modified sol-gel method: Topics by Science.gov

Sample records for modified sol-gel method

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

EPA Science Inventory

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...
Multicomponent micropatterned sol-gel materials by capillary molding

NASA Astrophysics Data System (ADS)

Lochhead, Michael J.; Yager, Paul

1997-10-01

A physically and chemically benign method for patterning multiple sol-gel materials onto a single substrate is described. Structures are demonstrated for potential micro- optical chemical sensor, biosensor, and waveguiding applications. Fabrication is based on the micro molding in capillaries (MIMIC) approach. A novel mold design allows several sols to be cast simultaneously. Closely spaced, organically modified silica ridges containing fluorescent dyes are demonstrated. Ridges have cross sectional dimensions from one to 50 micrometers and are centimeters in length. Processing issues, particularly those related to mold filling, are discussed in detail. Because sol-gel MIMIC avoids the harsh physical and chemical environments normally associated with patterning, the approach allows full exploitation of sol- gel processing advantages, such as the ability to entrap sensitive organic dopant molecules in the sol-gel matrix.
A Sol-Gel-Modified Poly(methyl methacrylate) Electrophoresis Microchip with a Hydrophilic Channel Wall

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Gang; Xu, Xuejiao; Lin, Yuehe

2007-07-27

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 27.4° compared with 66.3° for the pure PMMA. In addition, the electro-osmoticmore » flow increased from 2.13×10-4 cm2 V-1 s-1 for the native-PMMA channel to 4.86×10-4 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.« less
Surface modification of quartz fibres for dental composites through a sol-gel process.

PubMed

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

2017-05-01

In this study, quartz fibres (QFs) surface modification using a sol-gel method was proposed and dental posts reinforced with modified QFs were produced. A silica sol (SS) was prepared using tetraethoxysilane (TEOS) and 3-methacryloxypropyltrimethoxysilane (γ-MPS) as precursors. The amount of γ-MPS in the sol-gel system was varied from 0 to 24wt.% with a constant molar ratio of TEOS, ethanol, deionized water, and HCl. Thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), and contact angle (CA) measurements were used to characterize the modified QFs, which confirmed that SS had successfully coated the surface of QFs. SEM images showed good interfacial bonding between the modified QFs and the resin matrix. The results of three-point bending tests of the fibre reinforced composite (FRC) posts showed that the QFs modified by SS with 12wt.% γ-MPS presented the best mechanical properties, demonstrating improvements of 108.3% and 89.6% for the flexural strength and flexural modulus, respectively, compared with untreated QFs. Furthermore, the sorption and solubility of the prepared dental posts were also studied by immersing the posts in artificial saliva (AS) for 4weeks, and yielded favourable results. This sol-gel surface modification method promises to resolve interfacial bonding issues of fibres with the resin matrix, and produce FRC posts with excellent properties. Copyright © 2017. Published by Elsevier B.V.
Modified silica sol coatings for surface enhancement of leather.

PubMed

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.
Metal-oxide-based energetic materials and synthesis thereof

DOEpatents

Tillotson, Thomas M. , Simpson; Randall, L [Livermore, CA; Hrubesh, Lawrence W [Pleasanton, CA

2006-01-17

A method of preparing energetic metal-oxide-based energetic materials using sol-gel chemistry has been invented. The wet chemical sol-gel processing provides an improvement in both safety and performance. Essentially, a metal-oxide oxidizer skeletal structure is prepared from hydrolyzable metals (metal salts or metal alkoxides) with fuel added to the sol prior to gelation or synthesized within the porosity metal-oxide gel matrix. With metal salt precursors a proton scavenger is used to destabilize the sol and induce gelation. With metal alkoxide precursors standard well-known sol-gel hydrolysis and condensation reactions are used. Drying is done by standard sol-gel practices, either by a slow evaporation of the liquid residing within the pores to produce a high density solid nanocomposite, or by supercritical extraction to produce a lower density, high porous nanocomposite. Other ingredients may be added to this basic nanostructure to change physical and chemical properties, which include organic constituents for binders or gas generators during reactions, burn rate modifiers, or spectral emitters.
Solid-phase microfibers based on polyethylene glycol modified single-walled carbon nanotubes for the determination of chlorinated organic carriers in textiles.

PubMed

Zhang, Wei-Ya; Sun, Yin; Wang, Cheng-Ming; Wu, Cai-Ying

2011-09-01

Based on polyethylene glycol modified single-walled carbon nanotubes, a novel sol-gel fiber coating was prepared and applied to the headspace microextraction of chlorinated organic carriers (COCs) in textiles by gas chromatography-electron capture detection. The preparation of polyethylene glycol modified single-walled carbon nanotubes and the sol-gel fiber coating process was stated and confirmed by infrared spectra, Raman spectroscopy, and scanning electron microscopy. Several parameters affecting headspace microextraction, including extraction temperature, extraction time, salting-out effect, and desorption time, were optimized by detecting 11 COCs in simulative sweat samples. Compared with the commercial solid-phase microextraction fibers, the sol-gel polyethylene glycol modified single-walled carbon nanotubes fiber showed higher extraction efficiency, better thermal stability, and longer life span. The method detection limits for COCs were in the range from 0.02 to 7.5 ng L(-1) (S/N = 3). The linearity of the developed method varied from 0.001 to 50 μg L(-1) for all analytes, with coefficients of correlation greater than 0.974. The developed method was successfully applied to the analysis of trace COCs in textiles, the recoveries of the analytes indicated that the developed method was considerably useful for the determination of COCs in ecological textile samples.
Highly porous solid-phase microextraction fiber coating based on poly(ethylene glycol)-modified ormosils synthesized by sol-gel technology.

PubMed

da Costa Silva, Raquel Gomes; Augusto, Fabio

2005-04-22

The preparation and characteristics of solid-phase microextraction (SPME) fibers coated with Carbowax 20M ormosil (organically modified silica) are described here. Raw fused silica fibers were coated with Carbowax 20M-modified silica using sol-gel process. Scanning electron micrographs of fibers revealed a highly porous, sponge-like coating with an average thickness of (8 +/- 1) microm. The sol-gel Carbowax fibers were compared to commercial fibers coated with 100 microm polydimethylsiloxane (PDMS) and 65 microm Carbowax-divinylbenzene (DVB). Shorter equilibrium times were possible with the sol-gel Carbowax fiber: for headspace extraction of the test analytes, they ranged from less than 3 min for benzene to 15 min for o-xylene. Extraction efficiencies of the sol-gel Carbowax fiber were superior to those of conventional fibers: for o-xylene, the extracted masses were 230 and 540% of that obtained with 100 microm PDMS and 65 microm Carbowax-DVB fibers, respectively.
Sol-gel open tubular ODS columns with reversed electroosmotic flow for capillary electrochromatography.

PubMed

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

PubMed

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

PubMed

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%.
Epidemic models for phase transitions: application to a physical gel

NASA Astrophysics Data System (ADS)

Bilge, A. H.; Pekcan, O.; Kara, S.; Ogrenci, A. S.

2017-09-01

Carrageenan gels are characterized by reversible sol-gel and gel-sol transitions under cooling and heating processes and these transitions are approximated by generalized logistic growth curves. We express the transitions of carrageenan-water system, as a representative of reversible physical gels, in terms of a modified Susceptible-Infected-Susceptible epidemic model, as opposed to the Susceptible-Infected-Removed model used to represent the (irreversible) chemical gel formation in the previous work. We locate the gel point Tc of sol-gel and gel-sol transitions and we find that, for the sol-gel transition (cooling), Tc > Tsg (transition temperature), i.e. Tc is earlier in time for all carrageenan contents and moves forward in time and gets closer to Tsg as the carrageenan content increases. For the gel-sol transition (heating), Tc is relatively closer to Tgs; it is greater than Tgs, i.e. later in time for low carrageenan contents and moves backward as carrageenan content increases.
Raman study of TiO2 coatings modified by UV pulsed laser

NASA Astrophysics Data System (ADS)

Belka, Radosław; Keczkowska, Justyna; Sek, Piotr

2016-12-01

The TiO2 coatings were prepared by simple sol-gel method and modified by UV pulsed laser. TiO2, also know as titania, is a ceramic compound, existing in numerous polymorphic forms, mainly as tetragonal rutile and anatase, and rhomboidal brookite. Rutile is the most stable form of titanium dioxide, whereas anatase is a metastable form, created in lower temperatures than rutile. Anatase is marked with higher specific surface area, porosity and a higher number of surface hydroxyl groups as compared to rutile. The unique optical and electronic properties of TiO2 results in its use as semiconductors dielectric mirrors, sunscreen and UV-blocking pigments and especially as photocatalyst. In this paper, the tetraisopropoxide was used as Ti precursor according to sol-gel method. An organic base was applied during sol preparation. Prepared gel was coated on glass substrates and calcined in low temperature to obtain amorphous phase of titania. Prepared coatings were modified by UV picosecond pulse laser with different pulse repetition rate and pulse power. Physical modification of the coatings using laser pulses was intended in order change the phase content of the produced material. Raman spectroscopy (RS) method was applied to studies of modified coatings as it is one of the basic analytical techniques, supporting the identification of compounds and obtaining information about the structure. Especially, RS is a useful method for distinguishing the anatase and rutile phases. In these studies, anatase to rutile transformation was observed, depending on laser parameters.
Low Concentration Fe-Doped Alumina Catalysts Using Sol-Gel and Impregnation Methods: The Synthesis, Characterization and Catalytic Performance during the Combustion of Trichloroethylene

PubMed Central

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

2014-01-01

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%. PMID:28788556
Modified Au nanoparticles-imprinted sol-gel, multiwall carbon nanotubes pencil graphite electrode used as a sensor for ranitidine determination.

PubMed

Rezaei, B; Lotfi-Forushani, H; Ensafi, A A

2014-04-01

A new, simple, and disposable molecularly imprinted electrochemical sensor for the determination of ranitidine was developed on pencil graphite electrode (PGE) via cyclic voltammetry (CV). The PGEs were coated with MWCNTs containing the carboxylic functional group (f-MWCNTs), imprinted with sol-gel and Au nanoparticle (AuNPs) layers (AuNP/MIP-sol-gel/f-MWCNT/PGE), respectively, to enhance the electrode's electrical transmission and sensitivity. The thin film of molecularly imprinted sol-gel polymers with specific binding sites for ranitidine was cast on modified PGE by electrochemical deposition. The AuNP/MIP-sol-gel/f-MWCNT/PGE thus developed was characterized by electrochemical impedance spectroscopy (EIS) and CV. The interaction between the imprinted sensor and the target molecule was also observed on the electrode by measuring the current response of 5.0mMK3[Fe(CN)6] solution as an electrochemical probe. The pick currents of ranitidine increased linearly with concentration in the ranges of 0.05 to 2.0μM, with a detection limit of (S/N=3) 0.02μM. Finally, the modified electrode was successfully employed to determine ranitidine in human urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.
Sol-gel Derived Warfarin - Silica Composites for Controlled Drug Release.

PubMed

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.
Quantitative determination of Escherichia coli based on the electrochemical measurement of bacterial catalase activity using H2O2-selective organic/inorganic-hybrid sol-gel film-modified Pt electrode.

PubMed

Hasebe, Yasushi; Fukuzawa, Michiru; Matsuhisa, Hironori

2009-01-01

Quantitative determination of Escherichia coli (E. coli) concentration was achieved by measuring the intrinsic catalase activity of E. coli using novel H2O2-selective organic/inorganic-hybrid sol-gel film-modified platinum (Pt) wire electrode. This hybrid sol-gel film is composed of three kinds of organosilanes and two biopolymers (i.e., chitosan and bovine serum albumin), and exhibited an excellent permselectivity toward H2O2 based on a size-exclusive mechanism. The steady-state anodic current for 100 [xmol/L H2O2 at +0.6 V (vs. Ag/AgCl) in 0.1 mol/L phosphate buffer (pH 6.5) solution was apparently diminished by the addition of E. coli samples, due to the decomposition of H2O2 by intrinsic catalase activity of E. coli. The time-dependent decrease in current (-AI/At) was significantly dependent on the E. coli concentration. The -AI/At was enhanced by the permeabilization pretreatment of E. coli samples with the mixed solution of polymyxin B and lysozyme. This H2O2-selective organic/inorganic-hybrid sol-gel film-modified platinum (Pt) wire electrode allowed quantitative determination of E. coli concentration ranging from 10(6) to 10(9) CFU/mL within 30 min. This method required no label and complicated procedure, and allowed rapid, simple and cost-effective quantitative electrochemical determination of catalase-positive bacteria.
A new powder production route for transparent spinel windows: powder synthesis and window properties

NASA Astrophysics Data System (ADS)

Cook, Ronald; Kochis, Michael; Reimanis, Ivar; Kleebe, Hans-Joachim

2005-05-01

Spinel powders for the production of transparent polycrystalline ceramic windows have been produced using a number of traditional ceramic and sol-gel methods. We have demonstrated that magnesium aluminate spinel powders produced from the reaction of organo-magnesium compounds with surface modified boehmite precursors can be used to produce high quality transparent spinel parts. The new powder production method allows fine control over the starting particle size, size distribution, purity and stoichiometry. The new process involves formation of a boehmite sol-gel from the hydrolysis of aluminum alkoxides followed by surface modification of the boehmite nanoparticles using carboxylic acids. The resulting surface modified boehmite nanoparticles can then be metal exchanged at room temperature with magnesium acetylacetonate to make a precursor powder that is readily transformed into pure phase spinel.
Method of making ionic liquid mediated sol-gel sorbents

DOEpatents

Malik, Abdul; Shearrow, Anne M.

2017-01-31

Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.
Eu-doped BaTiO₃powder and film from sol-gel process with polyvinylpyrrolidone additive.

PubMed

García-Hernández, Margarita; García-Murillo, Antonieta; de J Carrillo-Romo, Felipe; Jaramillo-Vigueras, David; Chadeyron, Geneviève; De la Rosa, Elder; Boyer, Damien

2009-09-17

Transparent BaTiO(3):Eu(3+) films were prepared via a sol-gel method and dip-coating technique, using barium acetate, titanium butoxide, and polyvinylpyrrolidone (PVP) as modifier viscosity. BaTiO(3):Eu(3+) films ~500 nm thick, crystallized after thermal treatment at 700 masculineC. The powders revealed spherical and rod shape morphology. The optical quality of films showed a predominant band at 615 nm under 250 nm excitation. A preliminary luminescent test provided the properties of the Eu(3+) doped BaTiO(3).

Metal-silica sol-gel materials

NASA Technical Reports Server (NTRS)

Stiegman, Albert E. (Inventor)

2002-01-01

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

DOEpatents

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.
Surface analysis and biocorrosion properties of nanostructured surface sol-gel coatings on Ti6Al4V titanium alloy implants.

PubMed

Advincula, Maria C; Petersen, Don; Rahemtulla, Firoz; Advincula, Rigoberto; Lemons, Jack E

2007-01-01

Surfaces of biocompatible alloys used as implants play a significant role in their osseointegration. Surface sol-gel processing (SSP), a variant of the bulk sol-gel technique, is a relatively new process to prepare bioreactive nanostructured titanium oxide for thin film coatings. The surface topography, roughness, and composition of sol-gel processed Ti6Al4V titanium alloy coatings was investigated by atomic force microscopy (AFM) and X-ray electron spectroscopy (XPS). This was correlated with corrosion properties, adhesive strength, and bioreactivity in simulated body fluids (SBF). Electroimpedance spectroscopy (EIS) and polarization studies indicated similar advantageous corrosion properties between sol-gel coated and uncoated Ti6Al4V, which was attributed to the stable TiO2 composition, topography, and adhesive strength of the sol-gel coating. In addition, inductive coupled plasma (ICP) and scanning electron microscopy with energy dispersive spectrometry (SEM-EDS) analysis of substrates immersed in SBF revealed higher deposition of calcium and phosphate and low release rates of alloying elements from the sol-gel modified alloys. The equivalent corrosion behavior and the definite increase in nucleation of calcium apatite indicate the potential of the sol-gel coating for enhanced bioimplant applications. 2006 Wiley Periodicals, Inc.
Fabrication and Anti-Oxidation Ability of SiC-SiO₂ Coated Carbon Fibers Using Sol-Gel Method.

PubMed

Yang, Guangyuan; Huang, Zhixiong; Wang, Xu; Wang, Bo

2018-02-27

The paper proposed a method to improve the anti-oxidation performance of carbon fibers (CF) at high temperature environment by coating silicon dioxide (SiO₂) and silicon carbide (SiC). The modified sol-gel method had been used to ensure the proper interface between fibers and coating. We used polydimethylsiloxane and ethyl orthosilicate to make stable emulsion to uniformly disperse SiC nanoparticles. The modified SiO₂/SiC coating had been coated on CF successfully. Compared with the untreated CF, the coated fibers started to be oxidized around 900 °C and the residual weight was 57% at 1400 °C. The oxidation mechanism had been discussed. The structure of SiC/SiO₂ coated CF had been characterized by scanning electron microscope and X-ray diffraction analysis. Thermal gravimetric analysis was used to test the anti-oxidation ability of CF with different coatings.
Bioactivity of sol-gel-derived TiO2 coating on polyetheretherketone: In vitro and in vivo studies.

PubMed

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.
Site selective generation of sol-gel deposits in layered bimetallic macroporous electrode architectures.

PubMed

Lalo, Hélène; Bon-Saint-Côme, Yémima; Plano, Bernard; Etienne, Mathieu; Walcarius, Alain; Kuhn, Alexander

2012-02-07

The elaboration of an original composite bimetallic macroporous electrode containing a site-selective sol-gel deposit is reported. Regular colloidal crystals, obtained by a modified Langmuir-Blodgett approach, are used as templates for the electrogeneration of the desired metals in the form of a well-defined layered bimetallic porous electrode. This porous matrix shows a spatially modulated electroactivity which is subsequently used as a strategy for targeted electrogeneration of a sol-gel deposit, exclusively in one predefined part of the porous electrode.
Electrochemical luminescence determination of hyperin using a sol-gel@graphene luminescent composite film modified electrode for solid phase microextraction

NASA Astrophysics Data System (ADS)

Zou, Xiaojun; Shang, Fang; Wang, Sui

2017-02-01

In this paper, a novel electrochemiluminescence (ECL) sensor of sol-gel@graphene luminescent composite film modified electrode for hyperin determination was prepared using graphene (G) as solid-phase microextraction (SPME) material, based on selective preconcentration of target onto an electrode and followed by luminol ECL detection. Hyperin was firstly extracted from aqueous solution through the modified GCE. Hydrogel, electrogenerated chemiluminescence reagents, pH of working solution, extraction time and temperature and scan rate were discussed. Under the optimum conditions, the change of ECL intensity was in proportion to the concentration of hyperin in the range of 0.02-0.24 μg/mL with a detection limit of 0.01 μg/mL. This method showed good performance in stability, reproducibility and precision for the determination of hyperin.
High surface area neodymium phosphate nano particles by modified aqueous sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sankar, Sasidharan; Warrier, Krishna Gopakumar, E-mail: wwarrierkgk@yahoo.co.in; Komban, Rajesh

2011-12-15

Graphical abstract: Synthesis of nano rod shaped neodymium phosphate particles with specific surface area as high as 107 m{sup 2} g{sup -1} and particles could be compacted and sintered at as low as 1300 Degree-Sign C to a density of 98.5% (theoretical) with an average grain size of {approx}1 {mu}m. Highlights: Black-Right-Pointing-Pointer Nano size neodymium phosphate is synthesized and characterized using a novel modified aqueous sol gel process. Black-Right-Pointing-Pointer Specific surface area above 100 m{sup 2} g{sup -1} achieved without the addition of any complexing agents. Black-Right-Pointing-Pointer High sintered density reported than the density obtained for powder synthesized through conventionalmore » solid state reaction. Black-Right-Pointing-Pointer The particles are nano sized and have rod shape morphology and are retained at higher temperatures. Black-Right-Pointing-Pointer An average grain size of {approx}1 {mu}m obtained for sintered NdPO{sub 4} after thermal etching at 1400 Degree-Sign C. -- Abstract: Synthesis of nano rod shaped neodymium phosphate (NdPO{sub 4}) particles with specific surface area as high as 107 m{sup 2}g{sup -1} and an average length of 50 nm with aspect ratio 5 was achieved using modified sol gel method. Crystallite size calculated from the X-ray diffraction data by applying Scherer equation was 5 nm for the precursor gel after calcination at 400 Degree-Sign C. NdPO{sub 4} was first precipitated from neodymium nitrate solution using phosphoric acid followed by peptization using dilute nitric acid and further gelation in ammonia atmosphere. The calcined gel powders were further characterized by surface area (Brunauer-Emmet-Teller nitrogen adsorption analysis), Transmission electron microscopy, scanning electron microscopy, UV-vis and FT-IR analysis. Transmission electron microscopy confirms the formation of rod like morphology from the sol, gel and the calcined particles in nano size range. These particles could be compacted and sintered at as low as 1300 Degree-Sign C to a density of 98.5% (theoretical) with an average grain size of {approx}1 {mu}m.« less
Nanosilica coating for bonding improvements to zirconia.

PubMed

Chen, Chen; Chen, Gang; Xie, Haifeng; Dai, Wenyong; Zhang, Feimin

2013-01-01

Resin bonding to zirconia cannot be established from standard methods that are currently utilized in conventional silica-based dental ceramics. The solution-gelatin (sol-gel) process is a well developed silica-coating technique used to modify the surface of nonsilica-based ceramics. Here, we use this technique to improve resin bonding to zirconia, which we compared to zirconia surfaces treated with alumina sandblasting and tribochemical silica coating. We used the shear bond strength test to examine the effect of the various coatings on the short-term resin bonding of zirconia. Furthermore, we employed field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, and Fourier transform infrared spectroscopy to characterize the zirconia surfaces. Water-mist spraying was used to evaluate the durability of the coatings. To evaluate the biological safety of the experimental sol-gel silica coating, we conducted an in vitro Salmonella typhimurium reverse mutation assay (Ames mutagenicity test), cytotoxicity tests, and in vivo oral mucous membrane irritation tests. When compared to the conventional tribochemical silica coating, the experimental sol-gel silica coating provided the same shear bond strength, higher silicon contents, and better durability. Moreover, we observed no apparent mutagenicity, cytotoxicity, or irritation in this study. Therefore, the sol-gel technique represents a promising method for producing silica coatings on zirconia.
The influence of precursor addition order on the porosity of sol-gel bioactive glasses.

PubMed

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.
Eu-Doped BaTiO3 Powder and Film from Sol-Gel Process with Polyvinylpyrrolidone Additive

PubMed Central

García-Hernández, Margarita; García-Murillo, Antonieta; de J. Carrillo-Romo, Felipe; Jaramillo-Vigueras, David; Chadeyron, Geneviève; De la Rosa, Elder; Boyer, Damien

2009-01-01

Transparent BaTiO3:Eu3+ films were prepared via a sol-gel method and dip-coating technique, using barium acetate, titanium butoxide, and polyvinylpyrrolidone (PVP) as modifier viscosity. BaTiO3:Eu3+ films ~500 nm thick, crystallized after thermal treatment at 700 ºC. The powders revealed spherical and rod shape morphology. The optical quality of films showed a predominant band at 615 nm under 250 nm excitation. A preliminary luminescent test provided the properties of the Eu3+ doped BaTiO3. PMID:19865533
Thermal stability and degradation kinetics of kenaf/sol-gel silica hybrid

NASA Astrophysics Data System (ADS)

Yusof, F. A. M.; Hashim, A. S.; Tajudin, Z.

2017-12-01

Thermal stability and degradation kinetics of kenaf/sol-gel silica hybrid materials was investigated by thermogravimetric analysis (TGA). Model-free iso-conversion Flynn-Wall-Ozawa (FWO) and Coats-Redfern-modified (CRm) were chosen to evaluate the activation energy of the kenaf (KF) and kenaf/sol-gel silica (KFS) at heating rates (β) of 10, 20, 30 and 40 °C/min. The results shows that an apparent activation energy was increased for the kenaf/sol-gel silica hybrid (211.59 kJ/mol for FWO and 191.55 kJ/mol for CRm) as compared to kenaf fiber (202.84 kJ/mol for FWO and 186.20 kJ/mol for CRm). Other parameters such as integral procedure decomposition temperature (IPDT), final residual weight (Rf), temperature of maximum degradation rate (Tmax) and residual at maximum temperature (RTmax) were obtained from TGA curves, additionally confirmed the thermal stability of the kenaf/sol-gel silica hybrid. These activation energy values and other findings developed the simplified approach in order to understand the thermal stability and degradation kinetics behavior of kenaf/sol-gel silica hybrid materials.
Sol-gel method to fabricate CaP scaffolds by robocasting for tissue engineering.

PubMed

Houmard, Manuel; Fu, Qiang; Saiz, Eduardo; Tomsia, Antoni P

2012-04-01

Highly porous calcium phosphate (CaP) scaffolds for bone-tissue engineering were fabricated by combining a robocasting process with a sol-gel synthesis that mixed Calcium Nitrate Tetrahydrate and Triethyl Phosphite precursors in an aqueous medium. The resulting gels were used to print scaffolds by robocasting without the use of binder to increase the viscosity of the paste. X-ray diffraction analysis confirmed that the process yielded hydroxyapatite and β-tricalcium phosphate biphasic composite powders. Thus, the scaffold composition after crystallization of the amorphous structure could be easily modified by varying the initial Ca/P ratio during synthesis. The compressive strengths of the scaffolds are ~6 MPa, which is in the range of human cancellous bone (2-12 MPa). These highly porous scaffolds (~73 vol% porosity) are composed of macro-pores of ~260 μm in size; such porosity is expected to enable bone ingrowth into the scaffold for bone repair applications. The chemistry, porosity, and surface topography of such scaffolds can also be modified by the process parameters to favor bone formation. The studied sol-gel process can be used to coat these scaffolds by dip-coating, which induces a significant enhancement of mechanical properties. This can adjust scaffold properties such as composition and surface morphology, which consequently may improve their performances.
Biological influence of Ca/P ratio on calcium phosphate coatings by sol-gel processing.

PubMed

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.
Three-phase molecularly imprinted sol-gel based hollow fiber liquid-phase microextraction combined with liquid chromatography-tandem mass spectrometry for enrichment and selective determination of a tentative lung cancer biomarker.

PubMed

Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-Adergani, Behrouz; Abdel-Rehim, Mohamed

2015-07-15

In the present study, the modification of a polysulfone hollow fiber membrane with in situ molecularly imprinted sol-gel process (as a novel and one-step method) was prepared and investigated. 3-(propylmethacrylate)trimethoxysilane (3PMTMOS) as an inorganic precursor was used for preparation of molecularly imprinted sol-gel. The modified molecularly imprinted sol-gel hollow fiber membrane (MSHM) was used for the liquid-phase microextraction (LPME) of hippuric acid (HA) in human plasma and urine samples. MSHM as a selective, robust, and durable tool was used for at least 50 extractions without significant decrease in the extraction efficiency. The non-molecularly imprinted sol-gel hollow fiber membrane (NSHM) as blank hollow fiber membrane was prepared by the same process, only without HA. To achieve the best condition, influential parameters on the extraction efficiency were thoroughly investigated. The capability of this robust, green, and simple method for extraction of HA was successfully accomplished with LC/MS/MS. The limits of detection (LOD) and quantification (LOQ) in human plasma and urine samples were 0.3 and 1.0nmolL(-1), respectively. The standard calibration curves were obtained within the concentration range 1-2000nmolL(-1) for HA in human plasma and urine. The coefficients of determination (r(2)) were ≥0.998. The obtained data exhibited recoveries were higher than 89% for the extraction of HA in human plasma and urine samples. Copyright © 2015 Elsevier B.V. All rights reserved.
Spectroscopic studies of trimetoxypropylsilane and bis(trimethoxysilyl)ethane sol-gel coatings on aluminum and copper.

PubMed

Li, Ying-Sing; Tran, Tuan; Xu, Yue; Vecchio, Nicolas E

2006-11-01

Trimethoxypropylsilane (TMPS) and bis(trimethoxysilyl)ethane (BTMSE) were used as surface modifiers of metal vie the sol-gel process and dip coating. In addition to the single coating of Al, Cu and Sn, double treatments of Al were also conducted by combining coatings with these sol-gels in different sequences. Reflection and absorption infrared spectroscopy (RAIR) was employed to characterize and to trace the proceeding of the sol-gel process of the films. It was found that the silanol condensation occurs in the coating films on Al and the covalent linkage exists between the TMPS film and copper surface. From the assigned vibration modes, two conformers were identified in pure TMPS, TMPS sol-gel and coated film. A series of dip coating experiments with different concentrations of TMPS sol-gel was conducted, and the results from the collected RAIR spectra of the coated samples suggested that the coated Cu consistently has a better RAIR spectrum than that of the coated Al. The TMPS sol-gel appeared to have a better affinity to Cu than to Al. The temperature effect and the aging effect in the coating films were studied. X-ray photoelectronic spectroscopy (XPS) was employed to characterize the coated film, and the XPS data confirm the formation of the siloxane film from the silane coupling agents (SCA). Electrochemical impedance spectra (EIS) have been collected for bare Al and Cu, BTMSE sol-gel coated Al, and TMPS sol-gel coated Cu in 0.15M NaCl solution. The corresponding electronic circuit parameters have been determined to match the experimental EIS data.
Infrared wire-grid polarizer with sol-gel antireflection films on both sides

NASA Astrophysics Data System (ADS)

Yamada, Itsunari; Ishihara, Yoshiro

2017-12-01

We fabricated an infrared wire-grid polarizer with the high transverse magnetic (TM) polarization transmittance and high extinction ratio by soft imprint lithography, sol-gel method, and Al shadow coating processes. A zilconia film was coated on Si substrate by using sol-gel method and spin coating method. Then, sol-gel zirconia grating was formed on the back side using imprinting using a silicone mold. The polarizer was produced by depositing Al obliquely on the grating. The TM transmittance of the fabricated element was greater than 80% at a wavelength of 4.8 μm. The sol-gel zilconia films acted as antireflection films. The extinction ratio exceeded 26 dB at its wavelength.
Development of Novel Warfarin-Silica Composite for Controlled Drug Release.

PubMed

Parfenyuk, Elena V; Dolinina, Ekaterina S

2017-04-01

The work is devoted to synthesis and study of warfarin composites with unmodified, methyl and phenyl modified silica in order to develop controlled release formulation of the anticoagulant. The composites were prepared by two routes, adsorption and sol-gel, and characterized with FTIR spectroscopy, dynamic light scattering and DSC methods. The drug release behavior from the composites in media with pH 1.6, 6.8 and 7.4 was analyzed in vitro. The release kinetics of the warfarin - silica composites prepared by the two routes was compared among each other and with analogous silica composites with water soluble drug molsidomine. The comparative analysis showed that in general the kinetic regularities and mechanisms of release for both drugs are similar and determined by nonuniform distribution of the drugs over the silica matrixes and stability of the matrixes in the studied media for the adsorbed composites and uniformly distributed drug and more brittle structure for the sol-gel composites. The sol-gel composite of warfarin - phenyl modified silica is perspective for further development of novel warfarin formulation with controlled release because it releases warfarin according to zero-order kinetic law with approximately equal rate in the media imitating different segments of gastrointestinal tract.
Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

NASA Technical Reports Server (NTRS)

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.
Ultrasound-assisted sol-gel synthesis of ZrO2.

PubMed

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

Fabrication and Anti-Oxidation Ability of SiC-SiO2 Coated Carbon Fibers Using Sol-Gel Method

PubMed Central

Yang, Guangyuan; Huang, Zhixiong; Wang, Xu; Wang, Bo

2018-01-01

The paper proposed a method to improve the anti-oxidation performance of carbon fibers (CF) at high temperature environment by coating silicon dioxide (SiO2) and silicon carbide (SiC). The modified sol-gel method had been used to ensure the proper interface between fibers and coating. We used polydimethylsiloxane and ethyl orthosilicate to make stable emulsion to uniformly disperse SiC nanoparticles. The modified SiO2/SiC coating had been coated on CF successfully. Compared with the untreated CF, the coated fibers started to be oxidized around 900 °C and the residual weight was 57% at 1400 °C. The oxidation mechanism had been discussed. The structure of SiC/SiO2 coated CF had been characterized by scanning electron microscope and X-ray diffraction analysis. Thermal gravimetric analysis was used to test the anti-oxidation ability of CF with different coatings. PMID:29495499
Entrapment of subtilisin in ceramic sol-gel coating for antifouling applications.

PubMed

Regina, Viduthalai Rasheedkhan; Søhoel, Helmer; Lokanathan, Arcot Raghupathi; Bischoff, Claus; Kingshott, Peter; Revsbech, Niels Peter; Meyer, Rikke Louise

2012-11-01

Enzymes with antifouling properties are of great interest in developing nontoxic antifouling coatings. A bottleneck in developing enzyme-based antifouling coatings is to immobilize the enzyme in a suitable coating matrix without compromising its activity and stability. Entrapment of enzymes in ceramics using the sol-gel method is known to have several advantages over other immobilization methods. The sol-gel method can be used to make robust coatings, and the aim of this study was to explore if sol-gel technology can be used to develop robust coatings harboring active enzymes for antifouling applications. We successfully entrapped a protease, subtilisin (Savinase, Novozymes), in a ceramic coating using a sol-gel method. The sol-gel formulation, when coated on a stainless steel surface, adhered strongly and cured at room temperature in less than 8 h. The resultant coating was smoother and less hydrophobic than stainless steel. Changes in the coating's surface structure, thickness and chemistry indicate that the coating undergoes gradual erosion in aqueous medium, which results in release of subtilisin. Subtilisin activity in the coating increased initially, and then gradually decreased. After 9 months, 13% of the initial enzyme activity remained. Compared to stainless steel, the sol-gel-coated surfaces with active subtilisin were able to reduce bacterial attachment of both Gram positive and Gram negative bacteria by 2 orders of magnitude. Together, our results demonstrate that the sol-gel method is a promising coating technology for entrapping active enzymes, presenting an interesting avenue for enzyme-based antifouling solutions.
Secondary Crystal Growth on a Cracked Hydrotalcite-Based Film Synthesized by the Sol-Gel Method.

PubMed

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

2016-05-02

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

NASA Astrophysics Data System (ADS)

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

2017-03-01

Hydroxyapatite Ca10(PO4)6(OH)2 (HA) powder was successfully synthesized by a modified sol-gel method using a solution of calcium nitrate in ethanol, along with a solution of diammonium hydrogen phosphate in water and NH4OH as starting materials. The Ca/P molar ratio was maintained at 1.67. The powder was subjected to furnace and microwave heating to compare the decomposition of HA and study the crystallite sizes. It was found that microwave heated powders were pure HAP up to 230°C with absence of secondary phases. However, XRD patterns show that furnace heated powders convert completely to β-TCP when treated at 750°C and 1000°C. This result was confirmed by the absence of hydroxyl bands in the FT-IR spectra for these temperatures.
Modified thermoresponsive Poloxamer 407 and chitosan sol-gels as potential sustained-release vaccine delivery systems.

PubMed

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.
Effect of carrier properties on surface characteristics of sorbents modified with acetylacetonates Ni (II), Cu (II)

NASA Astrophysics Data System (ADS)

Faustova, Zhanna; Matveeva, Tatiana; Slizhov, Yuriy

2017-11-01

Sorbents based on Chromaton N-AW with layers of mesoporous silica gel modified with acetylacetonate nickel (II) and copper (II) were obtained. The porous structure of sorbents based on synthesized silica gel and industrial samples of Chromaton N, Silipore 075, Silochrom C-120 was studied. All studied samples are mesoporous. For sorbents based on commercially available Chromaton N, Silipore 075, and Silochrome 120, the mesopore dimensions vary in a wide range from 10 to 50 nm. For synthesized silica gel and chelate-containing sorbents, a narrower pore distribution is observed in the range of 5-15 nm, which indicates the uniformity of its surface. A comparative analysis of the effect of carrier properties on the acid-base properties of the surface of chelate-containing sorbents is carried out. The acid-base nature of the modifier is more pronounced in the case of synthesized silica gel by the sol-gel method.
Production of continuous mullite fiber via sol-gel processing

NASA Technical Reports Server (NTRS)

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.
Commercial and home-made nitrogen modified titanias. A short reflection about the advantageous/disadvantageous properties of nitrogen doping in the frame of their applicability

NASA Astrophysics Data System (ADS)

Pap, Zs.; Mogyorósi, K.; Veréb, G.; Dombi, A.; Hernádi, K.; Danciu, V.; Baia, L.

2014-09-01

As visible light driven photocatalysis became more and more intensively studied, the first commercial products showed up on the market. Simultaneously controversial results appeared in the literature generating an intensive debate regarding the advantages and draw-backs of nitrogen doping of titania. Hence, the present work focuses on two commercially available and four sol-gel made nitrogen modified titania powders regarding their structure and activity. It is demonstrated that the interstitial nitrogen entities “leak out” from the catalysts if the material is irradiated with UV light, while substitutional nitrogen remains stable. However, the latter one was proven to be less important in the photocatalytic point of view. These observations were also valid in the case of sol-gel made nitrogen modified titanias. Furthermore, the results obtained after applying different spectroscopic methods (IR, XPS and DRS) shown that the yellow color of the titanias, does not necessary mean that a successful doping is achieved.
Study of the Kinetics and Equilibrium of the Adsorption of Oils onto Hydrophobic Jute Fiber Modified via the Sol-Gel Method.

PubMed

Lv, Na; Wang, Xiaoli; Peng, Shitao; Zhang, Huaqin; Luo, Lei

2018-05-12

A new kind of hydrophobic and oil sorbent based on jute fiber was successfully prepared by the integration of silica onto a fiber surface via the sol-gel method and subsequent hydrophobic modification with octadecyltrichlorosilane (OTS). Compared with the hydrophilic raw fiber, the modified fiber had a water contact angle (CA) of 136.2°, suggesting that the material has good hydrophobicity. Furthermore, the ability of oil in the oil/water system (taking diesel for example) to absorb was revealed by the kinetics, the isotherm equation, and the thermodynamic parameters. Adsorption behavior was kinetically investigated using pseudo first-order and pseudo second-order models. The data mostly correlated with the pseudo first-order model. The equilibrium adsorption at 298 K was assessed by using the Langmuir and Freundlich isotherm models. The Freundlich model had greater consistency with the experimental data. The obtained thermodynamic parameters demonstrate that the adsorption of diesel is spontaneous, favorable, and exothermic.
Synthesis of CaCu3Ti4O12 by modified Sol-gel method with Hydrothermal process

NASA Astrophysics Data System (ADS)

Masingboon, C.; Rungruang, S.

2017-09-01

CaCu3Ti4O12 powders were synthesized by modified Sol-gel method with Hydrothermal process using Ca(NO3)2· 4H2O, Cu(NO3)2·3H2O, Ti(OC3H7)4 and freshly extracted egg white (ovalbumin) in aqueous medium. The precursor was calcined at 800, 900 and 1000 °C in air for 8 h to obtain nanocrystalline powders of CaCu3Ti4O12. The calcined CaCu3Ti4O12 powders were characterized by XRD, TEM and EDX. The XRD results indicated that all calcined samples have a typical perovskite CaCu3Ti4O12 structure and a small amount of CaTiO3, CuO and TiO2. TEM micrographs showed particle size 100 - 500 nm and EDX results showed elements of CaCu3Ti4O12 powders have calcium, copper, titanium and oxygen.
Methods for and products of processing nanostructure nitride, carbonitride and oxycarbonitride electrode power materials by utilizing sol gel technology for supercapacitor applications

DOEpatents

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.
Sol-gel Synthesis, Photo- and Electrocatalytic Properties of Mesoporous TiO2 Modified with Transition Metal Ions

NASA Astrophysics Data System (ADS)

Smirnova, N.; Petrik, I.; Vorobets, V.; Kolbasov, G.; Eremenko, A.

