to obtain ferrites having a single crystalline phase with cubic inverse spinel structure and a behavior near to that of superparamagnetic materials. Saturation magnetization values were higher for materials synthesized by sol-gel. Furthermore, in both cases particles have a spherical-like morphology and nanometric sizes (11–15 nm). Therefore, these materials can be used as thermoseeds for the treatment of cancer by magnetic hyperthermia. - Highlights: • Mg–Mn ferrites were synthesized by sol-gel and thermal decomposition methods. • Materials showed a single cubic inverse spinel crystalline structure. • Ferrites have a soft ferrimagnetic behavior close to superparamagnetic materials.

A Novel Microdialysis Glucose Sensor System Based on Co-immobilizing on AU Micro-Electrode by SOL-GEL Technique

National Research Council Canada - National Science Library

Yu, Ping

2001-01-01

.... The sensor is based on co_immobilizing glucose oxidase (COD) with the catalase by sol-gel technique on the surface of the silicon bases with two pattern of An microelectrodes. A graduated ("sandwich...

The Power of Non-Hydrolytic Sol-Gel Chemistry: A Review

Directory of Open Access Journals (Sweden)

Ales Styskalik

2017-05-01

Full Text Available This review is devoted to non-hydrolytic sol-gel chemistry. During the last 25 years, non-hydrolytic sol-gel (NHSG techniques were found to be attractive and versatile methods for the preparation of oxide materials. Compared to conventional hydrolytic approaches, the NHSG route allows reaction control at the atomic scale resulting in homogeneous and well defined products. Due to these features and the ability to design specific materials, the products of NHSG reactions have been used in many fields of application. The aim of this review is to present an overview of NHSG research in recent years with an emphasis on the syntheses of mixed oxides, silicates and phosphates. The first part of the review highlights well known condensation reactions with some deeper insights into their mechanism and also presents novel condensation reactions established in NHSG chemistry in recent years. In the second section we discuss porosity control and novel compositions of selected materials. In the last part, the applications of NHSG derived materials as heterogeneous catalysts and supports, luminescent materials and electrode materials in Li-ion batteries are described.

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

Energy Technology Data Exchange (ETDEWEB)

Atta, Nada F., E-mail: Nada_fah1@yahoo.com [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)

2010-05-14

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.

Highly efficient solid-state neutron scintillators based on hybrid sol-gel nanocomposite materials

International Nuclear Information System (INIS)

Kesanli, Banu; Hong, Kunlun; Meyer, Kent; Im, Hee-Jung; Dai, Sheng

2006-01-01

This research highlights opportunities in the formulation of neutron scintillators that not only have high scintillation efficiencies but also can be readily cast into two-dimensional detectors. Series of transparent, crack-free monoliths were prepared from hybrid polystyrene-silica nanocomposites in the presence of arene-containing alkoxide precursor through room temperature sol-gel processing. The monoliths also contain lithium-6 salicylate as a target material for neutron-capture reactions and amphiphilic scintillator solution as a fluorescent sensitizer. Polystyrene was functionalized by trimethoxysilyl group in order to enable the covalent incorporation of aromatic functional groups into the inorganic sol-gel matrices for minimizing macroscopic phase segregation and facilitating lithium-6 doping in the sol-gel samples. Neutron and alpha responses of these hybrid polystyrene-silica monoliths were explored

Synthesis and characterization of NiO nanopowder by sol-gel process

Energy Technology Data Exchange (ETDEWEB)

Ningsih, Sherly Kasuma Warda [Department of Chemistry, Faculty of Mathematics and Natural Sciences Padang State University, Kampus Air Tawar, Jl. Prof. Dr. Hamka, West Sumatera, 25161, Indonesia Email: sherly-kasuma@yahoo.com (Indonesia)

2015-09-30

Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms were produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.

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

Energy Technology Data Exchange (ETDEWEB)

Krueger, Hannes

2009-09-24

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

Application of response surface methodology for degradation of methyl orange with TiO{sub 2} sol-gel sulphated Ti; Aplicacion de metodologia de superficie de respuesta para la degradacion de naranja de metilo con TiO{sub 2} sol-gel sulfatado

Energy Technology Data Exchange (ETDEWEB)

Del Angel S, M. T.; Garcia A, R. [Instituto Tecnologico de Ciudad Madero, Av. 1o. de Mayo y Sor Juana I. de la Cruz, Col. Los Mangos, 89440 Ciudad Madero, Tamaulipas (Mexico); Garcia A, P.; Lagunes G, L. M. [Universidad Juarez Autonoma de Tabasco, Division Academica de Ciencias Agropecuarias, Av. Universidad s/n, Zona de la Cultura, Col. Magisterial, 86040 Villahermosa, Tabasco (Mexico); Cabrera C, E. G., E-mail: shish_kko@yahoo.com.mx [Instituto Tecnologico de Villahermosa, Carretera Villahermosa-Frontera Km. 3.5, Cd. Industrial, 86010 Villahermosa, Tabasco (Mexico)

2015-06-01

In this work we report the implementation of the response surface methodology for the optimization of photo catalytic degradation of methyl orange dye (MO) using as photo catalyst sulphated TiO{sub 2} prepared by sol-gel method. The variables studied were ph of the solution (3-11), catalyst concentration (0.1-1 g/L), and MO concentration (10-30 ppm). The effects of these parameters over the degradation of MO were evaluated according to a Box-Behnken design. The only crystal structure identified by X-ray diffraction was anatase phase. The optimum conditions for the photo catalytic degradation of MO according to the methodology applied were ph 6.0, 17.78 ppm MO concentration at each concentration level of the catalyst. (Author)

Moisture sensor based on evanescent wave light scattering by porous sol-gel silica coating

Science.gov (United States)

Tao, Shiquan; Singh, Jagdish P.; Winstead, Christopher B.