2017-03-01

Mesoporous nanosized titania films modified with Co2+, Ni2+, Mn3+, and Cu2+ ions have been produced by templated sol-gel method and characterized by optical spectroscopy, X-ray diffraction (XRD), and Brunauer, Emmett, and Teller (BET) surface area measurement. Band gap energy and the position of flat band potentials were estimated by photoelectrochemical measurements. The films doped with transition metals possessed higher photocurrent quantum yield, as well as photo- and electrochemical activity compared to undoped samples. Mn+/TiO2 (M-Co, Ni, Mn, Cu) electrodes with low dopant content demonstrate high efficiency in electrocatalytic reduction of dissolved oxygen. Polarization curves of TiO2, TiO2/Ni2+, TiO2/Co2+/3+, and TiO2/Mn3+ electrodes contain only one current wave (oxygen reduction current). It means that reaction proceeds without the formation of an intermediate product H2O2.
Sol-gel derived C-SiC composites and protective coatings for sustained durability in the space environment

NASA Astrophysics Data System (ADS)

Haruvy, Yair; Liedtke, Volker

2003-09-01

Composites and coatings were produced via the fast sol-gel process of a mixture of alkoxysilane precursors. The composites were comprised of carbon fibers, fabrics, or their precursors as reinforcement, and sol-gel-derived silicon carbide as matrix, aiming at high-temperature stable ceramics that can be utilized for re-entry structures. The protective coatings were comprised of fluorine-rich sol-gel derived resins, which exhibit high flexibility and coherence to provide sustained ATOX protection necessary for LEO space-exposed elements. For producing the composites, the sol-gel-derived resin is cast onto the reinforcement fibers/fabrics mat (carbon or its precursors) to produce a 'green' composite that is being cured. The 'green' composite is converted into a C-SiC composite via a gradual heat-pressure process under inert atmosphere, during which the organic substituents on the silicon atoms undergo internal oxidative pyrolysis via the schematic reaction: (SiRO3/2)n -> SiC + CO2 + H2O. The composition of the resultant silicon-oxi-carbide is tailorable via modifying the composition of the sol-gel reactants. The reinforcement, when made of carbon precursors, is converted into carbon during the heat-and-pressure processing as well. The C-SiC composites thus derived exhibit superior thermal stability and comparable thermal conductivity, combined with good mechanical strength features and failure resistance, which render them greatly applicable for re-entry shielding, heat-exchange pipes, and the like. Fluorine rich sol-gel derived coatings were developed as well, via the use of HF rich sol-gel process. These coatings provide oxidation-protection via the silica formation process, together with flexibility that allows 18,000 repetitive folding of the coating without cracking.
An abrasion-resistant and broadband antireflective silica coating by block copolymer assisted sol-gel method.

PubMed

Zou, Liping; Li, Xiaoguang; Zhang, Qinghua; Shen, Jun

2014-09-02

A double-layer broadband antireflective (AR) coating was prepared on glass substrate via sol-gel process using two kinds of acid-catalyzed TEOS-derived silica sols. The relative dense layer with a porosity of ∼10% was obtained from an as-prepared sol, while the porous layer with a porosity of ∼55% was from a modified one with block copolymer (BCP) Pluronic F127 as template which results in abundant ordered mesopores. The two layers give rise to a reasonable refractive index gradient from air to the substrate and thus high transmittance in a wide wavelength range, and both of them have the same tough skeleton despite different porosity, for which each single-layer and the double-layer coatings all behaved well in the mechanical property tests. The high transmittance and the strong ability of resisting abrasion make this coating promising for applications in some harsh conditions. In addition, the preparation is simple, low-cost, time-saving, and flexible for realizing the optical property.
Ferroelectric PLZT thick films grown by poly(1-vinylpyrrolidone-co-vinyl acetate) (PVP/VA)-modified sol-gel process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hu, Zhongqiang; Ma, Beihai; Li, Meiya

2016-03-01

We report the growth of ferroelectric Pb0.92La0.08Zr0.52Ti0.48O3 (PLZT) thick films using a poly(1-vinylpyrrolidone-co-vinyl acetate) (PVP/VA)-modified sol–gel process. A per-coating thickness of ≈0.66 μm has been demonstrated using PVP/VA-modified solution, which is more than doubled that of the PLZT films grown by PVP-modified method, and nearly 6 times the per-coating thickness of films prepared by conventional sol–gel process. PLZT thick films grown on LNO/Ni substrates exhibited denser microstructure, higher remanent polarization (11 μC/cm 2) and dielectric tunability (45%), lower leakage current density (≈1.2 × 10 -8 A/cm 2), and higher breakdown strength (≈1.6 MV/cm) than those for the samples grown onmore » PtSi substrates. These results demonstrated great potential of using PVP/VA-modified sol–gel process for high power film capacitor applications.« less
Selective determination of dopamine using quantum-sized gold nanoparticles protected with charge selective ligands

NASA Astrophysics Data System (ADS)

Kwak, Kyuju; Kumar, S. Senthil; Lee, Dongil

2012-06-01

We report here the selective determination of dopamine (DA) using quantum-sized gold nanoparticles coated with charge selective ligands. Glutathione protected gold nanoparticles (GS-Au25) were synthesized and immobilized into a sol-gel matrix via thiol linkers. The GS-Au25 modified sol-gel electrode was found to show excellent electrocatalytic activity towards the oxidation of DA but no activity towards the oxidation of ascorbic acid. The role of electrostatic charge in the selective electrocatalytic activity of GS-Au25 was verified by voltammetry of redox markers carrying opposite charges. The pH dependent sensitivity for the determination of DA further confirmed the charge screening effect of GS-Au25. Mechanistic investigation revealed that the selectivity is attained by the selective formation of an electrostatic complex between the negatively charged GS-Au25 and DA cation. The GS-Au25 modified sol-gel electrode also showed excellent selectivity for DA in the presence of an interferent, ascorbic acid.We report here the selective determination of dopamine (DA) using quantum-sized gold nanoparticles coated with charge selective ligands. Glutathione protected gold nanoparticles (GS-Au25) were synthesized and immobilized into a sol-gel matrix via thiol linkers. The GS-Au25 modified sol-gel electrode was found to show excellent electrocatalytic activity towards the oxidation of DA but no activity towards the oxidation of ascorbic acid. The role of electrostatic charge in the selective electrocatalytic activity of GS-Au25 was verified by voltammetry of redox markers carrying opposite charges. The pH dependent sensitivity for the determination of DA further confirmed the charge screening effect of GS-Au25. Mechanistic investigation revealed that the selectivity is attained by the selective formation of an electrostatic complex between the negatively charged GS-Au25 and DA cation. The GS-Au25 modified sol-gel electrode also showed excellent selectivity for DA in the presence of an interferent, ascorbic acid. Electronic supplementary information (ESI) available: TEM image of GS-Au25, SWV of GS-Au25 in solution, effect of scan rate on the CV of GS-Au25ME, CVs of DA and AA at the bare GCE and CVs of GS-Au25ME at different pHs. See DOI: 10.1039/c2nr30481c
Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method. Optimisation, characterisation and rheology.

PubMed

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.
Structural development and kinetic analysis of PbTiO3 powders processed at low-temperature via new sol-gel approach

NASA Astrophysics Data System (ADS)

Bel-Hadj-Tahar, Radhouane; Abboud, Mohamed

2018-04-01

The synthesis of crystalline lead titanate powder by a generic low-temperature sol-gel approach is developed. Acetoin was added as ligand, instead of the commonly used alkanolamines, to ensure total dissolution of the precursor compounds. The feasibility of the acetoin-Ti isopropoxide complex as a new precursor of PbTiO3 perovskite particles via sol-gel method has been demonstrated. No excess lead has been introduced. Nanometric PbTiO3 crystallites have been formed at 400 °C under atmospheric pressure from titanium isopropoxide and lead acetate in alcoholic solution by remarkably low activation energy of crystallization process of 90 kJ mol-1. The powders show tetragonal lattice and dendritic morphology. In addition to the effect of heat-treatment temperature, time, and atmosphere, the sol chemistry particularly influenced the phase composition, particle size, and particle morphology. The use of different ligands significantly modified powder morphology. The extent of the crystallization was quantitatively evaluated by differential thermal analysis and analyzed by Johnson-Mehl-Avrami approach. The crystallization followed two rate regimes depending on the interval of the crystallized fraction.
Porous alumina scaffold produced by sol-gel combined polymeric sponge method

NASA Astrophysics Data System (ADS)

Hasmaliza, M.; Fazliah, M. N.; Shafinaz, R. J.

2012-09-01

Sol gel is a novel method used to produce high purity alumina with nanometric scale. In this study, three-dimensional porous alumina scaffold was produced using sol-gel polymeric sponge method. Briefly, sol gel alumina was prepared by evaporation and polymeric sponge cut to designated sizes were immersed in the sol gel followed by sintering at 1250 and 1550°C. In order to study the cell interaction, the porous alumina scaffold was sterilized using autoclave prior to Human Mesenchymal Stem Cells (HMSCs) seeding on the scaffold and the cell proliferation was assessed by alamarBlue® assay. SEM results showed that during the 21 day period, HMSCs were able to attach on the scaffold surface and the interconnecting pores while maintaining its proliferation. These findings suggested the potential use of the porous alumina produced as a scaffold for implantation procedure.
Hybrid organic-inorganic sol-gel materials and components for integrated optoelectronics

NASA Astrophysics Data System (ADS)

Lu, Dong

On the technical platform of hybrid organic-inorganic sol-gel, the integrated optoelectronics in the forms of heterogeneous integration between the hybrid sol-gel waveguide and the high refractive index semiconductors and the nonlinear functional doping of disperse red chromophore into hybrid sol-gel is developed. The structure of hybrid sol-gel waveguide on high index semiconductor substrate is designed with BPM-CAD software. A hybrid sol-gel based on MAPTMS and TEOS suitable for lower cladding for the waveguide is developed. The multi-layer hybrid sol-gel waveguide with good mode confinement and low polarization dependence is fabricated on Si and InP. As proof of concept, a 1 x 12 beam splitter based on multimode interference is fabricated on silicon substrate. The device shows excess loss below 0.65 dB and imbalance below 0.28 dB for both TE and TM polarization. A nonlinear active hybrid sol-gel doped with disperse red 13 has been developed by simple co-solvent method. It permits high loading concentration and has low optical loss at 1550 nm. The second-order nonlinear property of the active sol-gel is induced with corona poling and studied with second harmonic generation. A 3-fold of enhancement in the poling efficiency is achieved by blue light assisted corona poling. The chromophore alignment stability is improved by reducing the free volume of the formed inorganic network from the sol-gel condensation reaction. An active sol-gel channel waveguide has been fabricated using active and passive hybrid sol-gel materials by only photopatterning and spin-coating. An amplitude modulator based on the active sol-gel containing 30 wt.% of DR13 shows an electro-optic coefficient of 14 pm/V at 1550 nm and stable operation within the observation time of 24 days.

Synthesis of zinc oxide thin films prepared by sol-gel for specific bioactivity

NASA Astrophysics Data System (ADS)

Adam, Tijjani; Basri, B.; Dhahi, Th. S.; Mohammed, Mohammed; Hashim, U.; Noriman, N. Z.; Dahham, Omar S.

2017-09-01

Zinc oxide (ZnO) thin films this device to used for many application like chemical sensor, biosensor, solar energy, etc but my project to use for bioactivity(biosensor). Zinc oxide (ZnO) thin films have been grown using sol-gel technique. Characterization was done using Scanning Electron Microscope (SEM), Energy Dispersive X-ray(EDX) and Electrical Measurement(I-V). ZnO thin film was successfully synthesized using low cost sol-gel spin coating method. The coupling of DNA probe to ZnO thin film supports modified with carboxylic acid (COOH) is certainly the best practical method to make DNA immobilization and it does not require any coupling agent which could be a source of variability during the spotting with an automatic device. So, selected this coupling procedure for further experiments. The sensor was tested with initial trial with low concentrated DNA and able to detect detection of the disease effectively. Silicon-on-insulator (SOI) wafer device with ZnO can detect at different concentration in order to valid the device capabilities for detecting development. The lowest concentration 1 µM HPV DNA probe can detect is 0.1 nM HPV target DNA.
Optical fiber sensor having a sol-gel fiber core and a method of making

DOEpatents

Tao, Shiquan; Jindal, Rajeev; Winstead, Christopher; Singh, Jagdish P.

2006-06-06

A simple, economic wet chemical procedure is described for making sol-gel fibers. The sol-gel fibers made from this process are transparent to ultraviolet, visible and near infrared light. Light can be guided in these fibers by using an organic polymer as a fiber cladding. Alternatively, air can be used as a low refractive index medium. The sol-gel fibers have a micro pore structure which allows molecules to diffuse into the fiber core from the surrounding environment. Chemical and biochemical reagents can be doped into the fiber core. The sol-gel fiber can be used as a transducer for constructing an optical fiber sensor. The optical fiber sensor having an active sol-gel fiber core is more sensitive than conventional evanescent wave absorption based optical fiber sensors.
Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process.

PubMed

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

PubMed Central

Li, Fa-Liang; Zhang, Hai-Jun

2017-01-01

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. PMID:28841188
One-step sol-gel imprint lithography for guided-mode resonance structures.

PubMed

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.
Method to produce alumina aerogels having porosities greater than 80 percent

DOEpatents

Poco, John F.; Hrubesh, Lawrence W.

2003-09-16

A two-step method for producing monolithic alumina aerogels having porosities of greater than 80 percent. Very strong, very low density alumina aerogel monoliths are prepared using the two-step sol-gel process. The method of preparing pure alumina aerogel modifies the prior known sol method by combining the use of substoichiometric water for hydrolysis, the use of acetic acid to control hydrolysis/condensation, and high temperature supercritical drying, all of which contribute to the formation of a polycrystalline aerogel microstructure. This structure provides exceptional mechanical properties of the alumina aerogel, as well as enhanced thermal resistance and high temperature stability.
Sol gel-derived hydroxyapatite films over porous calcium polyphosphate substrates for improved tissue engineering of osteochondral-like constructs.

PubMed

Lee, Whitaik David; Gawri, Rahul; Pilliar, Robert M; Stanford, William L; Kandel, Rita A

2017-10-15

Integration of in vitro-formed cartilage on a suitable substrate to form tissue-engineered implants for osteochondral defect repair is a considerable challenge. In healthy cartilage, a zone of calcified cartilage (ZCC) acts as an intermediary for mechanical force transfer from soft to hard tissue, as well as an effective interlocking structure to better resist interfacial shear forces. We have developed biphasic constructs that consist of scaffold-free cartilage tissue grown in vitro on, and interdigitated with, porous calcium polyphosphate (CPP) substrates. However, as CPP degrades, it releases inorganic polyphosphates (polyP) that can inhibit local mineralization, thereby preventing the formation of a ZCC at the interface. Thus, we hypothesize that coating CPP substrate with a layer of hydroxyapatite (HA) might prevent or limit this polyP release. To investigate this we tested both inorganic or organic sol-gel processing methods, asa barrier coating on CPP substrate to inhibit polyP release. Both types of coating supported the formation of ZCC in direct contact with the substrate, however the ZCC appeared more continuous in the tissue formed on the organic HA sol gel coated CPP. Tissues formed on coated substrates accumulated comparable quantities of extracellular matrix and mineral, but tissues formed on organic sol-gel (OSG)-coated substrates accumulated less polyP than tissues formed on inorganic sol-gel (ISG)-coated substrates. Constructs formed with OSG-coated CPP substrates had greater interfacial shear strength than those formed with ISG-coated and non-coated substrates. These results suggest that the OSG coating method can modify the location and distribution of ZCC and can be used to improve the mechanical integrity of tissue-engineered constructs formed on porous CPP substrates. Articular cartilage interfaces with bone through a zone of calcified cartilage. This study describes a method to generate an "osteochondral-like" implant that mimics this organization using isolated deep zone cartilage cells and a sol-gel hydroxyapatite coated bone substitute material composed of calcium polyphosphate (CPP). Developing a layer of calcified cartilage at the interface should contribute to enhancing the success of this "osteochondral-like" construct following implantation to repair cartilage defects. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Studies of (3-mercaptopropyl)trimethoxylsilane and bis(trimethoxysilyl)ethane sol-gel coating on copper and aluminum.

PubMed

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.
Sensing response of copper phthalocyanine salt dispersed glass with organic vapours

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ridhi, R.; Sachdeva, Sheenam; Saini, G. S. S.

2016-05-06

Copper Phthalocyanine and other Metal Phthalocyanines are very flexible and tuned easily to modify their structural, spectroscopic, optical and electrical properties by either functionalizing them with various substituent groups or by replacing or adding a ligand to the central metal atom in the phthalocyanine ring and accordingly can be made sensitive and selective to various organic species or gaseous vapours. In the present work, we have dispersed Copper Phthalocyanine Salt (CuPcS) in sol-gel glass form using chemical route sol-gel method and studied its sensing mechanism with organic vapours like methanol and benzene and found that current increases onto their exposuremore » with vapours. A variation in the activation energies was also observed with exposure of vapours.« less
Sensing response of copper phthalocyanine salt dispersed glass with organic vapours

NASA Astrophysics Data System (ADS)

Ridhi, R.; Sachdeva, Sheenam; Saini, G. S. S.; Tripathi, S. K.

2016-05-01

Copper Phthalocyanine and other Metal Phthalocyanines are very flexible and tuned easily to modify their structural, spectroscopic, optical and electrical properties by either functionalizing them with various substituent groups or by replacing or adding a ligand to the central metal atom in the phthalocyanine ring and accordingly can be made sensitive and selective to various organic species or gaseous vapours. In the present work, we have dispersed Copper Phthalocyanine Salt (CuPcS) in sol-gel glass form using chemical route sol-gel method and studied its sensing mechanism with organic vapours like methanol and benzene and found that current increases onto their exposure with vapours. A variation in the activation energies was also observed with exposure of vapours.
The Effect of Time, Temperature and Composition on Boron Carbide Synthesis by Sol-gel Method

NASA Astrophysics Data System (ADS)

Hadian, A. M.; Bigdeloo, J. A.

2008-02-01

To minimize free carbon residue in the boron carbide (B4C) powder, a modified sol-gel process is performed where the starting materials as boric acid and citric acid compositions are adjusted. Because of boron loss in the form of B2O2(g) during the reduction reaction of the stoichiometric starting composition, the final B4C powders contain carbon residues. Thus, an excess H3BO3 is used in the reaction to compensate the loss and to obtain stoichiometric powders. Parameters of production have been determined using x-ray diffraction analysis and particle size analyses. The synthesized B4C powder using an excess boric acid composition shows no trace of carbon.
Structural and Luminescence Properties of Lu2O3:Eu3+ F127 Tri-Block Copolymer Modified Thin Films Prepared by Sol-Gel Method

PubMed Central

de Jesus Morales Ramírez, Angel; Hernández, Margarita García; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Palmerin, Joel Moreno; Velazquez, Dulce Yolotzin Medina; Jota, María Luz Carrera

2013-01-01

Lu2O3:Eu3+ transparent, high density, and optical quality thin films were prepared using the sol-gel dip-coating technique, starting with lutetium and europium nitrates as precursors and followed by hydrolysis in an ethanol-ethylene glycol solution. Acetic acid and acetylacetonate were incorporated in order to adjust pH and as a sol stabilizer. In order to increment the thickness of the films and orient the structure, F127 Pluronic acid was incorporated during the sol formation. Structural, morphological, and optical properties of the films were investigated for different F127/Lu molar ratios (0–5) in order to obtain high optical quality films with enhanced thickness compared with the traditional method. X-ray diffraction (XRD) shows that the films present a highly oriented cubic structure <111> beyond 1073 K for a 3-layer film, on silica glass substrates. The thickness, density, porosity, and refractive index evolution of the films were investigated by means of m-lines microscopy along with the morphology by scanning electron microscope (SEM) and luminescent properties. PMID:28809336
Integrating sol-gel with cold plasmas modified porous polycaprolactone membranes for the drug-release of silver-sulfadiazine and ketoprofen

NASA Astrophysics Data System (ADS)

Mangindaan, Dave; Chen, Chao-Ting; Wang, Meng-Jiy

2012-12-01

A controlled release system composed of surface modified porous polycaprolactone (PCL) membranes combined with a layer of tetraorthosilicate (TEOS)-chitosan sol-gel was reported in this study. PCL is a hydrophobic, semi-crystalline, and biodegradable polymer with a relatively slow degradation rate. The drugs chosen for release experiments were silver-sulfadiazine (AgSD) and ketoprofen which were impregnated in the TEOS-chitosan sol-gel. The surface modification was achieved by O2 plasma and the surfaces were characterized by water contact angle (WCA) measurements, atomic force microscope (AFM), scanning electron microscope and electron spectroscopy for chemical analysis (ESCA). The results showed that the release of AgSD on O2 plasma treated porous PCL membranes was prolonged when compared with the pristine sample. On the contrary, the release rate of ketoprofen revealed no significant difference on pristine and plasma treated PCL membranes. The prepared PCL membranes showed good biocompatibility for the wound dressing biomaterial applications.
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.

PubMed

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) (4.2-26.3 ng L -1 ) for environmentally important analytes including polycyclic aromatic hydrocarbons, ketones and aliphatic hydrocarbons. In CME-GC experiments (n = 5), the capillary-to-capillary RSD value was ∼2.1%; such a low RSD value is indicative of excellent reproducibility of the sol-gel method used for the preparation of these CME coatings. The dual-ligand sol-gel coating provided stable performance in capillary microextraction of analytes from saline samples. Copyright © 2017 Elsevier B.V. All rights reserved.
Sol-Gel Chemistry for Carbon Dots.

PubMed

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.
Electrochemiluminescence detection of NADH and ethanol based on partial sulfonation of sol-gel network with gold nanoparticles.

PubMed

Deng, Liu; Zhang, Lihua; Shang, Li; Guo, Shaojun; Wen, Dan; Wang, Fuan; Dong, Shaojun

2009-03-15

We developed a stable, sensitive electrochemiluminescence (ECL) biosensor based on the synthesis of a new sol-gel material with the ion-exchange capacity sol-gel to coimmobilize the Ru(bpy)(3)(2+) and enzyme. The partial sulfonated (3-mercaptopropyl)-trimethoxysilane sol-gel (PSSG) film acted as both an ion exchanger for the immobilization of Ru(bpy)(3)(2+) and a matrix to immobilize gold nanoparticles (AuNPs). The AuNPs/PSSG/Ru(bpy)(3)(2+) film modified electrode allowed sensitive the ECL detection of NADH as low as 1 nM. Such an ability of AuNPs/PSSG/Ru(bpy)(3)(2+) film to promote the electron transfer between Ru(bpy)(3)(2+) and the electrode suggested a new, promising biocompatible platform for the development of dehydrogenase-based ECL biosensors. With alcohol dehydrogenase (ADH) as a model, we then constructed an ethanol biosensor, which had a linear range of 5 microM to 5.2 mM with a detection limit of 12nM.
Magnetic response of gelatin ferrogels across the sol-gel transition: the influence of high energy crosslinking on thermal stability.

PubMed

Wisotzki, Emilia I; Eberbeck, Dietmar; Kratz, Harald; Mayr, Stefan G

2016-05-07

As emerging responsive materials, ferrogels have demonstrated significant potential for applications in areas of engineering to regenerative medicine. Promising techniques to study the behavior of magnetic nanoparticles (MNPs) in such matrices include magnetic particle spectroscopy (MPS) and magnetorelaxometry (MRX). This work investigated the magnetic response of gelatin-based ferrogels with increasing temperatures, before and after high energy crosslinking. The particle response was characterized by the nonlinear magnetization using MPS and quasistatic magnetization measurements as well as MRX to discriminate between Néel and Brownian relaxation mechanisms. The effective magnetic response of MNPs in gelatin was suppressed, indicating that the magnetization of the ferrogels was strongly influenced by competing dipole-dipole interactions. Significant changes in the magnetic behavior were observed across the gelatin sol-gel transition, as influenced by the matrix viscosity. These relaxation processes were modeled by Fourier transformation of the Langevin function, combined with a Debye term for the nonlinear magnetic response, for single core MNPs embedded in matrices of changing viscosities. Using high energy electron irradiation as a crosslinking method, modified ferrogels exhibited thermal stability on a range of timescales. However, MRX relaxation times revealed a slight softening around the gelatin sol-gel transition felt by the smallest particles, demonstrating a high sensitivity to observe local changes in the viscoelasticity. Overall, MPS and MRX functioned as non-contact methods to observe changes in the nanorheology around the native sol-gel transition and in crosslinked ferrogels, as well as provided an understanding of how MNPs were integrated into and influenced by the surrounding matrix.
Ceria nanoparticles vis-à-vis cerium nitrate as corrosion inhibitors for silica-alumina hybrid sol-gel coating

NASA Astrophysics Data System (ADS)

Lakshmi, R. V.; Aruna, S. T.; Sampath, S.

2017-01-01

The present work provides a comparative study on the corrosion protection efficiency of defect free sol-gel hybrid coating containing ceria nanoparticles and cerium nitrate ions as corrosion inhibitors. Less explored organically modified alumina-silica hybrid sol-gel coatings are synthesized from 3-glycidoxypropyltrimethoxysilane and aluminium-tri-sec-butoxide. The microemulsion derived nanoparticles and the hybrid coatings are characterized and compared with coatings containing cerium nitrate. Corrosion inhibiting capability is assessed using electrochemical impedance spectroscopy. Scanning Kelvin probe measurements are also conducted on the coatings for identifying the apparent corrosion prone regions. Detailed X-ray photoelectron spectroscopy (XPS) analysis is carried out to comprehend the bonding and corrosion protection rendered by the hybrid coatings.
Fabrication of advanced electrochemical energy materials using sol-gel processing techniques

NASA Technical Reports Server (NTRS)

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

1995-01-01

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

PubMed Central

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

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

PubMed

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.
Spatially resolved speckle-correlometry of sol-gel transition

NASA Astrophysics Data System (ADS)

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

PubMed

Li, Ying-Sing; Ba, Abdul

2008-10-01

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

DOEpatents

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

2005-05-17

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

DOEpatents

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

2003-12-23

Sol-gel chemistry is used for the preparation of energetic materials (explosives, propellants and pyrotechnics) with improved homogeneity, and/or which can be cast to near-net shape, and/or made into precision molding powders. The sol-gel method is a synthetic chemical process where reactive monomers are mixed into a solution, polymerization occurs leading to a highly cross-linked three dimensional solid network resulting in a gel. The energetic materials can be incorporated during the formation of the solution or during the gel stage of the process. The composition, pore, and primary particle sizes, gel time, surface areas, and density may be tailored and controlled by the solution chemistry. The gel is then dried using supercritical extraction to produce a highly porous low density aerogel or by controlled slow evaporation to produce a xerogel. Applying stress during the extraction phase can result in high density materials. Thus, the sol-gel method can be used for precision detonator explosive manufacturing as well as producing precision explosives, propellants, and pyrotechnics, along with high power composite energetic materials.
Making MgO/SiO2 Glasses By The Sol-Gel Process

NASA Technical Reports Server (NTRS)

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.
Chemical Sensors Based on IR Spectroscopy and Surface-Modified Waveguides

NASA Technical Reports Server (NTRS)

Lopez, Gabriel P.; Niemczyk, Thomas

1999-01-01

Sol-gel processing techniques have been used to apply thin porous films to the surfaces of planar infrared (IR) waveguides to produce widely useful chemical sensors. The thin- film coating serves to diminish the concentration of water and increase the concentration of the analyte in the region probed by the evanescent IR wave. These porous films are composed of silica, and therefore, conventional silica surface modification techniques can be used to give the surface a specific functional character. The sol-gel film was surface-modified to make the film highly hydrophobic. These sensors were shown to be capable of detecting non-polar organic analytes, such as benzonitrile, in aqueous solution with detection limits in the ppb range. Further, these porous sol-gel structures allow the analytes to diffuse into and out of the films rapidly, thus reaching equilibrium in less than ten seconds. These sensors are unique because of the fact that their operation is based on the measurement of an IR absorption spectrum. Thus, these sensors are able to identify the analytes as well as measure concentration with high sensitivity. These developments have been documented in previous reports and publications. Recently, we have also targeted detection of the polar organic molecules acetone and isopropanol in aqueous solution. Polar organics are widely used in industrial and chemical processes, hence it is of interest to monitor their presence in effluents or decontamination process flows. Although large improvements in detection limits were expected with non-polar organic molecules in aqueous solutions using very hydrophobic porous sol-gel films on silicon attenuated total reflectance (Si ATR) waveguides, it was not as clear what the detection enhancements might be for polar organic molecules. This report describes the use of modified sol-gel-coated Si ATR sensors for trace detection and quantitation of small polar organic molecules in aqueous solutions. The detection of both acetone and isopropanol molecules in aqueous solution has been previously reported for chalcogenide fiber optic sensors. The sol-gel film was produced using a mixture of ethyltriethoxysilane and tetraethoxysilane and the surface modification was carried out using trimethylchlorosilane. We have demonstrated that this film concentrates the target polar analytes from aqueous solution in the region probed by the evanescent wave to improve detection limits by as much as a factor of 450.
A new strategy for surface modification of polysulfone membrane by in situ imprinted sol-gel method for the selective separation and screening of L-Tyrosine as a lung cancer biomarker.

PubMed

Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-adergani, Behrouz; Abdel-Rehim, Mohamed

2015-03-21

In this work, a novel method based on in situ molecularly imprinted sol-gel for the surface modification of a polysulfone membrane (PSM) was developed. A modified molecularly imprinted sol-gel polysulfone membrane (MSM) was placed in a homemade plastic tube and coupled on-line with LC/MS/MS for the selective extraction and screening of l-Tyrosine (Tyr) as a tentative lung cancer biomarker in human plasma samples. The existence of molecularly imprinted sol-gel layers on both sides of a PSM was examined using scanning electron microscopy (SEM). To evaluate the role of precursor in the extraction performance, repeatability, and selectivity of developed method, three precursors, 3-(propylmethacrylate) trimethoxysilane (P1), 3-(triethoxysilyl)-propylamine (P2), tetraethyl orthosilicate (P3), individually and together were used for treatment of PSM. Our investigation showed that a single precursor's route is more repeatable, straightforward, precise, accurate, and selective for the extraction of Tyr in plasma samples. Moreover, to achieve the best conditions and extraction efficiency, the effect of influential parameters, including the conditioning, washing, and elution of solvents, sample flow rate, loading time, desorption time, loading sample volume, salt effect, pH, and adsorption capacity for the most efficiently prepared membranes were truly investigated. The non-molecularly imprinted sol-gel polysulfone membrane (NSM) was prepared as a blank via the same process but in the absence of the Tyr. The LOD (S/N = 3/1) was 0.1 nmol L(-1) and the LOQ (S/N = 10/1) was 0.34 nmol L(-1) for Tyr in the plasma samples. The linearity for the Tyr was in the range of 0.34-2000 nmol L(-1) in the plasma samples. The coefficients of determination values were ≥0.998 for all runs. The extraction recovery was between 80%-85% for Tyr in the plasma samples. In addition, MSM could be used for up to 50 extractions without a significant change in recovery percentage.
Sol-gel method for encapsulating molecules

DOEpatents

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

2002-01-01

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

NASA Astrophysics Data System (ADS)

Shakeri, Amid; Abdizadeh, Hossein; Golobostanfard, Mohammad Reza

2014-09-01

Thick films of lead zirconate titanate (PZT) offer possibilities for micro-electro-mechanical systems such as high frequency ultrasonic transducers. In this paper, crack-free thick films of PZT have been prepared up to 45 μm thickness via modified sol-gel dip coating method. In this procedure, acetic acid-alcoholic based sol is used by applying diethanolamine (DEA) and deionized water as additives. The effects of DEA and water on the crystal structure and surface morphology of the films are investigated. The mechanisms of acetic acid and DEA complexations are introduced by using FTIR spectrometer which illustrates suitable substitution of complexing agents with alkoxide groups. DEA/(Ti + Zr) = 0.5 or water/(Ti + Zr) = 0.5 are determined as the optimum molar ratio of additives, which lead to the formation of almost pure perovskite phase with the tetragonal lattice parameters of ct = 4.16 Ǻ and at = 4.02 Ǻ and a distortion of 2%. Values of remanent polarization and dielectric constant of 7.8 μC cm-2 and 1630 were obtained for 45 μm thick films, respectively.
Octadecylsilane hybrid silicas prepared by the sol-gel method: morphological and textural aspects.

PubMed

Brambilla, Rodrigo; Pires, Gilvan P; dos Santos, João H Z; Lacerda Miranda, Márcia S

2007-08-15

A series of octadecylsilane-modified silicas was prepared by the sol-gel method through the hydrolysis and cocondensation of tetraethylorthosilicate (TEOS) with octadecyltriethoxysilane (ODS). The ODS:TEOS ratio was varied between 0:100 and 100:0. The resulting carbon content was between 2.5 and 53.4%. In the case of pure ODS, the resulting silica presented 68.6% of C. Hybrid silicas were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, and (29)Si nuclear magnetic resonance spectroscopy. Spheres of ca. 0.5-1.0 microm were obtained in the case of hydrolysis of pure TEOS. The combination of ODS:TEOS ratio yielded systems combining spherical and lamellar patterns zones. Monitoring the particle growth, it seems that spherical particles grow around lamellar zones, these latter concentrating the organosilicon moieties. The degree of cross-linking of ODS moieties was shown to be dependent on the ODS addition time and stirring speed.
Preparation of ZrO II/nano-TiO II composite powder by sol-gel method

NASA Astrophysics Data System (ADS)

Baharvandi, H. R.; Mohammadi, E.; Abdizadeh, H.; Hadian, A. M.; Ehsani, N.

2007-07-01

The effects of concentration of TTIP, amount of distilled water, and calcination temperature on morphology and particle size distribution of ZrO II/nano-TiO II catalysts were investigated. Mixed ZrO II/nano-TiO II powders were prepared by a modified sol-gel method by varying the mole fraction of TTIP from 0.002 to 0.01, H IIO/TTIP fraction from 2 to 8, and various stirring time (2, 4, and 10 h). The prepared ZrO II/nano-TiO II powders have been characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and TG/DTA. Each oxide was calcined at the temperature between 110 and 1000°C. The results showed that the calcinations temperature has a pronounced effect on the phase formation and particle size of the calcined zirconium titanate (ZT) powders.
Preparation of highly hydrophobic cotton fabrics by modification with bifunctional silsesquioxanes in the sol-gel process

NASA Astrophysics Data System (ADS)

Przybylak, Marcin; Maciejewski, Hieronim; Dutkiewicz, Agnieszka

2016-11-01

The surface modification of cotton fabrics was carried out using two types of bifunctional fluorinated silsesquioxanes with different ratios of functional groups. The modification was performed either by one- or two-step process. Two methods, the sol-gel and the dip coating method were used in different configurations. The heat treatment and the washing process were applied after modification. The wettability of cotton fabric was evaluated by measuring water contact angles (WCA). Changes in the surface morphology were examined by scanning electron microscopy (SEM, SEM-LFD) and atomic force microscopy (AFM). Moreover, the modified fabrics were subjected to analysis of elemental composition of the applied coatings using SEM-EDS techniques. Highly hydrophobic textiles were obtained in all cases studied and one of the modifications resulted in imparting superhydrophobic properties. Most of impregnated textiles remained hydrophobic even after multiple washing process which shows that the studied modification is durable.
Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: bonding to titanium and scanning electron microscopy.

PubMed

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.
Layer-by-Layer Self-Assembling Gold Nanorods and Glucose Oxidase onto Carbon Nanotubes Functionalized Sol-Gel Matrix for an Amperometric Glucose Biosensor.

PubMed

Wu, Baoyan; Hou, Shihua; Miao, Zhiying; Zhang, Cong; Ji, Yanhong

2015-09-18

A novel amperometric glucose biosensor was fabricated by layer-by-layer self-assembly of gold nanorods (AuNRs) and glucose oxidase (GOD) onto single-walled carbon nanotubes (SWCNTs)-functionalized three-dimensional sol-gel matrix. A thiolated aqueous silica sol containing SWCNTs was first assembled on the surface of a cleaned Au electrode, and then the alternate self-assembly of AuNRs and GOD were repeated to assemble multilayer films of AuNRs-GOD onto SWCNTs-functionalized silica gel for optimizing the biosensor. Among the resulting glucose biosensors, the four layers of AuNRs-GOD-modified electrode showed the best performance. The sol-SWCNTs-(AuNRs- GOD)₄/Au biosensor exhibited a good linear range of 0.01-8 mM glucose, high sensitivity of 1.08 μA/mM, and fast amperometric response within 4 s. The good performance of the proposed glucose biosensor could be mainly attributed to the advantages of the three-dimensional sol-gel matrix and stereo self-assembly films, and the natural features of one-dimensional nanostructure SWCNTs and AuNRs. This study may provide a new facile way to fabricate the enzyme-based biosensor with high performance.
Preparation of mesoporous silica microparticles by sol-gel/emulsion route for protein release.

PubMed

Vlasenkova, Mariya I; Dolinina, Ekaterina S; Parfenyuk, Elena V

2018-04-06

Encapsulation of therapeutic proteins into particles from appropriate material can improve both stability and delivery of the drugs, and the obtained particles can serve as a platform for development of their new oral formulations. The main goal of this work was development of sol-gel/emulsion method for preparation of silica microcapsules capable of controlled release of encapsulated protein without loss of its native structure. For this purpose, the reported in literature direct sol-gel/W/O/W emulsion method of protein encapsulation was used with some modifications, because the original method did not allow to prepare silica microcapsules capable for protein release. The particles were synthesized using sodium silicate and tetraethoxysilane as silica precursors and different compositions of oil phase. In vitro kinetics of bovine serum albumin (BSA) release in buffer (pH 7.4) was studied by Fourier transform infrared (FTIR) and fluorescence spectrometry, respectively. Structural state of encapsulated BSA and after release was evaluated. It was found that the synthesis conditions influenced substantially the porous structure of the unloaded silica particles, release properties of the BSA-loaded silica particles and structural state of the encapsulated and released protein. The modified synthesis conditions made it possible to obtain the silica particles capable of controlled release of the protein during a week without loss of the protein native structure.
Evaluation of tetraethoxysilane (TEOS) sol-gel coatings, modified with green synthesized zinc oxide nanoparticles for combating microfouling.

PubMed

Krupa, A Nithya Deva; Vimala, R

2016-04-01

Green synthesis of zinc oxide nanoparticles (ZnO-NPs) is gaining importance as an eco-friendly alternative to conventional methods due to its enormous applications. The present work reports the synthesis of ZnO-NPs using the endosperm of Cocos nucifera (coconut water) and the bio-molecules responsible for nanoparticle formation have been identified. The synthesized nanoparticles were characterized using UV-Visible spectroscopy (UV-Vis), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Zeta potential measurement. The results obtained reveal that the synthesized nanoparticles are moderately stable with the size ranging from 20 to 80 nm. The bactericidal effect of the nanoparticles was proved by well diffusion assay and determination of minimum inhibitory concentration (MIC) against marine biofilm forming bacteria. Further the green synthesized ZnO-NPs were doped with TEOS sol-gels (TESGs) in order to assess their antimicrofouling capability. Different volumes of liquid sol-gels were coated on to 96-well microtitre plate and cured under various conditions. The optimum curing conditions were found to be temperature 60 °C, time 72 h and volume 200 μl. Antiadhesion test of the undoped (SG) and ZnO-NP doped TEOS sol-gel (ZNSG) coatings were evaluated using marine biofilm forming bacteria. ZNSG coatings exhibited highest biofilm inhibition (89.2%) represented by lowest OD value against Pseudomonasotitidis strain NV1. Copyright © 2016 Elsevier B.V. All rights reserved.
Electrochemical and spectroscopic characterization of surface sol-gel processes.

PubMed

Chen, Xiaohong; Wilson, George S

2004-09-28

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

PubMed

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.
Solid-phase assays for small molecule screening using sol-gel entrapped proteins.

PubMed

Lebert, Julie M; Forsberg, Erica M; Brennan, John D

2008-04-01

With compound libraries exceeding one million compounds, the ability to quickly and effectively screen these compounds against relevant pharmaceutical targets has become crucial. Solid-phase assays present several advantages over solution-based methods. For example, a higher degree of miniaturization can be achieved, functional- and affinity-based studies are possible, and a variety of detection methods can be used. Unfortunately, most protein immobilization methods are either too harsh or require recombinant proteins and thus are not amenable to delicate proteins such as kinases and membrane-bound receptors. Sol-gel encapsulation of proteins in an inorganic silica matrix has emerged as a novel solid-phase assay platform. In this minireview, we discuss the development of sol-gel derived protein microarrays and sol-gel based monolithic bioaffinity columns for the high-throughput screening of small molecule libraries and mixtures.

Molecular receptors in metal oxide sol-gel materials prepared via molecular imprinting

DOEpatents

Sasaki, Darryl Y.; Brinker, C. Jeffrey; Ashley, Carol S.; Daitch, Charles E.; Shea, Kenneth J.; Rush, Daniel J.

2000-01-01

A method is provided for molecularly imprinting the surface of a sol-gel material, by forming a solution comprised of a sol-gel material, a solvent, an imprinting molecule, and a functionalizing siloxane monomer of the form Si(OR).sub.3-n X.sub.n, wherein n is an integer between zero and three and X is a functional group capable of reacting with the imprinting molecule, evaporating the solvent, and removing the imprinting molecule to form the molecularly imprinted metal oxide sol-gel material. The use of metal oxide sol-gels allows the material porosity, pore size, density, surface area, hardness, electrostatic charge, polarity, optical density, and surface hydrophobicity to be tailored and be employed as sensors and in catalytic and separations operations.
Sol-gel process for the manufacture of high power switches

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

According to one embodiment, a photoconductive semiconductor switch includes a structure of nanopowder of a high band gap material, where the nanopowder is optically transparent, and where the nanopowder has a physical characteristic of formation from a sol-gel process. According to another embodiment, a method includes mixing a sol-gel precursor compound, a hydroxy benzene and an aldehyde in a solvent thereby creating a mixture, causing the mixture to gel thereby forming a wet gel, drying the wet gel to form a nanopowder, and applying a thermal treatment to form a SiC nanopowder.
Sol-gel optics for biomeasurements

NASA Astrophysics Data System (ADS)

Lechna-Marczynska, Monika I.; Podbielska, Halina; Ulatowska-Jarza, Agnieszka; Holowacz, Iwona; Andrzejewski, Damian

2001-10-01

Sol-gel technique is a method for producing of glass-like materials without involving a melting process. Organic compounds such as alcoholates of silicon, sodium or calcium can be used. The irregular non-crystalline network forms a gel structure where the metallic atoms are bonded to oxygen atoms. Low-temperature treatment turns this gel into an inorganic glass-like structure. There are numbers of applications of these materials that can be produced in various forms and shapes. Here, silica based sol-gel bulks and thin films optodes for biomedical applications will be presented.
Tantala-based sol-gel coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

PubMed

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

NASA Technical Reports Server (NTRS)

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.
A comparative synthesis and physicochemical characterizations of Ni/Al2O3-MgO nanocatalyst via sequential impregnation and sol-gel methods used for CO2 reforming of methane.

PubMed

Aghamohammadi, Sogand; Haghighi, Mohammad; Karimipour, Samira

2013-07-01

Carbon dioxide reforming of methane is an interesting route for synthesis gas production especially over nano-sized catalysts. The present research deals with catalyst development for dry reforming of methane with the aim of reaching the most stable catalyst. Effect of preparation method, one of the most significant variables, on the properties of the catalysts was taken in to account. The Ni/Al2O3-MgO catalysts were prepared via sol-gel and sequential impregnation methods and characterized with XRD, FESEM, EDAX, BET and FTIR techniques. The reforming reactions were carried out using different feed ratios, gas hourly space velocities (GHSV) and reaction temperatures to identify the influence of operational variables. FESEM images indicate uniform particle size distribution for the sample synthesized with sol-gel method. It has been found that the sol-gel method has the potential to improve catalyst desired properties especially metal surface enrichment resulting in catalytic performance enhancement. The highest yield of products was obtained at 850 degrees C for both of the catalysts. During the 10 h stability test, CH4 and CO2 conversions gained higher values in the case of sol-gel made catalyst compared to impregnated one.
Short communication: Evaluation of a sol-gel-based stainless steel surface modification to reduce fouling and biofilm formation during pasteurization of milk.

PubMed

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.
A novel l-leucine modified Sol-Gel-Carbon electrode for simultaneous electrochemical detection of homovanillic acid, dopamine and uric acid in neuroblastoma diagnosis.

PubMed

Khamlichi, Redouan El; Bouchta, Dounia; Anouar, El Hassane; Atia, Mounia Ben; Attar, Aisha; Choukairi, Mohamed; Tazi, Saloua; Ihssane, Raissouni; Faiza, Chaoukat; Khalid, Draoui; Khalid, Riffi Temsamani

2017-02-01

Neuroblastoma is a pediatric neuroblastic tumor arising in the sympathetic nervous crest cells. A high grade of Neuroblastoma is characterized by a high urinary excretion of homovanillic acid and dopamine. In this work l-leucine modified Sol-Gel-Carbon electrode was used for a sensitive voltammetric determination of homovanillic acid and dopamine in urine. The electrochemical response characteristics were investigated by cyclic and differential pulse voltammetry; the modified electrode has shown an increase in the effective area of up to 40%, a well-separated oxidation peaks and an excellent electrocatalytic activity. High sensitivity and selectivity in the linear range of 0,4-100μML -1 of homovanillic acid and 10-120μML -1 of dopamine were also obtained. Moreover, a sub-micromolar limit of detection of 0.1μM for homovanillic acid and 1.0μM for the dopamine was achieved. Indeed, high reproducibility with simple preparation and regeneration of the electrode surface made this electrode very suitable for the determination of homovanillic acid and dopamine in pharmaceutical and clinical preparations. The mechanism of homovanillic acid and the electrochemical oxidation at l-leucine modified Sol-Gel-Carbon electrode is described out the B3P86/6-31+G(d,p) level of theory as implemented in Gaussian software. Copyright © 2016 Elsevier B.V. All rights reserved.
Spectroscopic characterization of zirconium(IV) and hafniumf(IV) gallate phthalocyanines in monolithic silica gels obtained by sol gel method

NASA Astrophysics Data System (ADS)

Gerasymchuk, Y. S.; Chernii, V. Ya.; Tomachynski, L. A.; Legendziewicz, J.; Radzki, St.

2005-07-01

The Zr(IV) and Hf(IV) phthalocyanines, with gallate as axial ligand coordinated to the central metal atom of phthalocyanine, were incorporated in silica gels during sol-gel process with using tetraethyl orthosilicate (TEOS) as precursor. The obtained mixed inorganic-organic composites were transparent and homogeneous. The absorption and emission properties of these materials in comparison with the spectra of the Zr(IV) and Hf(IV) phthalocyanines in various solvents were investigated. The spectra were correlated with various stage of the sol-gel process. It was established that in the gels concurrence of the monomer and dimer form is different in sol, alco-, hydro- and xerogels. The intensive 700-725 nm fluorescence emission upon relatively long-wavelength excitation and unusually large (about 45 nm) Stokes shift in the Q region, suggest that Zr(IV) and Hf(IV) phthalocyanines could be considered as photosensitizers in the PDT method (photodynamic therapy).
Application of surface analytical methods in thin film analysis

NASA Astrophysics Data System (ADS)

Wen, Xingu

Self-assembly and the sol-gel process are two promising methods for the preparation of novel materials and thin films. In this research, these two methods were utilized to prepare two types of thin films: self-assembled monolayers of peptides on gold and SiO2 sol-gel thin films modified with Ru(II) complexes. The properties of the resulting thin films were investigated by several analytical techniques in order to explore their potential applications in biomaterials, chemical sensors, nonlinear optics and catalysis. Among the analytical techniques employed in the study, surface analytical techniques, such as X-ray photoelectron spectroscopy (XPS) and grazing angle reflection absorption Fourier transform infrared spectroscopy (RA-FTIR), are particularly useful in providing information regarding the compositions and structures of the thin films. In the preparation of peptide thin films, monodisperse peptides were self-assembled on gold substrate via the N-terminus-coupled lipoic acid. The film compositions were investigated by XPS and agreed well with the theoretical values. XPS results also revealed that the surface coverage of the self-assembled films was significantly larger than that of the physisorbed films and that the chemisorption between the peptides and gold surface was stable in solvent. Studies by angle dependent XPS (ADXPS) and grazing angle RA-FTIR indicated that the peptides were on average oriented at a small angle from the surface normal. By using a model of orientation distribution function, both the peptide tilt angle and film thickness can be well calculated. Ru(II) complex doped SiO2 sol-gel thin films were prepared by low temperature sol-gel process. The ability of XPS coupled with Ar + ion sputtering to provide both chemical and compositional depth profile information of these sol-gel films was evaluated. This technique, together with UV-VIS and electrochemical measurements, was used to investigate the stability of Ru complexes in the composite films. The stability of Ru complexes with respect to dopant leaching was dependent on the film microstructures. Three methods aiming to improve the dopant stability were also explored. In addition, the ion exchange properties of the composite films, upon exposure to various ions in aqueous solutions, were investigated by XPS, and the ion exchange mechanism was elucidated.
Rheology of polyaniline-dinonylnaphthalene disulfonic acid (DNNDSA) montmorillonite clay nanocomposites in the sol state: shear thinning versus pseudo-solid behavior.

PubMed

Garai, Ashesh; Nandi, Arun K

2008-04-01

The melt rheology of polyaniline (PANI)-dinonylnaphthalenedisulfonic acid (DNNDSA) gel nanocomposites (GNCs) with organically modified (modified with cetyl trimethylammonium bromide)-montmorillonite (om-MMT) clay has been studied for three different clay concentrations at the temperature range 120-160 degrees C. Field emission scanning electron microscopy (FE-SEM), wide angle X-ray scattering (WAXS), differential scanning calorimetry (DSC) and dc-conductivity data (approximately 10(-3) S/cm) indicate that the PANI-DNNDSA melt is in sol state and it is not de-doped at that condition. The WAXS data indicate that in GNC-1 sol clay tactoids are in exfoliated state but in the other sols they are in intercalated state. The zero shear viscosity (eta0), storage modulus (G') and loss modulus (G") increase than that of pure gel in the GNCs. The pure sol and the sols of gel nanocomposites (GNCs) exhibit Newtonian behavior for low shear rate (< 6 x 10(-3) s(-1)) and power law variation for the higher shear rate region. The characteristic time (A) increase with increasing clay concentration and the power law index (n) decreases with increase in clay concentration in the GNCs indicating increased shear thinning for the clay addition. Thus the sols of om-clay nanocomposites of PANI-DNNDSA system are easily processible. The storage modulus (G') of GNC sols are higher than that of pure PANI-DNNDSA sol, GNC1 sol shows a maximum of 733% increase in storage modulus and the percent increase decreases with increase in temperature. Exfoliated nature of clay tactoids has been attributed for the above dramatic increase of G'. The PANI-DNNDSA sol nanocomposites behave as a pseudo-solid at higher frequency where G' and loss modulus (G") show a crossover point in the frequency sweep experiment at a fixed temperature. The crossover frequency decreases with increase in clay concentration and it increases with increase in temperature for GNC sols. The pseudo-solid behavior has been explained from jamming or network formation of clay tactoids under shear. A probable explanation of the two apparently contradictory phenomena of shear thinning versus pseudo-solid behavior of the nanocomposite sols is discussed.
Sol-gel processed porous silica carriers for the controlled release of diclofenac diethylamine.

PubMed

Czarnobaj, Katarzyna; Czarnobaj, Joanna

2008-10-01

Silica xerogels doped with diclofenac diethylamine were prepared by the sol-gel method from a hydrolysed tetraethoxysilane (TEOS) solution containing diclofenac diethylamine. Two different catalysts, drying conditions and levels of water content were used to alter the microstructure of the silica xerogels. The aim of this study was to determine the rate of Diclofenac release from the silica xerogels. This in vitro study showed that the sol-gel method is useful for entrapping Diclofenac in the pores of xerogels. It also showed that, in vitro, Diclofenac is released from the silica xerogel, through the pores, by diffusion. Base-catalysed gels proved to be much more effective than acid-catalyzed gels. (c) 2008 Wiley Periodicals, Inc.
Polymer modified sol-gel materials for photochromic applications

NASA Astrophysics Data System (ADS)

Janik, Ryszard; Kucharski, Stanislaw

2006-08-01

The chromophoric materials were prepared by copolymerization of various methacrylic monomers. The incorporation of the chromophore groups was done by coupling reaction of diazonium salts of the sulfonamide such as: sulfomethazine or sulfisomidine). The copolymers having free OH groups were able to react with 3-triethoxypropyl isocyanate forming intermediates used to prepare hybrid transparent films by sol-gel technique. The films of both copolymers as well as of hybrid sol-gel structures showed photochromic properties via trans-cis isomerization of the diazo groups. The absorption maximum of the trans form was ca. 435-445 nm depending on chemical composition of the material. Illumination of the films with coherent laser beams (two-beam coupling) resulted in formation of diffraction grating. The diffraction efficiency reached 4-5 % and refractive index modulation was in the range up to 0.0032.
Detection of Hydrofluoric Acid by a SiO2 Sol-Gel Coating Fiber-Optic Probe Based on Reflection-Based Localized Surface Plasmon Resonance

PubMed Central

Chen, I-Cherng; Lin, Shiu-Shiung; Lin, Tsao-Jen; Du, Je-Kang

2011-01-01

A novel fiber-optic probe based on reflection-based localized surface plasmon resonance (LSPR) was developed to quantify the concentration of hydrofluoric acid (HF) in aqueous solutions. The LSPR sensor was constructed with a gold nanoparticle-modified PMMA fiber, integrated with a SiO2 sol-gel coating. This fiber-sensor was utilized to assess the relationship between HF concentration and SiO2 sol-gel layer etching reduction. The results demonstrated the LSPR sensor was capable of detecting HF-related erosion of hydrofluoric acid solutions of concentrations ranging from 1% to 5% using Relative RI Change Rates. The development of the LSPR sensor constitutes the basis of a detector with significant sensitivity for practical use in monitoring HF solution concentrations. PMID:22319388
Improvement of the titanium implant biological properties by coating with poly (ε-caprolactone)-based hybrid nanocomposites synthesized via sol-gel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando

When bioactive coatings are applied to medical implants by means of sol-gel dip coating technique, the biological proprieties of the implant surface can be modified to match the properties of the surrounding tissues. In this study organo-inorganic nanocomposites materials were synthesized via sol-gel. They consisted of an inorganic zirconium-based and silica-based matrix, in which a biodegradable polymer (the poly-ε-caprolactone, PCL) was incorporated in different weight percentages. The synthesized materials, in sol phase, were used to dip-coat a substrate of commercially pure titanium grade 4 (CP Ti gr. 4) in order to improve its biological properties. A microstructural analysis of themore » obtained films was carried out by scanning electron microscopy (SEM) and attenuated total reflectance (ATR) Fourier transform infrared spectroscopy (FT-IR). Biological proprieties of the coated substrates were investigated by means of in vitro tests.« less
Magneto-Sensitive Adsorbents Modified by Functional Nitrogen-Containing Groups

NASA Astrophysics Data System (ADS)

Melnyk, Inna V.; Gdula, Karolina; Dąbrowski, Andrzej; Zub, Yuriy L.

2016-02-01

In order to obtain amino-functionalized silica materials with magnetic core, one-step synthesis was carried out. Several materials, differ in number and structure of amino groups, were synthesized on the basis of sol-gel method. The synthesized materials were examined by several analytical techniques. The presence and content of amino groups were measured by using Diffuse Reflectance Infrared Fourier Transform (DRIFT) spectroscopy and acid-base titration, respectively. Specific surface areas were measured by nitrogen/adsorption desorption isotherms. It was proved that sol-gel approach leads to obtain materials with high content of amino groups built into their surfaces (in the range 1.6-2.7 mmol/g). As-obtained materials were tested as potential adsorbents for copper(II) ions. The received maximum adsorption capacities were in the range 0.4-0.7 mmol/g.
Influence of surfactants on the release behaviour and structural properties of sol-gel derived silica xerogels embedded with metronidazole.

PubMed

Czarnobaj, Katarzyna; Sawicki, Wiesław

2013-01-01

The aim of this study was to obtain stable and controlled release silica xerogels containing metronidazole (MT) prepared with surfactants with different charges: cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulphate (SDS) and hydroxypropyl cellulose (HPC), which could be the promising carrier materials used as the implantable drug delivery systems. The xerogels were prepared by the sol-gel method. The influence of various formulation precursors on porosity parameters and drug release were investigated. Addition of surfactants showed a promising result in controlling the MT release. Dissolution study revealed increased release of MT from silica modified SDS and CTAB, whereas the release of MT from silica modified HPC considerably decreased, in comparison with unmodified silica. The addition of surfactants showed slight changes in porosity parameters. All xerogels are characterized by a highly developed surface area (701-642 m(2) g(-1)) and mesoporous structure. The correlation between pore size obtained matrices and release rate of drug was also observed. Based on the presented results of this study, it may be stated that applied xerogel matrices: pure silica and surfactants-modified silica could be promising candidates for the formulation in local delivery systems.
Material for surface-enhanced Raman spectroscopy, and SER sensors and method for preparing same

NASA Technical Reports Server (NTRS)

Farquharson, Stuart (Inventor); Nelson, Chad (Inventor); Lee, Yuan-Hsiang (Inventor)

2003-01-01

Metal-doped sol-gel materials, suitable for use as sensors for surface-enhanced Raman spectroscopic analysis for trace chemical detection, are produced by effecting gelation and solvent removal of a doped sol-gel under mild temperature conditions. At least in certain instances reaction and drying will desirably be effected in an oxygen-starved environment. The metal of the sol-gel material functions, when irradiated, to produce a plasmon field for interaction with molecules of an analyte in contact therewith, increasing by orders of magnitude Raman photons that are generate by excitation radiation, and the method allows matching of the metal and metal particle size to a wavelength of light (or incident radiation, e.g., laser radiation) to generate surface plasmons. The porosity of the sol-gel material dramatically increases the surface area, and thereby the amount of metal exposed for analyte interaction. The sensors provided may be in the form of glass vials, fiber optics, multi-well micro-sample plates, etc., having surface coatings of the doped sol-gel material, to provide sampling systems for use in a Raman instrument.
Sol-gel derived sorbents

DOEpatents

Sigman, Michael E.; Dindal, Amy B.

2003-11-11

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

PubMed

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.

Layer-by-Layer Self-Assembling Gold Nanorods and Glucose Oxidase onto Carbon Nanotubes Functionalized Sol-Gel Matrix for an Amperometric Glucose Biosensor

PubMed Central

Wu, Baoyan; Hou, Shihua; Miao, Zhiying; Zhang, Cong; Ji, Yanhong

2015-01-01

A novel amperometric glucose biosensor was fabricated by layer-by-layer self-assembly of gold nanorods (AuNRs) and glucose oxidase (GOD) onto single-walled carbon nanotubes (SWCNTs)-functionalized three-dimensional sol-gel matrix. A thiolated aqueous silica sol containing SWCNTs was first assembled on the surface of a cleaned Au electrode, and then the alternate self-assembly of AuNRs and GOD were repeated to assemble multilayer films of AuNRs-GOD onto SWCNTs-functionalized silica gel for optimizing the biosensor. Among the resulting glucose biosensors, the four layers of AuNRs-GOD-modified electrode showed the best performance. The sol-SWCNTs-(AuNRs-GOD)4/Au biosensor exhibited a good linear range of 0.01–8 mM glucose, high sensitivity of 1.08 μA/mM, and fast amperometric response within 4 s. The good performance of the proposed glucose biosensor could be mainly attributed to the advantages of the three-dimensional sol-gel matrix and stereo self-assembly films, and the natural features of one-dimensional nanostructure SWCNTs and AuNRs. This study may provide a new facile way to fabricate the enzyme-based biosensor with high performance. PMID:28347080
Preparation and Optoelectrical Properties of p-CuO/n-Si Heterojunction by a Simple Sol-Gel Method

NASA Astrophysics Data System (ADS)

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

PubMed Central

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
Preparation of long alumina fibers by sol-gel method using tartaric acid

NASA Astrophysics Data System (ADS)

Tan, Hong-Bin

2011-12-01

Long alumina fibers were prepared by sol-gel method. The spinning sol was obtained by mixing aluminum nitrate, tartaric acid, and polyvinylpyrrolidone with a mass ratio of 10:3:1.5. Thermogravimetry-differential scanning calorimetry (TG-DSC), Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD), and scanning electron microscopy (SEM) were used to characterize the properties of the gel and ceramic fibers. A little of α-Al2O3 phase is observed in the alumina precursor gel fibers sintered at 1273 K. The fibers with a uniform diameter can be obtained when sintered at 1473 K, and its main phase is also indentified as α-Al2O3.
Evaluation of sol-gel based magnetic 45S5 bioglass and bioglass-ceramics containing iron oxide.

PubMed

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.
Phospho-silicate and silicate layers modified by hydroxyapatite particles

NASA Astrophysics Data System (ADS)

Rokita, M.; Brożek, A.; Handke, M.

2005-06-01

Common used metal materials do not ensure good connection between an implant and biological neighbourhood. Covering implants by thin silicate or phosphate layers enable to improve biological properties of implants and create conditions for producing the non-concrete bonding between the implant and tissue. The project includes preparing silicate sols of different concentrations and proper (powder) fraction of synthetic as well as natural ox hydroxyapatite, depositing the sol mixed with hydroxyapatite onto the base material (metal, ceramic carbon) and heat treatment. Our work includes also preparation of phospho-silicate layers deposited onto different base materials using sol-gel method. Deposited sols were prepared regarding composition, concentration and layer heat treatment conditions. The prepared layers are examined to determine their phase composition (XRD, IR spectroscopy methods), density and continuity (scanning microscopy with EDX methods). Biological activity of layers was evaluated by means of estimation of their corrosive resistance in synthetic body fluids ('in vitro' method) and of bone cells growth on the layers surface. Introducing hydroxyapatite to the layer sol should improve connection between tissue and implant as well as limit the disadvantageous, corrosive influence of implant material (metal) on the tissue.
Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: dissolution behaviour and biological properties after crystallisation.

PubMed

Tredwin, Christopher J; Young, Anne M; Abou Neel, Ensanya A; Georgiou, George; Knowles, Jonathan C

2014-01-01

Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) were synthesised by the sol-gel method as possible implant coating or bone-grafting materials. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride were incorporated for the preparation of the FHA and FA sol-gels. After heating and powdering the sol-gels, dissolution behaviour was assessed using ion chromatography to measure Ca(2+) and PO4 (3-) ion release. Biological behaviour was assessed using cellular proliferation with human osteosarcoma cells and alamarBlue™ assay. Statistical analysis was performed with a two way analysis of variance and post hoc testing with a Bonferroni correction. Increasing fluoride substitution into an apatite structure decreased the dissolution rate. Increasing the firing temperature of the HA, FHA and FA sol-gels up to 1,000 °C decreased the dissolution rate. There was significantly higher cellular proliferation on highly substituted FHA and FA than on HA or Titanium. The properties of an implant coating or bone grafting material can be tailored to meet specific requirements by altering the amount of fluoride that is incorporated into the original apatite structure. The dissolution behaviour can further be altered by the temperature at which the sol-gel is fired.
Electrical and optical properties of sol-gel derived La modified PbTiO 3 thin films

NASA Astrophysics Data System (ADS)

Chopra, Sonalee; Sharma, Seema; Goel, T. C.; Mendiratta, R. G.

2004-09-01

Lanthanum modified lead titanate (Pb 1- xLa xTi 1- x/4 O 3) PLT x ( x=0.08 i.e. PLT8) sol-gel derived thin films have been prepared on indium tin oxide (ITO) coated glass and quartz substrates using lead acetate trihydrate, lanthanum acetate hydrate and titanium isopropoxide as precursors along with 2-methoxyethanol as solvent and acetic acid as catalyst by spin coating method. The microstructure and surface morphology of the films annealed at 650 °C have been studied by X-ray diffraction technique and atomic force microscope (AFM). XRD has shown a single phase with tetragonal structure and AFM images have confirmed a smooth and crack-free surface with low surface roughness. The dependence of leakage current on applied voltage show ohmic behavior at low field region with a space charge conduction mechanism at high fields. The wavelength dispersion curve of thin films obtained from the transmission spectrum of thin films show that the films have high optical transparency in the visible region.
Photocatalytic degradation of methylene blue dye by zinc oxide nanoparticles obtained from precipitation and sol-gel methods.

PubMed

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).
Macroporous ceramics by colloidal templating

NASA Astrophysics Data System (ADS)

Subramaniam, G.; Pine, David J.

2000-04-01

We describe a novel method of fabricating macroporous ceramics employing colloidal dispersion of ultrafine ceramic particles with latex particles as the templates. The colloidal particles form a particulate gel on drying and fill the voids of the ordered latex templates. Subsequent removal of the template by calcination results in the formation of an ordered macroporous ceramic. The process has significant advantages over the traditional sol-gel process employing alkoxide precursors. Most importantly, the much lower shrinkage compared to the sol-gel process enabled us to produce larger pieces of the sample. The larger shrinkage involved in the sol-gel process often results in small and fragile pieces of the macroporous material which has to be subsequently heat treated to induce crystallization. The ability to choose crystalline colloidal particles in our method obviates the need for heat treatment to achieve crystallinity. We have synthesized a variety of materials such as macroporous silica, titania, alumina and recently have also extended the approach to macroporous silicon which is not amenable to the sol-gel process.
Sol-gel deposition of buffer layers on biaxially textured metal substances

DOEpatents

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.
Site-specific protein immobilization in a microfluidic chip channel via an IEF-gelation process.

PubMed

Shi, Mianhong; Peng, Youyuan; Yu, Shaoning; Liu, Baohong; Kong, Jilie

2007-05-01

A novel strategy for site-specific protein immobilization via combining chip IEF with low-temperature sol-gel technology, called IEF-GEL here, in the channel of a modified poly(methyl methacrylate) (PMMA) microfluidic chip is proposed in this work. The IEF-GEL process involves firstly IEF for homogeneously dissolved protein in PBS containing alumina sol and carrier ampholyte with prearranged pH gradient, and then gelation locally for protein encapsulation. The process and feasibility of proposed IEF-GEL were investigated by EOF measurements, fluorescence microscopic photography, Raman spectrum and further demonstrated by glucose oxidase (GOx) reactors integrated with end-column electrochemical detection. Site-controllable immobilization of protein was realized in a 30 mm long microfluidic chip channel by the strategy to create a approximately 1.7 mm concentrated FITC-BSA band, which leads to great improvement of the elute peak shape, accomplished with remarkably increased sensitivity, approximately 20 times higher than that without IEF-GEL treatment to GOx reactors. The kinetic response of GOx after IEF-GEL treatment was also investigated. The proposed system holds the advantages of IEF and low-temperature sol-gel technologies, i.e. concentrating the protein to be focused and retaining the biological activity for the gel-embedded protein, thus realizes site-specific immobilization of low-concentration protein at nL volume level.
STUDY ON SYNTHESIS AND EVOLUTION OF NANOCRYSTALLINE Mg4Ta2O9 BY AQUEOUS SOL-GEL PROCESS

NASA Astrophysics Data System (ADS)

Wu, H. T.; Yang, C. H.; Wu, W. B.; Yue, Y. L.

2012-06-01

Nanosized and highly reactive Mg4Ta2O9 were successfully synthesized by aqueous sol-gel method compared with conventional solid-state method. Ta-Mg-citric acid solution was first formed and then evaporated resulting in a dry gel for calcination in the temperature ranging from 600°C to 800°C for crystallization in oxygen atmosphere. The crystallization process from the gel to crystalline Mg4Ta2O9 was identified by thermal analysis and phase evolution of powders was studied using X-ray diffraction (XRD) technique during calcinations. Particle size and morphology were examined by transmission electron microscopy (TEM) and high resolution scanning electron microscopy (HR-SEM). The results revealed that sol-gel process showed great advantages over conventional solid-state method and Mg4Ta2O9 nanopowders with the size of 20-30 nm were obtained at 800°C.
Environmentally benign sol-gel antifouling and foul-releasing coatings.

PubMed

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

DOEpatents

Bartl, Michael H.; Barhoum, Moussa; Riassetto, David

2016-08-02

A versatile and rapid sol-gel technique for the fabrication of high quality one-dimensional photonic bandgap materials. For example, silica/titania multi-layer materials may be fabricated by a sol-gel chemistry route combined with dip-coating onto planar or curved substrate. A shock-cooling step immediately following the thin film heat-treatment process is introduced. This step was found important in the prevention of film crack formation--especially in silica/titania alternating stack materials with a high number of layers. The versatility of this sol-gel method is demonstrated by the fabrication of various Bragg stack-type materials with fine-tuned optical properties by tailoring the number and sequence of alternating layers, the film thickness and the effective refractive index of the deposited thin films. Measured optical properties show good agreement with theoretical simulations confirming the high quality of these sol-gel fabricated optical materials.
Preparation of hydrophobic organic aeorgels

DOEpatents

Baumann, Theodore F.; Satcher, Jr., Joe H.; Gash, Alexander E.

2007-11-06

Synthetic methods for the preparation of hydrophobic organics aerogels. One method involves the sol-gel polymerization of 1,3-dimethoxybenzene or 1,3,5-trimethoxybenzene with formaldehyde in non-aqueous solvents. Using a procedure analogous to the preparation of resorcinol-formaldehyde (RF) aerogels, this approach generates wet gels that can be dried using either supercritical solvent extraction to generate the new organic aerogels or air dried to produce an xerogel. Other methods involve the sol-gel polymerization of 1,3,5 trihydroxy benzene (phloroglucinol) or 1,3 dihydroxy benzene (resorcinol) and various aldehydes in non-aqueous solvents. These methods use a procedure analogous to the one-step base and two-step base/acid catalyzed polycondensation of phloroglucinol and formaldehyde, but the base catalyst used is triethylamine. These methods can be applied to a variety of other sol-gel precursors and solvent systems. These hydrophobic organics aerogels have numerous application potentials in the field of material absorbers and water-proof insulation.
Preparation of hydrophobic organic aeorgels

DOEpatents

Baumann, Theodore F.; Satcher, Jr., Joe H.; Gash, Alexander E.

2004-10-19

Synthetic methods for the preparation of hydrophobic organics aerogels. One method involves the sol-gel polymerization of 1,3-dimethoxybenzene or 1,3,5-trimethoxybenzene with formaldehyde in non-aqueous solvents. Using a procedure analogous to the preparation of resorcinol-formaldehyde (RF) aerogels, this approach generates wet gels that can be dried using either supercritical solvent extraction to generate the new organic aerogels or air dried to produce an xerogel. Other methods involve the sol-gel polymerization of 1,3,5 trihydroxy benzene (phloroglucinol) or 1,3 dihydroxy benzene (resorcinol) and various aldehydes in non-aqueous solvents. These methods use a procedure analogous to the one-step base and two-step base/acid catalyzed polycondensation of phloroglucinol and formaldehyde, but the base catalyst used is triethylamine. These methods can be applied to a variety of other sol-gel precursors and solvent systems. These hydrophobic organics aerogels have numerous application potentials in the field of material absorbers and water-proof insulation.
Sol-Gel Matrices For Direct Colorimetric Detection Of Analytes

DOEpatents

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

2002-11-26

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.
Sol-gel matrices for direct colorimetric detection of analytes

DOEpatents

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.
Preparation and optical properties of iron-modified titanium dioxide obtained by sol-gel method

NASA Astrophysics Data System (ADS)

Hreniak, Agnieszka; Gryzło, Katarzyna; Boharewicz, Bartosz; Sikora, Andrzej; Chmielowiec, Jacek; Iwan, Agnieszka

2015-08-01

In this paper twelve TiO2:Fe powders prepared by sol-gel method were analyzed being into consideration the kind of iron compound applied. As a precursor titanium (IV) isopropoxide (TIPO) was used, while as source of iron Fe(NO3)3 or FeCl3 were tested. Fe doped TiO2 was obtained using two methods of synthesis, where different amount of iron was added (1, 5 or 10% w/w). The size of obtained TiO2:Fe particles depends on the iron compound applied and was found in the range 80-300 nm as it was confirmed by SEM technique. TiO2:Fe particles were additionally investigated by dynamic light scattering (DLS) method. Additionally, for the TiO2:Fe particles UV-vis absorption and the zeta potential were analyzed. Selected powders were additionally investigated by magnetic force microscopy (MFM) and X-ray diffraction techniques. Photocatalytic ability of Fe doped TiO2 powders was evaluated by means of cholesteryl hemisuccinate (CHOL) degradation experiment conducted under the 30 min irradiation of simulated solar light.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 slidesmore » 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.« less
Titanium (IV) sol-gel chemistry in varied gravity environments

NASA Astrophysics Data System (ADS)

Hales, Matthew; Martens, Wayde; Steinberg, Theodore

Sol-gel synthesis in reduced gravity is a relatively new topic in the literature and further inves-tigation is essential to realise its potential and application to other sol-gel systems. The sol-gel technique has been successfully applied to the synthesis of silica systems of varying porosity for many diverse applications [1-5]. It is proposed that current methods for the synthesis of silica sol-gels in reduced gravity may be applied to titanium sol-gel processing in order to enhance desirable physical and chemical characteristics of the final materials. The physical and chemical formation mechanisms for titanium alkoxide based sol-gels, to date, is not fully understood. However, various authors [6-9] have described potential methods to control the hydrolysis and condensation reactions of titanium alkoxides through the use of chemical inhibitors. A preliminary study of the reaction kinetics of titanium alkoxide sol-gel reaction in normal gravity was undertaken in order to determine reactant mixtures suitable for further testing under varied gravity conditions of limited duration. Through the use of 1H Nuclear Magnetic Resonance spectroscopy (NMR) for structural analysis of precursor materials, Ultra-Violet-Visible spectroscopy (UV-VIS) and viscosity measurements, it was demonstrated that not only could the rate of the chemical reaction could be controlled, but directed linear chain growth within the resulting gel structure was achievable through the use of increased inhibitor concentrations. Two unique test systems have been fabricated to study the effects of varied gravity (reduced, normal, high) on the formation of titanium sol-gels. Whilst the first system is to be used in conjunction with the recently commissioned drop tower facility at Queensland University of Technology in Brisbane, Australia to produce reduced gravity conditions. The second system is a centrifuge capable of providing high gravity environments of up to 70 G's for extended periods of time. The test systems and experimental results obtained will be presented. 1. Okubo, T., Tsuchida, A., Okuda, T., Fujitsuna, K., Ishikawa, M., Morita, T., Tada, T. , Kinetic Analyses of Colloidal Crystallization in Microgravity -Aircraft Experiments. . Colloids and Surfaces A: Physicochemical and Engineering Aspects, 1999. 153: p. 515-524. 2. Okubo, T., Tsuchida, A., Kobayashi, K., Kuno, A., Morita, T., Fujishima, M., Kohno, Y., Kinetic Study of the Formation Reaction of Colloidal Silica Spheres in Microgravity Using Aircraft. Colloid Polymer Science, 1999. 277(5): p. 474-478. 3. Pienaar, C.L., Chiffoleau, G. J. A., Follens, L. R. A., Martens, J. A., Kirschhock, C. E. A., Steinberg, T. A., Effect of Gravity on the Gelation of Silica Sols. Chem. Mater., 2007. 19(4): p. 660-664. 4. Smith, D.D., et al., Effect of Microgravity on the Growth of Silica Nanostructures. Langmuir, 2000. 16(26): p. 10055-10060. 5. Zhang, X., Johnson, D.P., Manerbino, A.R., Moore, J.J., Schowengerdt, F. , Recent Mi-crogravity Results in the Synthesis of Porous Materials. AIP Conference Proceedings (Space Technology and Applications International Forum-1999, Pt. 1), 1999. 458: p. 88-93. 6. Dunbar, P.B., Bendzko, N.J.,, 1H and 13C NMR observation of the reaction of acetic acid with titanium isopropoxide. Materials Chemistry and Physics, 1999. 59: p. 26-35. 7. Krunks, M., Oja, I., T˜nsuaadu, K., Es-Souni, M., Gruselle, M., Niinistü,. L, Thermoanalytical study of acetylacetonate-modified titanium (iv) isopropoxide as precursor for TiO2 films. Journal of Thermal Analysis and Calorimetry, 2005: p. 483-488. 8. Moran, P.D., Bowmaker, G. A., Cooney, R. P., Vibrational Spectra and Molecular Associa-tion of Titanium Tetraisopropoxide. Inorg. Chem., 1998. 37(1): p. 2741-2748. 9. Somogyvari, A., Serpone, N.,, Evidence for five-coordination in titanium(1V) complexes. A nuclear magnetic resonance investigation. Canadian Journal of Chemistry, 1977. 56: p. 316-319.
Enhancement of Ce/Cr Codopant Solubility and Chemical Homogeneity in TiO2 Nanoparticles through Sol-Gel versus Pechini Syntheses.

PubMed

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.
Robust aptamer sol-gel solid phase microextraction of very polar adenosine from human plasma.

PubMed

Mu, Li; Hu, Xiangang; Wen, Jianping; Zhou, Qixing

2013-03-01

Conventional solid phase microextraction (SPME) has a limited capacity to extract very polar analytes, such as adenosine. To solve this problem, aptamer conjugating sol-gel methodology was coupled with an SPME fiber. According to the authors' knowledge, this is the first reported use of aptamer SPME. The fiber of aptamer sol-gel SPME with a mesoporous structure has high porosity, large surface area, and small water contact angle. Rather than employing direct entrapment, covalent immobilization was the dominant method of aptamer loading in sol-gel. Aptamer sol-gel fiber captured a specified analyte from among the analog molecules, thereby, exhibiting an excellent selective property. Compared with commercial SPME fibers, this aptamer fiber was suitable for extracting adenosine, presenting an extraction efficiency higher than 20-fold. The values of repeatability and reproducibility expressed by relative standard deviation were low (9.4%). Interestingly, the sol-gel network enhanced the resistance of aptamer SPME to both nuclease and nonspecific proteins. Furthermore, the aptamer sol-gel fiber was applied in human plasma with LOQ 1.5 μg/L, which is an acceptable level. This fiber also demonstrates durability and regeneration over 20-cycles without significant loss of efficiency. Given the various targets (from metal ions to biomacromolecules and cells) of aptamers, this methodology will extend the multi-domain applications of SPME. Copyright © 2013 Elsevier B.V. All rights reserved.
Preparation and characterization of conductive and transparent ruthenium dioxide sol-gel films.

PubMed

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.
Study on the Effect of Various Sol-Gel Concentration to the Electrical, Structural and Optical Properties of the Nanostructured Titanium Dioxide Thin Films

NASA Astrophysics Data System (ADS)

Ahmad, M. K.; Rusop, M.

2009-06-01

Nanostructured Titanium Dioxide (TiO2) thin film with various sol-gel concentration has been successfully prepared using sol-gel spin coating method. The sol-gel concentration of nanostructured TiO2 thin films are varied at 0.1 M, 0.2 M, 0.3 M and 0.4 M, respectively. The effects of different sol-gel concentration of nanostructured TiO2 thin film structural, electrical and optical properties have been studied. The effects of these properties were characterized using X-Ray Diffractometer (XRD), 2-point probe I-V measurement and UV-Vis-NIR Spectrophotometer. For electrical properties, 0.2 M of sol-gel concentration gives the lowest sheet resistance among other concentrated sol-gels. As for structural properties, 0.1 M of concentration gives very weak peak, and continues stronger as in comes to 0.2 M until 0.4 M. It is due to amount of solute (i.e Titanium Isopropoxide) increases in the solution and therefore the intensity of (101) planes become higher. The optical transmission in the visible region (450-1000 nm) for 0.1 M and 0.2 M are the highest (>80%), indicating that the films are transparent in the visible region. The transmission decreases sharply near the ultraviolet region due to the band gap absorption.
Synthesis and adsorption of silica gel modified 3-aminopropyltriethoxysilane (APTS) from corn cobs against Cu(II) in water

NASA Astrophysics Data System (ADS)

Purwanto, Agung; Yusmaniar, Ferdiani, Fatmawati; Damayanti, Rachma

2017-03-01

Silica gel modified APTS was synthesized from silica gel which was obtained from corn cobs via sol-gel process. Silica gel was synthesized from corn cobs and then chemically modified with silane coupling agent which has an amine group (NH2). This process resulting modified silica gel 3-aminopropyltriethoxysilane (APTS). Characterization of silica gel modified APTS by SEM-EDX showed that the size of the particles of silica gel modified APTS was 20µm with mass percentage of individual elements were nitrogen (N) 15.56%, silicon (Si) 50.69% and oxygen (O) 33.75%. In addition, silica gel modified APTS also showed absorption bands of functional groups silanol (Si-OH), siloxane (Si-O-Si), and an aliphatic chain (-CH2-), as well as amine (NH2) from FTIR spectra. Based on the characterization of XRD, silica gel 2θ of 21.094° and 21.32° respectively. It indicated that both material were amorphous. Determination of optimum pH and contact time on adsorption of silica gel 3-aminopropyltriethoxysilane (APTS) against Cu(II). The optimum pH and contact time was measured by using AAS. Optimum pH of adsorption silica gel modified APTS against metal Cu(II) could be obtained at pH 6 while optimum contact time was at 30 minutes, with the process of adsorption metal Cu(II) occured based on the model Freundlich isotherm.
A review of photocatalysts prepared by sol-gel method for VOCs removal.