2006-05-02

An optical fiber moisture sensor that can be used to sense moisture present in gas phase in a wide range of concentrations is provided, as well techniques for making the same. The present invention includes a method that utilizes the light scattering phenomenon which occurs in a porous sol-gel silica by coating an optical fiber core with such silica. Thus, a porous sol-gel silica polymer coated on an optical fiber core forms the transducer of an optical fiber moisture sensor according to an embodiment. The resulting optical fiber sensor of the present invention can be used in various applications, including to sense moisture content in indoor/outdoor air, soil, concrete, and low/high temperature gas streams.

Protic ionic liquid as additive on lipase immobilization using silica sol-gel.

Science.gov (United States)

de Souza, Ranyere Lucena; de Faria, Emanuelle Lima Pache; Figueiredo, Renan Tavares; Freitas, Lisiane dos Santos; Iglesias, Miguel; Mattedi, Silvana; Zanin, Gisella Maria; dos Santos, Onélia Aparecida Andreo; Coutinho, João A P; Lima, Álvaro Silva; Soares, Cleide Mara Faria

2013-03-05

Ionic liquids (ILs) have evolved as a new type of non-aqueous solvents for biocatalysis, mainly due to their unique and tunable physical properties. A number of recent review papers have described a variety of enzymatic reactions conducted in IL solutions, on the other hand, to improve the enzyme's activity and stability in ILs; major methods being explored include the enzyme immobilization (on solid support, sol-gel, etc.), protic ionic liquids used as an additive process. The immobilization of the lipase from Burkholderia cepacia by the sol-gel technique using protic ionic liquids (PIL) as additives to protect against inactivation of the lipase due to release of alcohol and shrinkage of the gel during the sol-gel process was investigated in this study. The influence of various factors such as the length of the alkyl chain of protic ionic liquids (monoethanolamine-based) and a concentration range between 0.5 and 3.0% (w/v) were evaluated. The resulting hydrophobic matrices and immobilized lipases were characterised with regard to specific surface area, adsorption-desorption isotherms, pore volume (V(p)) and size (d(p)) according to nitrogen adsorption and scanning electron microscopy (SEM), physico-chemical properties (thermogravimetric - TG, differential scanning calorimetry - DSC and Fourier transform infrared spectroscopy - FTIR) and the potential for ethyl ester and emulsifier production. The total activity yields (Y(a)) for matrices of immobilized lipase employing protic ionic liquids as additives always resulted in higher values compared with the sample absent the protic ionic liquids, which represents 35-fold increase in recovery of enzymatic activity using the more hydrophobic protic ionic liquids. Compared with arrays of the immobilized biocatalyst without additive, in general, the immobilized biocatalyst in the presence of protic ionic liquids showed increased values of surface area (143-245 m(2) g(-1)) and pore size (19-38 Å). Immobilization with

Development of fluorocarbon/silica composites via sol/gel process

International Nuclear Information System (INIS)

Ferreira, Max P.; Maria, Daniel A.; Gomes, Luiza M.F.

2009-01-01

Fluorocarbon/silica composites have interesting physical-chemical properties, combining the great resistance to chemical products, the electric insulation, and the thermal stability of fluorine polymers with the optical, magnetic, and dielectric properties of silica. Due to the unique mechanical, thermal, and dielectric properties of fluorocarbon and silica composites, there is interest in their application in the development of fuel cells, the production of integrated circuit boards (ICB), and packages for the transportation of integrated circuits. The sol-gel process is a chemical route to prepare ceramic materials with specific properties that are hard or impossible to obtain by conventional methods. Fluorocarbon/silica composites were obtained by the sol-gel method from tetramethoxysilane - TMOS and fluorinated hydrocarbons with low molecular weight and main chains with 10 - 20 carbon atoms previously obtained from PTFE scraps irradiated with a 60 Co γ source in oxygen atmosphere with a dose of 1 MGy. Syntheses were performed in 125-mL reaction flasks in basic medium at 35 deg C and in acid medium at 60 deg C with N-N dimethylformamide as a chemical additive for drying control. After synthesis, the material was thermally treated in an oven with electronic temperature control. The monoliths obtained were characterized by Fourier transform infrared spectroscopy (FTIR), electron microprobe and by a standard nitrogen adsorption-desorption technique. (author)

Microstructure of Zirconia-Based Sol-Gel Glasses Studied by SANS

Czech Academy of Sciences Publication Activity Database

Ryukhtin, Vasyl; Strunz, Pavel; Kopitsa, G. P.; Ezdakova, K. V.; Gubanova, N. N.; Ivanov, V. K.; Baranchikov, A. Y.; Angelov, Borislav; Feoktistov, A.; Pipich, V.; Levinský, P.

2015-01-01

Roč. 128, č. 4 (2015), s. 582-584 ISSN 0587-4246. [ISPMA 13 - 13th INTERNATIONAL SYMPOSIUM ON PHYSICS OF MATERIALS. Praha, 31.08.2014 - 04.09.2014] R&D Projects: GA ČR GB14-36566G; GA MŠk LM2011019 Institutional support: RVO:61389013 ; RVO:61389005 Keywords : sol-gel method * SANS * USANS Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.525, year: 2015

The role sol-gel process for nuclear fuels - an overview

International Nuclear Information System (INIS)

Sood, D.D.