PubMed

Tseng, Ting Ke; Lin, Yi Shing; Chen, Yi Ju; Chu, Hsin

2010-05-28

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.
The thickness correction of sol-gel coating using ion-beam etching in the preparation of antireflection coating

NASA Astrophysics Data System (ADS)

Dong, Siyu; Xie, Lingyun; He, Tao; Jiao, Hongfei; Bao, Ganghua; Zhang, Jinlong; Wang, Zhanshan; Cheng, Xinbin

2017-09-01

For the sol-gel method, it is still challenging to achieve excellent spectral performance when preparing antireflection (AR) coating by this way. The difficulty lies in controlling the film thickness accurately. To correct the thickness error of sol-gel coating, a hybrid approach that combined conventional sol-gel process with ion-beam etching technology was proposed in this work. The etching rate was carefully adjusted and calibrated to a relatively low value for removing the redundant material. Using atomic force microscope (AFM), it has been demonstrated that film surface morphology will not be changed in this process. After correcting the thickness error, an AR coating working at 1064 nm was prepared with transmittance higher than 99.5%.
Investigation on the path process of M doped ZnO (M = Gd, Mg) via the sol-gel method from dried gel to stable nanostructure powder

NASA Astrophysics Data System (ADS)

Suharno; Soegijono, B.; Budiawanti, S.; Fadillah, L.

2017-04-01

Doping is one of the effective methods to modify the physical properties of ZnO material in order to extend its applications. An investigation on Zn1-xMxO (M = Gd, Mg and x = 0.00, 0.03) nanopowders that have been synthesized by sol-gel method and sintered at 600 °C for 2 hours was reported. The decomposition process of the dried gel system was investigated by thermal gravimetric analysis (TGA) and the nanopowders with different heating temperature were studied using FT-IR spectroscopy. The crystal structure of the nanopowders after sintering at 600 °C was obtained using X-ray diffraction (XRD). The TGA curves of the samples showed the various weight loss regions corresponding to the removal of starting materials and no weight loss was observed in the temperature range of 300 to 800 °C which corresponded to the phase-crystallization step. The FTIR spectra showed that ZnO band was assigned to the stretching frequency at 669 cm-1 while Gd/Mg doped ZnO was at 668 cm-1 and 666 cm-1. From the XRD studies, the crystal structure of the samples indicated single phase ZnO crystalline and confirmed hexagonal wurtzite structure (space group of P63mc).
The impact of thermal treatment conditions on the formation of crystalline structure of Ce-Zr-oxide composite obtained by a modified sol-gel technique

NASA Astrophysics Data System (ADS)

Trusova, E. A.; Khrushcheva, A. A.; Shvorneva, L. I.

2012-02-01

We present the results of the modified sol-gel synthesis of ultrafine ceria-doped zirconia powder for medical ceramics (implants) and catalytic purposes (environmental catalysis and petrochemistry). Special attention has been paid to study the influence of thermal treatment on crystallite size and crystal lattice parameters of zirconia doped by ceria. Zirconyl chloride and cerium nitrate were used as metal sources, and tetraethylammonium hydroxide (TEAH) was used as a sol stabilizer at molar ratio TEAH/Σ (Ce + Zr) equal to 0.5. It was proved that zirconium and cerium practically completely were included in the obtained solid solutions, since their phase compositions fully correspond to initial quantities of cerium and zirconium in reaction mixture. It was shown that average crystallite size of the obtained powders did not exceed 75Å, and the powders were resistant to thermal treatment. It was established that stabilization of the crystal lattice of ZrO2 occurs through formation of a cubic ceria sublattice.
Sol-gel synthesis of mesoporous CaCu{sub 3}Ti{sub 4}O{sub 12} thin films and their gas sensing response

DOE Office of Scientific and Technical Information (OSTI.GOV)

Parra, R., E-mail: rparra@fi.mdp.edu.a; Savu, R.; Ramajo, L.A.

2010-06-15

A new sol-gel synthesis procedure of stable calcium copper titanate (CaCu{sub 3}Ti{sub 4}O{sub 12}-CCTO) precursor sols for the fabrication of porous films was developed. The composition of the sol was selected in order to avoid the precipitation of undesired phases; ethanol was used as solvent, acetic acid as modifier and poly(ethyleneglycol) as a linker agent. Films deposited by spin-coating onto oxidized silicon substrates were annealed at 700 {sup o}C. The main phase present in the samples, as detected by X-ray diffraction and Raman spectroscopy, was CaCu{sub 3}Ti{sub 4}O{sub 12}. Scanning electron microscopy analysis showed that mesoporous structures, with thicknesses betweenmore » 200 and 400 nm, were developed as a result of the processing conditions. The films were tested regarding their sensibility towards oxygen and nitrogen at atmospheric pressure using working temperatures from 200 to 290 {sup o}C. The samples exhibited n-type conductivity, high sensitivity and short response times. These characteristics indicate that CCTO mesoporous structures obtained by sol-gel are suitable for application in gas sensing. - Graphical abstract: A sol-gel synthesis procedure toward stable CaCu{sub 3}Ti{sub 4}O{sub 12}-precursor sols avoiding the precipitation of undesired compounds is proposed. Films deposited by spin-coating onto oxidized silicon substrates were annealed at 700 {sup o}C. The thickness varied between 200 and 400 nm depending on sol composition. The films, tested as gas sensors for O{sub 2}, showed n-type conductivity, good sensitivity and short response times.« less
Systematic study of inorganic functionalization of ZnO nanorods by Sol-Gel method

NASA Astrophysics Data System (ADS)

Gamarra, J. K.; Solano, C.; Piñeres, I.; Gómez, H.; Mass, J.; Montenegro, D. N.

2017-01-01

A systematic study of the inorganic surface functionalization of ZnO nanostructures by sol-gel method is shown. We have emphasized on the evolution of morphology properties of samples as a function of functionalization parameters. In addition, the effects on thermal stability and some optical properties of samples are discussed.
Infiltration of methylammonium metal halide in highly porous membranes using sol-gel-derived coating method

NASA Astrophysics Data System (ADS)

Kwon, Seung Lee; Jin, Young Un; Kim, Byeong Jo; Han, Man Hyung; Han, Gill Sang; Shin, Seunghak; Lee, Sangwook; Jung, Hyun Suk

2017-09-01

Organic-inorganic halide perovskites (OIHPs) has emerged as promising optoelectronic materials for solar cells and light-emitting diodes. OIHPs are usually coated on a flat surface or mesoporous scaffold for the applications. Herein, we report a facile sol-gel-derived solution route for coating methylammonium lead iodide (MAPbI3) perovskite layers onto various nanoporous structures. We found that lead-acetate solution has superior infiltration property onto surface of oxide membranes, and it can easily be converted to MAPbI3 by sequential transform to PbO, PbI2, and finally MAPbI3. Excellent pore-filling and full coverage of the nanostructures with the final MAPbI3 perovskite material are demonstrated via this sol-gel-derived solution route, using mesoporous TiO2, TiO2 nanorods, and high-aspect ratio nanopores in anodic aluminum oxide membranes. Given that this sol-gel-based method fills nanopores better than other conventional coating methods for OIHPs, this method may find wide applications in nanostructured OIHPs-based optoelectronic systems.
Room temperature ferromagnetism of tin oxide nanocrystal based on synthesis methods

NASA Astrophysics Data System (ADS)

Sakthiraj, K.; Hema, M.; Balachandrakumar, K.

2016-04-01

The experimental conditions used in the preparation of nanocrystalline oxide materials play an important role in the room temperature ferromagnetism of the product. In the present work, a comparison was made between sol-gel, microwave assisted sol-gel and hydrothermal methods for preparing tin oxide nanocrystal. X-ray diffraction analysis indicates the formation of tetragonal rutile phase structure for all the samples. The crystallite size was estimated from the HRTEM images and it is around 6-12 nm. Using optical absorbance measurement, the band gap energy value of the samples has been calculated. It reveals the existence of quantum confinement effect in all the prepared samples. Photoluminescence (PL) spectra confirms that the luminescence process originates from the structural defects such as oxygen vacancies present in the samples. Room temperature hysteresis loop was clearly observed in M-H curve of all the samples. But the sol-gel derived sample shows the higher values of saturation magnetization (Ms) and remanence (Mr) than other two samples. This study reveals that the sol-gel method is superior to the other two methods for producing room temperature ferromagnetism in tin oxide nanocrystal.
A Sol-gel Integrated Dual-readout Microarray Platform for Quantification and Identification of Prostate-specific Antigen.

PubMed

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.
A Urea Biosensor from Stacked Sol-Gel Films with Immobilized Nile Blue Chromoionophore and Urease Enzyme

PubMed Central

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 optical biosensor constructed from three layers of sol-gel films that contained urease demonstrated a much wider linear response range of up to 100 mM urea when compared with biosensors that constructed from 1-2 layers of films. Analysis of urea in urine samples with this optical urea biosensor yielded results similar to that determined by a spectrophotometric method using the reagent p-dimethylaminobenzaldehyde (R2 = 0.982, n = 6). The average recovery of urea from urine samples using this urea biosensor is approximately 103%.
Sol gel method for synthesis of semiconducting ferrite and the study of FTIR, DTA, SEM and CV

NASA Astrophysics Data System (ADS)

Alva, Sagir; Hua, Tang Ing; Kalmar Nizar, Umar; Wahyudi, Haris; Sundari, Rita

2018-03-01

In this study, a sol gel method using citric acid as anionic surfactant is used for synthesis of magnesium ferrite. Calcinations of magnesium ferrite at temperature (300°C, 600°C and 800°C) have been conducted after sol gel process. Characterization study of the prepared magnesium ferrite related to calcinations using Fourier transform infrared spectrometry (FTIR), Differential thermogravic analysis (DTA), and Scanning electron microscope (SEM) has been discussed. The study of Cyclic voltammetry (CV) of the prepared magnesium ferrite has been examined to assay the semiconducting behavior of magnesium ferrite in relation to its electrochemical behavior.
Neutron detector using sol-gel absorber

DOEpatents

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.
Sol-Gel Synthesis and Crystallization of Magnesium and Calcium Rich Silicate Dust Analogs

NASA Astrophysics Data System (ADS)

Gillot, J.; Roskosz, M.; Depecker, C.; Roussel, P.; Leroux, H.

2009-03-01

A new sol-gel method optimized to synthesize amorphous and porous silicate dust analogs is proposed. The crystallization of such analogs is metastable and polyphasic. Their high reactivity is probably due to high surface/volume ratio.

Novel sol-gel organic-inorganic hybrid materials for drug delivery.

PubMed

Catauro, Michelina; Verardi, Duilio; Melisi, Daniela; Belotti, Federico; Mustarelli, Piercarlo

2010-01-01

The aim of the present study was to synthetize and characterize novel sol-gel organic-inorganic hybrid materials to be used for controlled drug delivery application. Organic-inorganic hybrid class I materials based on poly(epsilon-caprolactone) (PCL 6, 12, 24 and 50 wt%) and zirconia-yttria (ZrO2-5%Y2O3) were synthesized by a sol-gel method, from a multicomponent solution containing zirconium propoxide [Zr(OC2H7)4], yttrium chloride (YCl3), PCL, water and chloroform (CHCl3). The structure of the hybrids was obtained by means of hydrogen bonds between the Zr-OH group (H-donor) in the sol-gel intermediate species and the carboxylic group (H-acceptor) in the repeating units of the polymer. The presence of hydrogen bonds between organic-inorganic components of the hybrid materials was suggested by Fourier transform infrared (FTIR) analysis, and strongly supported by solid-state NMR. A single-step, sol-gel process was then used to precipitate microspheres containing ketoprofen or indomethacin for controlled drug delivery applications. Release kinetics in a simulated body fluid (SBF) were subsequently investigated. The amount of drug released was detected by UV-VIS spectroscopy. Pure anti-inflammatory agents exhibited linear release with time, in contrast drugs entrapped in the organic-inorganic hybrids were released with a logarithmic time dependence, starting with an initial burst effect followed by a gradual decrease. The synthesis of amorphous materials containing drugs, obtained by sol-gel methods, helps to devise new strategies for controlled drug delivery system design.
Process for preparing energetic materials

DOEpatents

Simpson, Randall L [Livermore, CA; Lee, Ronald S [Livermore, CA; Tillotson, Thomas M [Tracy, CA; Hrubesh, Lawrence W [Pleasanton, CA; Swansiger, Rosalind W [Livermore, CA; Fox, Glenn A [Livermore, CA

2011-12-13

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

NASA Astrophysics Data System (ADS)

Huang, Li; Zheng, Chan; Guo, Qiaohang; Huang, Dongdong; Wu, Xiukai; Chen, Ling

2018-02-01

Freely dispersed carbon nanodots (CNDs) were introduced into a 3-glycidoxy-propyltrimethoxysilane modified silicate gel glass (i.e. an organically modified silica or ORMOSIL) by a highly efficient and simple sol-gel process, which could be easily extended to prepare functional molecules/nanoparticles solid state optoelectronic devices. Scanning electron microscope imaging, Fourier transform infrared spectroscopy, pore structure measurements, ultraviolet-visible spectroscopy, and fluorescence spectroscopy were used to investigate the surface characteristics, structure, texture, and linear optical properties of the CND/SiO2 ORMOSIL gel glasses. Images and UV/Vis spectra confirmed the successful dispersion of CNDs in the ORMOSIL gel glass. The surface characteristics and pore structure of the host SiO2 matrix were markedly changed through the introduction of the CNDs. The linear optical properties of the guest CNDs were also affected by the sol-gel procedure. The nonlinear optical (NLO) properties of the CNDs were investigated by a nanosecond open-aperture Z-scan technique at 532 nm both in liquid and solid matrices. We found that the NLO response of the CNDs was considerably improved after their incorporation into the ORMOSIL gel glasses. Possible enhancement mechanisms were also explored. The nonlinear extinction coefficient gradually increased while the optical limiting (OL) threshold decreased as the CND doping level was increased. This result suggests that the NLO and OL properties of the composite gel glasses can be optimized by tuning the concentration of CNDs in the gel glass matrix. Our findings show that CND/SiO2 ORMOSIL gel glasses are promising candidates for optical limiters to protect sensitive instruments and human eyes from damage caused by high power lasers.
Effect of Sol Concentration, Aging and Drying Process on Cerium Stabilization Zirconium Gel Produced by External Gelation

NASA Astrophysics Data System (ADS)

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 to release the decomposition of the material during heating. Larger the concentration of nitric metal in sol solution, yields a gel with a larger diameter of gels. This research allows us to plan the diameter of the sintered particles to be made.
Evidence of modifications of micellar interface in sol-gel glass

DOE Office of Scientific and Technical Information (OSTI.GOV)

Catuara, C.M.; Lin, C.T.

1994-12-31

A new sol-gel procedure using micellar solutions has been developed to immobilize local anesthetic drugs in optically transparent glass. Dibucaine was selected as a direct emission probe at 77 K for determining the forms of the anesthetic drug (free base, monoprotonated, and/or diprotonated) and its location (hydrophobic core, interfacial layer or hydrophilic region) in micelles. The photophysical properties of local anesthetics obtained in gels are compared to those in solutions. During the gelation stage, the predominant drug species was identified as free base dibucaine embedded in the hydrophobic core of neutral as well as charged micelles. This observation suggests thatmore » the micellar interface was modified by the large hydrophilic gel surface during the gelation stage. The modified micellar interface allows an increase in the partition of free base dibucaine into the hydrophobic region. At the xerogel stage, however, the collapse of micellar structure provides a direct interaction of dibucaine with the acidic gel surface, leading to a formation of diprotonated dibucaine. The results are discussed in terms of molecular basis of pharmacological implications such as drug delivery, release, and transport under microencapsulation conditions.« less
Electrochemical sensor based on molecularly imprinted polymer film via sol-gel technology and multi-walled carbon nanotubes-chitosan functional layer for sensitive determination of quinoxaline-2-carboxylic acid.

PubMed

Yang, Yukun; Fang, Guozhen; Liu, Guiyang; Pan, Mingfei; Wang, Xiaomin; Kong, Lingjie; He, Xinlei; Wang, Shuo

2013-09-15

Quinoxaline-2-carboxylic acid (QCA) is difficult to measure since only trace levels are present in commercial meat products. In this study, a rapid, sensitive and selective molecularly imprinted electrochemical sensor for QCA determination was successfully constructed by combination of a novel modified glassy carbon electrode (GCE) and differential pulse voltammetry (DPV). The GCE was fabricated via stepwise modification of multi-walled carbon nanotubes (MWNTs)-chitosan (CS) functional composite and a sol-gel molecularly imprinted polymer (MIP) film on the surface. MWNTs-CS composite was used to enhance the electron transfer rate and expand electrode surface area, and consequently amplify QCA reduction electrochemical response. The imprinted mechanism and experimental parameters affecting the performance of MIP film were discussed in detail. The resulting MIP/sol-gel/MWNTs-CS/GCE was characterized using various electrochemical methods involving cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and DPV. The sensor using MIP/sol-gel/MWNTs-CS/GCE as working electrode showed a linear current response to the target QCA concentration in the wide range from 2.0×10(-6) to 1.0×10(-3)molL(-1) with a low detection limit of 4.4×10(-7)molL(-1) (S/N=3). The established sensor with excellent reproductivity and stability was applied to evaluate commercial pork products. At five concentration levels, the recoveries and standard deviations were calculated as 93.5-98.6% and 1.7-3.3%, respectively, suggesting the proposed sensor is promising for the accurate quantification of QCA at trace levels in meat samples. Copyright © 2013 Elsevier B.V. All rights reserved.
Electroanalytical applications of screen-printable surfactant-induced sol-gel graphite composites

DOEpatents

Guadalupe, Ana R.; Guo, Yizhu

2001-05-15

A process for preparing sol-gel graphite composite electrodes is presented. This process preferably uses the surfactant bis(2-ethylhexyl) sulfosuccinate (AOT) and eliminates the need for a cosolvent, an acidic catalyst, a cellulose binder and a thermal curing step from prior art processes. Fabrication of screen-printed electrodes by this process provides a simple approach for electroanalytical applications in aqueous and nonaqueous solvents. Examples of applications for such composite electrodes produced from this process include biochemical sensors such as disposable, single-use glucose sensors and ligand modified composite sensors for metal ion sensitive sensors.
Ultra-small dye-doped silica nanoparticles via modified sol-gel technique

NASA Astrophysics Data System (ADS)

Riccò, R.; Nizzero, S.; Penna, E.; Meneghello, A.; Cretaio, E.; Enrichi, F.

2018-05-01

In modern biosensing and imaging, fluorescence-based methods constitute the most diffused approach to achieve optimal detection of analytes, both in solution and on the single-particle level. Despite the huge progresses made in recent decades in the development of plasmonic biosensors and label-free sensing techniques, fluorescent molecules remain the most commonly used contrast agents to date for commercial imaging and detection methods. However, they exhibit low stability, can be difficult to functionalise, and often result in a low signal-to-noise ratio. Thus, embedding fluorescent probes into robust and bio-compatible materials, such as silica nanoparticles, can substantially enhance the detection limit and dramatically increase the sensitivity. In this work, ultra-small fluorescent silica nanoparticles (NPs) for optical biosensing applications were doped with a fluorescent dye, using simple water-based sol-gel approaches based on the classical Stöber procedure. By systematically modulating reaction parameters, controllable size tuning of particle diameters as low as 10 nm was achieved. Particles morphology and optical response were evaluated showing a possible single-molecule behaviour, without employing microemulsion methods to achieve similar results. [Figure not available: see fulltext.
A new sol-gel synthesis of 45S5 bioactive glass using an organic acid as catalyst.

PubMed

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.
Magnetic studies of cobalt doped barium hexaferrite nanoparticles prepared by modified sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shalini, M. Govindaraj; Sahoo, Subasa C., E-mail: subasa@cukerala.ac.in

2016-05-06

M-type barium hexaferrite (BaFe{sub 12}O{sub 19}) and cobalt doped barium hexaferrite (BaFe{sub 11}CoO{sub 19}) nanopowders were synthesized by modified sol-gel auto-combustion technique and were annealed at 900°C in air for 4 hours. The annealed powders were studied in the present work and X-ray diffraction studies showed pure phase formation after annealing. The average grain size in the nanopowder sample was decreased after doping. Magnetization value of 60 emu/g was observed at 300 K for the barium hexaferrite and was reduced to 54 emu/g after doping. The coercivity of 5586 Oe was observed at 300 K for the undoped sample andmore » was found to be decreased in the doped sample. As the measurement temperature was decreased from 300 K to 60 K, magnetization value was increased in both the samples compared to those at 300 K. The coercivity of the undoped sample was found to decrease whereas it was increased for the doped sample at 60 K. The observed magnetic properties may be understood on the basis of modified exchange interaction and anisotropy in the doped sample compared to that of pure barium hexaferrite.« less
A Review of Photocatalysts Prepared by Sol-Gel Method for VOCs Removal

PubMed Central

Tseng, Ting Ke; Lin, Yi Shing; Chen, Yi Ju; Chu, Hsin

2010-01-01

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. PMID:20640156
Sol-gel methods for synthesis of aluminosilicates for dental applications.

PubMed

Cestari, Alexandre

2016-12-01

Amorphous aluminosilicates glasses containing fluorine, phosphorus and calcium are used as a component of the glass ionomer dental cement. This cement is used as a restorative, basis or filling material, but presents lower mechanical resistance than resin-modified materials. The Sol-Gel method is a possible route for preparation of glasses with lower temperature and energy consumption, with higher homogeneity and with uniform and nanometric particles, compared to the industrial methods Glass ionomer cements with uniform, homogeneous and nanometric particles can present higher mechanical resistance than commercial ionomers. The aim of this work was to adapt the Sol-Gel methods to produce new aluminosilicate glass particles by non-hydrolytic, hydrolytic acid and hydrolytic basic routes, to improve glass ionomer cements characteristics. Three materials were synthesized with the same composition, to evaluate the properties of the glasses produced from the different methods, because multicomponent oxides are difficult to prepare with homogeneity. The objective was to develop a new route to produce new glass particles for ionomer cements with possible higher resistance. The particles were characterized by thermal analysis (TG, DTA, DSC), transmission electron microscopy (TEM), X-ray diffraction (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS). The glasses were tested with polyacrylic acid to form the glass ionomer cement by the setting reaction. It was possible to produce distinct materials for dental applications and a sample presented superior characteristics (homogeneity, nanometric particles, and homogenous elemental distribution) than commercial glasses for ionomer cements. The new route for glass production can possible improve the mechanical resistance of the ionomer cements. Copyright Â© 2016 Elsevier Ltd. All rights reserved.
A review on development of solid phase microextraction fibers by sol-gel methods and their applications.

PubMed

Kumar, Ashwini; Gaurav; Malik, Ashok Kumar; Tewary, Dhananjay Kumar; Singh, Baldev

2008-03-03

Solid phase microextraction (SPME) is an innovative, solvent free technology that is fast, economical and versatile. SPME is a fiber coated with a liquid (polymer), a solid (sorbent) or a combination of both. The fiber coating takes up the compounds from the sample by absorption in the case of liquid coatings or adsorption in the case of solid coatings. The SPME fiber is then transferred with the help of a syringe like device into the analytical instrument for desorption and analysis of the target analytes. The sol-gel process provides a versatile method to prepare size, shape and charge selective materials of high purity and homogeneity by means of preparation techniques different from the traditional ones, for the chemical analysis. This review is on the current state of the art and future trends in the developments of solid phase microextraction (SPME) fibers using sol-gel method. To achieve more selective determination of different compound classes, the variety of different coating material for SPME fibers has increased. Further developments in SPME as a highly efficient extraction technique, will greatly depend on new breakthroughs in the area of new coating material developments for the SPME fibers. In sol-gel approach, appropriate sol-gel precursors and other building blocks can be selected to create a stationary phase with desired structural and surface properties. This approach is efficient in integrating the advantageous properties of organic and inorganic material systems and thereby increasing and improving the extraction selectivity of the produced amalgam organic-inorganic stationary phases. This review is mainly focused on recent advanced developments in the design, synthesis, characterisation, properties and application of sol-gel in preparation of coatings for the SPME fibers.
The Effect of Different Coupling Agents on Nano-ZnO Materials Obtained via the Sol-Gel Process.

PubMed

Purcar, Violeta; Şomoghi, Raluca; Niţu, Sabina Georgiana; Nicolae, Cristian-Andi; Alexandrescu, Elvira; Gîfu, Ioana Cătălina; Gabor, Augusta Raluca; Stroescu, Hermine; Ianchiş, Raluca; Căprărescu, Simona; Cinteză, Ludmila Otilia

2017-12-12

Hybrid nanomaterials based on zinc oxide were synthesized via the sol-gel method, using different silane coupling agents: (3-glycidyloxypropyl)trimethoxysilane (GPTMS), phenyltriethoxysilane (PhTES), octyltriethoxysilane (OTES), and octadecyltriethoxysilane (ODTES). Morphological properties and the silane precursor type effect on the particle size were investigated using dynamic light scattering (DLS), environmental scanning electron microscopy (ESEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). The bonding characteristics of modified ZnO materials were investigated using Fourier transform infrared spectroscopy (FTIR). The final solutions were deposited on metallic substrate (aluminum) in order to realize coatings with various wettability and roughness. The morphological studies, obtained by ESEM and TEM analysis, showed that the sizes of the ZnO nanoparticles are changed as function of silane precursor used in synthesis. The thermal stability of modified ZnO materials showed that the degradation of the alkyl groups takes place in the 300-500 °C range. Water wettability study revealed a contact angle of 142 ± 5° for the surface covered with ZnO material modified with ODTES and showed that the water contact angle increases as the alkyl chain from the silica precursor increases. These modified ZnO materials, therefore, can be easily incorporated in coatings for various applications such as anti-corrosion and anti-icing.
Structural analysis and corrosion studies on an ISO 5832-9 biomedical alloy with TiO2 sol-gel layers.

PubMed

Burnat, B; Dercz, G; Blaszczyk, T

2014-03-01

The aim of this study was to demonstrate the relationship between the structural and corrosion properties of an ISO 5832-9 biomedical alloy modified with titanium dioxide (TiO2) layers. These layers were obtained via the sol-gel method by acid-catalyzed hydrolysis of titanium isopropoxide in isopropanol solution. To obtain TiO2 layers with different structural properties, the coated samples were annealed at temperatures of 200, 300, 400, 450, 500, 600 and 800 °C for 2 h. For all the prepared samples, accelerated corrosion measurements were performed in Tyrode's physiological solution using electrochemical methods. The most important corrosion parameters were determined: corrosion potential, polarization resistance, corrosion rate, breakdown and repassivation potentials. Corrosion damage was analyzed using scanning electron microscopy. Structural analysis was carried out for selected TiO2 coatings annealed at 200, 400, 600 and 800 °C. In addition, the morphology, chemical composition, crystallinity, thickness and density of the deposited TiO2 layers were determined using suitable electron and X-ray measurement methods. It was shown that the structure and character of interactions between substrate and deposited TiO2 layers depended on annealing temperature. All the obtained TiO2 coatings exhibit anticorrosion properties, but these properties are related to the crystalline structure and character of substrate-layer interaction. From the point of view of corrosion, the best TiO2 sol-gel coatings for stainless steel intended for biomedical applications seem to be those obtained at 400 °C.
Method for fabrication of ceramic dielectric films on copper foils

DOEpatents

Ma, Beihai; Narayanan, Manoj; Dorris, Stephen E.; Balachandran, Uthamalingam

2015-03-10

The present invention provides a method for fabricating a ceramic film on a copper foil. The method comprises applying a layer of a sol-gel composition onto a copper foil. The sol-gel composition comprises a precursor of a ceramic material suspended in 2-methoxyethanol. The layer of sol-gel is then dried at a temperature up to about 250.degree. C. The dried layer is then pyrolyzed at a temperature in the range of about 300 to about 450.degree. C. to form a ceramic film from the ceramic precursor. The ceramic film is then crystallized at a temperature in the range of about 600 to about 750.degree. C. The drying, pyrolyzing and crystallizing are performed under a flowing stream of an inert gas. In some embodiments an additional layer of the sol-gel composition is applied onto the ceramic film and the drying, pyrolyzing and crystallizing steps are repeated for the additional layer to build up a thicker ceramic layer on the copper foil. The process can be repeated one or more times if desired.
Determination of Insulator-to-Semiconductor Transition in Sol-Gel Oxide Semiconductors Using Derivative Spectroscopy.

PubMed

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.
Resistance of dichromated gelatin as photoresist

NASA Astrophysics Data System (ADS)

Lin, Pang; Yan, Yingbai; Jin, Guofan; Wu, Minxian

1999-09-01

Based on the photographic chemistry, chemically hardening method was selected to enhance the anti-etch capability of gelatin. With the consideration of hardener and permeating processing, formaldehyde is the most ideal option due to the smallest molecule size and covalent cross-link with gelatin. After hardened in formaldehyde, the resistance of the gelatin was obtained by etched in 1% HF solution. The result showed that anti-etch capability of the gelatin layer increased with tanning time, but the increasing rate reduced gradually and tended to saturation. Based on the experimental results, dissolving-flaking hypothesis for chemically hardening gelatin was presented. Sol-gel coatings were etched with 1% HF solution. Compared with the etching rate of gelatin layer, it showed that gelatin could be used as resist to fabricate optical elements in sol-gel coating. With the cleaving-etch method and hardening of dichromated gelatin (DCG), DCG was used as a photoresist for fabricating sol-gel optical elements. As an application, a sol-gel random phase plate was fabricated.
Development of a functionalized coating for inhibition of marine corrosion and biofouling

NASA Astrophysics Data System (ADS)

Gittens, Jeanette Elizabeth

The financial loss incurred by corrosion of metals in the marine environment has led to a need to develop effective, economic and environmentally friendly methods of protection. Traditional methods of counteracting the development of surface biofilms and biofouling within aqueous environments have involved implementing chemical biocides, often with a deleterious effect on non-target organisms. Sol gel coating technology offers a convenient route for immobilizing functional additives, such as inhibitors or, in the case of this study, biologically active microorganisms. Paenibacillus polymyxa biofilms inhibit the corrosion of metal substrates and this strain has the advantage of forming endospores can withstand the solvent and acid concentrations required in sol-gel formulation. Encapsulation of viable P. polymyxa endospores within the sol-gel matrix allowed germination on exposure to nutrients, when germinating endospores and vegetative cells were seen after fluorescence microscopy to be distributed throughout the coating. Laboratory electrochemical impedance tests were used to characterize the corrosion behaviour of the endospore-containing (biotic) sol-gel coating in comparison to an abiotic (no endospores) sol-gel only coating and one containing non-viable (killed) endospores. The technology enabled manipulation of the sol-gel formulation and the method of application to produce biotic sol-gel with enhanced corrosion inhibition properties on aluminium alloy. Field trials in a marine environment confirmed the corrosion protecting properties of the biotic coating and that the biotic coatings inhibited macroscopic biofouling for at least 29 weeks relative to the controls without encapsulated live endospores. Production of polymyxin by the encapsulated bacteria, which was proposed as a mechanism by which they inhibit MIC, was less than 1 mug per ml and below the threshold of detection by liquid chromatography mass spectrometry and antimicrobial bioassay. Microcosm experiments were used to study differences in the corrosion of abiotic and biotic coatings in the presence of a corrosion-causing sulphate-reducing bacterium. Scanning electrochemical microscopy was developed as a technique to study electrochemical processes on the coating surface and showed differences in the distribution of copper ions on the surface of abiotic and biotic coatings.The results of the experimental work in this thesis show the potential of encapsulating metabolically active bacterial cells within a sol-gel coating on metals for the control of marine corrosion and biofouling.
Spectroscopic and electrochemical characterization of cytochrome c encapsulated in a bio sol-gel matrix.

PubMed

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 < 2.5) dramatically limited their application to 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.

Analysis of Zinc Oxide Thin Films Synthesized by Sol-Gel via Spin Coating

NASA Astrophysics Data System (ADS)

Wolgamott, Jon Carl

Transparent conductive oxides are gaining an increasingly important role in optoelectronic devices such as solar cells. Doped zinc oxide is a candidate as a low cost and nontoxic alternative to tin doped indium oxide. Lab results have shown that both n-type and p-type zinc oxide can be created on a small scale. This can allow zinc oxide to be used as either an electrode as well as a buffer layer to increase efficiency and protect the active layer in solar cells. Sol-gel synthesis is emerging as a low temperature, low cost, and resource efficient alternative to producing transparent conducting oxides such as zinc oxide. For sol-gel derived zinc oxide thin films to reach their potential, research in this topic must continue to optimize the known processing parameters and expand to new parameters to tighten control and create novel processing techniques that improve performance. The processing parameters of drying and annealing temperatures as well as cooling rate were analyzed to see their effect on the structure of the prepared zinc oxide thin films. There were also preliminary tests done to modify the sol-gel process to include silver as a dopant to produce a p-type thin film. The results from this work show that the pre- and post- heating temperatures as well as the cooling rate all play their own unique role in the crystallization of the film. Results from silver doping show that more work needs to be done to create a sol-gel derived p-type zinc oxide thin film.
Fluorescent Dye-doped Sol-gel Sensor for Highly Sensitive Carbon Dioxide Gas Detection below Atmospheric Concentrations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dansby-Sparks, Royce N.; Jin, Jun; Mechery, Shelly J

2009-01-01

Optical fluorescence sol-gel sensors have been developed for the detection of carbon dioxide gas in the 0.03?30% range with a detection limit of 0.008% (or 80 ppm) and a quantitation limit of 0.02% (or 200 ppm) CO{sub 2}. Sol?gels were spin-coated on glass slides to create an organically modified silica-doped matrix with the 1-hydroxypyrene-3,6,8-trisulfonate (HPTS) fluorescent indicator. The luminescence intensity of the HPTS indicator (513 nm) is quenched by CO{sub 2}, which protonates the anionic form of HPTS. An ion pair technique was used to incorporate the lipophilic dye into the hydrophilic sol?gel matrix. TiO{sub 2} particles (<5 {mu}m diameter)more » were added to induce Mie scattering and increase the incident light interaction with the sensing film, thus increasing the signal-to-noise ratio. Moisture-proof overcoatings have been used to maintain a constant level of water inside the sensor films. The optical sensors are inexpensive to prepare and can be easily coupled to fiber optics for remote sensing capabilities. A fiber-optic bundle was used for the gas detection and shown to work as part of a multianalyte platform for simultaneous detection of multiple analytes. The studies reported here resulted in the development of sol?gel optical fluorescent sensors for CO{sub 2} gas with sensitivity below that in the atmosphere (ca. 387 ppm). These sensors are a complementary approach to current FT-IR measurements for real-time carbon dioxide detection in environmental applications.« less
The effect of silica-coating by sol-gel process on resin-zirconia bonding.

PubMed

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

2013-01-01

The effect of silica-coating by sol-gel process on the bond strength of resin composite to zirconia was evaluated and compared against the sandblasting method. Four groups of zirconia samples were silica-coated by sol-gel process under varied reagent ratios of ethanol, water, ammonia and tetraethyl orthosilicate and for different deposition times. One control group of zirconia samples were treated with sandblasting. Within each of these five groups, one subgroup of samples was kept in dry storage while another subgroup was aged by thermocycling for 6,000 times. Besides shear bond testing, the surface topography and surface elemental composition of silica-coated zirconia samples were also examined using scanning electron microscopy and X-ray photoelectron spectroscopy. Comparison of silica coating methods revealed significant differences in bond strength among the Dry groups (p<0.001) and Thermocycled groups (p<0.001). Comparison of sol-gel deposition times also revealed significant differences in bond strength among the Dry groups (p<0.01) and Thermocycled groups (p<0.001). Highest bond strengths were obtained after 141-h deposition: Dry (7.97±3.72 MPa); Thermocycled (2.33±0.79 MPa). It was concluded that silica-coating of zirconia by sol-gel process resulted in weaker resin bonding than by sandblasting.
Graphene oxide based sol-gel stainless steel fiber for the headspace solid-phase microextraction of organophosphate ester flame retardants in water samples.

PubMed

Jin, Tingting; Cheng, Jing; Cai, Cuicui; Cheng, Min; Wu, Shiju; Zhou, Hongbin

2016-07-29

In this paper, graphene oxide was coated onto a stainless steel wire through sol-gel technique and it was used as a solid phase microextraction (SPME) fiber. The prepared fiber was characterized by scanning electron microscopy (SEM), which displayed that the fiber had crinkled surface and porous structure The application of the fiber was evaluated through the headspace SPME of nine organophosphate ester flame retardants (OPFRs) with different characteristics in water samples followed by gas chromatography and nitrogen-phosphorous detector (GC/NPD). The major factors influencing the extraction efficiency, including the extraction and desorption conditions, were studied and optimized. Under the optimum conditions, the proposed method was evaluated, and applied to the analysis of organophosphate ester flame retardants in real environmental water samples. The results demonstrated the HS-SPME method based on GO sol-gel fiber had good linearity (R>0.9928), and limits of detection (1.4-135.6ngL(-1)), high repeatability (RSD<9.8%) and good recovery (76.4-112.4%). The GO based sol-gel fiber displayed bigger extraction capability than the commercial PDMS fiber and the pure sol-gel fiber for both polar and apolar organophosphate esters, especially for the OPFRs containing benzene rings. Copyright © 2016 Elsevier B.V. All rights reserved.
Infrared and Raman spectra of triacetoxyvinylsilane, aqueous sol-gel and xerogel

NASA Astrophysics Data System (ADS)

Li, Ying-Sing; Ba, Abdul; Mahmood, Maleeha S.

2009-04-01

Triacetoxyvinylsilane (TAVS) has been used as a precursor to prepare sol-gel under aqueous conditions. The sol-gel product has been applied for the surface treatment of aluminum. Infrared and Raman spectra have been collected for TAVS and for TAVS sol-gel, xerogel and sol-gel-coated aluminum. Vibrational analyses have been suggested for the recorded spectra based essentially on the group frequencies and the spectral variation with the change of the sol-gel product states and the vibrational assignments of similar molecules. From the recorded infrared and Raman spectra of the sol-gel and xerogel, it is found that the sol-gel produced in the process with TAVS is essentially the same as that prepared from vinyltriethoxysilane. Thermo-gravimetric analysis (TGA) of TAVS xerogel has been conducted, and an explanation has been given in coordination with the results obtained from IR spectroscopic study of the xerogels cured at different temperatures. The study has demonstrated the thermal effect on the condensation of the sol-gel process and on the vinyl decomposition of TAVS xerogel.
Versatile bio-ink for covalent immobilization of chimeric avidin on sol-gel substrates.

PubMed

Heikkinen, Jarkko J; Kivimäki, Liisa; Määttä, Juha A E; Mäkelä, Inka; Hakalahti, Leena; Takkinen, Kristiina; Kulomaa, Markku S; Hytönen, Vesa P; Hormi, Osmo E O

2011-10-15

A bio-ink for covalent deposition of thermostable, high affinity biotin-binding chimeric avidin onto sol-gel substrates was developed. The bio-ink was prepared from heterobifunctional crosslinker 6-maleimidohexanoic acid N-hydroxysuccinimide which was first reacted either with 3-aminopropyltriethoxysilane or 3-aminopropyldimethylethoxysilane to form silane linkers 6-maleimide-N-(3-(triethoxysilyl)propyl)hexanamide or -(ethoxydimethylsilyl)propyl)-hexanamide. C-terminal cysteine genetically engineered to chimeric avidin was reacted with the maleimide group of silane linker in methanol/PBS solution to form a suspension, which was printed on sol-gel modified PMMA film. Different concentrations of chimeric avidin and ratios between silane linkers were tested to find the best properties for the bio-ink to enable gravure or inkjet printing. Bio-ink prepared from 3-aminopropyltriethoxysilane was found to provide the highest amount of active immobilized chimeric avidin. The developed bio-ink was shown to be valuable for automated fabrication of avidin-functionalized polymer films. Copyright © 2011 Elsevier B.V. All rights reserved.
Construction of flame retardant coating on polyamide 6.6 via UV grafting of phosphorylated chitosan and sol-gel process of organo-silane.