2009-01-01

The paper reviews the sol-gel methods used for the preparation of fuel materials in the form of microspheres. It also discusses how these microspheres can be fabricated into nuclear fuels for reactors like High Temperature Gas Cooled Reactors and Fast Reactors. Performance of these microsphere based fuels is reviewed. More recent applications, like transmutation of minor actinides, (Np, Am and Cm) and hydrogen production, are also briefly covered. (author)

Peri-tumor administration of 5-fluorouracil sol-gel using a hollow microneedle for treatment of gastric cancer.

Science.gov (United States)

Jung, Yoon Suk; Koo, Dong-Hoe; Yang, Jeong-Yoon; Lee, Hee-Young; Park, Jung-Hwan; Park, Jung Ho

2018-11-01

The aim of this study was to investigate the effectiveness of treating gastric cancer by injecting a pluronic F-127 sol-gel formulation of 5-fluorouracil (5-FU) into normal tissue surrounding the tumor using a hollow microneedle. The MTS tetrazolium assay was performed to assess the cytotoxicity of 5-FU after application to gastric cancer cells at different concentrations for 1, 5 and 10 h. Gastric cancer cells were inoculated subcutaneously into 30 male nude mice (CrjBALB/c-nu/nu mice, male); the inoculated mouse were divided into three groups. One group received no treatment, whereas the two other groups received free 5-FU gel (40 mg/kg) and 5-FU gel (40 mg/kg) for 4 days, respectively. Mean tumor volume, apoptotic index (TUNEL) and proliferative index (Ki 67) were evaluated in all groups. Cell viability was 77.3% when 1.22 g of free 5-FU was administered, whereas cell viability was 37.4% and 43.5% when 0.122 g of free 5-FU was administered per hour for 10 h and 0.244 g of free 5-FU was administered for 5 h (p sol-gel induced apoptosis and significantly inhibited cell proliferation compared to the free 5-FU (p sol-gel formulation to inoculated mice (p sol-gel formulation into normal tissue surrounding the tumor mass using a hollow microneedle is an effective method for treating gastric cancer.

Sol-gel derived flexible silica aerogel as selective adsorbent for water decontamination from crude oil.

Science.gov (United States)

Abolghasemi Mahani, A; Motahari, S; Mohebbi, A

2018-04-01

Oil spills are the most important threat to the sea ecosystem. The present study is an attempt to investigate the effects of sol-gel parameters on seawater decontamination from crude oil by use of flexible silica aerogel. To this goal, methyltrimethoxysilane (MTMS) based silica aerogels were prepared by two-step acid-base catalyzed sol-gel process, involving ambient pressure drying (APD) method. To investigate the effects of sol-gel parameters, the aerogels were prepared under two different acidic and basic pH values (i.e. 4 and 8) and varied ethanol/MTMS molar ratios from 5 to 15. The adsorption capacity of the prepared aerogels was evaluated for two heavy and light commercial crude oils under multiple adsorption-desorption cycles. To reduce process time, desorption cycles were carried out by using roll milling for the first time. At optimum condition, silica aerogels are able to uptake heavy and light crude oils with the order of 16.7 and 13.7, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparation of Flame Retardant Polyacrylonitrile Fabric Based on Sol-Gel and Layer-by-Layer Assembly.

Science.gov (United States)

Ren, Yuanlin; Huo, Tongguo; Qin, Yiwen; Liu, Xiaohui

2018-03-23

This paper aims to develop a novel method, i.e., sol-gel combined with layer-by-layer assembly technology, to impart flame retardancy on polyacrylonitrile (PAN) fabrics. Silica-sol was synthesized via the sol-gel process and acted as cationic solution, and phytic acid (PA) was used as the anionic medium. Flame-retardant-treated PAN fabric (FR-PAN) could achieve excellent flame retardancy with 10 bilayer (10BL) coating through layer-by-layer assembly. The structure of the fabrics was characterized by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The thermal stability and flame retardancy were evaluated by thermogravimetric (TG) analysis, cone calorimetry (CC) and limiting oxygen index (LOI). The LOI value of the coated fabric was up to 33.2 vol % and the char residue at 800 °C also increased to 57 wt %. Cone calorimetry tests revealed that, compared to the control fabric, the peak of heat release rate (PHRR) and total heat release (THR) of FR-PAN decreased by 66% and 73%, respectively. These results indicated that sol-gel combined with layer-by-layer assembly technique could impart PAN fabric with satisfactory flame-retardant properties, showing an efficient flame retardant strategy for PAN fabric.

Safe and Environmentally Acceptable Sol-Gel-Derived Pyrophoric Pyrotechnics

National Research Council Canada - National Science Library

Simpson, Randall L; Hubble, William; Stevenson, Bradley; Gash, Alexander; Satcher, Joe; Metcalf, Patricia

2004-01-01

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...

Effects of inorganic acids and divalent hydrated metal cations (Mg(2+), Ca(2+), Co(2+), Ni(2+)) on γ-AlOOH sol-gel process.