PubMed

Kundu, Chanchal Kumar; Wang, Xin; Hou, Yanbei; Hu, Yuan

2018-02-01

Phosphorylated chitosan (PCS) was synthesized and grafted onto the surface of polyamide 6.6 (PA 6.6) fabrics via UV-induced grafting polymerization in order to improve the flame retardant properties. Subsequently, PCS grafted PA 6.6 fabrics were modified by (3-aminopropyl) triethoxysilane (APTES) through sol-gel process in order to form a cross-linking coating. The results obtained from the vertical burning test indicated that only the PCS grafted and simultaneously sol-gel treated fabrics could stop the melt dripping. A maximum reduction (30%) in the peak heat release rate was achieved for the PA6.6-PCS-4W-SG fabric sample. The optimal flame retardant effect was achieved for the PA6.6 fabrics treated by PCS and APTES simultaneously, which was attributed to the joint effect of thermal shielding exerted by the silica and char-forming effect derived from PCS. Copyright © 2017 Elsevier Ltd. All rights reserved.
Titanium dioxide nanoparticles: Impact of increasing ionic strength during synthesis, reflux, and hydrothermal aging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Isley, Sara L.; Jordan, David S.; Penn, R. Lee

2009-01-08

This work investigates the role of ionic strength during synthesis, reflux, and hydrothermal aging of sol-gel synthesized titanium dioxide. Research presented here uses X-ray diffraction data and Rietveld refinements to quantify anatase, brookite, and rutile phases as functions of synthetic and aging variables. In addition, the Scherrer equation is used to obtain average crystallite sizes for each phase quantified. Results presented in this work demonstrate that the most control over the sol-gel products can be obtained by modifying the pH during hydrolysis. In addition, while varying the ionic strength during reflux and hydrothermal aging can result in enhanced control overmore » the crystalline phase and crystallite size, the most control can be achieved by varying the ionic strength during synthesis. Finally, sol-gel synthesis at low pH (-0.6) and high-chloride concentration (3 M NaCl) produced a heterogeneous sample composed of nanocrystalline anatase (3.8 nm) and rutile (2.9 nm)« less
Growth and Characterization of CuO Nanostructures on Si for the Fabrication of CuO/p-Si Schottky Diodes

PubMed Central

Çetinkaya, S.; Çetinkara, H. A.; Bayansal, F.; Kahraman, S.

2013-01-01

CuO interlayers in the CuO/p-Si Schottky diodes were fabricated by using CBD and sol-gel methods. Deposited CuO layers were characterized by SEM and XRD techniques. From the SEM images, it was seen that the film grown by CBD method is denser than the film grown by sol-gel method. This result is compatible with XRD results which show that the crystallization in CBD method is higher than it is in sol-gel method. For the electrical investigations, current-voltage characteristics of the diodes have been studied at room temperature. Conventional I-V and Norde's methods were used in order to determine the ideality factor, barrier height, and series resistance values. It was seen that the morphological and structural analysis are compatible with the results of electrical investigations. PMID:23766670
Administration of a Sol-Gel Formulation of Phenylephrine Using Low-Temperature Hollow Microneedle for Treatment of Intermittent Fecal Incontinence.

PubMed

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.
Production of monodisperse cerium oxide microspheres with diameters near 100 μm by internal-gelation sol–gel methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 slidesmore » 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.« less
Preparation and Application of Immobilized Surfactant-Modified PANi-CNT/TiO2 under Visible-Light Irradiation

PubMed Central

Yuan, Ching; Hung, Chung-Hsuang; Yuan, Chung-Shin; Li, Huei-Wen

2017-01-01

Hydrothermally and sol-gel-synthesized immobilized surfactant-modified polyaniline-carbon nanotubes/TiO2 (PANi-CNT/TiO2) photocatalysts were prepared and their application in the degradation of diethyl phthalate (DEP) under visible light at 410 nm was investigated in this sturdy. To improve the dispersion of nanoparticles and the transfer of electrons, the TiO2 surface was modified with both sodium dodecyl sulfate (SDS) and functionalized carbon nanotubes (CNT-COOH and CNT-COCl). With the addition of PANi, which was increased from 1–5%, the adsorption edge of the prepared photocatalysts shifted to 442 nm. The SDS linked the PANi polymers to achieve a thickness of coating of the film of up to 314–400 nm and 1301–1600 nm for sol-gel hydrolysis and hydrothermally-synthesized photocatalysts, respectively. An appropriate film thickness would extend the transfer path of the electrons and inhibit the recombination of the electrons and the electron-holes. The photo-degradation performance of DEP by the hydrothermally-synthesized photocatalysts was better than those by sol-gel hydrolysis. The results revealed that the hydroxyl radicals were the key oxidant in the degradation of DEP using hydrothermally-synthesized PANi-CNT/TiO2 photocatalysts. The morphology and functional groups of the raw materials of photocatalysts were characterized and a comparison of photocatalytic activity with other TiO2-based photocatalysts was also provided. PMID:28773238
Coating and curing apparatus and methods

DOEpatents

Brophy, Brenor L; Maghsoodi, Sina; Neyman, Patrick J; Gonsalves, Peter R; Hirsch, Jeffrey G; Yang, Yu S

2015-02-24

Disclosed are coating apparatus including flow coating and roll-coating that may be used for uniform sol-gel coating of substrates such as glass, solar panels, windows or part of an electronic display. Also disclosed are methods for substrate preparation, flow coating and roll coating. Lastly systems and methods for skin curing sol-gel coatings deposited onto the surface of glass substrates using a high temperature air-knife are disclosed.
Sol-gel processing to form doped sol-gel monoliths inside hollow core optical fiber and sol-gel core fiber devices made thereby

NASA Technical Reports Server (NTRS)

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.
Sol-gel layers for ceramic microsystems application

NASA Astrophysics Data System (ADS)

Czok, Mateusz; Golonka, Leszek

2016-11-01

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

NASA Astrophysics Data System (ADS)

Krebs, J. K.; Hobson, Christopher; Silversmith, Ann

2004-03-01

Sol-gel produced materials have recently gained attention for their use in producing nanoscale dielectric materials for confinement studies. Lanthanide impurities in the dielectric enable experimenters to optically probe the structure and dynamic properties of the nanoparticle hosts. We report on an alkoxide sol-gel production method used to produce trivalent europium doped yttrium oxide. Our process follows the standard hydrolysis of an alkoxide precursor with water containing the lanthanide ions. The sol is then aged and calcined at 800 ^oC to produce the powder samples. X-ray diffraction confirms the structure of the powder is that of Y_2O_3. The emission and excitation of the europium impurities is consistent with that of europium doped single crystal yttrium oxide, where it is known that the europium ions substitute for yttrium in the lattice. We therefore conclude that the sol-gel process enables the incorporation of europium ions into the yttrium oxide structure at temperatures far below the melting temperature. The results of preliminary dynamics measurements will also be discussed.
Fundamental electrochemiluminescence characteristics of fluorine-doped tin oxides synthesized by sol-gel combustion.

PubMed

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

PubMed

Segro, Scott S; Malik, Abdul

2008-09-26

A sol-gel polydimethyldiphenylsiloxane (PDMDPS) coating was developed for capillary microextraction on-line hyphenated with high-performance liquid chromatography (HPLC). This coating was created using methyltrimethoxysilane (MTMS) as the sol-gel precursor and di-hydroxy-terminated PDMDPS as the sol-gel active polymer. The methyl and phenyl groups on the sol-gel active polymer and the methyl groups on the sol-gel precursor ultimately turned into pendant groups providing the ability to extract non-polar analytes. A 40-cm segment of 0.25 mm I.D. fused silica capillary containing the sol-gel PDMDPS coating was installed as an external sampling loop in an HPLC injection port. Aqueous samples containing polycyclic aromatic hydrocarbons (PAHs), aromatic compounds, ketones, and aldehydes were passed through this capillary wherein the analytes were extracted by the sol-gel coating. The extracted analytes were then transferred to the HPLC column using isocratic or gradient elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for non-polar (e.g., polycyclic aromatic hydrocarbons and aromatic compounds) as well as moderately polar compounds, such as aromatic amines, ketones, and aldehydes. The test results indicate that PDMDPS can be successfully immobilized into a sol-gel network and that the resulting solvent-resistant sol-gel organic-inorganic hybrid coating can be effectively used for on-line hyphenation of capillary microextraction with high-performance liquid chromatography. The test results also indicate that the sol-gel PDMDPS coated capillary is resistant to high-temperature solvents, making it suitable for applications in high-temperature HPLC. To the best of our knowledge, this is the first report on the creation of a silica-based sol-gel PDMDPS coating used in capillary microextraction on-line hyphenated to HPLC.
Radiation hardening in sol-gel derived Er{sup 3+}-doped silica glasses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hari Babu, B., E-mail: hariphy2012@gmail.com, E-mail: matthieu.lancry@u-psud.fr; León Pichel, Mónica; Institut de Chimie Moléculaire et des Matériaux d'Orsay, UMR CNRS-UPSud 8182, Université Paris Sud, 91405 Orsay

2015-09-28

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

DOEpatents

Brophy, Brenor L.; Gonsalves, Peter R.; Maghsoodi, Sina; Colson, Thomas E.; Yang, Yu S.; Abrams, Ze'ev R.

2016-04-19

Disclosed is a coating apparatus including flow coating and roll-coating that may be used for uniform sol-gel coating of substrates such as glass, solar panels, windows or part of an electronic display. Also disclosed are methods for substrate preparation, flow coating and roll coating. Lastly, systems and methods for curing sol-gel coatings deposited onto the surface of glass substrates using high temperature air-knives, infrared emitters and direct heat applicators are disclosed.

Spectrofluorimetric assessment of hydrochlorothiazide using optical sensor nano-composite terbium ion doped in sol-gel matrix.

PubMed

Youssef, A O

2012-05-01

A new, simple, sensitive and selective spectrofluorimetric method for the determination of Hydrochlorothiazide was developed in acetonitrile at pH 6.2. The Hydrochlorothiazide can remarkably enhance the luminescence intensity of the Tb(3+) ion doped in sol-gel matrix at λ(ex) = 370 nm. The intensity of the emission band of Tb(3+) ion doped in sol-gel matrix was increased due to the energy transfer from the triplet excited state of Hydrochlorothiazide to ((5)D(4)) excited energy state of Tb(3) ion. The enhancement of the emission band of Tb(3+) ion doped in sol-gel matrix at ((5)D(4)→(7)F(5)) 545 nm was directly proportion to the concentration of Hydrochlorothiazide with a dynamic ranges of 5.0 × 10(-10)-5.0 × 10(-6) mol L(-1) and detection limit of 2.2 × 10(-11) mol L(-1).
Highly sensitive and selective spectrofluorimetric determination of metoclopramide hydrochloride in pharmaceutical tablets and serum samples using Eu3+ ion doped in sol-gel matrix.

PubMed

Attia, M S; Aboaly, M M

2010-06-30

A simple, sensitive and selective spectrofluorimetric method for the determination of Metoclopramide hydrochloride (MCP) is developed. The MCP can remarkably enhances the luminescence intensity of the Eu(3+) ion doped in sol-gel matrix at lambda(ex)=380 nm in DMSO at pH 8.7. The intensity of the emission band of Eu(3+) ion doped in sol-gel matrix increases due to energy transfer from MCP to Eu(3+) in the excited state. The enhancement of the emission band of Eu(3+) ion doped in sol-gel matrix at 617 nm was found to be directly proportional to the concentration of MCP with a dynamic range of 5 x 10(-9) - 1.0 x 10(-6) mol L(-1) and detection limit of 2.2 x10(-11) mol L(-1). Copyright 2010 Elsevier B.V. All rights reserved.
A new sol-gel process for producing Na(2)O-containing bioactive glass ceramics.

PubMed

Chen, Qi-Zhi; Li, Yuan; Jin, Li-Yu; Quinn, Julian M W; Komesaroff, Paul A

2010-10-01

The sol-gel process of producing SiO(2)-CaO bioactive glasses is well established, but problems remain with the poor mechanical properties of the amorphous form and the bioinertness of its crystalline counterpart. These properties may be improved by incorporating Na(2)O into bioactive glasses, which can result in the formation of a hard yet biodegradable crystalline phase from bioactive glasses when sintered. However, production of Na(2)O-containing bioactive glasses by sol-gel methods has proved to be difficult. This work reports a new sol-gel process for the production of Na(2)O-containing bioactive glass ceramics, potentially enabling their use as medical implantation materials. Fine powders of 45S5 (a Na(2)O-containing composition) glass ceramic have for the first time been successfully synthesized using the sol-gel technique in aqueous solution under ambient conditions, with the mean particle size being approximately 5 microm. A comparative study of sol-gel derived S70C30 (a Na(2)O-free composition) and 45S5 glass ceramic materials revealed that the latter possesses a number of features desirable in biomaterials used for bone tissue engineering, including (i) the crystalline phase Na(2)Ca(2)Si(3)O(9) that couples good mechanical strength with satisfactory biodegradability, (ii) formation of hydroxyapatite, which may promote good bone bonding and (iii) cytocompatibility. In contrast, the sol-gel derived S70C30 glass ceramic consisted of a virtually inert crystalline phase CaSiO(3). Moreover, amorphous S70C30 largely transited to CaCO(3) with minor hydroxyapatite when immersed in simulated body fluid under standard tissue culture conditions. In conclusion, sol-gel derived Na(2)O-containing glass ceramics have significant advantages over related Na(2)O-free materials, having a greatly improved combination of mechanical capability and biological absorbability. 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Catalytic activity of acid and base with different concentration on sol-gel kinetics of silica by ultrasonic method.

PubMed

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.
Tuning of thermally induced sol-to-gel transitions of moderately concentrated aqueous solutions of doubly thermosensitive hydrophilic diblock copolymers poly(methoxytri(ethylene glycol) acrylate)-b-poly(ethoxydi(ethylene glycol) acrylate-co-acrylic acid).

PubMed

Jin, Naixiong; Zhang, Hao; Jin, Shi; Dadmun, Mark D; Zhao, Bin

2012-03-15

We report in this article a method to tune the sol-to-gel transitions of moderately concentrated aqueous solutions of doubly thermosensitive hydrophilic diblock copolymers that consist of two blocks exhibiting distinct lower critical solution temperatures (LCSTs) in water. A small amount of weak acid groups is statistically incorporated into the lower LCST block so that its LCST can be tuned by varying solution pH. Well-defined diblock copolymers, poly(methoxytri(ethylene glycol) acrylate)-b-poly(ethoxydi(ethylene glycol) acrylate-co-acrylic acid) (PTEGMA-b-P(DEGEA-co-AA)), were prepared by reversible addition-fragmentation chain transfer polymerization and postpolymerization modification. PTEGMA and PDEGEA are thermosensitive water-soluble polymers with LCSTs of 58 and 9 °C, respectively, in water. A 25 wt % aqueous solution of PTEGMA-b-P(DEGEA-co-AA) with a molar ratio of DEGEA to AA units of 100:5.2 at pH = 3.24 underwent multiple phase transitions upon heating, from a clear, free-flowing liquid (<15 °C) to a clear, free-standing gel (15-46 °C) to a clear, free-flowing hot liquid (47-56 °C), and a cloudy mixture (≥57 °C). With the increase of pH, the sol-to-gel transition temperature (T(sol-gel)) shifted to higher values, while the gel-to-sol transition (T(gel-sol)) and the clouding temperature (T(clouding)) of the sample remained essentially the same. These transitions and the tunability of T(sol-gel) originated from the thermosensitive properties of two blocks of the diblock copolymer and the pH dependence of the LCST of P(DEGEA-co-AA), which were confirmed by dynamic light scattering and differential scanning calorimetry studies. Using the vial inversion test method, we mapped out the C-shaped sol-gel phase diagrams of the diblock copolymer in aqueous buffers in the moderate concentration range at three different pH values (3.24, 5.58, and 5.82, all measured at ~0 °C). While the upper temperature boundaries overlapped, the lower temperature boundary shifted upward and the critical gelation concentration increased with the increase of pH. The AA content in PTEGMA-b-P(DEGEA-co-AA) was found to have a significant effect on the pH dependence of T(sol-gel). For PTEGMA-b-P(DEGEA-co-AA) with a molar ratio of DEGEA to AA units of 100:10, the T(sol-gel) of its 25 wt % aqueous solution increased faster with the increase of pH than that of PTEGMA-b-P(DEGEA-co-AA) with a DEGEA-to-AA molar ratio of 100:5.2. © 2012 American Chemical Society
Sol-Gel Synthesis of Carbon Xerogel-ZnO Composite for Detection of Catechol

PubMed Central

Li, Dawei; Zang, Jun; Zhang, Jin; Ao, Kelong; Wang, Qingqing; Dong, Quanfeng; Wei, Qufu

2016-01-01

Carbon xerogel-zinc oxide (CXZnO) composites were synthesized by a simple method of sol-gel condensation polymerization of formaldehyde and resorcinol solution containing zinc salt followed by drying and thermal treatment. ZnO nanoparticles were observed to be evenly dispersed on the surfaces of the carbon xerogel microspheres. The as-prepared CXZnO composites were mixed with laccase (Lac) and Nafion to obtain a mixture solution, which was further modified on an electrode surface to construct a novel biosensing platform. Finally, the prepared electrochemical biosensor was employed to detect the environmental pollutant, catechol. The analysis result was satisfactory, the sensor showed excellent electrocatalysis towards catechol with high sensitivity (31.2 µA·mM−1), a low detection limit (2.17 µM), and a wide linear range (6.91–453 µM). Moreover, the biosensor also displayed favorable repeatability, reproducibility, selectivity, and stability besides being successfully used in the trace detection of catechol existing in lake water environments. PMID:28773407
Effects of lithium doping on microstructure, electrical properties, and chemical bonds of sol-gel derived NKN thin films

NASA Astrophysics Data System (ADS)

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

2015-02-01

Highly (100/110) oriented lead-free Lix(Na0.5K0.5)1-xNbO3 (LNKN, x = 0, 0.02, 0.04, and 0.06) thin films are fabricated on Pt/Ti/SiO2/Si substrates via a sol-gel processing method. The lithium (Li) dopants modify the microstructure and chemical bonds of the LNKN films, and therefore improve their electrical properties. The optimal values of the remnant polarization (Pr = 14.3 μC/cm2), piezoelectric coefficient (d33 = 48.1 pm/V), and leakage current (<10-5 A/cm2) are obtained for a lithium addition of x = 0.04 (i.e., 4 at. %). The observation results suggest that the superior electrical properties are the result of an improved crystallization, a larger grain size, and a smoother surface morphology. It is shown that the ion transport mechanism is dominated by an Ohmic behavior under low electric fields and the Poole-Frenkel emission effect under high electric fields.
Synthesis and characterization of nanosized MgxMn1-xFe2O4 ferrites by both sol-gel and thermal decomposition methods

NASA Astrophysics Data System (ADS)

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

2017-04-01

This work reports the synthesis of MgxMn1-xFe2O4 (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.
Crystallization behaviour of nanostructured hybrid SiO2-TiO2 gel glasses to nanocomposites.

PubMed

Tsvetelina, Gerganova; Yordanka, Ivanova; Yuliya, Vueva; Miranda, Salvado Isabel M; Helena, Fernandes Maria

2010-04-01

The crystallization behaviour of hybrid SiO2-TiO2 nanocomposites derived from titanosiloxanes by sol-gel method has been investigated depending on the type of siloxane precursor and the pirolysis temperature. The resulting hybrid titanosiloxanes, crosslinked with trimethylsilil isocyanate (nitrogen-modified) or methyltrietoxisilane (carbon-modified), were pirolyzed in an inert atmosphere in the temperature range between 600 to 1100 degrees C in order to form C-(N)-Si-O-TiO2 nanocomposites. By means of XRD, FTIR, 29Si NMR, SEM, TEM and AFM investigations have been established that the transformation of the nanostructured SiO2-TiO2 hybrid materials into nanocomposites as well as the crystalline size depend on the titanium content and the type of cross-linking agents used in the synthesizes.
Sol-gel applications for ceramic membrane preparation

NASA Astrophysics Data System (ADS)

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.
Studies on modification of ZnO sol-gel spin coated on flexible substrate at low temperature: Effect of time exposure

NASA Astrophysics Data System (ADS)

Kamardin, Ili Liyana Khairunnisa; Ainuddin, Ainun Rahmahwati

2017-04-01

Transparent Conducting Oxide (TCO) Film has been chosen as flexible substrate recently in the application of a device. One of the TCO mostly used is ITO/PET substrates. Through this communication, the effect of time exposure of ZnO thin film by modified sol-gel deposited on flexible substrates was investigated. 0.75 M of NaOH and C6H8O7 were dropped directly into precursor solution right before aging process in order to modified precursor solution environment condition. x-ray diffraction pattern recorded plane (100) and (101) as preferential growth orientation. The (101) plane was selected to calculate the average crystallite. The atomic force microscopy indicated RMS value for NaOH samples increased with time exposure. Meanwhile, for C6H8O7 samples decreased with hot water treatment time exposure.
Sol-gel hybrid films based on organosilane and montmorillonite for corrosion inhibition of AA2024.

PubMed

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

2014-07-15

The present work reports the production of films on AA2024-T3 composed of vinyltrimethoxysilane (VTMS)/tetraethylorthosilicate (TEOS) with incorporation of montmorillonite (sodium montmorillonite and montmorillonite modified with quaternary ammonium salt, abbreviated Na and 30B, respectively), generated by the sol-gel process. According to FT-IR analyses the incorporation of montmorillonite does not affect silica network. Electrochemical characterization was performed by electrochemical impedance spectroscopy measurement in 0.05 mol L(-1) NaCl solution. Results indicate that montmorillonite incorporation improves the corrosion protection compared to the non-modified system. Scanning electron microscopy micrographs reveal that high concentrations of montmorillonite provide agglomerations on the metallic surface, which is in detriment of the anticorrosive performance. The VTMS/TEOS/30B films with the lowest concentration (22 mg L(-1)) of embedded clay provide the highest corrosion protection. Copyright © 2014 Elsevier Inc. All rights reserved.
Outdoor weathering of sol-gel-treated wood

Treesearch

Mandla A Tshabalala; Ryan Libert; Nancy Ross Sutherland

2009-01-01

Outdoor weathering of wood specimens treated with sol-gel formulations based on methyltrimethoxysilane (MTMOS), hexadecyltrimethoxysilane (HDTMOS), and ferric-zirconia-titania (Fe-Zr-Ti) sol was evaluated. The sol-gel process allowed deposition of a thin film of hybrid inorganic-organic networks (gel) in the wood cell wall that resulted in improved outdoor weathering...
Characterisation of well-adhered ZrO2 layers produced on structured reactors using the sonochemical sol-gel method

NASA Astrophysics Data System (ADS)

Jodłowski, Przemysław J.; Chlebda, Damian K.; Jędrzejczyk, Roman J.; Dziedzicka, Anna; Kuterasiński, Łukasz; Sitarz, Maciej

2018-01-01

The aim of this study was to obtain thin zirconium dioxide coatings on structured reactors using the sonochemical sol-gel method. The preparation method of metal oxide layers on metallic structures was based on the synergistic combination of three approaches: the application of ultrasonic irradiation during the synthesis of Zr sol-gel based on a precursor solution containing zirconium(IV) n-propoxide, the addition of stabilszing agents, and the deposition of ZrO2 on the metallic structures using the dip-coating method. As a result, dense, uniform zirconium dioxide films were obtained on the FeCrAlloy supports. The structured reactors were characterised by various physicochemical methods, such as BET, AFM, EDX, XRF, XRD, XPS and in situ Raman spectroscopy. The results of the structural analysis by Raman and XPS spectroscopy confirmed that the metallic surface was covered by a ZrO2 layer without any impurities. SEM/EDX mapping revealed that the deposited ZrO2 covered the metallic support uniformly. The mechanical and high temperature tests showed that the developed ultrasound assisted sol-gel method is an efficient way to obtain thin, well-adhered zirconium dioxide layers on the structured reactors. The prepared metallic supports covered with thin ZrO2 layers may be a good alternative to layered structured reactors in several dynamics flow processes, for example for gas exhaust abatement.
How to design cell-based biosensors using the sol-gel process.

PubMed

Depagne, Christophe; Roux, Cécile; Coradin, Thibaud

2011-05-01

Inorganic gels formed using the sol-gel process are promising hosts for the encapsulation of living organisms and the design of cell-based biosensors. However, the possibility to use the biological activity of entrapped cells as a biological signal requires a good understanding and careful control of the chemical and physical conditions in which the organisms are placed before, during, and after gel formation, and their impact on cell viability. Moreover, it is important to examine the possible transduction methods that are compatible with sol-gel encapsulated cells. Through an updated presentation of the current knowledge in this field and based on selected examples, this review shows how it has been possible to convert a chemical technology initially developed for the glass industry into a biotechnological tool, with current limitations and promising specificities.
Sol-gel chemistry-based Ucon-coated columns for capillary electrophoresis.

PubMed

Hayes, J D; Malik, A

1997-07-18

A sol-gel chemistry-based novel approach for the preparation of a Ucon-coated fused-silica capillary column in capillary electrophoresis is presented. In this approach the sol-gel process is carried out inside 25 microm I.D. fused-silica capillaries. The sol solution contained appropriate quantities of an alkoxide-based sol-gel precursor, a polymeric coating material (Ucon), a crosslinking reagent, a surface derivatizing reagent, controlled amounts of water and a catalyst dissolved in a suitable solvent system. The coating procedure involves filling a capillary with the sol solution and allowing the sol-gel process to proceed for an optimum period. Hydrolysis of the alkoxide precursor and polycondensation of the hydrolyzed products with the surface silanol groups and the hydroxy-terminated Ucon molecules lead to the formation of a surface-bonded sol-gel coating on the inner walls of the capillary. The thickness of the coated film can be controlled by varying the reaction time, coating solution composition and experimental conditions. Commercial availability of high purity sol-gel precursors (e.g., TEOS 99.999%), the ease of coating, run-to-run and column-to-column reproducibility, and long column lifetimes make sol-gel coating chemistry very much suitable for being applied in analytical microseparations column technology. Test samples of basic proteins and nucleotides were used to evaluate the column performance. These results show that the sol-gel coating scheme has allowed for the generation of bio-compatible surfaces characterized by high separation efficiencies in CE. For different types of solutes, the sol-gel coated Ucon column consistently provided migration time R.S.D. values of the order of 0.5%.
Sol-gel approach to in situ creation of high pH-resistant surface-bonded organic-inorganic hybrid zirconia coating for capillary microextraction (in-tube SPME).

PubMed

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

2005-01-07

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

PubMed

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

PubMed

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.
All optical controlled photonic integrated circuits using azo dye functionized sol-gel material

NASA Astrophysics Data System (ADS)

Ke, Xianjun

The main focus of this dissertation is development and characterization of all-optical controllable azo dye functionized sol gel material, demonstrating a PIC fabrication technique on glass substrate using such material, and exploration and feasibility demonstration of three PIC functional devices namely optical variable attenuator, optical switches, and optical tunable filters using the material. The realization of all the devices in this dissertation are based on one material: dye functionalized sol-gel material. A photochromic sol-gel material functionalized with azo dye was synthesized and characterized. It possesses a photochromic characteristic under the control of green laser beam illumination. The material characteristics suggest the possibility of a new promising material platform candidate for the fabrication of alloptical controlled photonic integrated circuits. As the first potential application of the dye functionalized sol-gel material, an alloptical variable attenuator was designed and demonstrated. The optical variable attenuation is achieved in Mach-Zehnder interferometric configuration through all-optical modulation of sol-gel waveguide phase shifters. A 2 x 2 optical switch based on multimode interference (MMI) waveguide structure is proposed in the dissertation. The schematic configuration of the optical switch consists of a cascade of two identical MMIs with two all-optical controlled phase shifters realized by using the photochromic sol-gel material. The cross or bar switch state of the optical switch is determined by the phase difference between the two sol-gel waveguide phase shifters. An all-optical tunable filter is designed and its feasibility demonstrated by using the sol-gel photochromic material. Except for the phase change demonstrated on sol-gel waveguide phase shifters, dynamic gratings were observed on sol-gel film when exposed to two interference beams. This reveals the possibility of realizing Bragg grating-based tunable filters. The schematic configuration of proposed tunable filters consists of a single straight waveguide embedded with a sol-gel waveguide. The wavelength tuning of the tunable filters is accomplished by varying the grating period.

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

NASA Astrophysics Data System (ADS)

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

2014-05-01

The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of the sol-gel approach.The entrapment of lipases in hydrophobic silicate matrices formed by sol-gel mediated hydrolysis of RSi(OCH3)3/Si(OCH3)4 as originally reported in 1996 has been improved over the years by a number of modifications. In the production of second-generation sol-gel lipase immobilizates, a variety of additives during the sol-gel process leads to increased activity and enhanced stereoselectivity in esterifying kinetic resolution. Recent advances in this type of lipase immobilization are reviewed here, in addition to new results regarding the sol-gel entrapment of the lipase from Burkholderia cepacia. It constitutes an excellent heterogeneous biocatalyst in the acylating kinetic resolution of two synthetically and industrially important chiral alcohols, rac-sulcatol and rac-trans-2-methoxycyclohexanol. The observation that the catalyst can be used 10 times in recycling experiments without losing its significant activity or enantioselectivity demonstrates the practical viability of the sol-gel approach. Dedicated to the pioneer of sol-gel enzyme immobilization, Professor David Avnir, on the occasion of his 65th birthday.
Structural and morphological characterization of anatase TiO 2 coating on χ-Alumina scale fiber fabricated by sol-gel dip-coating method

NASA Astrophysics Data System (ADS)

Nguyen, Hue Thi; Miao, Lei; Tanemura, Sakae; Tanemura, Masaki; Toh, Shoichi; Kaneko, Kenji; Kawasaki, Masahiro

2004-10-01

Anatase TiO 2 coatings 0.4 μm thick have been successfully fabricated by sol-gel dip-coating process on χ-Al 2O 3 fibers 100 μm by 10 cm long with a surface fish-scale. This was achieved by adjustment of the sol-gel parameters such as molar ratio of the precursors in TiO 2-sols, dip-coating time, drying duration in air, heating processes and number of cyclical repetitions of the process. Two samples were prepared using two sols containing different molar ratios of precursors. XRD, TEM, EDS and SEM characterization confirmed: (1) the similarity of the growth of anatase-TiO 2 from two sols under the optimal sol-gel parameters, (2) that the coatings are composed of aggregated crystallites of 10-25 nm in diameter, (3) the good compositional uniformity of Ti in the fabricated anatase-TiO 2 crystallites, (4) a surface covering ratio of anatase-TiO 2 around the fiber of at least 90%, and (5) that there is a good adherence of the fabricated anatase-TiO 2 layer on alumina fiber as evidenced by the lack of cracking and peeling off traces around the boundary between the coating and the fiber.
A novel tantalum-based sol-gel packed microextraction syringe for highly specific enrichment of phosphopeptides in MALDI-MS applications.

PubMed

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 was packed into a standard syringe (0.5 mL) to enhance the ease of use of the sol-gel material and for the elimination of additional mixing and separation procedures during the adsorption, washing and elution steps of the enrichment procedure. It was found that up to 28 phosphopeptides in milk digest were easily detectable by MALDI-MS at femtomole levels (around 20 fmol) using the microextraction syringe within less than one minute.
Method for fabrication of ceramic dielectric films on copper foils

DOEpatents

Ma, Beihai; Narayanan, Manoj; Dorris, Stephen E.; Balachandran, Uthamalingam

2017-06-14

The present invention provides copper substrate coated with a lead-lanthanum-zirconium-titanium (PLZT) ceramic film, which is prepared by a method comprising applying a layer of a sol-gel composition onto a copper foil. The sol-gel composition comprises a precursor of a ceramic material suspended in 2-methoxyethanol. The layer of sol-gel is then dried at a temperature up to about 250.degree. C. The dried layer is then pyrolyzed at a temperature in the range of about 300 to about 450.degree. C. to form a ceramic film from the ceramic precursor. The ceramic film is then crystallized at a temperature in the range of about 600 to about 750.degree. C. The drying, pyrolyzing and crystallizing are performed under a flowing stream of an inert gas.
Optical properties of Na2O-TiO2-SiO2 glass films prepared by the sol-gel method

NASA Astrophysics Data System (ADS)

Barton, Ivo; Matejec, Vlastimil; Mrazek, Jan; Predoana, Luminita; Zaharescu, Maria

2017-12-01

Layers based on TiO2-SiO2 systems fabricated by sol-gel method have been investigated for the preparation of planar waveguides, antireflective coatings, Bragg mirrors, etc. However, at high titania contents such materials exhibit high viscosities and tendency to phase separation. In this paper we present optical properties of films containing TiO2 which are prepared via a novel approach sol-gel on the basis of ternary Na2O-TiO2-SiO2 glasses and which can exhibit lower viscosities. Films of Na2O-TiO2-SiO2 systems were prepared from input sols mixed of silica, titania and sodium oxide sols. The silica sol was prepared from tetraethyl orthosilicate (TEOS), ethanol, hydrochloric acid and water, with a TEOS c= 2 mol/l and water/alkoxide ratio 1.75. The titania sol was mixed from titanium tetraisopropoxide (TiPr), propan-2-ol, nitric acid and water, c= 0.5 mol/l, RW= 0.42. The sodium oxide sols with c= 0.474 mol/l were prepared from sodium ethoxide and ethanol. Input sols were prepared by mixing the silica and titania sols first and then the sodium sol was added. The input sols were aged for one hour. Stable input sols were obtained. The input sols were deposited on glass and silica slides by dip-coating technique at a withdrawing speeds of 200 mm/min. Applied gel layers were thermally treated at temperatures of 450 and 900°C. Layers containing sodium oxide and titania in concentration ranges of 0-20 mol.% and 0-30 mol.% respectively have been fabricated. Optical properties of layers were determined by UV-VIS-NIR transmission and reflection spectrophotometry. Refractive indices of layers were determined by spectral ellipsometry and from transmission spectra. Optical properties were correlated with results of XRD spectroscopy, optical microscopy, and atomic force microscopy. Transparent homogenous films with a maximum refractive index of 1.61 at a wavelength of 600 nm have been obtained.
Determination of Aromatic Amines Using Solid-Phase Microextraction Based on an Ionic Liquid-Mediated Sol-Gel Technique.

PubMed

Abbasi, Vajihe; Sarafraz-Yazdi, Ali; Amiri, Amirhassan; Vatani, Hossein

2016-04-01

A headspace solid-phase microextraction (HS-SPME) method was developed for isolation of monocyclic aromatic amines from water samples followed by gas chromatography-flame ionization detector (GC-FID). In this work, the effect of the presence of ionic liquid (namely, 1-hexyl-3-methyl-imidazolium hexafluorophosphate [C6MIM][PF6]) was investigated in the sol-gel coating solutions on the morphology and extraction behavior of the resulting hybrid organic-inorganic sol-gel sorbents utilized in SPME. Hydroxy-terminated poly(dimethylsiloxane) (PDMS) was used as the sol-gel active organic component for sol-gel hybrid coatings. Two different coated fibers that were prepared are PDMS and PDMS-IL ([C6MIM][PF6]) fibers. Under the optimal conditions, the method detection limits (S/N = 3) with PDMS-IL were in the range of 0.001-0.1 ng/mL and the limits of quantification (S/N = 10) between 0.005 and 0.5 ng/mL. The relative standard deviations for one fiber (n = 5) were obtained from 3.1 up to 8.5% and between fibers or batch to batch (n = 3) in the range of 5.3-10.1%. The developed method was successfully applied to real water and juice fruits samples while the relative recovery percentages obtained for the spiked water samples at 0.1 ng/mL were from 83.3 to 95.0%. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
Diamond nanoparticles as a way to improve electron transfer in sol-gel L-lactate biosensing platforms.

PubMed

Briones, M; Casero, E; Vázquez, L; Pariente, F; Lorenzo, E; Petit-Domínguez, M D

2016-02-18

In the present work, we have included for the first time diamond nanoparticles (DNPs) in a sol-gel matrix derived from (3-mercaptopropyl)-trimethoxysilane (MPTS) in order to improve electron transfer in a lactate oxidase (LOx) based electrochemical biosensing platform. Firstly, an exhaustive AFM study, including topographical, surface potential (KFM) and capacitance gradient (CG) measurements, of each step involved in the biosensing platform development was performed. The platform is based on gold electrodes (Au) modified with the sol-gel matrix (Au/MPTS) in which diamond nanoparticles (Au/MPTS/DNPs) and lactate oxidase (Au/MPTS/DNPs/LOx) have been included. For the sake of comparison, we have also characterized a gold electrode directly modified with DNPs (Au/DNPs). Secondly, the electrochemical behavior of a redox mediator (hydroxymethyl-ferrocene, HMF) was evaluated at the platforms mentioned above. The response of Au/MPTS/DNPs/LOx towards lactate was obtained. A linear concentration range from 0.053 mM to 1.6 mM, a sensitivity of 2.6 μA mM(-1) and a detection limit of 16 μM were obtained. These analytical properties are comparable to other biosensors, presenting also as advantages that DNPs are inexpensive, environment-friendly and easy-handled nanomaterials. Finally, the developed biosensor was applied for lactate determination in wine samples. Copyright © 2016 Elsevier B.V. All rights reserved.
The low temperature synthesis, characterization and properties of ferroelectrics

NASA Astrophysics Data System (ADS)

Xu, Jie

2000-10-01

PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.
Sol-Gel deposition of inorganic alkoxides on wood surfaces to enhance their durability under exposure to sunlight and moisture

Treesearch

Mandla A. Tshabalala

2005-01-01

Wood specimens were coated with sol-gel deposits of aluminum isopropoxide, titanium isopropoxide, or zirconium propoxide in the presence of methytrimethoxysilane. Both zirconium propoxide and titanium isopropoxide sol-gel deposits reduced water sorption, whereas aluminum isopropoxide sol-gel deposit increased water sorption, compared with uncoated wood specimens. There...
Agar/gelatin bilayer gel matrix fabricated by simple thermo-responsive sol-gel transition method.

PubMed

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.
Synthesis and properties of nanostructured sol-gel sorbents for simultaneous removal of sulfur dioxide and nitrogen oxides from flue gas

NASA Astrophysics Data System (ADS)

Buelna Quijada, Genoveva

2001-07-01

Regenerative, alumina-supported, copper-based sorbent/catalysts provide a promising technique for simultaneous removal of SO2 and NO x from flue gas. These sorbents can remove over 90% of SO2 and 70+% of NOx while generating no wastes, reducing energy consumption, and producing valuable by-products. The lack of a cost-effective sorbent with low attrition rate and good reactivity has been the main hurdle to commercialization of this copper oxide process. Developing such a sorbent is the focus of this dissertation. This work examines using sol-gel techniques rather than traditional processes to produce gamma-alumina and copper coated 7-alumina granular sorbents. Important modifications to the established sol-gel synthesis process were made, which minimized generated wastes and reduced preparation time and sorbent cost. A laboratory scale semi-continuous process providing a basis for large-scale synthesis was developed. The effect of the copper content on the surface area and dispersion of the active species on sol-gel-derived sorbents coated by the one step and wet-impregnation methods was studied. The sol-gel-derived sorbents showed superior sulfation and regeneration properties than the existing commercial sorbents used in the copper oxide process in terms of sulfation capacity, fast regeneration, recovery of sorption capacity, and SO2 concentration in the regenerated effluent. The optimum temperature for NO reduction by NH3 over sol-gel-derived CuO/gamma-Al2O3 was found to be 350°C for both fresh and sulfated catalysts. This was also the optimum operating temperature for simultaneous removal of SO2 and NOx from simulated flue gas. At 350°C, the adsorption capacity of the sol-gel sorbent/catalyst was higher than UOP's sorbent, and very close to the capacity of ALCOA's sorbent, while the catalytic activity for NO reduction of the sol-gel-derived CuO/gamma-Al 2O3 sorbent fell between the commercial sorbents. The new mesoporous sol-gel-derived materials showed larger surface area, better mechanical strength, and more uniform dispersion of the copper species than existing commercially available sorbents. The superior mechanical properties, better cost effectiveness, and comparable efficiency for simultaneous removal of SO2 and NOx of the sol-gel-derived CuO/gamma-Al 2O3 sorbents with respect to the commercial ones make them a good option for use in the copper oxide process for combined removal of SO2 and NOx from flue gas.
Sol-Gel Synthesis of Non-Silica Monolithic Materials

PubMed Central

Gaweł, Bartłomiej; Gaweł, Kamila; Øye, Gisle

2010-01-01

Monolithic materials have become very popular because of various applications, especially within chromatography and catalysis. Large surface areas and multimodal porosities are great advantages for these applications. New sol-gel preparation methods utilizing phase separation or nanocasting have opened the possibility for preparing materials of other oxides than silica. In this review, we present different synthesis methods for inorganic, non-silica monolithic materials. Some examples of application of the materials are also included.
Sintering and microstructure of silicon carbide ceramic with Y3Al5O12 added by sol-gel method*

PubMed Central

Guo, Xing-zhong; Yang, Hui

2005-01-01

Silicon carbide (SiC) ceramic with YAG (Y3Al5O12) additive added by sol-gel method was liquid-phase sintered at different sintering temperatures, and the sintering mechanism and microstructural characteristics of resulting silicon carbide ceramics were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and elemental distribution of surface (EDS). YAG (yttrium aluminum garnet) phase formed before the sintering and its uniform distribution in the SiC/YAG composite powder decreased the sintering temperature and improved the densification of SiC ceramic. The suitable sintering temperature was 1860 °C with the specimen sintered at this temperature having superior sintering and mechanical properties, smaller crystal size and fewer microstructure defects. Three characteristics of improved toughness of SiC ceramic with YAG added by sol-gel method were microstructural densification, main-crack deflection and crystal ‘bridging’. PMID:15682507
Sol-gel based oxidation catalyst and coating system using same

NASA Technical Reports Server (NTRS)

Leighty, Bradley D. (Inventor); Watkins, Anthony N. (Inventor); Patry, JoAnne L. (Inventor); Schryer, Jacqueline L. (Inventor); Oglesby, Donald M. (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.
Synthesis and Microstructure of Highly Oriented PbTiO3 Thin Films Prepared by a Sol-Gel Method

DTIC Science & Technology

1989-06-01

lead acetate with titanium isopropoxide * in 2-methoxyethanol,* in a method similar to that reported by Gurkovitch and Blum." The resulting yellow-gold...orientation by a sol-gel processing method. EXPERIMENTAL Precursor Solution Preparation Stock solutions of complex Pb-Ti alkoxide were prepared by reacting... solution had an equivalent PbTiO 3 concentration of approximately 66 wt%. The alkoxide solutions were handled as moisture-sensitive reagents and, as
Oxide Ceramic Fibers by the Sol-Gel Methods

DTIC Science & Technology

1989-02-10

AFWAL-TR-88-4199 OXIDE CERAMIC FIBERS BY THE SOL-GEL METHOD J . D. Mackenzie If) K. Ono The Regents of the University of California (Los Angeles) V...METHOD 12. PERSONAL AUTHOR(S) J . D. MACKENZIE, K. ONO 13a. TYPE OF REPORT 13b. TIME COVERED 114. DATE OF REPORT (Year,Month, Day) 15. PAGE COUNT...to Mary Colby who performed, under the direction of J . D. Mackenzie, the bulk of the experimental studies and contributed extensively to the
Comparative study of RF reactive magnetron sputtering and sol-gel deposition of UV induced superhydrophilic TiOx thin films

NASA Astrophysics Data System (ADS)

Vrakatseli, V. E.; Amanatides, E.; Mataras, D.

2016-03-01

TiOx and TiOx-like thin films were deposited on PEEK (Polyether ether ketone) substrates by low-temperature RF reactive magnetron sputtering and the sol-gel method. The resulting films were compared in terms of their properties and photoinduced hydrophilicity. Both techniques resulted in uniform films with good adhesion that can be switched to superhydrophilic after exposure to UVA radiation for similar time periods. In addition, the sputtered films can also be activated and switched to superhydrophilic by natural sunlight due to the higher absorption in the visible spectrum compared to the sol-gel films. On the other hand, the as deposited sol-films remain relatively hydrophilic for a longer time in dark compared to the sputtered film due to the differences in the morphology and the porosity of the two materials. Thus, depending on the application, either method can be used in order to achieve the desirable TiOx properties.
Application of Sol-Gel Method as a Protective Layer on a Specular Reflective Surface for Secondary Reflector in a Solar Receiver

DOE Office of Scientific and Technical Information (OSTI.GOV)

Afrin, Samia; Dagdelen, John; Ma, Zhiwen

Highly-specular reflective surfaces that can withstand elevated-temperatures are desirable for many applications including reflective heat shielding in solar receivers and secondary reflectors, which can be used between primary concentrators and heat collectors. A high-efficiency, high-temperature solar receiver design based on arrays of cavities needs a highly-specular reflective surface on its front section to help sunlight penetrate into the absorber tubes for effective flux spreading. Since this application is for high-temperature solar receivers, this surface needs to be durable and to maintain its optical properties through the usable life. Degradation mechanisms associated with elevated temperatures and thermal cycling, which include cracking,more » delamination, corrosion/oxidation, and environmental effects, could cause the optical properties of surfaces to degrade rapidly in these conditions. Protected mirror surfaces for these applications have been tested by depositing a thin layer of SiO2 on top of electrodeposited silver by means of the sol-gel method. To obtain an effective thin film structure, this sol-gel procedure has been investigated extensively by varying process parameters that affect film porosity and thickness. Endurance tests have been performed in a furnace at 150 degrees C for thousands of hours. This paper presents the sol-gel process for intermediate-temperature specular reflective coatings and provides the long-term reliability test results of sol-gel protected silver-coated surfaces.« less
Sol-gel modification of wood substrates to retard weathering

Treesearch

Mandla A Tshabalala; Sam Williams

2008-01-01

Wood specimens were treated with sol-gel systems based on metalorganic precursors of silicon (Si), iron (Fe), zirconium (Zr), and titanium (Ti). The effect of these sol-gel systems on weathering properties of wood was investigated. These sol-gel systems were found to have a positive effect on surface color stability and water vapor resistance of the specimens. Under...
rhEGF-containing thermosensitive and mucoadhesive polymeric sol-gel for endoscopic treatment of gastric ulcer and bleeding.

PubMed

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.

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

PubMed

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
Hydrophobicity of hemp shiv treated with sol-gel coatings

NASA Astrophysics Data System (ADS)

Hussain, Atif; Calabria-Holley, Juliana; Schorr, Diane; Jiang, Yunhong; Lawrence, Mike; Blanchet, Pierre

2018-03-01

This is the first time sol-gel technology is used in the treatment of hemp shiv to develop sustainable thermal insulation building materials. The impact on the hydrophobicity of hemp shiv by depositing functionalised sol-gel coatings using hexadecyltrimethoxysilane (HDTMS) has been investigated. Bio-based materials have tendency to absorb large amounts of water due to their hydrophilic nature and highly porous structure. In this work, the influence of catalysts, solvent dilution and HDTMS loading in the silica sols on the hydrophobicity of hemp shiv surface has been reported. The hydrophobicity of sol-gel coated hemp shiv increased significantly when using acid catalysed sols which provided water contact angles of up to 118° at 1% HDTMS loading. Ethanol diluted sol-gel coatings enhanced the surface roughness of the hemp shiv by 36% as observed under 3D optical profilometer. The XPS results revealed that the surface chemical composition of the hemp shiv was altered by the sol-gel coating, blocking the hydroxyl sites responsible for hydrophilicity.
Fabrication and characterization of highly transparent and conductive indium tin oxide films made with different solution-based methods

NASA Astrophysics Data System (ADS)

Xia, N.; Gerhardt, R. A.

2016-11-01

Solution-based fabrication methods can greatly reduce the cost and broaden the applications of transparent conducting oxides films, such as indium tin oxide (ITO) films. In this paper, we report on ITO films fabricated by spin coating methods on glass substrates with two different ITO sources: (1) a commercial ITO nanopowder water dispersion and (2) a sol-gel ITO solution. A simple and fast air annealing process was used to treat as-coated ITO films on a controlled temperature hot plate. Thermogravimetric analysis and x-ray diffraction showed that highly crystalline ITO films were formed after the annealing steps. The final ITO films had a good combination of optical properties and electrical properties, especially for films made from five layers of sol-gel ITO (92.66% transmittance and 8.7 × 10-3 Ω cm resistivity). The surface morphology and conducting network on the ITO films were characterized by non-contact and current atomic force microscopy. It was found that conducting paths were only partially connected for the nanoparticle ITO dispersion films, whereas the sol-gel ITO films had a more uniformly distributed conducting network on the surface. We also used the sol-gel ITO films to fabricate a simple liquid crystal display (LCD) device to demonstrate the excellent properties of our films.
Optical Fiber Chemical Sensor with Sol-Gel Derived Refractive Material as Transducer for High Temperature Gas Sensing in Clean Coal Technology

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 fibermore » 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 fiber optic sensors uses sol-gel derived porous silica materials doped with nanometer particles of noble metals in the form of fiber or coating for sensing trace H{sub 2}, NH{sub 3} and HCl in gas samples at for applications ambient temperature. The third classes of fiber optic sensors use sol-gel derived semiconductor metal oxide coating on the surface of silica optical fiber as transducers for selectively sensing H{sub 2}, CH{sub 4} and CO at high temperature. In addition, optical fiber temperature sensors use the fluorescence signal of rare-earth metal ions doped porous silica optical fiber or the optical absorption signal of thermochromic metal oxide materials coated on the surface of silica optical fibers have also been developed for monitoring gas temperature of corrosive gas. Based on the results obtained from this project, the principle of fiber optic sensor techniques for monitoring matrix gas components as well as trace components of coal gasification derived syngas has been established. Prototype sensors for sensing trace ammonia and hydrogen sulfide in gasification derived syngas have been built up in our laboratory and have been tested using gas samples with matrix gas composition similar to that of gasification derived fuel gas. Test results illustrated the feasibility of these sensors for applications in IGCC processes.« less
Synthesis and Properties of Carbon Nanotube-Grafted Silica Nanoarchitecture-Reinforced Poly(Lactic Acid)

PubMed Central

Hsu, Yao-Wen; Wu, Chia-Ching; Wu, Song-Mao

2017-01-01

A novel nanoarchitecture-reinforced poly(lactic acid) (PLA) nanocomposite was prepared using multi-walled carbon nanotube (MWCNT)-grafted silica nanohybrids as reinforcements. MWCNT-grafted silica nanohybrids were synthesized by the generation of silica nanoparticles on the MWCNT surface through the sol-gel technique. This synthetic method involves organo-modified MWCNTs that are dispersed in tetrahydrofuran, which incorporates tetraethoxysilane that undergoes an ultrasonic sol-gel process. Gelation yielded highly dispersed silica on the organo-modified MWCNTs. The structure and properties of the nanohybrids were established using 29Si nuclear magnetic resonance, Raman spectroscopy, wide-angle X-ray diffraction, thermogravimetric analysis, and transmission electron microscopy. The resulting MWCNT nanoarchitectures were covalently assembled into silica nanoparticles, which exhibited specific and controllable morphologies and were used to reinforce biodegradable PLA. The tensile strength and the heat deflection temperature (HDT) of the PLA/MWCNT-grafted silica nanocomposites increased when the MWCNT-grafted silica was applied to the PLA matrix; by contrast, the surface resistivity of the PLA/MWCNT-grafted silica nanocomposites appeared to decline as the amount of MWCNT-grafted silica in the PLA matrix increased. Overall, the reinforcement of PLA using MWCNT-grafted silica nanoarchitectures was efficient and improved its mechanical properties, heat resistance, and electrical resistivity. PMID:28773187
Effects of ion irradiation on the surface mechanical behavior of hybrid sol-gel derived silicate thin films

NASA Astrophysics Data System (ADS)

Ghisleni, Rudy

A study on the effects of ion irradiation on the surface mechanical behavior of hybrid sol-gel derived thin films has been performed. Hybrid organic/inorganic modified silicate thin films were synthesized by sol-gel processing from tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES) precursors and spin-coated onto (100) Si substrates. The synthesized films were investigated by nanoindentation, photoluminescence spectroscopy, and Raman spectroscopy. Hybrid TEOS/MTES sol-gel films modified by ion irradiation with deposited electronic energies of 1.87 x 1025 eV/cm3 or higher showed higher values of reduced elastic modulus and hardness than 800°C heat treated films. Thus, ion irradiation was found to be an effective means in converting the polymer sol into ceramic type coatings. The ions used in this study were Cu2+, N2+, Si+, O+, N+, He+, and H+, with incident energies ranging from 100 keV to 2 MeV, and fluences ranging from 1 x 1014 to 1 x 1017 ions/cm2. Both the reduced elastic modulus and hardness were seen to increase monotonically with the increase in ion fluence, with an observed maximum hardness of 7.7 GPa (an unirradiated film hardness was 0.4 GPa) and a maximum reduced elastic modulus of 84.0 GPa (an unirradiated film reduced elastic modulus was 7.1 GPa) for 250 keV N2+ irradiation with a 5 x 1016 ions/cm2 fluence. The electronic stopping power was found to be principally responsible for the film hardening, while the role of nuclear stopping power was minimal. A monotonic increase in hardness with increase in electronic energy deposited to the film surface was found. A model describing the hardening of ion irradiated films was developed. This model characterizes the hardening effectiveness of the ion species considered by two parameters: the constant hardening cross-section and the hardening coefficient. Where the hardening cross-section represents the cross-sectional area hardened by the interaction of an incident ion with the target, and the hardening coefficient represents an index of the cross-sectional area gradient as a function of fluence. The increase in hardness of hybrid sol-gel films following ion irradiation was linked to structural changes. Ion irradiation results in a cross-linked silica film as well as the segregation of amorphous carbon clusters, both of which contributed to increase the mechanical properties of the films.
Effect of Adding SiO2-Al2O3 Sol into Anodizing Bath on Corrosion Resistance of Oxidation Film on Magnesium Alloy

NASA Astrophysics Data System (ADS)

Liu, Huicong; Zhu, Liqun; Li, Weiping

Due to the widely use in automobile and construction field, AZ91D magnesium alloy need to be protected more effectively for its high chemical activity. In this paper, three kinds of films were formed on magnesium alloy. The first kind of film, named as anodic oxidation film, was prepared by anodic oxidation in the alkaline solution. The processes for preparing the second kind of film, named as multiple film, involved coating sol-gel on the samples and heat-treating before anodic oxidation. The third kind of film was prepared by anodic oxidation in the alkaline oxidation solution containning 5% (vol) SiO2-Al2O3 sol, named as modified oxidation film. The corrosion resistance of the three different films was investigated. The results showed that the modified oxidation film had the highest corrosion resistance due to the largest thickness and most dense surface morphology. Sol was discussed to react during the film forming process, which leaded to the difference between modified oxidation film and anodic oxidation film.
Synthesis and Study of Gel Calcined Cd-Sn Oxide Nanocomposites

NASA Astrophysics Data System (ADS)

De, Arijit; Kundu, Susmita

2016-07-01

Cd-Sn oxide nanocomposites were synthesized by sol-gel method from precursor sol containing Cd:Sn = 2:1 and 1:1 mol ratio. Instead of coprecipitation, a simple novel gel calcination route was followed. Cd (NO3)2. 4H2O and SnCl4. 5H2O were used as starting materials. Gel was calcined at 1050 °C for 2 h to obtain nanocomposites. XRD analysis reveals the presence of orthorhombic, cubic Cd2SnO4 along with orthorhombic, hexagonal CdSnO3 phases in both the composites. SEM and TEM studies indicate the development of nanocomposites of different shapes suggesting different degrees of polymerization in precursor sol of different composition. UV-Vis absorption spectra show a blue shift for both the composites compared to bulk values. Decrease of polarization with frequency, dipole contribution to the polarization, and more sensitivity to ethanol vapor were observed for the nanocomposite derived from precursor sol containing Cd:Sn = 2:1 mol ratio.
Sol-gel titania-coated needles for solid phase dynamic extraction-GC/MS analysis of desomorphine and desocodeine.

PubMed

Su, Chi-Ju; Srimurugan, Sankarewaran; Chen, Chinpiao; Shu, Hun-Chi

2011-01-01

Novel sol-gel titania film coated needles for solid-phase dynamic extraction (SPDE)-GC/MS analysis of desomorphine and desocodeine are described. The high thermal stability of titania film permits efficient extraction and analysis of poorly volatile opiate drugs. The influences of sol-gel reaction time, coating layer, extraction and desorption time and temperature on the SPDE needle performance were investigated. The deuterium labeled internal standard was introduced either during the extraction of analyte or directly injected to GC after the extraction process. The latter method was shown to be more sensitive for the analysis of water and urine samples containing opiate drugs. The proposed conditions provided a wide linear range (from 5-5000 ppb), and satisfactory linearity, with R(2) values from 0.9958 to 0.9999, and prominent sensitivity, LOQs (1.0-5.0 ng/g). The sol-gel titania film coated needle with SPDE-GC/MS will be a promising technique for desomorphine and desocodeine analysis in urine.
Generation of a mesoporous silica MSU shell onto solid core silica nanoparticles using a simple two-step sol-gel process.

PubMed

Allouche, Joachim; Dupin, Jean-Charles; Gonbeau, Danielle

2011-07-14

Silica core-shell nanoparticles with a MSU shell have been synthesized using several non-ionic poly(ethylene oxide) based surfactants via a two step sol-gel method. The materials exhibit a typical worm-hole pore structure and tunable pore diameters between 2.4 nm and 5.8 nm.
Cholesterol biosensor based on a plastic optical fibre with sol-gel: structural analysis and sensing properties

NASA Astrophysics Data System (ADS)

Razo-Medina, D. A.; Trejo-Durán, M.; Alvarado-Méndez, E.

2018-02-01

In this paper, we report the design and characterization of an optical fibre cholesterol biosensor by using sol-gel immobilization technique. The cholesterol enzyme is encapsulated inside of the sol-gel film onto an end of a plastic optical fibre. Two film deposition methods (Dip-Coating and Immersion) were studied. The morphology analysis and sensing properties permit us to determine the best film deposition to sense cholesterol concentration. The range of measured is 4.4-5.2 mM in real time and our results were validated by comparing them with other previously published results. The biosensor is portable, simple cheap, and easy to use.
An investigation of GaN thin films on AlN on sapphire substrate by sol-gel spin coating method

NASA Astrophysics Data System (ADS)

Amin, Nur Fahana Mohd; Ng, Sha Shiong

2017-12-01

In this research, the gallium nitride (GaN) thin films were deposited on aluminium nitride on sapphire (AlN/Al2O3) substrate by sol-gel spin coating method. Simple ethanol-based precursor with the addition of diethanolamine solution was used. The structural and morphology properties of synthesized GaN thin films were characterized by using X-ray Diffraction, Field-Emission Scanning Electron Microscopy and Atomic Force Microscopy. While the elemental compositions and the lattice vibrational properties of the films were investigated by means of the Energy Dispersive X-ray spectroscopy and Raman spectroscopy. All the results revealed that the wurtzite structure GaN thin films with GaN(002) preferred orientation and smooth surface morphology were successfully grown on AlN/Al2O3 substrate by using inexpensive and simplified sol-gel spin coating technique. The sol-gel spin coated GaN thin film with lowest oxygen content was also achieved.FESEM images show that GaN thin films with uniform and packed grains were formed. Based on the obtained results, it can be concluded that wurtzite structure GaN thin films were successfully deposited on AlN/Al2O3 substrate.
Investigation of Annealing Temperature on Copper Oxide Thin Films Using Sol-Gel Spin Coating Technique

NASA Astrophysics Data System (ADS)

Hashim, H.; Samat, S. F. A.; Shariffudin, S. S.; Saad, P. S. M.

2018-03-01

Copper (II) Oxide or cupric oxide (CuO) is one of the well-known materials studied for thin films applications. This paper was studied on the effect of annealing temperature to CuO thin films using sol-gel method and spin coating technique. The solution was prepared by sol-gel method and the thin films were synthesized at various temperatures from 500°C to 700°C that deposited onto the quartz substrates. After the annealing process, the thin films were uniform and brownish black in colour. The measurements were performed by atomic force microscopy (AFM), surface profiler (SP), two-point probe and Ultraviolet-visible (UV-Vis-NIR) spectrometer. From the optical measurement, the band gap was estimated to be 1.44eV for sample annealed at 550°C.
Solventless sol-gel chemistry through ring-opening polymerization of bridged disilaoxacyclopentanes

DOE Office of Scientific and Technical Information (OSTI.GOV)

RAHIMIAN,KAMYAR; LOY,DOUGLAS A.

2000-04-04

Disilaoxacyclopentanes have proven to be excellent precursors to sol-gel type materials. These materials have shown promise as precursors for encapsulation and microelectronics applications. The polymers are highly crosslinked and are structurally similar to traditional sol-gels, but unlike typical sol-gels they are prepared without the use of solvents and water, they have low VOC's and show little shrinkage during processing.
Effect of complexing agents on the electrochemical performance of LiFePO4/C prepared by sol-gel method

PubMed Central

2012-01-01

LiFePO4/C is synthesized via sol-gel method using Fe3+ as iron sources and different complexing agents, followed by sintering at high temperature for crystallization. The amount of carbon in these composites is less than 6.8 wt.%, and the X-ray diffraction experiment confirms that all samples are pure single phase indexed with the orthorhombic Pnma space group. The particle size of the LiFePO4/C synthesized by acetic acid as a complexing agent is very fine with a size of 200 nm. The electrochemical performance of this material, including reversible capacity, cycle number, and charge-discharge characteristics, is better than those of LiFePO4/C synthesized by other complexing agents. The cell of this sample can deliver a discharge capacity of 161.1 mAh g-1 at the first cycle. After 30 cycles, the capacity decreases to 157.5 mAh g-1, and the capacity fading rate is 2.2%. The mechanism is studied to explain the effect of a complexing agent on the synthesis of LiFePO4/C by sol-gel method. The results show that the complexing agent with a low stability constant may be proper for the synthetic process of LiFePO4/C via sol-gel method. PMID:22221711
Effect of complexing agents on the electrochemical performance of LiFePO4/C prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Yang, Rong; Kang, Erwei; Jiang, Bailing; Ahn, Jou-Hyeon

2012-01-01

LiFePO4/C is synthesized via sol-gel method using Fe3+ as iron sources and different complexing agents, followed by sintering at high temperature for crystallization. The amount of carbon in these composites is less than 6.8 wt.%, and the X-ray diffraction experiment confirms that all samples are pure single phase indexed with the orthorhombic Pnma space group. The particle size of the LiFePO4/C synthesized by acetic acid as a complexing agent is very fine with a size of 200 nm. The electrochemical performance of this material, including reversible capacity, cycle number, and charge-discharge characteristics, is better than those of LiFePO4/C synthesized by other complexing agents. The cell of this sample can deliver a discharge capacity of 161.1 mAh g-1 at the first cycle. After 30 cycles, the capacity decreases to 157.5 mAh g-1, and the capacity fading rate is 2.2%. The mechanism is studied to explain the effect of a complexing agent on the synthesis of LiFePO4/C by sol-gel method. The results show that the complexing agent with a low stability constant may be proper for the synthetic process of LiFePO4/C via sol-gel method.
Low temperature synthesis of CaO-SiO2 glasses having stable liquid-liquid immiscibility by sol-gel process

NASA Technical Reports Server (NTRS)

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

NASA Technical Reports Server (NTRS)

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.
Synthesis and thermochromic property studies on W doped VO2 films fabricated by sol-gel method.

PubMed

Pan, Guoping; Yin, Jinhua; Ji, Keli; Li, Xiang; Cheng, Xingwang; Jin, Haibo; Liu, Jiping

2017-07-21

Tungsten-doped VO 2 thin films have been synthesized by a modified sol-gel process and followed by a post annealing. Vanadium pentoxide and tungstic acid as raw materials with the addition of hydrogen peroxide, concentrated hydrochloric acid (catalyst) and oxalic acid used as reducing agent were reacted in isobutanol. Finally, the uniform sol of vanadyl oxalate in isobutanol solvent was obtained as precursor. Detailed study suggested that W doped in VO 2 introduces additional electron carriers and induces the formation of V 3+ . Post annealing under vacuum promotes the releasing of chemical stress and generates oxygen vacancies in the samples. Temperature dependent transmittance study revealed that the releasing of chemical stress and deliberately introducing oxygen vacancies in W-doped VO 2 films have positive effects on enhancing its switching ability in the infrared transmittance as the metal-insulator transition (MIT) occurs. The largest switching of transmittance was obtained about 48% in the infrared range at 43 °C in 1.5%W doped VO 2 films, which is significantly larger than the reported ones. The findings in this work open a new way to synthesize the novel and thermochromic W doped VO 2 films with facility and low cost. Therefore, it has extensive application to construct smart windows and electronic devices.
Integrating nanohybrid membranes of reduced graphene oxide: chitosan: silica sol gel with fiber optic SPR for caffeine detection

NASA Astrophysics Data System (ADS)

Kant, Ravi; Tabassum, Rana; Gupta, Banshi D.

2017-05-01

Caffeine is the most popular psychoactive drug consumed in the world for improving alertness and enhancing wakefulness. However, caffeine consumption beyond limits can result in lot of physiological complications in human beings. In this work, we report a novel detection scheme for caffeine integrating nanohybrid membranes of reduced graphene oxide (rGO) in chitosan modified silica sol gel (rGO: chitosan: silica sol gel) with fiber optic surface plasmon resonance. The chemically synthesized nanohybrid membrane forming the sensing route has been dip coated over silver coated unclad central portion of an optical fiber. The sensor works on the mechanism of modification of dielectric function of sensing layer on exposure to analyte solution which is manifested in terms of red shift in resonance wavelength. The concentration of rGO in polymer network of chitosan and silica sol gel and dipping time of the silver coated probe in the solution of nanohybrid membrane have been optimized to extricate the supreme performance of the sensor. The optimized sensing probe possesses a reasonably good sensitivity and follows an exponentially declining trend within the entire investigating range of caffeine concentration. The sensor boasts of an unparalleled limit of detection value of 1.994 nM and works well in concentration range of 0-500 nM with a response time of 16 s. The impeccable sensor methodology adopted in this work combining fiber optic SPR with nanotechnology furnishes a novel perspective for caffeine determination in commercial foodstuffs and biological fluids.

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

PubMed

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

PubMed

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

NASA Astrophysics Data System (ADS)

Motalebi, Abolfazl; Nasr-Esfahani, Mojtaba

2013-06-01

The corrosion resistance of AISI 316L stainless steel for biomedical applications, was significantly enhanced by means of hybrid organic-inorganic sol-gel thin films deposited by spin-coating. Thin films of less than 100 nm with different hybrid characters were obtained by incorporating rosemary extract as green corrosion inhibitor. The morphology, composition, and adhesion of hybrid sol-gel coatings have been examined by SEM, EDX, and pull-off test, respectively. Addition of high additive concentrations (0.1%) did not disorganize the sol-gel network. Direct pull-off test recorded a mean coating-substrate bonding strength larger than 21.2 MPa for the hybrid sol-gel coating. The effect of rosemary extract, with various added concentrations from 0.012 to 0.1%, on the anticorrosion properties of sol-gel films have been characterized by electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization tests in simulated body fluid (SBF) solution and has been compared to the bare metal. Rosemary extract additions (0.05%) have significantly increased the corrosion protection of the sol-gel thin film to higher than 90%. The in vitro bioactivity of prepared films indicates that hydroxyapatite nuclei can form and grow on the surface of the doped sol-gel thin films. The present study shows that due to their excellent anticorrosion properties, bioactivity and bonding strength to substrate, doped sol-gel thin films are practical hybrid films in biomedical applications.
Sol-gel derived CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics: Synthesis, characterization and electrical properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu Laijun; Fan Huiqing; Fang Pinyang

2008-07-01

The giant dielectric constant material CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) has been synthesized by sol-gel method, for the first time, using nitrate and alkoxide precursor. The electrical properties of CCTO ceramics, showing an enormously large dielectric constant {epsilon} {approx} 60,000 (100 Hz at RT), were investigated in the temperature range from 298 to 358 K at 0, 5, 10, 20, and 40 V dc. The phases, microstructures, and impedance properties of final samples were characterized by X-ray diffraction, scanning electron microscopy, and precision impedance analyzer. The dielectric permittivity of CCTO synthesized by sol-gel method is at least three times ofmore » magnitude larger than that synthesized by other low-temperature method and solid-state reaction method. Furthermore, the results support the internal barrier layer capacitor (IBLC) model of Schottky barriers at grain boundaries between semiconducting grains.« less
Sol-gel synthesis and characterisation of nano-scale hydroxyapatite

NASA Astrophysics Data System (ADS)

Bilton, M.; Brown, A. P.; Milne, S. J.

2010-07-01

Hydroxyapatite (HAp) forms the main mineral component of bone and teeth. This naturally occurring HAp is in the form of nano-metre sized crystallites of Ca10(PO4)6(OH)2 that contain a number of cation and anion impurities, for example CO32-, F-, Na+, Mg2+ and Sr2+. Synthetic nano-sized HAp particles exhibit favourable biocompatibility and bioactivity and in order to better match the composition to natural HAp there is great interest in producing a range of chemically modified powders. In this study, two HAp powders have been synthesised via a water-based low-temperature sol-gel method and a third, commercial powder from Sigma-Aldrich have been analysed. Subsequent powder calcination has been carried out within the temperature range of 500-700 °C and the products characterised by bulk chemical analysis, X-ray diffraction and electron microscopy. Energy dispersive X-ray spectroscopy (EDX) in the TEM has been used to assess the composition of individual HAp particles. In order to do this accurately it is first necessary to account for the sensitivity of the HAp structure and composition to irradiation by the high energy electron beam of the TEM. This was done by monitoring the estimated Ca/P ratio derived from TEM-EDX of stoichiometric HAp under increasing levels of electron fluence. A fluence threshold (at a given beam energy) was established below which the measured Ca/P ratio can be considered to be stable. Subsequent elemental analysis at or below this threshold has enabled the variation in composition between particles both within and between synthesis batches to be accurately assessed. Compositional variability between particles is also evident, even in the commercial powder, but is far greater in the powders prepared by the sol-gel method.
Synthesis of polymeric fluorinated sol-gel precursor for fabrication of superhydrophobic coating

NASA Astrophysics Data System (ADS)

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

2016-03-01

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

PubMed

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.
Surface Modification of Zirconia Substrate by Calcium Phosphate Particles Using Sol-Gel Method.

PubMed

Jin, So Dam; Um, Sang Cheol; Lee, Jong Kook

2015-08-01

Surface modification with a biphasic composition of hydroxyapatite (HA) and tricalcium phosphate (TCP) was performed on a zirconia substrate using a sol-gel method. An initial calcium phosphate sol was prepared by mixing a solution of Ca(NO3)2 · 4H20 and (C2H5O)3P(O), while both porous and dense zirconia were used as substrates. The sol-gel coating was performed using a spin coater. The coated porous zirconia substrate was re-sintered at 1350 °C 2 h, while coated dense zirconia substrate was heat-treated at 750 °C 1 h. The microstructure of the resultant HA/TCP coatings was found to be dependent on the type of zirconia substrate used. With porous zirconia as a starting substrate, numerous isolated calcium phosphate particles (TCP and HA) were uniformly dispersed on the surface, and the particle size and covered area were dependent on the viscosity of the calcium phosphate sol. Conversely, when dense zirconia was used as a starting substrate, a thick film of nano-sized HA particles was obtained after heat treatment, however, substantial agglomeration and cracking was also observed.
Preparation, characterization, and biological properties of organic-inorganic nanocomposite coatings on titanium substrates prepared by sol-gel.

PubMed

Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando

2014-02-01

When surface-reactive (bioactive) coatings are applied to medical implants by means of the sol-gel dip-coating technique, the biological proprieties of the surface of the implant can be locally modified to match the properties of the surrounding tissues to provide a firm fixation of the implant. The aim of this study has been to synthesize, via sol-gel, organoinorganic nanoporous materials and to dip-coat a substrate to use in dental applications. Different systems have been prepared consisting of an inorganic zirconium-based matrix, in which a biodegradable polymer, the poly-ε-caprolactone was incorporated in different percentages. The materials synthesized by the sol-gel process, before gelation, when they were still in sol phase, have been used to coat a titanium grade 4 (Ti-4) substrate to change its surface biological properties. Thin films have been obtained by means of the dip-coating technique. A microstructural analysis of the obtained coatings was performed using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy. The biological proprieties have been investigated by means of tests in vitro. The bone-bonding capability of the nanocomposite films has been evaluated by examining the appearance of apatite on their surface when plunged in a simulated body fluid (SBF) with ion concentrations nearly equal to those of human blood plasma. The examination of apatite formation on the nanocomposites, after immersion in SBF, has been carried out by SEM equipped with energy-dispersive X-ray spectroscopy. To evaluate cells-materials interaction, human osteosarcoma cell line (Saos-2) has been seeded on specimens and cell vitality evaluated by WST-8 assay. © 2013 Wiley Periodicals, Inc.
Sol-gel technique for the preparation of beta-cyclodextrin derivative stationary phase in open-tubular capillary electrochromatography.

PubMed

Wang, Y; Zeng, Z; Guan, N; Cheng, J

2001-07-01

A novel open-tubular capillary electrochromatography (OT-CEC) column coated with 2,6-dibutyl-beta-cyclodextrin (DB-beta-CD) was prepared using sol-gel technique. In the sol-gel approach, owing to the three-dimensional 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. We achieved high efficiencies of 5-14 x 10(4) plates/m for the isomeric nitrophenols using the sol-gel-derived DB-beta-CD columns. The migration time reproducibility of the separation of the isomeric nitrophenols was better than 2.2% over five runs and 4.5% from column to column. These sol-gel-coated DB-beta-CD columns have shown improved separations of isomeric aminophenols, isomeric dihydroxybenzenes and isomeric nitrophenols, in comparison with the sol-gel matrix capillary column. The influences of buffer pH and methanol solvent on separation were investigated. The chiral resolution of enantiomers such as ibuprofen and binaphthol was explored primarily.
Sol-gel immobilized short-chain poly(ethylene glycol) coating for capillary microextraction of underivatized polar analytes.

PubMed

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

2007-12-07

Sol-gel coating with covalently bonded low-molecular-weight (MW<300 Da) poly(ethylene glycol) (PEG) chains was developed for capillary microextraction (CME). The sol-gel chemistry proved effective in the immobilization of low-molecular-weight PEGs thanks to the formation of chemical bonds between the organic-inorganic hybrid sol-gel PEG coating and the fused silica capillary inner surface. This chemical anchorage provided excellent thermal and solvent stability to the created sol-gel PEG coating as is evidenced by its high upper limit of allowable conditioning temperature (340 degrees C) and its practically identical performance before and after rinsing with various solvents. The prepared sol-gel PEG coating provided simultaneous extraction of moderately polar and highly polar analytes from aqueous samples without requiring derivatization, pH adjustment or salting-out procedures. Detection limits on the order of nanogram per liter (ng/L) were achieved in CME-GC-flame ionization detection experiments designed for the preconcentration and trace analysis of both highly polar and moderately polar compounds extracted directly from aqueous media using sol-gel short-chain PEG coated microextraction capillaries.
Evolution of heterogeneity accompanying sol-gel transitions in a supramolecular hydrogel.

PubMed

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.
Preparation of MTMS based transparent superhydrophobic silica films by sol-gel method.

PubMed

Venkateswara Rao, A; Latthe, Sanjay S; Nadargi, Digambar Y; Hirashima, H; Ganesan, V

2009-04-15

Superhydrophobic surfaces with water contact angle higher than 150 degrees generated a lot of interest both in academia and in industry because of the self-cleaning properties. Optically transparent superhydrophobic silica films were synthesized at room temperature (27 degrees C) using sol-gel process by a simple dip coating technique. The molar ratio of MTMS:MeOH:H(2)O (5 M NH(4)OH) was kept constant at 1:10.56:4.16, respectively. Emphasis is given to the effect of the surface modifying agents on the hydrophobic behavior of the films. Methyl groups were introduced in the silica film by post-synthesis grafting from two solutions using trimethylchlorosilane (TMCS) and hexamethyldisilazane (HMDZ) silylating agents in hexane solvent, individually. The percentage of silylating agents and silylation period was varied from 2.5 to 7.5% and 1 to 3 h, respectively. The TMCS modified films exhibited a very high water contact angle (166+/-2 degrees) in comparison to the HMDZ (138+/-2 degrees) modified films, indicating the water repellent behavior of the surface. When the TMCS and HMDZ modified films were heated at temperatures higher than 350 degrees C and 335 degrees C, respectively, the films became superhydrophilic; the contact angle for water on the films was smaller than 5 degrees. Further, the humidity study was carried out at a relative humidity of 85% at 30 degrees C temperature over 30 days. The films have been characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FT-IR), % optical transmission, humidity tests and contact angle (CA) measurements.
Processing of non-oxide ceramics from sol-gel methods

DOEpatents

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.
Selective filling for patterning in microfluidic channels and integration of chromatography in "lab-on-a-chip" devices using sol-gel technology

NASA Astrophysics Data System (ADS)

Jindal, Rohit

The last decade has seen tremendous advancement in the development of miniaturized chemical analysis system also known as "lab-on-a-chip". It is believed that the true potential of these devices will be achieved by integrating various functions such as separation, reaction, sensing, mixing, pumping, injection and detection onto a single chip. The ability to pattern different functionalities is indispensable for the development of highly integrated devices. In this work, a simple method based on the concept of selective filling is described for patterning in the microfluidic channels. It is based on the difference in the free energy of filling between an open and a covered part of the channel. This method was used for the integration of chromatography in the microfluidic devices. A chromatographic column was realized by utilizing sol-gel as an immobilization matrix for entrapping reversed phase chromatographic particles. Localization of the stationary phase was achieved using the selective filling technique. Channels were fabricated in quartz using photolithography and wet etching. Electroosmotic flow was used for manipulating fluid movement in the channels. Cross channel design was used for making a pulse injection of the solutes in the separation channel. An optical fiber setup was developed for carrying out on-chip UV absorbance detection. Stationary phase was created under different sol-gel synthesis conditions. It was established that the sol-gel synthesis carried out under acidic conditions provides the optimum synthesis conditions for creating separation column. Chromatographic performance of the stationary phase material was demonstrated by separating peptides present in a mixture. The sol-gel immobilization method was extended for the integration of micropump in the chip. The micropump enables pumping of the fluid in field free channels. Preliminary results, demonstrating the potential of carbon nanotubes as a support material in the microfluidic channels, were obtained using CVD (chemical vapor deposition) grown tubes in the channel. Results obtained in this work demonstrate the potential of selective filling technique along with sol-gel technology as a useful tool for the fabrication of multifunctional "lab-on-a-chip" devices.
Growth and properties of gradient free sol-gel lead zirconate titanate thin films

NASA Astrophysics Data System (ADS)

Calame, F.; Muralt, P.