Science.gov (United States)

Zhang, Jian; Xia, Yuguo; Zhang, Li; Chen, Dairong; Jiao, Xiuling

2015-11-07

In-depth understanding of the sol-gel process plays an essential role in guiding the preparation of new materials. Herein, the effects of different inorganic acids (HCl, HNO3 and H2SO4) and divalent hydrated metal cations (Mg(2+), Ca(2+), Co(2+), Ni(2+)) on γ-AlOOH sol-gel process were studied based on experiments and density functional theory (DFT) calculations. In these experiments, the sol originating from the γ-AlOOH suspension was formed only with the addition of HCl and HNO3, but not with H2SO4. Furthermore, the DFT calculations showed that the strong adsorption of HSO4(-) on the surface of the γ-AlOOH particles, and the hydrogen in HSO4(-) pointing towards the solvent lead to an unstable configuration of electric double layer (EDL). In the experiment, the gelation time sequence of γ-AlOOH sol obtained by adding metal ions changed when the ionic strength was equal to or greater than 0.198 mol kg(-1). The DFT calculations demonstrated that the adsorption energy of hydrated metal ions on the γ-AlOOH surface can actually make a difference in the sol-gel process.

A Urea Biosensor from Stacked Sol-Gel Films with Immobilized Nile Blue Chromoionophore and Urease Enzyme

OpenAIRE

Alqasaimeh, Muawia Salameh; Heng, Lee Yook; Ahmad, Musa

2007-01-01

An optical urea biosensor was fabricated by stacking several layers of sol-gel films. The stacking of the sol-gel films allowed the immobilization of a Nile Blue chromoionophore (ETH 5294) and urease enzyme separately without the need of any chemical attachment procedure. The absorbance response of the biosensor was monitored at 550 nm, i.e. the deprotonation of the chromoionophore. This multi-layer sol-gel film format enabled higher enzyme loading in the biosensor to be achieved. The urea op...

Moment scaling at the sol-gel transition

International Nuclear Information System (INIS)

Botet, R.

1998-01-01

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)

Colloidal probe dynamics in gelatin solution during the sol-gel transition.

Science.gov (United States)

Hong, Wei; Xu, Guozhi; Ou, Xiaogang; Sun, Weixiang; Wang, Tao; Tong, Zhen

2018-05-16

The dynamics of the colloidal probes in a gelatin solution during the time-dependent sol-gel transition was investigated by multi-particle tracking. The relationship between the relaxation of the medium at the critical gel point and the mean square displacement of the probes was elucidated. Based on this understanding, the critical gel point of gelatin and the corresponding critical exponent n were unambiguously determined by the loss angle criterion and the time-cure superposition. The shift factors of the latter are further used to estimate the time/length-scale evolution of the gelatin during the sol-gel transition. The growth of the medium length scale crossed with the two measuring length scales successively at the pre-gel regime. Coinciding with the length-scale crossovers, the probability density function (PDF) of the probe displacements displayed two transient peaks of non-Gaussianity. In the post-gel regime, the third peak of Gaussianity suggested inhomogeneity in the gel network. The non-Gaussianity results from the bifurcation of diffusivity. The present work showed that the non-Gaussian dynamics of the probes are not the direct equivalence of that of the medium, but an effect of length-scale coupling.

Nano crystals of Ni doped Zn O semiconductor by Sol-Gel combustion method

Energy Technology Data Exchange (ETDEWEB)

Carrero, A.; Sagredo, V. [Universidad de Los Andes, Departamento de Fisica, Laboratorio de Magnetismo, 5101 Merida (Venezuela, Bolivarian Republic of); Larionova, J., E-mail: aneelyc@gmail.com [Universite Montpellier II, 2 Place Eugene Bataillon, 34090 Montpellier (France)

2016-11-01

Nanoparticles of the system Zn{sub 0.95}O were prepared by sol-gel self - combustion method and a study of their structural, optical and magnetic properties were conducted. X-ray diffraction study shows a hexagonal wurtzite structure for the nano compound. The formation of the wurtzite structure in Ni doped Zn O was further confirmed by Fourier transform infra-red spectrometry. Transmission electron microscopy revealed an average size of 31 nm for the particles. Optical absorption spectra shows that the band energy of Zn{sub 0.95}Ni{sub 0.}9{sub 5}O powders is about 2.54 eV at room temperature. A study of the magnetic properties of the nano powders of Zn O: Ni, reveals paramagnetic behavior, with interaction ferromagnetic between particles. (Author)

Sol-gel processes and materials. January 1970-August 1988 (Citations from the US Patent data base). Report for January 1970-August 1988

International Nuclear Information System (INIS)

1988-08-01

This bibliography contains citations of selected patents concerning Sol-Gel processes and Sol-Gel derived materials and products. Selected patents include Sol-Gel compositions, ceramic and refractory materials, fabrication of silica glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, Sol-Gel production of microspheres, Sol-Gel thin films and coatings, photographic materials, and dental materials. (Contains 71 citations fully indexed and including a title list.)

Athermal silicon optical add-drop multiplexers based on thermo-optic coefficient tuning of sol-gel material.

Science.gov (United States)

Namnabat, Soha; Kim, Kyung-Jo; Jones, Adam; Himmelhuber, Roland; DeRose, Christopher T; Trotter, Douglas C; Starbuck, Andrew L; Pomerene, Andrew; Lentine, Anthony L; Norwood, Robert A

2017-09-04

Silicon photonics has gained interest for its potential to provide higher efficiency, bandwidth and reduced power consumption compared to electrical interconnects in datacenters and high performance computing environments. However, it is well known that silicon photonic devices suffer from temperature fluctuations due to silicon's high thermo-optic coefficient and therefore, temperature control in many applications is required. Here we present an athermal optical add-drop multiplexer fabricated from ring resonators. We used a sol-gel inorganic-organic hybrid material as an alternative to previously used materials such as polymers and titanium dioxide. In this work we studied the thermal curing parameters of the sol-gel and their effect on thermal wavelength shift of the rings. With this method, we were able to demonstrate a thermal shift down to -6.8 pm/°C for transverse electric (TE) polarization in ring resonators with waveguide widths of 325 nm when the sol-gel was cured at 130°C for 10.5 hours. We also achieved thermal shifts below 1 pm/°C for transverse magnetic (TM) polarization in the C band under different curing conditions. Curing time compared to curing temperature shows to be the most important factor to control sol-gel's thermo-optic value in order to obtain an athermal device in a wide temperature range.

Sol-gel synthesis of magnesium oxide-silicon dioxide glass compositions

Science.gov (United States)

Bansal, Narottam P.

1988-01-01

MgO-SiO2 glasses containing up to 15 mol pct MgO, which could not have been prepared by the conventional glass melting method due to the presence of stable liquid-liquid immiscibility, were synthesized by the sol-gel technique. Clear and transparent gels were obtained from the hydrolysis and polycondensation of silicon tetraethoxide (TEOS) and magnesium nitrate hexahydrate when the water/TEOS mole ratio was four or more. The gelling time decreased with increase in magnesium content, water/TEOS ratio, and reaction temperature. Magnesium nitrate hexahydrate crystallized out of the gels containing 15 and 20 mol pct MgO on slow drying. This problem was partially alleviated by drying the gels quickly at higher temperatures. Monolithic gel samples were prepared using glycerol as the drying control additive. The gels were subjected to various thermal treatments and characterized by several methods. No organic groups could be detected in the glasses after heat treatments to approx. 800 C, but trace amounts of hydroxyl groups were still present. No crystalline phase was found from X-ray diffraction in the gel samples to approx. 890 C. At higher temperatures, alpha quartz precipitated out as the crystalline phase in gels containing up to 10 mol pct MgO. The overall activation energy for gel formation in 10MgO-90SiO2 (mol pct) system for water/TEOS mole ratio of 7.5 was calculated to be 58.7 kJ/mol.

Encapsulation of biological species in sol-gel matrices

International Nuclear Information System (INIS)

Finnie, K.S.; Bartlett, J.R.; Woolfrey, J.L.

2000-01-01

Two examples are given of the gelation of silica sols containing bio catalysts, resulting in their encapsulation in porous matrices. Urease was encapsulated in gels made from a mixture of TMOS and alkyltrimethoxysilane. Enzyme activities, monitored by measuring the rate of production of ammoniacal nitrogen as urea was decomposed, ranged up to 60% of that of the unencapsulated species. Anaerobic sulphate-reducing bacteria were encapsulated in a gel produced from colloidal silica, thus avoiding contact with alcohol. The detection of H 2 S produced in the doped gel indicated that the bacteria were able to continue normal metabolic function within the gel matrix. A gel initially doped with ∼ 5 x 10 5 cells cm -3 , exhibited an optimum sulphate reduction rate of 11 ug h -1 cm -3 ; this reduction rate was quickly re-established after storage of the gel for 14 weeks. Copyright (2000) The Australian Ceramic Society

Properties of Zn O/Cr thin films prepared by Sol-Gel

International Nuclear Information System (INIS)

Tirado G, S.; Olvera A, R.

2014-08-01

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)

Preparation of Aligned ZnO Nanorod Arrays on Sn-Doped ZnO Thin Films by Sonicated Sol-Gel Immersion Fabricated for Dye-Sensitized Solar Cell

Directory of Open Access Journals (Sweden)

I. Saurdi

2014-01-01

Full Text Available Aligned ZnO Nanorod arrays are deposited on the Sn-doped ZnO thin film via sonicated sol-gel immersion method. The structural, optical, and electrical properties of the Sn-doped ZnO thin films were investigated. Results show that the Sn-doped ZnO thin films with small grain size (~20 nm, high average transmittance (96% in visible region, and good resistivity 7.7 × 102 Ω·cm are obtained for 2 at.% Sn doping concentration. The aligned ZnO nanorod arrays with large surface area were also obtained for 2 at.% Sn-doped ZnO thin film. They were grown on sol-gel derived Sn-doped ZnO thin film, which acts as a seed layer, via sonicated sol-gel immersion method. The grown aligned ZnO nanorod arrays show high transmittance at visible region. The fabricated dye-sensitised solar cell based on the 2.0 at.% Sn-doped ZnO thin film with aligned ZnO nanorod arrays exhibits improved current density, open-circuit voltage, fill factor, and conversion efficiency compared with the undoped ZnO and 1 at.% Sn-doped ZnO thin films.

Sol-gel optical thin films for an advanced megajoule-class Nd:glass laser ICF-driver

International Nuclear Information System (INIS)

Floch, H.G.; Belleville, P.F.; Pegon, P.M.; Dijonneau, C.S.; Guerain, J.

1995-01-01

It is well established by manufacturers and users that optical coatings are generally prepared by the well known Physical Vapor Deposition (PVD) technology. In the authors' opinion sol-gel technology is an effective and competitive alternative. The aim of this paper is to emphasize on the sol-gel thin film work carried out at Centre d'Etudes de Limeil-Valenton (CEL-V) and concerning the technology for high power lasers. The authors will briefly discuss the chemistry of the sol-gel process, the production of optical coatings and the related deposition techniques. Finally, the paper describes the preparation and performance of sol-gel optical coatings they have developed to fulfill the requirements of a future 2 MJ/500 TW (351 nm) pulsed Nd:glass laser so-called LMJ (Laser MegaJoules). This powerful laser is to be used for their national Inertial Confinement Fusion (ICF) program, to demonstrate at the laboratory scale, ignition of deuterium-tritium fusion fuel. Moreover, the aim of this article is, hopefully, to provide a convincing argument that coatings and particularly optical coatings, are some of the useful products available from sol-gel technology, and that exciting developments in other areas are almost certain to emerge within the coming decade

Ring-Resonator/Sol-Gel Interferometric Immunosensor

Science.gov (United States)

Bearman, Gregory; Cohen, David

2007-01-01

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.