2007-02-01

Pb(Zrx,Ti1-x)O3 thin films of homogeneous composition were synthesized by means of a modified sol-gel route on Pt(111)/TiOx/SiO2/Si substrates. The gradient in B-site composition as obtained by standard routes could be lowered, reducing Zr concentration fluctuations form ±12to±2.5at.%. The 2μm thick, dense and crack-free films exhibited a {100}-texture index of 98.4%. Grain diameters increased by 50%. Dielectric and piezoelectric properties were remarkably improved. The relative dielectric constant ɛ33,f was obtained as 1620, and the remanent transverse piezoelectric coefficient e31,f was measured as -17.7Cm2.
Synthesis of nano-sized lithium cobalt oxide via a sol-gel method

NASA Astrophysics Data System (ADS)

Li, Guangfen; Zhang, Jing

2012-07-01

In this study, nano-structured LiCoO2 thin film were synthesized by coupling a sol-gel process with a spin-coating method using polyacrylic acid (PAA) as chelating agent. The optimized conditions for obtaining a better gel formulation and subsequent homogenous dense film were investigated by varying the calcination temperature, the molar mass of PAA, and the precursor's molar ratios of PAA, lithium, and cobalt ions. The gel films on the silicon substrate surfaces were deposited by multi-step spin-coating process for either increasing the density of the gel film or adjusting the quantity of PAA in the film. The gel film was calcined by an optimized two-step heating procedure in order to obtain regular nano-structured LiCoO2 materials. Both atomic force microscopy (AFM) and scanning electron microscopy (SEM) were utilized to analyze the crystalline and the morphology of the films, respectively.
Polyethylene glycol assisted growth of Sn-doped ZnO nanorod arrays prepared via sol-gel immersion method

NASA Astrophysics Data System (ADS)

Ismail, A. S.; Mamat, M. H.; Malek, M. F.; Saidi, S. A.; Yusoff, M. M.; Mohamed, R.; Sin, N. D. Md; Suriani, A. B.; Rusop, M.

2018-05-01

Tin-doped zinc oxide (SZO) nanorod films at different concentrations of polyethylene glycol (PEG) were successfully deposited on zinc oxide (ZnO) seeded layer catalyst using sol-gel immersion method. The morphology of the samples were characterized using field emission scanning electron microscopy (FESEM), optical properties using UV-Vis spectrophotometer and electrical properties using I-V measurement system. The current-voltage (I-V) characteristics displayed that 5 wt % sample produced the highest conductivity.
Electrophoretically active sol-gel processes to backfill, seal, and/or densify porous, flawed, and/or cracked coatings on electrically conductive material

DOEpatents

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

1999-01-01

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

PubMed

Nishigami, Yukinori; Ichikawa, Masatoshi; Kazama, Toshiya; Kobayashi, Ryo; Shimmen, Teruo; Yoshikawa, Kenichi; Sonobe, Seiji

2013-01-01

Amoeboid locomotion is one of the typical modes of biological cell migration. Cytoplasmic sol-gel conversion of an actomyosin system is thought to play an important role in locomotion. However, the mechanisms underlying sol-gel conversion, including trigger, signal, and regulating factors, remain unclear. We developed a novel model system in which an actomyosin fraction moves like an amoeba in a cytoplasmic extract. Rheological study of this model system revealed that the actomyosin fraction exhibits shear banding: the sol-gel state of actomyosin can be regulated by shear rate or mechanical force. Furthermore, study of the living cell indicated that the shear-banding property also causes sol-gel conversion with the same order of magnitude as that of shear rate. Our results suggest that the inherent sol-gel transition property plays an essential role in the self-regulation of autonomous translational motion in amoeba.

3-(Triethoxysilyl)propionitrile sol-gel coating.

PubMed

Li, Ying-Sing; Xiao, Yun; Wright, Paul B; Tran, Tuan

2005-05-01

3-(Triethoxysilyl)propionitrile (TESPN) sol-gel has been prepared under different conditions. It was employed for coating the surfaces of quartz and aluminum. Infrared (IR) and Raman spectra of TESPN and TESPN sol-gels have been recorded in the study of the sol-gel process. Transmission and reflection absorption IR (RAIR) spectra of TESPN sol-gel coated quartz and aluminum have also been collected for better understanding the film formation on the substrate surfaces. Spectra collected at different temperatures indicated that the silane film on quartz decomposes at 700 degrees C. Results from thermal gravimetric analysis (TGA) supported this result. Based on the group frequencies and the spectral behavior in different states, some vibrational modes were assigned to the observed bands. The anticorrosion behavior of the sol-gel coated aluminum in comparison with the uncoated metal was evaluated by measuring the potentiodynamic polarization and electrochemical impedance spectra (EIS).
pH-resistant titania hybrid organic-inorganic sol-gel coating for solid-phase microextraction of polar compounds.

PubMed

Li, Xiujuan; Gao, Jie; Zeng, Zhaorui

2007-05-02

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

PubMed Central

Spijksma, Gerald I.; Blank, Dave H. A.; Bouwmeester, Henny J. M.; Kessler, Vadim G.

2009-01-01

Modification of different zirconium propoxide precursors with H2dea was investigated by characterization of the isolated modified species. Upon modification of zirconium n-propoxide and [Zr(OnPr)(OiPr)3(iPrOH)]2 with ½ a mol equivalent of H2dea the complexes [Zr2(OnPr)6(OCH2CH2)2NH]2 (1) and [Zr2(OnPr)2(OiPr)4(OCH2CH2)2NH]2 (2) were obtained. However, 1H-NMR studies of these tetranuclear compounds showed that these are not time-stable either in solution or solid form. The effect of this time instability on material properties is demonstrated by light scattering and TEM experiments. Modification of zirconium isopropoxide with either ½ or 1 equivalent mol of H2dea results in formation of the trinuclear complex, Zr{η3μ2-NH(C2H4O)2}3[Zr(OiPr)3]2(iPrOH)2 (3) countering a unique nona-coordinated central zirconium atom. This complex 3 is one of the first modified zirconium propoxide precursors shown to be stable in solution for long periods of time. The particle size and morphology of the products of sol-gel synthesis are strongly dependent on the time factor and eventual heat treatment of the precursor solution. Reproducible sol-gel synthesis requires the use of solution stable precursors. PMID:20087472
Sol concentration effect on ZnO nanofibers photocatalytic activity synthesized by sol-gel dip coating method

NASA Astrophysics Data System (ADS)

Toubane, M.; Tala-Ighil, R.; Bensouici, F.; Bououdina, M.; Souier, M.; Liu, S.; Cai, W.; Iratni, A.

2017-03-01

ZnO thin films were deposited onto glass substrate by sol-gel dip coating method. The initial sol concentrations were varied from 0.2 to 0.5 M. Zinc acetate dihydrate, ethanol and Diethanolamine (DEA) were used as staring material, solvent and stabilizer respectively. The evolution of structural, optical properties and methylene blue (MB) photodegradation of the as-deposited films on sol concentration was investigated. Rietveld refinements of x-ray patterns reveal that all the as-prepared thin films have a Zincite-type structure with grain orientation along to c-axis. The strongest sol concentration is favorable for the highest crystallization quality. However, the high preferred orientation factor (POF) occurs for 0.3 M sol concentration. The field emission scanning electron microscopy observations reveals nanofibrous morphology with different lengths. The nanofibers density increases with increasing sols concentrations until forming a flower-like morphology. The EDS analysis confirms the high purity of the as-deposited ZnO films. It is found that all films present good transparency greater than 95% in the visible range; the optical band gap is slightly reduced with the increase in sol concentration. The photocatalytic degradation is enhanced by 90% with the sol concentration. The K app rate reaction increased with increasing sol concentration. The films stability is found to slightly decrease after the third cycle, especially for 0.5 M sol concentration.
Hydrogen permeation through steel coated with erbium oxide by sol-gel method

NASA Astrophysics Data System (ADS)

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

2009-04-01

Er 2O 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 2O 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.
Physically incorporated extraction phase of solid-phase microextraction by sol-gel technology.

PubMed

Liu, Wenmin; Hu, Yuan; Zhao, Jinghong; Xu, Yuan; Guan, Yafeng

2006-01-13

A sol-gel method for the preparation of solid-phase microextraction (SPME) fiber was described and evaluated. The extraction phase of poly(dimethysiloxane) (PDMS) containing 3% vinyl group was physically incorporated into the sol-gel network without chemical bonding. The extraction phase itself is then partly crosslinked at 320 degrees C, forming an independent polymer network and can withstand desorption temperature of 290 degrees C. The headspace extraction of BTX by the fiber SPME was evaluated and the detection limit of o-xylene was down to 0.26 ng/l. Extraction and determination of organophosphorus pesticides (OPPs) in water, orange juice and red wine by the SPME-GC thermionic specified detector (TSD) was validated. Limits of detection of the method for OPPs were below 10 ng/l except methidathion. Relative standard deviations (RSDs) were in the range of 1-20% for pesticides being tested.
Highly efficient up-conversion and bright white light in RE co-doped KYF4 nanocrystals in sol-gel silica matrix

NASA Astrophysics Data System (ADS)

Méndez-Ramos, J.; Yanes, A. C.; Santana-Alonso, A.; del-Castillo, J.

2013-01-01

Transparent nano-glass-ceramics comprising Yb3+, Er3+ and Tm3+ co-doped KYF4 nanocrystals have been developed from sol-gel method. A structural analysis by means of X-ray diffraction confirmed the precipitation of cubic KYF4 nanocrystals into a silica matrix. Visible luminescence has been analyzed as function of treatment temperature of precursor sol-gel glasses. Highly efficient up-conversion emissions have been obtained under 980 nm excitation and studied by varying the doping level, processing temperature and pump power. Color tuneability has been quantified in terms of CIE diagram and in particular, a white-balanced overall emission has been achieved for a certain doping level and thermal treatment.
Moisture sensor based on evanescent wave light scattering by porous sol-gel silica coating

DOEpatents

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.
The effect of microwave and conventional heating on a modified sol-gel derived biphasic calcium phosphate

NASA Astrophysics Data System (ADS)

Herradi, S.; Bouhazma, S.; Khaldi, M.; El Hachadi, A.; El Bali, B.; Lachkar, M.

2018-03-01

A facile sol-gel method was used to synthesize either hydroxyapatite (HA) or beta-tricalcium phosphate (β-TCP) as the major phase. Herein, we report, on the one hand, the effect of a very low maturation temperature on the final powder composition after drying step, and on the other hand, we compare the effect of calcination of this powder by microwave or electric furnace. It was found that microwave heating has led to the formation of hydroxyapatite phase upon 180°C for 20 minutes, however, XRD patterns show that the powder becomes less crystallized upon 220°C and amorphous upon 230°C. In contrast, furnace heating at 600°C and 700°C converts the as-synthesized powder to β-TCP as the major phase together with HA as the minor phase. This work shows the possibility to obtain the as-prepared BCP at much lower maturation temperature; it also gives an insight into the role, of either microwave or conventional heating, in controlling the ratio between HA and β-TCP in the sintered powder.
Imprinted propyl gallate electrochemical sensor based on graphene/single walled carbon nanotubes/sol-gel film.

PubMed

Xu, Guilin; Chi, Yu; Li, Lu; Liu, Shouhua; Kan, Xianwen

2015-06-15

A novel imprinted sol-gel electrochemical sensor for the determination of propyl gallate (PG) was developed based on a composite of graphene and single walled carbon nanotubes (GR-SWCNTs). It was fabricated by stepwise modifying GR-SWCNTs and molecularly imprinted polymers and stored in 0.10 mol L(-1) phosphate buffer solution pH 6.0, which endowed the sensor good sensitivity and selective recognition towards template molecules. The morphology and specific adsorption capacity of the sensor was characterized by scanning electron microscope and electrochemical methods, respectively. Under the optimized conditions, a linear range of the sensor to PG was 8.0 × 10(-8)-2.6 × 10(-3)mo lL(-1) with a limit of detection of 5.0 × 10(-8)mol L(-1) (S/N=3). The sensor exhibited specificity and selectivity towards template molecules as well as excellent reproducibility, regeneration and stability. Furthermore, the sensor could be applied to determine PG in edible oils, instant noodles and cookies with satisfactory results. Copyright © 2015 Elsevier Ltd. All rights reserved.
Synthesis, Fabrication and Characterization of ZnO-Based Thin Films Prepared by Sol-Gel Process and H2 Gas Sensing Performance

NASA Astrophysics Data System (ADS)

Dey, Anup; Roy, Subhashis; Sarkar, Subir Kumar

2018-03-01

In this paper, an attempt is made to deposit ZnO thin films using sol-gel process followed by dip-coating method on p-silicon (100) substrates for intended application as a hydrogen gas sensor owing to the low toxic nature and thermal stability of ZnO. The thin films are annealed under annealing temperatures of 350, 450 and 550 °C for 25 min. The crystalline quality of the fabricated thin films is then analyzed by field-emission scanning electron microscopy and transmission electron microscope. The gas sensing performance analysis of ZnO thin films is demonstrated at different annealing temperatures and hydrogen gas concentrations ranging from 100 to 3000 ppm. Results obtained show that the sensitivity is significantly improved as annealing temperature increases with maximum sensitivity being achieved at 550 °C annealing temperature and operating temperature of 150 °C. Hence, the modified ZnO thin films can be applicable as H2 gas sensing device showing to the improved performance in comparison with unmodified thin-film sensor.
Thermally activated charge transport in modified tetragonal zirconia thin films prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Aboulkacem, Khiali; Abdelkader, Ammari; Bediaf, Benrabah; Amar, Bouaza; Abdelmalek, Kharoubi; Hadj, Benhebal

2018-04-01

Films of Sn-doped ZrO2 were prepared using the sol-gel based dip-coating technique. The X-ray diffraction patterns showed a tetragonal structure with a preferential orientation along the (111) plane. The average grain size of the samples varies from 9.53 to 12.64 nm. Thermal analysis revealed endothermic peaks in the range 84-90 °C and exothermic peaks appearing in the range 489-531 °C. Fourier transform infrared (FTIR) spectra depicted bands located at 612 and 736 cm-1, which are attributed to stretching mode and asymmetric vibrations of Zr-O and O-Zr-O bonds respectively. All films exhibited high transmittance in the visible range above 60% and the optical band gap (E g) decreases from 4.085 to 4.061 eV. The impedance measurements show that the equivalent circuit of the samples is an R p C p where C p is the capacitance of the layer and R p its resistance. The electrical conductivity was found to follows an Arrhenius law with two activation energies.
An improved biosensor for acetaldehyde determination using a bienzymatic strategy at poly(neutral red) modified carbon film electrodes.

PubMed

Ghica, Mariana Emilia; Pauliukaite, Rasa; Marchand, Nicolas; Devic, Eric; Brett, Christopher M A

2007-05-15

Improved biosensors for acetaldehyde determination have been developed using a bienzymatic strategy, based on a mediator-modified carbon film electrode and co-immobilisation of NADH oxidase and aldehyde dehydrogenase. Modification of the carbon film electrode with poly(neutral red) mediator resulted in a sensitive, low-cost and reliable NADH detector. Immobilisation of the enzymes was performed using encapsulation in a sol-gel matrix or cross-linking with glutaraldehyde. The bienzymatic biosensors were characterized by studying the influence of pH, applied potential and co-factors. The sol-gel and glutaraldehyde biosensors showed a linear response up to 60 microM and 100 microM, respectively, with detection limits of 2.6 microM and 3.3 microM and sensitivities were 1.7 microA mM(-1) and 5.6 microA mM(-1). The optimised biosensors showed good stability and good selectivity and have been tested for application for the determination of acetaldehyde in natural samples such as wine.
Deactivation of photocatalytically active ZnO nanoparticle and enhancement of its compatibility with organic compounds by surface-capping with organically modified silica

NASA Astrophysics Data System (ADS)

Cao, Zhi; Zhang, Zhijun

2011-02-01

Tetraethyl orthosilicate (TEOS) and dimethyldiethoxysilane (DEDMS) were used as co-precursors to prepare organically modified silica (ormosil) via sol-gel process. The resultant ormosil was adopted for surface-capping of ZnO nanoparticle, where methyl (organic functional group) and silica (inorganic component) were simultaneously introduced onto the surface of the nanoparticles for realizing dual surface-modification. The ormosil-capped ZnO nanoparticle showed strong hydrophobicity and good compatibility with organic phases, as well as effectively decreased photocatalytic activity and almost unchanged ultraviolet (UV)-shielding ability. More importantly, the comprehensive properties of ormosil-capped ZnO nanoparticle could be manipulated by adjusting the molar ratio of TEOS to DEDMS during sol-gel process. This should help to open a wider window to better utilizing the unique and highly attractive properties such as high UV-shielding ability and high-visible light transparency of ZnO nanoparticle in sunscreen cosmetics.
Synthesis and characterization of TiC nanopowders via sol-gel and subsequent carbothermal reduction process

NASA Astrophysics Data System (ADS)

Chen, Xu; Fan, Jinglian; Lu, Qiong

2018-06-01

TiC nanocrystalline powders were synthesized by in-situ carbothermic reduction of Ti-O-C precursor under vacuum atmosphere. And the Ti-O-C precursor was formed by sol-gel method from titanium butyrate (TBOT) and sucrose. To obtain stable sol, TBOT was directly added into mixed solution which contains water, sucrose, acetic acid (AcOH) and acetylacetone (ACAC). This procedure is more convenient and economical because it avoids the use of alcohol which is used as solvent in most reports of alkoxide hydrolysis sol-gel method. TG-DSC, XRD, FTIR and SEM/TEM were employed to analyze and characterize the product during the entire process. The phase composition and crystalline structure parameters of powders with different C/Ti molar ratio were investigated by Rietveld refinement method, and elemental quantitative analysis of the samples were performed. Furthermore, the optimal parameters of carbothermal reduction were obtained and the grain growth mechanism was demonstrated. The results show that TiC nanocrystalline powders (C/Ti molar ratio is 3.5 in the precursor) were synthesized at 1300 °C for 2 h, which have near standard lattice parameter, well crystallinity and fine average grain size ( 37.4 nm).
Electrophoretically active sol-gel processes to backfill, seal, and/or densify porous, flawed, and/or cracked coatings on electrically conductive material

DOEpatents

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

1999-07-20

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

PubMed

Carrasquilla, Carmen; Brennan, John D

2013-10-01

Functional nucleic acids (FNAs) are single-stranded DNA or RNA molecules, typically generated through in vitro selection, that have the ability to act as receptors for target molecules (aptamers) or perform catalysis of a chemical reaction (deoxyribozymes and ribozymes). Fluorescence-signaling aptamers and deoxyribozymes have recently emerged as promising biological recognition and signaling elements, although little has been done to evaluate their potential for solid-phase assays, particularly with species made of RNA due to their lack of chemical stability and susceptibility to nuclease attack. Herein, we present a detailed overview of the methods utilized for solid-phase immobilization of FNAs using a sol-gel entrapment method that can provide protection from nuclease degradation and impart long-term chemical stability to the FNA reporter systems, while maintaining their signaling capabilities. This article will also provide a brief review of the results of such entrapment studies involving fluorescence-signaling versions of a DNA aptamer, selected RNA-cleaving deoxyribozymes, and two different RNA aptamers in a series of sol-gel derived composites, ranging from highly polar silica to hydrophobic methylsilsesquioxane-based materials. Given the ability to produce sol-gel derived materials in a variety of configurations, particularly as thin film coatings on electrodes, optical fibers, and other devices, this entrapment method should provide a useful platform for numerous solid-phase FNA-based biosensing applications. Copyright © 2013 Elsevier Inc. All rights reserved.
Ultra-small dye-doped silica nanoparticles via modified sol-gel technique.

PubMed

Riccò, R; Nizzero, S; Penna, E; Meneghello, A; Cretaio, E; Enrichi, F

2018-01-01

In modern biosensing and imaging, fluorescence-based methods constitute the most diffused approach to achieve optimal detection of analytes, both in solution and on the single-particle level. Despite the huge progresses made in recent decades in the development of plasmonic biosensors and label-free sensing techniques, fluorescent molecules remain the most commonly used contrast agents to date for commercial imaging and detection methods. However, they exhibit low stability, can be difficult to functionalise, and often result in a low signal-to-noise ratio. Thus, embedding fluorescent probes into robust and bio-compatible materials, such as silica nanoparticles, can substantially enhance the detection limit and dramatically increase the sensitivity. In this work, ultra-small fluorescent silica nanoparticles (NPs) for optical biosensing applications were doped with a fluorescent dye, using simple water-based sol-gel approaches based on the classical Stöber procedure. By systematically modulating reaction parameters, controllable size tuning of particle diameters as low as 10 nm was achieved. Particles morphology and optical response were evaluated showing a possible single-molecule behaviour, without employing microemulsion methods to achieve similar results. Graphical abstractWe report a simple, cheap, reliable protocol for the synthesis and systematic tuning of ultra-small (< 10 nm) dye-doped luminescent silica nanoparticles.
Effect of synthesis route on the uptake of Ni and Cd by MgFe2O4 nanopowders

NASA Astrophysics Data System (ADS)

Al-Najar, B.; Khezami, L.; Judith Vijaya, J.; Lemine, O. M.; Bououdina, M.

2017-01-01

In this study, MgFe2O4 nanopowders were synthesized through two different methods, sol-gel method (SG) and modified sol-gel with Ammonia (MSG-A). The influence of synthesis route was investigated in terms of phase stability, pores size and surface area, magnetic properties and uptake of Ni and Cd metals from aqueous solution. Rietveld refinements of x-ray diffraction patterns confirmed the formation of single spinel phase for SG sample, while minor impurity was detected for SGM-A sample (few amount of MgO). The crystallite size was found to be sensitive to the preparation method; it ranges from 4 nm for SG to 15 nm for MSG-A. Magnetization experiment at room temperature showed ferromagnetic behavior with a saturation magnetization ( M s) ranging from 5.39 emu/g for SG to 9.93 emu/g for MSG-A. Preliminary results showed that SG and MSG-A samples are efficient adsorbent for Ni and Cd metal ions from aqueous solution. Maximum quantity of 62.67 and 61.2 mg of Ni(II) and 36.49 and 32.84 mg of Cd(II) was adsorbed per gram of MgFe2O4 synthesized by SG and MSG-A, respectively.
A novel sensor made of Antimony Doped Tin Oxide-silica composite sol on a glassy carbon electrode modified by single-walled carbon nanotubes for detection of norepinephrine.

PubMed

Wang, Zhao; Wang, Kai; Zhao, Lu; Chai, Shigan; Zhang, Jinzhi; Zhang, Xiuhua; Zou, Qichao

2017-11-01

In this study, we designed a novel molecularly imprinted polymer (MIP), Antimony Doped Tin Oxide (ATO)-silica composite sol, which was made using a sol-gel method. Then a sensitive and selective imprinted electrochemical sensor was constructed with the ATO-silica composite sol on a glassy carbon electrode modified by single-walled carbon nanotubes (SWNTs). The introduction of SWNTs increased the sensitivity of the MIP sensor. The surface morphology of the MIP and MIP/SWNTs were characterized by scanning electron microscopy (SEM), and the optimal conditions for detection were determined. The oxidative peak current increased linearly with the concentration of norepinephrine in the range of 9.99×10 -8 M to 1.50×10 -5 M, as detected by cyclic voltammetry (CV), the detection limit was 3.33×10 -8 M (S/N=3). In addition, the proposed electrochemical sensors were successfully applied to detect the norepinephrine concentration in human blood serum samples. The recoveries of the sensors varied from 99.67% to 104.17%, indicating that the sensor has potential for the determination of norepinephrine in clinical tests. Moreover, the imprinted electrochemical sensor was used to selectively detect norepinephrine. The analytical application was conducted successfully and yielded accurate and precise results. Copyright © 2017. Published by Elsevier B.V.

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

PubMed Central

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
Tubular structured hierarchical mesoporous titania material derived from natural cellulosic substances and application as photocatalyst for degradation of methylene blue

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Haiqing; Liu, Xiaoyan; Huang, Jianguo, E-mail: jghuang@zju.edu.cn

Graphical abstract: Bio-inspired, tubular structured hierarchical mesoporous titania material with high photocatalytic activity under UV light was fabricated employing natural cellulosic substance (cotton) as hard template and cetyltrimethylammonium bromide (CTAB) surfactant as soft template using a one-pot sol-gel method. Highlights: {yields} Tubular structured mesoporous titania material was fabricated by sol-gel method. {yields} The titania material faithfully recorded the hierarchical structure of the template substrate (cotton). {yields} The titania material exhibited high photocatalytic activity in decomposition of methylene blue. -- Abstract: Bio-inspired, tubular structured hierarchical mesoporous titania material was designed and fabricated employing natural cellulosic substance (cotton) as hard template andmore » cetyltrimethylammonium bromide (CTAB) surfactant as soft template by one-pot sol-gel method. The tubular structured hierarchical mesoporous titania material processes large specific surface area (40.23 m{sup 2}/g) and shows high photocatalytic activity in the photodegradation of methylene blue under UV light irradiation.« less
Antimicrobial activity of thin solid films of silver doped hydroxyapatite prepared by sol-gel method.

PubMed

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.
Flexible freestanding sandwich type ZnO/rGO/ZnO electrode for wearable supercapacitor

NASA Astrophysics Data System (ADS)

Ghorbani, Mina; Golobostanfard, Mohammad Reza; Abdizadeh, Hossein

2017-10-01

The development of flexible supercapacitors with high energy and power density as one of the main components of wearable electronics is in an enormous interest. In this report, a unique flexible electrode based on freestanding sandwich type ZnO/rGO/ZnO paper is fabricated by a simple low cost sol-gel method for utilizing in flexible supercapacitor. ZnO layers are deposited on both sides of rGO paper which is prepared by a modified Hummer's method and evaporation induced assembly. The uniform and densely packed ZnO layers are formed on graphene oxide paper and the paper is simultaneously reduced. Structural analysis reveals the formation of ZnO thin films on both sides of rGO nanosheets, which leads to the sandwich architecture. Also, the effect of ZnO sol-gel process parameters on microstructure of sandwich paper are investigated and the most suitable condition for highest supercapacity performance is the solvent of 1-PrOH, stabilizer of TeA, sol concentration of 0.2 M, deposition speed of 30 mm min-1, and 10 deposited layers. The results of electrochemical impedance spectroscopy, galvanostatic charge-discharge, and cyclic voltammetry confirm that the incorporation of ZnO improves the capacitive performance of rGO electrode. Moreover, ZnO/rGO/ZnO flexible electrode exhibits suitable capacitance value of 60.63 F g-1 at scan rate of 5 mV/s.
Structural Modification of Sol-Gel Materials through Retro Diels-Alder Reaction

DOE Office of Scientific and Technical Information (OSTI.GOV)

SHALTOUT,RAAFAT M.; LOY,DOUGLAS A.; MCCLAIN,MARK D.

1999-12-08

Hydrolysis and condensation of organically bridged bis-triethoxysilanes, (EtO){sub 3}Si-R-Si(OEt){sub 3}, results in the formation of three dimensional organic/inorganic hybrid networks (Equation 1). Properties of these materials, including porosity, are dependent on the nature of the bridging group, R. Flexible groups (akylene-spacers longer than five carbons in length) polymerize under acidic conditions to give non-porous materials. Rigid groups (such as arylene-, alkynylene-, or alkenylene) form non-porous, microporous, and macroporous gels. In many cases the pore size distributions are quite narrow. One of the motivations for preparing hybrid organic-inorganic materials is to extend the range of properties available with sol-gel systems bymore » incorporating organic groups into the inorganic network. For example, organically modified silica gels arc either prepared by co-polymerizing an organoalkoxysilane with a silica precursor or surface silylating the inorganic gel. This can serve to increase hydrophobicity or to introduce some reactive organic functionality. However, the type and orientation of these organic functionalities is difficult to control. Furthermore, many organoalkoxysilanes can act to inhibitor even prevent gelation, limiting the final density of organic functionalities. We have devised a new route for preparing highly functionalized pores in hybrid materials using bridging groups that are thermally converted into the desired functionalities after the gel has been obtained. In this paper, we present the preparation and characterization of bridged polysilsesquioxanes with Diels-Alder adducts as the bridging groups from the sol-gel polymerization of monomers 2 and 4. The bridging groups are constructed such that the retro Diela-Alder reaction releases the dienes and leaves the dienophiles as integral parts of the network polymers. In the rigid architecture of a xerogel, this loss of organic functionality should liberate sufficient space to modify the overall porosity. Furthermore, the new porosity will be functionalized with the dienophilic olefin bridging group. We also demonstrate that by changing the type of Diels-Alder adduct used as the bridging group, we can change the temperature at which the retro-Diels-Alder reaction will occur.« less
Sol-gel chemical sensors for surface-enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Lee, Vincent Y.; Farquharson, Stuart; Kwon, Hueong-Chan; Shahriari, Mahmoud R.; Rainey, Petrie M.

1999-02-01

Surface-enhanced Raman spectroscopy (SERS) promises to be one of the most sensitive methods for chemical detection. Unfortunately, the inability of SERS to perform quantitative chemical analysis has slowed its general use in laboratories. This is largely due to the difficulty of manufacturing either active surfaces that yield reproducible enhancements, or surfaces that are capable of reversible chemical adsorption, or both. In an effort to meet this need, we have developed metal-doped sol-gels that provide surface-enhancement of Raman scattering. The porous silica network offers a unique environment for stabilizing SER active metal particles and the high surface area increases the interaction between the analyte and metal particles. This eliminates the need to concentrate the analyte on the surface by evaporating the solvent. The sol-gel is easily coated on a variety of surfaces, such as fiber optics, glass slides, or glass tubing, and can be designed into sample flow systems. Here we present the development of both gold- and silver-doped sol-gels, which have been used to coat the inside walls of glass sample vials for SERS applications. The performance of the metal-doped sol-gels was evaluated using p-aminobenzoic acid, to establish enhancement factors, detection limits, dynamic response range, reversibility, reproducibility, and suitability to commercial spectrometers. Measurements of trace chemicals, such as adenine and cocaine, are also presented.
Athermal silicon optical add-drop multiplexers based on thermo-optic coefficient tuning of sol-gel material.

PubMed

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.
KOH catalysed preparation of activated carbon aerogels for dye adsorption.

PubMed

Ling, Sie King; Tian, H Y; Wang, Shaobin; Rufford, Thomas; Zhu, Z H; Buckley, C E

2011-05-01

Organic carbon aerogels (CAs) were prepared by a sol-gel method from polymerisation of resorcinol, furfural, and hexamethylenetetramine catalysed by KOH at around pH 9 using ambient pressure drying. The effect of KOH in the sol-gel on CA synthesis was studied. It was found that addition of KOH prior to the sol-gel polymerisation process improved thermal stability of the gel, prevented the crystallinity of the gel to graphite, increased the microporosity of CA and promoted activation of CA. The CAs prepared using the KOH catalyst exhibited higher porosity than uncatalysed prepared samples. Activation in CO(2) at higher temperature also enhanced the porosity of CAs. Adsorption tests indicated that the CAs were effective for both basic and acid dye adsorption and the adsorption increased with increasing surface area and pore volume. The kinetic adsorption of dyes was diffusion control and could be described by the second-order kinetic model. The equilibrium adsorption of dyes was higher than activated carbon. Copyright © 2011 Elsevier Inc. All rights reserved.
Production of Monodisperse Cerium Oxide Microspheres with Diameters near 100 µm by Internal-Gelation Sol-Gel Methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

Cerium dioxide microspheres with uniform diameters between 65 – 211 µm were fabricated using internal gelation sol-gel methods. Although uniform microspheres are produced for nuclear fuel applications with diameters above 300 µm, sol-gel microspheres with diameters of 50 - 200 µm have historically been made by emulsion techniques and had poor size uniformity [1, 2]. An internal gelation, sol-gel apparatus was designed and constructed to accommodate the production of small, uniform microspheres whereby cerium-containing solutions were dispersed into flowing silicone oil and heated in a gelation column to initiate solidification [3, 4]. Problems with premature feed gelation and microsphere coalescencemore » were overcome by equipment modifications unique among known internal gelation setups. Microspheres were fabricated and sized in batches as a function of dispersing needle diameter and silicone oil flow rate in the two-fluid nozzle in order to determine the range of sizes possible and corresponding degree of monodispersity. Initial experiments with poor size uniformity were linked to microsphere coalescence in the gelation column prior to solidification as well as excessive flow rates for the cerium feed solution. Average diameter standard deviations as low as 2.23% were observed after optimization of flow rates and minimization of coalescence reactions.« less
Sol-gel-based biosensing applied to medicinal science.

PubMed

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.
Fabrication and characterization of sol-gel derived 45S5 Bioglass®-ceramic scaffolds.

PubMed

Chen, Qi-Zhi; Thouas, George A

2011-10-01

Although Bioglass® has existed for nearly half a century its ability to trigger bone formation and tuneable degradability is vastly superior to other bioceramics, such as SiO(2)-CaO bioactive glasses. The sol-gel process of producing glass foams is well established for SiO(2)-CaO compositions, but not yet established for 45S5 composites containing Na(2)O. In this work the sol-gel derived 45S5 Bioglass® has for the first time been foamed into highly porous three-dimensional scaffolds using a surfactant, combined with vigorous mechanical stirring and subsequent sintering at 1000°C for 2 h. It was found that the mechanical strength of the sintered sol-gel derived Bioglass® scaffolds was significantly improved, attributable to the small fraction of material on the pore walls. More importantly, the compressive strength of the three-dimensional scaffolds produced by this surfactant foaming method could be predicted using Gibson and Ashby's closed cell model of porous networks. A comparative experiment revealed that ion release from the sol-gel derived Bioglass® foams was faster than that of counterparts produced by the replication technique. In vitro evaluation using osteoblast-like cells demonstrated that the sol-gel derived 45S5 Bioglass foams supported the proliferation of viable cell populations on the surface of the scaffolds, although few cells were observed to migrate into the virtually closed pores within the foams. Further work should be focused on modifications of the reaction conditions or alternative foaming techniques to improve pore interconnection. Copyright © 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
The incorporation of calix[6]arene and cyclodextrin derivatives into sol-gels for the preparation of stationary phases for gas chromatography.

PubMed

Delahousse, Guillaume; Peulon-Agasse, Valérie; Debray, Jean-Christophe; Vaccaro, Marie; Cravotto, Giancarlo; Jabin, Ivan; Cardinael, Pascal

2013-11-29

New polyethylene-glycol-based sol-gels containing cyclodextrin or calix[6]arene derivatives have been synthesized. An original method for sol-gel preparation and capillary column coating, which consumes smaller quantities of selectors and allows for control of their amounts in the stationary phase, is reported herein. The new stationary phases exhibited excellent column efficiencies over a large range of temperatures and thermal stability up to 280°C. The cyclodextrin derivative generally showed the best separation factors for aromatic positional isomers. The calix[6]arene derivative exhibited the best selectivity for the polychlorobiphenyl congeners and some polycyclic aromatic hydrocarbon isomers. The relationship between the structure and the chromatographic properties of the selectors is discussed. The tert-butyl groups on the upper rim of the calix[6]arene were found to possibly play an important role in the recognition of solutes. The incorporation of the cyclodextrin derivative into the sol-gel matrix did not affect its enantioselective recognition capabilities. Copyright © 2013 Elsevier B.V. All rights reserved.
Sol-gel derived flexible silica aerogel as selective adsorbent for water decontamination from crude oil.

PubMed

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.
Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation.

PubMed

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.
Effects of sol-gel processing parameters on the phases and microstructures of HA films.

PubMed

Wang, Diangang; Chen, Chuanzhong; Liu, Xiuna; Lei, Tingquan

2007-06-15

Bioactive hydroxyapatite (HA) films were fabricated by a sol-gel method and triethylphosphate and calcium nitrate were used as the phosphorus and calcium precursors, respectively. The effects of the heat treatment temperature, pH level and substrate materials on the phases and microstructures of HA films were studied by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and electronic probe microanalysis (EPMA) and so on. The results show that all the sol-gel films are composed of the phases of HA, CaO, TiO(2) and CaTiO(3). With increasing the calcining temperature, the crystallinity of the films increases, the structure becomes more compact and changes from granular and lamellar to cellular structure, and the Ca/P ratio increases slightly because of the loss of P in the films. The addition of ammonia (adjusting the pH level to be about 7.5) can increase the HA content in the films, and the difference of substrate materials only has a little influence on the microstructure of the sol-gel films.
Functionalizable Sol-Gel Silica Coatings for Corrosion Mitigation

PubMed Central

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
Nanocrystal/sol-gel nanocomposites

DOEpatents

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.
Nanocrystal/sol-gel nanocomposites

DOEpatents

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

2012-06-12

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
Solventless sol-gel chemistry through ring-opening polymerization of bridged disilaoxacyclopentanes

DOE Office of Scientific and Technical Information (OSTI.GOV)

RAHIMIAN,KAMYAR; LOY,DOUGLAS A.

2000-05-01

Ring-opening polymerization (ROP) of disilaoxacyclopentanes has proven to be an excellent approach to sol-gel type hybrid organic-inorganic materials. These materials have shown promise as precursors for encapsulation and microelectronics applications. The polymers are highly crosslinked and are structurally similar to traditional sol-gels, but unlike typical sol-gels they are prepared by an organic base or Bronsted acid (formic or triflic acid), without the use of solvents and water, they have low VOC's and show little shrinkage during processing.
Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

PubMed

Catauro, M; Papale, F; Bollino, F

2016-01-01

The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0

Method of making particles from an aqueous sol

DOEpatents

Rankin, G.W.; Hooker, J.R.

1973-07-24

A process for preparing gel particles from an aqueous sol by forming the sol into droplets in a liquid system wherein the liquid phase contains a liquid organic solvent and a barrier agent. The barrier agent prevents dehydration from occurring too rapidly and permits surface tension effects to form sol droplets into the desired spheroidal shape. A preferred barrier agent is mineral oil. (Official Gazette)
Sol gel derived hydroxyapatite coatings on titanium and its alloy Ti6Al4V

NASA Astrophysics Data System (ADS)

Stoch, A.; Jastrzebski, W.; Długoń, E.; Lejda, W.; Trybalska, B.; Stoch, G. J.; Adamczyk, A.

2005-06-01

Titanium has been used for many medical and dental applications; however, its joining to a living bone is not satisfactorily good or the implant integration with bone tissue takes several months.The aim of this work is to produce hydroxyapatite (HAP) coatings on titanium and its alloy for facilitating and shortening the processes towards osseointegration. HAP coatings were obtained by sol-gel method with sol solutions prepared from calcium nitrate tetrahydrate and triammonium phosphate trihydrate as the calcium and phosphorous sources. Two types of gelatine were added to the sol: agar-agar or animals gelatine. Both were found to enhance the formation and stability of amorphous HAP using soluble salts as the sources of calcium and phosphate. HAP coatings were deposited from HAP-GEL sol using dip-withdrawal technique, then the plates were dried and annealed at temperatures 460-750 °C. FTIR spectroscopy and XRD analysis were used to study the phase composition of phosphate coatings. Morphology and chemical analysis of HAP layers was performed using a scanning electron microscope equipped with an energy dispersive X-ray analyser (SEM+EDX). The biological activity of sol-gel phosphate coatings was observed during thermostatic held in simulated body fluid (SBF). It was found that chemical composition and structure of HAP coatings depends on pH and final thermal treatment of the layer.
Fabrication of silica ceramic membrane via sol-gel dip-coating method at different nitric acid amount

NASA Astrophysics Data System (ADS)

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.
Thermostability of glucose oxidase in silica gel obtained by sol-gel method and in solution studied by fluorimetric method.

PubMed

Przybyt, Małgorzata; Miller, Ewa; Szreder, Tomasz

2011-04-04

The thermostability of glucose oxidase entrapped in silica gel obtained by sol-gel method was studied by thermostimulated fluorescence of FAD at pH 5 and 7 and compared with that of the native enzyme in the solution and at the presence of ethanol. The unfolding temperatures were found to be lower for the enzyme immobilised in gel as compared with the native enzyme but higher as for the enzyme at the presence of ethanol. In gel, the thermal denaturation of glucose oxidase is independent on pH while in solution the enzyme is more stable at pH 5. The investigation the enzyme in different environment by steady-state fluorescence of FAD and tryptophan, synchronous fluorescence and time-resolved fluorescence of tryptophan indicates that the state of the molecule (tertiary structure and molecular dynamics) is different in gel and in solution. The ethanol produced during gel precursor hydrolysis is not the main factor influencing the thermostability of the enzyme but more important are interactions of the protein with the gel lattice. Copyright © 2011 Elsevier B.V. All rights reserved.
Ultrapure glass optical waveguide development in microgravity by the sol-gel process

NASA Technical Reports Server (NTRS)

Mukherjee, S. P.; Holman, R. A.

1981-01-01

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 referred to here 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. The use of gels offers several advantages such as high purity and lower melting times and temperatures. The sol-gel process is studied for utilization in the preparation of multicomponent ultrapure glass batches for subsequent containerless melting of the batches in space to prepare glass blanks for optical waveguides.
One pot synthesis of exchange coupled Nd2Fe14B/alpha-Fe by pechini type sol-gel method.