Zr alkoxide chain effect on the sol-gel synthesis of lithium metazirconate

International Nuclear Information System (INIS)

Pfeiffer, Heriberto; Bosch, Pedro; Bulbulian, Silvia

2003-01-01

Lithium metazirconate (Li 2 ZrO 3 ) was synthesized by the sol-gel method, using four different Zr alkoxides: zirconium ethoxide, zirconium iso-propoxide, zirconium propoxide and zirconium butoxide. The syntheses were made under two different catalytic regimes, acid and basic. The resulting powders were mixtures of Li 2 ZrO 3 and ZrO 2 . The best yield of Li 2 ZrO 3 (100%) was obtained when the sol-gel reaction was developed with lithium methoxide and zirconium ethoxide under acid catalysis regime. This study establishes that, for base-catalyzed reactions the ZrO 2 formation decreases when the alkyl-chain increases in the alkoxides. By contrast, for acid-catalyzed reactions the ZrO 2 formation increases as the alkyl-chain increases. Finally, when Zr propoxide and Zr iso-propoxide were used, the Li 2 ZrO 3 amounts were different due to steric effects

Nano sized La2Co2O6 double perovskite synthesized by sol gel method

Science.gov (United States)

Solanki, Neha; Lodhi, Pavitra Devi; Choudhary, K. K.; Kaurav, Netram

2018-05-01

We report here the synthesis of double perovskite La2Co2O6 (LCO) compound by a sol gel route method. The double perovskite structure of LCO system was confirmed via X-ray diffraction (XRD) analysis. Further, the lattice parameter, unit cell volume and bond length were refined by means of rietveld analysis using the full proof software. Debye Scherer formula was used to determine the particle size. The compound crystallized in triclinic structure with space group P-1 in ambient condition. We also obtained Raman modes from XRD spectra of poly-crystalline LCO sample. These results were interpreted for the observation of phonon excitations in this compound.

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

NARCIS (Netherlands)

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

2013-01-01

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

Sol-to-Gel Transition in Fast Evaporating Systems Observed by in Situ Time-Resolved Infrared Spectroscopy.

Science.gov (United States)

Innocenzi, Plinio; Malfatti, Luca; Carboni, Davide; Takahashi, Masahide

2015-06-22

The in situ observation of a sol-to-gel transition in fast evaporating systems is a challenging task and the lack of a suitable experimental design, which includes the chemistry and the analytical method, has limited the observations. We synthesise an acidic sol, employing only tetraethylorthosilicate, SiCl4 as catalyst and deuterated water; the absence of water added to the sol allows us to follow the absorption from the external environment and the evaporation of deuterated water. The time-resolved data, obtained by attenuated total reflection infrared spectroscopy on an evaporating droplet, enables us to identify four different stages during evaporation. They are linked to specific hydrolysis and condensation rates that affect the uptake of water from external environment. The second stage is characterized by a decrease in hydroxyl content, a fast rise of condensation rate and an almost stationary absorption of water. This stage has been associated with the sol-to-gel transition. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of preparation methods of microwave, sol-gel, and hydrothermal on structural and optical properties of lanthania nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Goharshadi, Elaheh K.; Mahvelati, Tahereh; Yazdanbakhsh, Mohammad [Ferdowsi Univ., Mashhad (Iran, Islamic Republic of). Dept. of Chemistry

2016-01-15

In this work, the nearly pure hexagonal phase of lanthania nanoparticles (NPs) was successfully synthesized using three methods: microwave, sol-gel, and hydrothermal. The samples were characterized using nine techniques including powder X-ray powder diffraction, thermogravimetry, transmission electron microscopy, scanning electron microscopy, field emission microscopy, energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, far infrared spectroscopy, and ultraviolet-visible absorption spectroscopy. This study showed that the method of synthesizing lanthania NPs can affect the size, which in turn has impact on structural, morphological, and optical properties.

Thickness controlled sol-gel silica films for plasmonic bio-sensing devices

Energy Technology Data Exchange (ETDEWEB)

Figus, Cristiana, E-mail: cristiana.figus@dsf.unica.it; Quochi, Francesco, E-mail: cristiana.figus@dsf.unica.it; Artizzu, Flavia, E-mail: cristiana.figus@dsf.unica.it; Saba, Michele, E-mail: cristiana.figus@dsf.unica.it; Marongiu, Daniela, E-mail: cristiana.figus@dsf.unica.it; Mura, Andrea; Bongiovanni, Giovanni [Dipartimento di Fisica - University of Cagliari, S.P. Km 0.7, I-09042 Monserrato (Canada) (Italy); Floris, Francesco; Marabelli, Franco; Patrini, Maddalena; Fornasari, Lucia [Dipartimento di Fisica - University of Pavia, Via Agostino Bassi 6, I-27100 Pavia (PV) (Italy); Pellacani, Paola; Valsesia, Andrea [Plasmore S.r.l. -Via Grazia Deledda 4, I-21020 Ranco (Vatican City State, Holy See) (Italy)

2014-10-21

Plasmonics has recently received considerable interest due to its potentiality in many fields as well as in nanobio-technology applications. In this regard, various strategies are required for modifying the surfaces of plasmonic nanostructures and to control their optical properties in view of interesting application such as bio-sensing, We report a simple method for depositing silica layers of controlled thickness on planar plasmonic structures. Tetraethoxysilane (TEOS) was used as silica precursor. The control of the silica layer thickness was obtained by optimizing the sol-gel method and dip-coating technique, in particular by properly tuning different parameters such as pH, solvent concentration, and withdrawal speed. The resulting films were characterized via atomic force microscopy (AFM), Fourier-transform (FT) spectroscopy, and spectroscopic ellipsometry (SE). Furthermore, by performing the analysis of surface plasmon resonances before and after the coating of the nanostructures, it was observed that the position of the resonance structures could be properly shifted by finely controlling the silica layer thickness. The effect of silica coating was assessed also in view of sensing applications, due to important advantages, such as surface protection of the plasmonic structure.

Luminescence properties of europium (III) cryptates trapped in sol-gel glass

International Nuclear Information System (INIS)

Zaitoun, M.A.; Kim, T.; Jaradat, Q.M.; Momani, K.; Qaseer, H.A.; El-Qisairi, A.K.; Qudah, A.; Radwan, N.E.

2008-01-01

The Lanthanide complexes Eu-2.2.1 and Eu-2.2.2 were synthesized and then incorporated into silica based transparent organic-inorganic hybrid material by the sol-gel method as an example of how doped xerogel materials are emerging as an important means of producing new materials. The produced gels were diagnosed to monitor emission spectra of the luminescent trivalent europium (Eu 3+ ) complexes; emissions were compared to those for gels containing uncomplexed Eu 3+ . Results of the experiments (emission and lifetimes) concerning the coordination sphere composition showed that a cryptand ligand with aromatic groups (short range effect) and the hydrophobic gel host (long range effect) settle efficient action in the antenna effect and isolate the central ion from efficient quenchers, as e.g. water molecules. Each ligand imposed a distinct splitting pattern on the europium emission bands that helps identify them

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

Science.gov (United States)

1982-01-01

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.

A copper ion-selective electrode with high selectivity prepared by sol-gel and coated wire techniques.

Science.gov (United States)

Mazloum Ardakani, M; Salavati-Niasari, M; Khayat Kashani, M; Ghoreishi, S M

2004-03-01

A sol-gel electrode and a coated wire ion-selective poly(vinyl chloride) membrane, based on thiosemicarbazone as a neutral carrier, were successfully developed for the detection of Cu (II) in aqueous solutions. The sol-gel electrode and coated electrode exhibited linear response with Nernstian slopes of 29.2 and 28.1 mV per decade respectively, within the copper ion concentration ranges 1.0 x 10(-5) - 1.0 x 10(-1) M and 6.0 x 10(-6) - 1.0 x 10(-1) M for coated and sol-gel sensors. The coated and sol-gel electrodes show detection limits of 3.0 x 10(-6) and 6.0 x 10(-6) M respectively. The electrodes exhibited good selectivities for a number of alkali, alkaline earth, transition and heavy metal ions. The proposed electrodes have response times ranging from 10-50 s to achieve a 95% steady potential for Cu2+ concentration. The electrodes are suitable for use in aqueous solutions over a wide pH range (4-7.5). Applications of these electrodes for the determination of copper in real samples, and as an indicator electrode for potentiometric titration of Cu2+ ion using EDTA, are reported. The lifetimes of the electrodes were tested over a period of six months to investigate their stability. No significant change in the performance of the sol-gel electrode was observed over this period, but after two months the coated wire copper-selective electrode exhibited a gradual decrease in the slope. The selectivity of the sol-gel electrode was found to be better than that of the coated wire copper-selective electrode. Based on these results, a novel sol-gel copper-selective electrode is proposed for the determination of copper, and applied to real sample assays.

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

KAUST Repository

Ramos-Gonzá lez, R.; Garcí a-Cerda, L. A.; Alshareef, Husam N.; Gnade, Bruce E.; Quevedo-Ló pez, Manuel Angel Quevedo

2010-01-01

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

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

KAUST Repository

Ramos-González, R.

2010-03-01

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

Ternary Phase-Separation Investigation of Sol-Gel Derived Silica from Ethyl Silicate 40

Science.gov (United States)

Wang, Shengnan; Wang, David K.; Smart, Simon; Diniz da Costa, João C.

2015-01-01

A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification. PMID:26411484

Fabrication of superhydrophobic and antibacterial surface on cotton fabric by doped silica -based sols with nanoparticles of copper

Science.gov (United States)

Berendjchi, Amirhosein; Khajavi, Ramin; Yazdanshenas, Mohammad Esmaeil

2011-11-01

The study discussed the synthesis of silica sol using the sol-gel method, doped with two different amounts of Cu nanoparticles. Cotton fabric samples were impregnated by the prepared sols and then dried and cured. To block hydroxyl groups, some samples were also treated with hexadecyltrimethoxysilane. The average particle size of colloidal silica nanoparticles were measured by the particle size analyzer. The morphology, roughness, and hydrophobic properties of the surface fabricated on cotton samples were analyzed and compared via the scanning electron microscopy, the transmission electron microscopy, the scanning probe microscopy, with static water contact angle (SWC), and water shedding angle measurements. Furthermore, the antibacterial efficiency of samples was quantitatively evaluated using AATCC 100 method. The addition of 0.5% (wt/wt) Cu into silica sol caused the silica nanoparticles to agglomerate in more grape-like clusters on cotton fabrics. Such fabricated surface revealed the highest value of SWC (155° for a 10-μl droplet) due to air trapping capability of its inclined structure. However, the presence of higher amounts of Cu nanoparticles (2% wt/wt) in silica sol resulted in the most slippery smooth surface on cotton fabrics. All fabricated surfaces containing Cu nanoparticles showed the perfect antibacterial activity against both of gram-negative and gram-positive bacteria.

Effect of templates on inverse opals fabricated through annular self-assembly/sol-gel method

International Nuclear Information System (INIS)

Ge Dengteng; Yang Lili; Fan Zeng; Zhao Jiupeng; Li Yao

2011-01-01

Highlights: → Flexible inverse opals could be facilely prepared through annular growth method. → The infiltrated materials are highly densified due to the existence of templates. → The crystalline grains are refined due to the the existence of templates. - Abstract: There is a strong interest in simple preparation of flexible inverse opals for applications. In this article, indium tin oxides (ITO) flexible inverse opals were prepared through annular growth of templates and sol-gel process. It is shown that this method provides a facile route for large scale flexible inverse opals with excellent ordered structures. ITO materials are found much denser in inverse opals, which is due to the increased capillary force during drying process and enhanced shrinkage during annealing process. It is also found that the crystalline grains are refined and the photoluminescence performance is strengthened in low frequency.

Bioorganically doped sol-gel materials containing amyloglucosidase activity

Directory of Open Access Journals (Sweden)

Vlad-Oros Beatrice

2006-01-01

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.

Synthesis of ZrO2-TiO2 mixed oxide spheres by sol-gel method and investigation of Sr adsorption behaviours by experimental design approach

International Nuclear Information System (INIS)

Cetinkaya, B.; Tel, H.; Altas, Y.; Eral, M.; Sert, S.; Inan, S.; Talip, Z.

2009-01-01

ZrO 2 -TiO 2 gel spheres were synthesized by sol-gel method. Zr-Ti sol solution was prepared from ZrCl 4 and TiCl 4 (1:1 mol ratio) via partial neutralization by ammonia to obtain 0.5M final metal concentration. ZrO 2 -TiO 2 sol was transferred to vibrating nozzle system by peristaltic pump. Vibrating nozzle system was designed and produced in Institute of Nuclear Sciences. Sol drops formed by nozzle were gelled in gelation column. Synthesized ZrO 2 -TiO 2 spheres were aged for 24h then washed with deionized water and dried in oven. Sr + 2 adsorption behaviors of ZrO 2 -TiO 2 mixed oxides were investigated with central composite design (CCD). Four independent parameters (pH, initial Sr + 2 concentration, temperature and contact time) were investigated with 7 replicates at central points. Sorption data have been interpreted in terms of Langmuir, Freundlich and Dubinin Radushkevich equations. Thermodynamic parameters for the sorption system have been determined.

{sup 90}Y microspheres prepared by sol-gel method, promising medical material for radioembolization of liver malignancies

Energy Technology Data Exchange (ETDEWEB)

Łada, Wiesława, E-mail: w.lada@ichtj.waw.pl [Institute of Nuclear Chemistry and Technology, 03-195 Warsaw, Dorodna 16 (Poland); Iller, Edward [National Centre for Nuclear Research, Radioisotope Centre POLATOM, 05-400 Otwock, Andrzej Sołtan 7 (Poland); Wawszczak, Danuta [Institute of Nuclear Chemistry and Technology, 03-195 Warsaw, Dorodna 16 (Poland); Konior, Marcin, E-mail: marcin.konior@polatom.pl [National Centre for Nuclear Research, Radioisotope Centre POLATOM, 05-400 Otwock, Andrzej Sołtan 7 (Poland); Dziel, Tomasz [National Centre for Nuclear Research, Radioisotope Centre POLATOM, 05-400 Otwock, Andrzej Sołtan 7 (Poland)

2016-10-01

A new technology for the production of radiopharmaceutical {sup 90}Y microspheres in the form of spherical yttrium oxide grains obtained by sol-gel method has been described. The authors present and discuss the results of investigations performed in the development of new production technology of yttrium microspheres and determination of their physic-chemical properties. The final product has the structure of spherical yttrium oxide grains with a diameter 25–100 μm, is stable and free from contaminants. Irradiation of 20 mg samples of grains with diameter of 20–50 μm in the thermal neutron flux of 1.7 × 10{sup 14} cm{sup −2} s{sup −1} at the core of MARIA research nuclear reactor allowed to obtain microspheres labelled with the {sup 90}Y isotope on the way of the nuclear reaction {sup 89}Y(n, γ){sup 90}Y. Specific activity of irradiated microspheres has been determined by application of absolute triple to double coincidence ratio method (TDCR) and has been evaluated at 190 MBq/mg Y. {sup 90}Y microspheres prepared by the proposed technique can be regarded as a promising medical material for radioembolization of liver malignancies. - Highlights: • Sol-gel methods for preparation of spherical yttrium trioxide grains have been proposed. • Determination condition for irradiation {sup 89}Y{sub 2}O{sub 3} grains in nuclear reactor • Evaluation of specific activity of {sup 90}Y microspheres • Estimation of {sup 90}Y microspheres as promising medical material for radioembolization.