PubMed

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

2013-11-01

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

PubMed

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.
Improved magnetic properties and growth anisotropy of chemically modified Sr ferrites

NASA Astrophysics Data System (ADS)

Lee, Jung W.; Cho, Yong S.; Amarakoon, Vasantha R. W.

1999-04-01

Magnetic properties and microstructural characteristics of SrOṡ5.9Fe2O3 chemically modified with Si and Ca were investigated by changing experimental parameters such as additive composition, the ratio of Ca/Si, and sintering condition. A novel particulate coating method utilizing sol-gel reactions was used to uniformly incorporate the additives of Si and Ca. This method was very successful in obtaining homogeneous grain growth and fine grains. A sample containing the gel additives of 0.6 wt % SiO2 and 0.7 wt % CaO and sintered at 1200 °C for 4 h was found to significantly suppress abnormal grain growth, resulting in submicron-sized grains and high density. A distinct grain boundary phase containing Si and Ca was observed by increasing the sintering temperature to 1250 °C. The resultant microstructural characteristics favorably affected magnetic properties. For example, the chemically modified sample exhibited a higher coercivity of 3530 Oe compared to a value of 2050 Oe obtained for the sample without the additives. On the other hand, an increase in the ratio of Ca/Si or in sintering temperature tended to induce a large anisotropy during grain growth.
Synthesis of phthalocyanine doped sol-gel materials

NASA Technical Reports Server (NTRS)

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 section ratio, 4, however, the tetrasulfonate groups make the dye soluble in water which greatly facilitates its incorporation into the sol-gel matrix. The nonlinear transmission of CuPc4S in a pH 2 buffer solution and in a silica xerogel were compared. It is evident that the CuPc4S preserves its optical limiting behavior in the sol-gel matrix, indicating that the fundamental excited state absorption process is essentially the same for a molecule in solution or in the solid state. Although the spectroscopic details of energy level lifetimes are unknown, the significance is that passive optical limiting has been achieved in the solid state via incorporation of a dye into an inorganic host. The only compromise occurs at the extremely high energy regime where photobleaching is observed. This is a result of the limited mobility of the dye molecules in the solid silica host relative to a liquid host. The effects of photodegradation in the xerogel are additive, whereas the solution provides a supply of fresh molecules that are free to enter the active volume between pulses.
Nanostructured aluminium titanate (Al{sub 2}TiO{sub 5}) particles and nanofibers: Synthesis and mechanism of microstructural evolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Azarniya, Abolfazl, E-mail: abolfazl_azarniya@mehr.sharif.ir; Azarniya, Amir, E-mail: a.azarnia91@gmail.com; Hosseini, Hamid Reza Madaah, E-mail: madaah@sharif.ir

In this study, aluminium titanate (AT) particles and nanofibers were synthesized through citrate sol gel and sol gel-assisted electrospinning methods in both nanostructured powder and nanofiber forms. The results of X-ray diffraction analysis, field-emission scanning electron microscopy and differential thermal analysis showed that the synthetic products benefit a nanostructured nature with a grain size less than 70 nm. The optimal values for time and temperature at which a roughly pure AT is attained were determined as 2 h and 900 °C, respectively. It was found that the sol gel precursor bears an amorphous structure till 700 °C and begins tomore » be crystallized to alumina, anatase and AT at higher temperatures. Moreover, AT tends to decompose into rutile and alumina at temperatures higher than 900 °C and its degradation rate reaches a maximum at temperatures near to 1100 °C. In this synthesis, citric acid was used as a chelating agent for Al{sup 3} {sup +} and Ti{sup 4} {sup +} ions and it was shown that a low citric acid-to-metal cation ratio leads to larger numbers of nuclei during crystallization and smaller grain size. Finally, a model was suggested to describe the microstructural evolution of AT compound based on a nucleation and growth regime. - Graphical abstract: Display Omitted - Highlights: • We synthesized aluminium titanate ceramic in both powder and nanofiber forms. • The methods in use were citrate sol gel and sol gel-assisted electrospinning. • Powders and nanofibers bear a nanostructured nature with a grain size less than 70 nm. • A model is suggested to describe microstructural evolution of synthetic products.« less
Comparing nanostructured hydroxyapatite coating on AZ91 alloy samples via sol-gel and electrophoretic deposition for biomedical applications.

PubMed

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.
Solid-state NMR study of geopolymer prepared by sol-gel chemistry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsai, Yi-Ling; Hanna, John V.; Lee, Yuan-Ling, E-mail: yuanlinglee@ntu.edu.t

2010-12-15

Geopolymers are a new class of materials formed by the condensation of aluminosilicates and silicates obtained from natural minerals or industrial wastes. In this work, the sol-gel method is used to synthesize precursor materials for the preparation of geopolymers. The geopolymer samples prepared by our synthetic route have been characterized by a series of physical techniques, including Fourier-transform infrared, X-ray diffraction, and multinuclear solid-state NMR. The results are very similar to those obtained for the geopolymers prepared from natural kaolinite. We believe that our synthetic approach can offer a good opportunity for the medical applications of geopolymer. -- Graphical abstract:more » Geopolymer prepared by the sol-gel route has the same spectroscopic properties as the sample prepared from the natural kaolinite. Display Omitted« less
Development and application of a sol-gel immunosorbent-based method for the determination of isoproturon in surface water.

PubMed

Zhang, Xiuli; Martens, Dieter; Krämer, Petra M; Kettrup, Antonius A; Liang, Xinmiao

2006-01-13

An immunosorbent was fabricated by encapsulation of monoclonal anti-isoproturon antibodies in sol-gel matrix. The immunosorbent-based loading, rinsing and eluting processes were optimized. Based on these optimizations, the sol-gel immunosorbent (SG-IS) selectively extracted isoproturon from an artificial mixture of 68 pesticides. In addition to this high selectivity, the SG-IS proved to be reusable. The SG-IS was combined with liquid chromatography-tandem mass spectrometry (LC-MS-MS) to determine isoproturon in surface water, and the linear range was up to 2.2 microg/l with correlation coefficient higher than 0.99 and relative standard deviation (RSD) lower than 5% (n=8). The limit of quantitation (LOQ) for 25-ml surface water sample was 5 ng/l.
Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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.
Method and apparatus for controlled size distribution of gel microspheres formed from aqueous dispersions. [Patent application

DOEpatents

Ryon, A.D.; Haas, P.A.; Vavruska, J.S.

1982-01-19

The present invention is directed to a method and apparatus for making a population of dense, closely size-controlled microspheres by sol-gel procedures wherein said microspheres are characterized by a significant percentage of said population being within a predetermined, relatively narrow size range. This is accomplished by subjecting aqueous dispersions of a sol, within a water-immiscible organic liquid to a turbulent flow. Microsphere populations thus provided are useful in vibratory-packed processes for nuclear fuels to be irradiated in LWR- and FBR-type nuclear reactors.
Preparation of Flame Retardant Polyacrylonitrile Fabric Based on Sol-Gel and Layer-by-Layer Assembly

PubMed Central

Ren, Yuanlin; Huo, Tongguo; Qin, Yiwen; Liu, Xiaohui

2018-01-01

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. PMID:29570646
Preparation of Flame Retardant Polyacrylonitrile Fabric Based on Sol-Gel and Layer-by-Layer Assembly.

PubMed

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.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Chitralekha, C. S.; Rasi, Mohammed; Nair, Swapna S., E-mail: swapna.s.nair@gmail.com

A modified sol-gel method was introduced by employing a cost effective novel template to synthesize coaxial one dimensional (1-D) composite nanostructures based on CoFe{sub 2}O{sub 4} (CFO) - K{sub 0.5}Na{sub 0.5}NbO{sub 3} (KNN) and magnetic nanostructures based on CoFe{sub 2}O{sub 4} (CFO). The studies with scanning electron microscopy (SEM) and atomic force microscopy (AFM) revealed that the composite material is characterized by the 1-D tubular structure. The absorption edge is blue shifted for both KNN and CFO nanotubes due to the lattice strain effect.
Switchable vanadium oxide films by a sol-gel process

NASA Astrophysics Data System (ADS)

Partlow, D. P.; Gurkovich, S. R.; Radford, K. C.; Denes, L. J.

1991-07-01

Thin polycrystalline films of VO2 and V2O3 were deposited on a variety of substrates using a sol-gel process. The orientation, microstructure, optical constants, and optical and electrical switching behavior are presented. These films exhibited sharp optical switching behavior even on an amorphous substrate such as fused silica. The method yields reproducible results and is amenable to the coating of large substrates and curved surfaces such as mirrors and lenses.
COLLABORATIVE RESEARCH AND DEVELOPMENT (CR&D) Delivery Order 0065: Nanostructured Dynamic Modulus Materials

DTIC Science & Technology

2008-03-01

solution-gelation (sol- gel) technique, to form hybrids of these materials with high-Tg open-cell foams so as to enhance shape memory characteristics , and...did not demonstrate the shape memory properties of the original Morthane thermoplastic due to the suppression of crystallinity following sol-gel...method. The utilization of photolatent bases to allow for improved reaction control and the combination of this system with Basotect™ open-cell foam in

Peri-tumor administration of 5-fluorouracil sol-gel using a hollow microneedle for treatment of gastric cancer.

PubMed

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 < .01). The 5-FU sol-gel induced apoptosis and significantly inhibited cell proliferation compared to the free 5-FU (p < .01). In addition, xenografted tumor growth was significantly suppressed by administration of the 5-FU sol-gel formulation to inoculated mice (p < .01), and 71% (5/7) of xenografted tumors disappeared after 4 weeks. In conclusion, peri-tumor injection of a 5-FU sol-gel formulation into normal tissue surrounding the tumor mass using a hollow microneedle is an effective method for treating gastric cancer.
Brilliant molecular nanocrystals emerging from sol-gel thin films: towards a new generation of fluorescent biochips.

PubMed

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

2009-08-05

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 Förster 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.
Influence of polyols on the formation of nanocrystalline nickel ferrite inside silica matrices

NASA Astrophysics Data System (ADS)

Stoia, Marcela; Barvinschi, Paul; Barbu-Tudoran, Lucian; Bunoiu, Mădălin

2017-01-01

We have synthesized nickel ferrite/silica nanocomposites, using a modified sol-gel method that combines the sol-gel processing with the thermal decomposition of metal-organic precursors, leading to a homogenous dispersion of ferrite nanoparticles within the silica matrix and a narrow size distribution. We used as starting materials tetraethyl orthosilicate (TEOS) as source of silica, Fe(III) and Ni(II) nitrates as sources of metal cations, and polyols as reducing agent (polyvinyl alcohol, 1,4-butanediol and their mixture). TG/DTA coupled technique evidenced the redox interaction between the polyol and the mixture of metal nitrates during the heating of the gel, with formation of nickel ferrite precursors in the pores of the silica-gels. FT-IR spectroscopy confirmed the formation of metal carboxylates inside the silica-gels and the interaction of the polyols with the Si-OH groups of the polysiloxane network. X-ray diffractometry evidenced that in case of nanocomposites obtained by using a single polyol, nickel ferrite forms as single crystalline phase inside the amorphous silica matrix, while in case of using a mixture of polyols the nickel oxide appears as a secondary phase. TEM microscopy and elemental mapping evidenced the fine nature of the obtained nickel ferrite nanoparticles that are homogenously dispersed within the silica matrix. The obtained nanocomposites exhibit magnetic behavior very close to superparamagnetism slightly depending on the presence and nature of the organic compounds used in synthesis; the magnetization reached at 5 kOe magnetic field was 7 emu/g for all composites.
PREPARATION OF HIGH-DENSITY, COMPACTIBLE THORIUM OXIDE PARTICLES

DOEpatents

McCorkle, K.H.; Kleinsteuber, A.T.; Schilling, C.E.; Dean, O.C.

1962-05-22

A method is given for preparing millimeter-size, highdensity thorium oxide particles suitable for fabrication into nuclear reactor feel elements by means of vibratory compaction. A thorium oxide gel containing 3.7 to 7 weight per cent residual volatile nitrate and water is prepared by drying a thorium oxide sol. The gel is then slowly heated to a temperature of about 450DEC, and the resulting gel fragments are calcined. The starting sol is prepared by repeated dispersion of oxalate-source thorium oxide in a nitrate system or by dispersion of steam-denitrated thorium oxide in water. (AEC)
Electrospun Polyhydroxybutyrate/Poly(ε-caprolactone)/58S Sol-Gel Bioactive Glass Hybrid Scaffolds with Highly Improved Osteogenic Potential for Bone Tissue Engineering.

PubMed

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

2016-07-13

Electrospinning of biopolymer and inorganic substances is one of the efficient ways to combine various advantageous properties in one single fibrous structure with potential for tissue engineering applications. In the present study, to integrate the high stiffness of polyhydroxybutyrate (PHB), the flexibility of poly(ε-caprolactone) (PCL) and the bioactivity of 58S bioactive glass, PHB/PCL/58S sol-gel bioactive glass hybrid scaffolds were fabricated using combined electrospinning and sol-gel method. Physical features such as fiber diameter distribution, mechanical strength and Young's modulus were characterized thoroughly. FTIR analysis demonstrated the successful incorporation of 58S bioactive glass into the blend polymers, which greatly improved the hydrophilicity of PHB/PCL fibermats. The primary biological response of MG-63 osteoblast-like cells on the prepared fibrous scaffolds was evaluated, proving that the 58S glass sol containing hybrid scaffold were not only favorable to MG-63 cell adhesion but also slightly enhanced cell viability and significantly increased alkaline phosphate activity .
Study of the sodium phenytoin effect on the formation of sol-gel SiO 2 nanotubes by TEM

NASA Astrophysics Data System (ADS)

López, T.; Asomoza, M.; Picquart, M.; Castillo-Ocampo, P.; Manjarrez, J.; Vázquez, A.; Ascencio, J. A.

2005-04-01

Microencapsulation is a versatile technology that allows controlling the release of different active molecules. Recently the sol-gel process has emerged like a promising method to immobilization and stabilization of biologically active compounds like enzymes, antigens, microorganisms and drugs. Porous silica and titanium dioxide materials made by low temperature sol-gel processes are promising host matrixes for encapsulation of biological molecules. The preparation of a low-temperature silica sol followed by gelation to neutral pH with water for injection containing the antiepileptic drug is reported here. The structure is very important so the analysis of the new developed material is also reported. Particularly interesting is the presence of nanotubes and microtubes, produced in the inorganic matrix in the presence of the sodium phenytoin. The use of transmission electron microscopy and quantum mechanics molecular simulation allows determining a micelle-like effect during the synthesis of these materials, which controls the size, structure and stability of them.
Investigation of corrosion protection performance of sol-gel surface treatments on AA2024-T3

NASA Astrophysics Data System (ADS)

Voevodin, Natalia Nikolajevna

The dissertation research project addresses the technologically important problem of replacement of chromate based coatings for corrosion protection of aircraft. A review of corrosion processes in high-strength aluminum alloys indicated that the strengthening intermetallic precipitates provide local cathodic areas, which may initiate surface pitting. The mechanisms of chromate inhibition in these localized corrosion processes were identified. The environmental hazard of chromates was also highlighted, serves as the impetus for chromate coating replacement. Sol-gel coatings are shown as an excellent alternative, based on environment compliance, flexibility in the composition control, and reasonable costs. Several sol-gel coatings were formulated and applied to the surface of an AA2024-T3 alloy. The coating composition and bonding were analyzed with XPS and FTIR, surface morphology was studied with SEM and AFM, and corrosion protection properties were tested with EIS, PDS, salt water immersion, and salt-fog exposure. The results demonstrated that epoxy-zirconate sol-gel coatings can provide excellent barrier properties. A novel SVET technique was applied for studies of local electrochemical processes in the pitting formation. This technique was further refined in model studies of aluminum surfaces with artificially created local cathodic regions, experimental studies of chromate inhibition with pit formation, and pitting development studies in sol-gel coatings with artificially introduced defects. Mechanisms of pitting development and inhibition with the pit initiation and growth kinetics were established. The Zr-epoxy coatings are subjected to the pit development and undercutting in the absence of the corrosion inhibitors. Several organic and non-organic inhibitors were evaluated in the sol-gel coating composition. Organic inhibitors had a better compliance with sol-gel chemistry and were identified for future studies. Experiments were performed to verify that sol-gel coatings can be used as barrier layers in complex coating systems. The results clearly demonstrated that Zr-epoxy sol-gel coatings are a viable replacement for the currently used chromate-based surface treatments. This work expands the fundamental knowledge of chromate coating replacement with chromate-free sol-gel coatings and identifies possible ways to implement this goal.
Uniform thin films of CdSe and CdSe(ZnS) core(shell) quantum dots by sol-gel assembly: enabling photoelectrochemical characterization and electronic applications.

PubMed

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

2013-02-26

Optoelectronic properties of quantum dot (QD) films are limited by (1) poor interfacial chemistry and (2) nonradiative 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 interparticle 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.
Uniform Thin Films of CdSe and CdSe(ZnS) Core(shell) Quantum Dots by Sol-Gel Assembly: Enabling Photoelectrochemical Characterization and Electronic Applications

PubMed Central

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
Mayenite Synthesized Using the Citrate Sol-Gel Method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ude, Sabina N; Rawn, Claudia J; Meisner, Roberta A

2014-01-01

A citrate sol-gel method has been used to synthesize mayenite (Ca12Al14O33). X-ray powder diffraction data show that the samples synthesized using the citrate sol-gel method contained CaAl2O4 and CaCO3 along with mayenite when fired ex-situ in air at 800 C but were single phase when fired at 900 C and above. Using high temperature x-ray diffraction, data collected in-situ in air at temperatures of 600 C and below showed only amorphous content; however, data collected at higher temperatures indicated the first phase to crystallize is CaCO3. High temperature x-ray diffraction data collected in 4% H2/96% N2 does not show themore » presence of CaCO3, and Ca12Al14O33 starts to form around 850 C. In comparison, x-ray powder diffraction data collected ex-situ on samples synthesized using traditional solid-state synthesis shows that single phase was not reached until samples were fired at 1350 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method suggest the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is very different depending on the environment. Brunauer-Emmett-Teller (BET) measurements showed a slightly higher surface area of 7.4 0.1 m2/g in the citrate gel synthesized samples compared to solid-state synthesized sample with a surface area of 1.61 0.02 m2/g. SEM images show a larger particle size for samples synthesized using the solid-state method compared to those synthesized using the citrate gel method.« less
The Complex Sol-Gel Process for producing small ThO2 microspheres

NASA Astrophysics Data System (ADS)

Brykala, Marcin; Rogowski, Marcin

2016-05-01

Thorium based fuels offer several benefits compared to uranium based fuels thus they might be an attractive alternative to conventional fuel types. This study is devoted to the synthesis and the characterization of small thorium dioxide microspheres (Ø <50 μm). Their application involves using powder-free process, called the Complex Sol-Gel Process. The source sols used for the processes were prepared by the method where in the starting ascorbic acid solution the solid thorium nitrate was dissolved and partially neutralized by aqueous ammonia under pH control. The microspheres of thorium-ascorbate gel were obtained using the ICHTJ Process (INCT in English). Studies allowed to determine an optimal heat treatment with calcination temperature of 700 °C and temperature rate not higher than 2 °C/min which enabled us to obtain a crack-free surface of microspheres. The main parameters which have a strong influence on the synthesis method and features of the spherical particles of thorium dioxide are described in this article.
Microstructural changes in NiFe2O4 ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

NASA Astrophysics Data System (ADS)

Chauhan, Lalita; Bokolia, Renuka; Sreenivas, K.

2016-05-01

Structural properties of Nickel ferrite (NiFe2O4) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe2O4 powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe2O4 ceramics with a uniform microstructure and a large grain size.
Two-Step Sintering Behavior of Sol-Gel Derived Dense and Submicron-Grained YIG Ceramics

NASA Astrophysics Data System (ADS)

Chen, Ruoyuan; Zhou, Jijun; Zheng, Liang; Zheng, Hui; Zheng, Peng; Ying, Zhihua; Deng, Jiangxia

2018-04-01

In this work, dense and submicron-grain yttrium iron garnet (YIG, Y3Fe5O12) ceramics were fabricated by a two-step sintering (TSS) method using nano-size YIG powder prepared by a citrate sol-gel method. The densification, microstructure, magnetic properties and ferromagnetic resonance (FMR) linewidth of the ceramics were investigated. The sample prepared at 1300°C in T 1, 1225°C in T 2 and 18 h holding time has a density higher than 98% of the theoretical value and exhibits a homogeneous microstructure with fine grain size (0.975 μm). In addition, the saturation magnetization ( M S) of this sample reaches 27.18 emu/g. High density and small grain size can also achieve small FMR linewidth. Consequently, these results show that the sol-gel process combined with the TSS process can effectively suppress grain-boundary migration while maintaining active grain-boundary diffusion to obtain dense and fine-grained YIG ceramics with appropriate magnetic properties.
Biocatalysis with Sol-Gel Encapsulated Acid Phosphatase

ERIC Educational Resources Information Center

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…
Passive and active sol-gel materials and devices

NASA Astrophysics Data System (ADS)

Andrews, Mark P.; Najafi, S. Iraj

1997-07-01

This paper examines sol-gel materials for photonics in terms of partnerships with other material contenders for processing optical devices. The discussion in four sections identifies semiconductors, amorphous and crystalline inorganic dielectrics, and amorphous and crystalline organic dielectrics as strategic agents in the rapidly evolving area of materials and devices for data communications and telecommunications. With Zyss, we trace the hierarchical lineage that connects molecular hybridization (chemical functionality), through supramolecular hybridization (collective properties and responses), to functional hybridization (device and system level constructs). These three concepts thread their way through discussions of the roles sol-gel glasses might be anticipated to assume in a photonics marketplace. We assign a special place to glass integrated optics and show how high temperature consolidated sol-gel derived glasses fit into competitive glass fabrication technologies. Low temperature hybrid sol-gel glasses that combine attractive features of organic polymers and inorganic glasses are considered by drawing on examples of our own new processes for fabricating couplers, power splitters, waveguides and gratings by combining chemical synthesis and sol-gel processing with simple photomask techniques.
Vibrational spectroscopic studies of (3-mercaptopropyl)trimethoxylsilane sol-gel and its coating.

PubMed

Li, Ying-Sing; Wang, Yu; Tran, Tuan; Perkins, Anshion

2005-10-01

Organosilane sol-gels have been prepared under different conditions from mercaptopropyltrimethoxysilane (MPTMS) and mercaptopropyltriethoxysilane (MPTES). These sol-gels were applied for the thin film coating on aluminum. Vibrational spectroscopy has been employed to trace and to study the proceeding of the sol-gel formation and the curing of the coated films on Al. Based on the group frequencies as well as their spectral behavior under different conditions, vibrational assignments have been made for most of the observed bands. Surface enhanced Raman scattering has revealed the chemical adsorption of MPTMS sol-gel on silver particles. Recorded reflection and absorption infrared (RAIR) spectra of coated tiles cured at different temperatures have indicated that surface reaction may occur at high temperature. The anticorrosion characters of the coated metals have been evaluated with the measured electrochemical data. Results from cyclic voltammographs have indicated that each layer of sol-gel coating would reduce the redox current across the electrode/electrolyte solution interface. Tafel plots have shown that the anodic current of the coated electrode decreases significantly and the corrosion potentials shift to the positive side.
Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films.

PubMed

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

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 degrees water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 degrees C and 500 degrees C.
Preparation and characterization of silica xerogels as carriers for drugs.

PubMed

Czarnobaj, K

2008-11-01

The aim of the present study was to utilize the sol-gel method to synthesize different forms of xerogel matrices for drugs and to investigate how the synthesis conditions and solubility of drugs influence the change of the profile of drug release and the structure of the matrices. Silica xerogels doped with drugs were prepared by the sol-gel method from a hydrolyzed tetraethoxysilane (TEOS) solution containing two model compounds: diclofenac diethylamine, (DD)--a water-soluble drug or ibuprofen, (IB)--a water insoluble drug. Two procedures were used for the synthesis of sol-gel derived materials: one-step procedure (the sol-gel reaction was carried out under acidic or basic conditions) and the two-step procedure (first, hydrolysis of TEOS was carried out under acidic conditions, and then condensation of silanol groups was carried out under basic conditions) in order to obtain samples with altered microstructures. In vitro release studies of drugs revealed a similar release profile in two steps: an initial diffusion-controlled release followed by a slower release rate. In all the cases studied, the released amount of DD was higher and the released time was shorter compared with IB for the same type of matrices. The released amount of drugs from two-step prepared xerogels was always lower than that from one-step base-catalyzed xerogels. One-step acid-catalyzed xerogels proved unsuitable as the carriers for the examined drugs.
Combining inkjet printing and sol-gel chemistry for making pH-sensitive surfaces.

PubMed

Orsi, Gianni; De Maria, Carmelo; Montemurro, Francesca; Chauhan, Veeren M; Aylott, Jonathan W; Vozzi, Giovanni

2015-01-01

Today biomedical sciences are experiencing the importance of imaging biological parameters with luminescence methods. Studying 2D pH distribution with those methods allows building knowledge about complex cellular processes. Immobilizing pH sensitive nanoparticles inside hydrogel matrixes, in order to guarantee a proper SNR, could easily make stable and biocompatible 2D sensors. Inkjet printing is also well known as tool for printing images onto porous surfaces. Recently it has been used as a free-form fabrication method for building three-dimensional parts, and now is being explored as a way of printing electrical and optical devices. Inkjet printing was used either as a rapid prototyping method for custom biosensors. Sol-gel method is naturally bound with inkjet, because the picoliter-sized ink droplets evaporate quickly, thus allowing quick sol-gel transitions on the printed surface. In this work will be shown how to merge those technologies, in order to make a nanoparticles doped printable hydrogel, which could be used for making 2D/3D smart scaffolds able to monitor cell activities. An automated image analysis system was developed in order to quickly have the pH measurements from pH nanosensors fluorescence images.
Effect of SiN x diffusion barrier thickness on the structural properties and photocatalytic activity of TiO2 films obtained by sol-gel dip coating and reactive magnetron sputtering.

PubMed

Ghazzal, Mohamed Nawfal; Aubry, Eric; Chaoui, Nouari; Robert, Didier

2015-01-01

We investigate the effect of the thickness of the silicon nitride (SiN x ) diffusion barrier on the structural and photocatalytic efficiency of TiO2 films obtained with different processes. We show that the structural and photocatalytic efficiency of TiO2 films produced using soft chemistry (sol-gel) and physical methods (reactive sputtering) are affected differentially by the intercalating SiN x diffusion barrier. Increasing the thickness of the SiN x diffusion barrier induced a gradual decrease of the crystallite size of TiO2 films obtained by the sol-gel process. However, TiO2 obtained using the reactive sputtering method showed no dependence on the thickness of the SiN x barrier diffusion. The SiN x barrier diffusion showed a beneficial effect on the photocatalytic efficiency of TiO2 films regardless of the synthesis method used. The proposed mechanism leading to the improvement in the photocatalytic efficiency of the TiO2 films obtained by each process was discussed.

Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Cao, Peng; Huang, Saifang; Zhang, Weijun; Huang, Zhaohui; Gao, Wei

2015-07-01

CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.
Matrix molecularly imprinted mesoporous sol-gel sorbent for efficient solid-phase extraction of chloramphenicol from milk.

PubMed

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 inter-assay RSD values were less than 13% and accuracy expressed as relative recovery ranged from 85 to 106%. Copyright © 2016 Elsevier B.V. All rights reserved.
Sol-Gel Derived Hafnia Coatings

NASA Technical Reports Server (NTRS)

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.
ZrO2-modified mesoporous nanocrystalline TiO2-xNx as efficient visible light photocatalysts.

PubMed

Wang, Xinchen; Yu, Jimmy C; Chen, Yilin; Wu, Ling; Fu, Xianzhi

2006-04-01

Mesoporous nanocrystalline TiO2-xNx and TiO2-xNx/ZrO2 visible-light photocatalysts have been prepared by a sol-gel method. The photocatalysts were characterized by XRD, N2 adsorption-desorption, TEM, XPS, UV/Vis, and IR spectroscopy. The photocatalytic activity of the samples was evaluated by the decomposition of ethylene in air under visible light (lambda > 450 nm) illumination. Results revealed that nitrogen was doped into the lattice of TiO2 by the thermal treatment of NH3-adsorbed TiO2 hydrous gels, converting the TiO2 into a visible-light responsive catalyst. The introduction of ZrO2 into TiO2-xNx considerably inhibits the undesirable crystal growth during calcination. Consequently, the ZrO2-modified TiO2-xNx displays higher porosity, higher specific surface area, and an improved thermal stability over the corresponding unmodified TiO2-xNx samples.
Theoretical Design of Multilayer Dental Posts Using CAD-Based Approach and Sol-Gel Chemistry.

PubMed

Maietta, Saverio; De Santis, Roberto; Catauro, Michelina; Martorelli, Massimo; Gloria, Antonio

2018-05-07

A computer-aided design (CAD)-based approach and sol-gel chemistry were used to design a multilayer dental post with a compositional gradient and a Young’s modulus varying from 12.4 to 2.3 GPa in the coronal-apical direction. Specifically, we propose a theoretical multilayer post design, consisting of titanium dioxide (TiO₂) and TiO₂/poly(ε-caprolactone) (PCL) hybrid materials containing PCL up to 24% by weight obtained using the sol-gel method. The current study aimed to analyze the effect of the designed multilayer dental post in endodontically treated anterior teeth. Stress distribution was investigated along and between the post and the surrounding structures. In comparison to a metal post, the most uniform distributions with lower stress values and no significant stress concentration were found when using the multilayer post.
Preparation of titanium dioxide films by sol-gel route for gas sensors

NASA Astrophysics Data System (ADS)

Schiopu, Vasilica; Matei, Alina; Cernica, Ileana; Podaru, Cecilia

2009-01-01

Semiconductor oxides such as SnO2, TiO2, WO3, ZnO2 etc. have been shown to be useful as gas sensor materials for monitoring various pollutant gases like H2S, NOx, NH3 etc. In this work, we would like to present the preparation of titanium dioxide films for gas sensor application, via the sol-gel technique. The coating solution was prepared by using titanium isopropoxide precursor, which was hydrolyzed with distilled water under the catalytic effect of different acids (HNO3, HCl or CH3COOH). Titanium dioxide films have been deposited using spin coating method and then synthesized at different temperatures. Fourier transform infrared spectroscopy observation has been used to analyze the sol-gel process. The morphology and the structure of the thin films were analyzed.
Photoluminescence from trivalent-cerium-doped silica glass prepared by sol-gel method with aluminum co-dopant

NASA Astrophysics Data System (ADS)

Tokumitsu, Seika; Murakami, Yukon; Oda, Hisaya; Kawabe, Yutaka

2018-01-01

Trivalent cerium is an important luminescent center giving light emission in short wavelength region depending on host materials. Sol-gel formed silica glass is an ideal matrix due to its high transparency, robustness, and low-temperature processability, but the emission from cerium in silica matrix is often mixed up with that from defects in the matrix, making it difficult to obtain well-determined characteristics. Bright emission from Ce ions peaking at about 400 nm was observed in sol-gel silica glasses synthesized with aluminum co-dopant. From luminescence decay time, the origin was confirmed to be d-f transition in trivalent Ce. From dependence of emission characteristics and UV absorbance on aluminum concentration, it was found that the co-dopant plays an important role to convert the optically inactive tetravalent ions to emissive trivalent state.
A fluorescence study of liposomes entrapped in sol-gel materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yamanaka, S.A.; Singh, S.; Sasaki, D.Y.

1997-12-31

Liposomes of phosphatidylcholine lipids were successfully entrapped in silicates using the sol-gel method with complete retention of the molecular aggregates over long periods in aqueous solution. Fluorescent studies of the small unilamellar vesicles of 5% pyrene labeled lipid PSIDA with DSPC remobilized in the gel found significant lipid reorganization upon aging in aqueous solutions. Monitoring of pyrene excimer (470 nm) to monomer (375 nm) ratios in the bilayer reveals that the silicate matrix tends to disperse PSIDA lipid aggregates from that observed in free solution. On an interesting note, the liposomes in the gel at pH 7.5. The PSIDA/DSPC liposomes,more » sensitive to heavy metal ions in free solution, maintain similar sensitivity in the gel yet the sensor material can not be recycled.« less
Synthesis of In2O3nanoparticles by thermal decomposition of a citrate gel precursor

NASA Astrophysics Data System (ADS)

Rey, J. F. Q.; Plivelic, T. S.; Rocha, R. A.; Tadokoro, S. K.; Torriani, I.; Muccillo, E. N. S.

2005-06-01

This paper describes the synthesis of indium oxide by a modified sol-gel method, and the study of thermal decomposition of the metal complex in air. The characterization of the intermediate as well as the final compounds was carried out by thermogravimetry, differential thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and small angle X-ray scattering. The results show that the indium complex decomposes to In2O3 with the formation of an intermediate compound. Nanoparticles of cubic In2O3 with crystallite sizes in the nanosize range were formed after calcination at temperatures up to 900°C. Calcined materials are characterized by a polydisperse distribution of spherical particles with sharp and smooth surfaces.
Down- and up-conversion luminescent carbon dot fluid: inkjet printing and gel glass fabrication.

PubMed

Wang, Fu; Xie, Zheng; Zhang, Bing; Liu, Yun; Yang, Wendong; Liu, Chun-yan

2014-04-07

Room temperature liquid-like nanoparticles have emerged as an exciting new research and development area, because their properties could be tailored over a broad range by manipulating geometric and chemical characteristics of the inorganic core and organic canopy. However, related applications are rarely reported due to the multi-step synthesis process and potential toxicity of cadmium based nanomaterials. In this study, we prepared inexpensive and eco-friendly carbon dot fluid by the direct thermal decomposition method. The carbon dot fluid can be excited from UV to near infrared light, and can be prepared as highly concentrated luminescent ink or incorporated into sol-gel derived organically modified silicate glass, suggesting that it has great application potential in the field of printable electronics, solid state lighting and so on.
Innovative Sol-Gel Routes for the Bottom-up Preparation of Heterogeneous Catalysts.

PubMed

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.
Preparation of fullerene/glass composites

DOEpatents

Mattes, Benjamin R.; McBranch, Duncan W.; Robinson, Jeanne M.; Koskelo, Aaron C.; Love, Steven P.

1995-01-01

Synthesis of fullerene/glass composites. A direct method for preparing solid solutions of C.sub.60 in silicon dioxide (SiO.sub.2) glass matrices by means of sol-gel chemistry is described. In order to produce highly concentrated fullerene-sol-gel-composites it is necessary to increase the solubility of these "guests" in a delivery solvent which is compatible with the starter sol (receiving solvent). Sonication results in aggregate disruption by treatment with high frequency sound waves, thereby accelerating the rate of hydrolysis of the alkoxide precursor, and the solution process for the C.sub.60. Depending upon the preparative procedure, C.sub.60 dispersed within the glass matrix as microcrystalline domains, or dispersed as true molecular solutions of C.sub.60 in a solid glass matrix, is generated by the present method.
Preparation of fullerene/glass composites

DOEpatents

Mattes, B.R.; McBranch, D.W.; Robinson, J.M.; Koskelo, A.C.; Love, S.P.

1995-05-30

Synthesis of fullerene/glass composites is described. A direct method for preparing solid solutions of C{sub 60} in silicon dioxide (SiO{sub 2}) glass matrices by means of sol-gel chemistry is described. In order to produce highly concentrated fullerene-sol-gel-composites it is necessary to increase the solubility of these ``guests`` in a delivery solvent which is compatible with the starter sol (receiving solvent). Sonication results in aggregate disruption by treatment with high frequency sound waves, thereby accelerating the rate of hydrolysis of the alkoxide precursor, and the solution process for the C{sub 60}. Depending upon the preparative procedure, C{sub 60} dispersed within the glass matrix as microcrystalline domains, or dispersed as true molecular solutions of C{sub 60} in a solid glass matrix, is generated by the present method.
Hydrogen Production by Steam Reforming of Ethanol over Nickel Catalysts Supported on Sol Gel Made Alumina: Influence of Calcination Temperature on Supports

PubMed Central

Yaakob, Zahira; Bshish, Ahmed; Ebshish, Ali; Tasirin, Siti Masrinda; Alhasan, Fatah H.

2013-01-01

Selecting a proper support in the catalyst system plays an important role in hydrogen production via ethanol steam reforming. In this study, sol gel made alumina supports prepared for nickel (Ni) catalysts were calcined at different temperatures. A series of (Ni/AlS.G.) catalysts were synthesized by an impregnation procedure. The influence of varying the calcination temperature of the sol gel made supports on catalyst activity was tested in ethanol reforming reaction. The characteristics of the sol gel alumina supports and Ni catalysts were affected by the calcination temperature of the supports. The structure of the sol gel made alumina supports was transformed in the order of γ → (γ + θ) → θ-alumina as the calcination temperature of the supports increased from 600 °C to 1000 °C. Both hydrogen yield and ethanol conversion presented a volcano-shaped behavior with maximum values of 4.3 mol/mol ethanol fed and 99.5%, respectively. The optimum values were exhibited over Ni/AlS.G800 (Ni catalyst supported on sol gel made alumina calcined at 800 °C). The high performance of the Ni/AlS.G800 catalyst may be attributed to the strong interaction of Ni species and sol gel made alumina which lead to high nickel dispersion and small particle size. PMID:28809270
Enzymatic liquefaction of agarose above the sol-gel transition temperature using a thermostable endo-type β-agarase, Aga16B.

PubMed

Kim, Jung Hyun; Yun, Eun Ju; Seo, Nari; Yu, Sora; Kim, Dong Hyun; Cho, Kyung Mun; An, Hyun Joo; Kim, Jae-Han; Choi, In-Geol; Kim, Kyoung Heon

2017-02-01

The main carbohydrate of red macroalgae is agarose, a heterogeneous polysaccharide composed of D-galactose and 3,6-anhydro-L-galactose. When saccharifying agarose by enzymes, the unique physical properties of agarose, namely the sol-gel transition and the near-insolubility of agarose in water, limit the accessibility of agarose to the enzymes. Due to the lower accessibility of agarose to enzymes in the gel state than to the sol state, it is important to prevent the sol-gel transition by performing the enzymatic liquefaction of agarose at a temperature higher than the sol-gel transition temperature of agarose. In this study, a thermostable endo-type β-agarase, Aga16B, originating from Saccharophagus degradans 2-40 T , was characterized and introduced in the liquefaction process. Aga16B was thermostable up to 50 °C and depolymerized agarose mainly into neoagarooligosaccharides with degrees of polymerization 4 and 6. Aga16B was applied to enzymatic liquefaction of agarose at 45 °C, which was above the sol-gel transition temperature of 1 % (w/v) agarose (∼35 °C) when cooling agarose. This is the first systematic demonstration of enzymatic liquefaction of agarose, enabled by determining the sol-gel temperature of agarose under specific conditions and by characterizing the thermostability of an endo-type β-agarase.
Hydrogen Production by Steam Reforming of Ethanol over Nickel Catalysts Supported on Sol Gel Made Alumina: Influence of Calcination Temperature on Supports.

PubMed

Yaakob, Zahira; Bshish, Ahmed; Ebshish, Ali; Tasirin, Siti Masrinda; Alhasan, Fatah H

2013-05-30

Selecting a proper support in the catalyst system plays an important role in hydrogen production via ethanol steam reforming. In this study, sol gel made alumina supports prepared for nickel (Ni) catalysts were calcined at different temperatures. A series of (Ni/Al S.G. ) catalysts were synthesized by an impregnation procedure. The influence of varying the calcination temperature of the sol gel made supports on catalyst activity was tested in ethanol reforming reaction. The characteristics of the sol gel alumina supports and Ni catalysts were affected by the calcination temperature of the supports. The structure of the sol gel made alumina supports was transformed in the order of γ → (γ + θ) → θ-alumina as the calcination temperature of the supports increased from 600 °C to 1000 °C. Both hydrogen yield and ethanol conversion presented a volcano-shaped behavior with maximum values of 4.3 mol/mol ethanol fed and 99.5%, respectively. The optimum values were exhibited over Ni/Al S.G800 (Ni catalyst supported on sol gel made alumina calcined at 800 °C). The high performance of the Ni/Al S.G800 catalyst may be attributed to the strong interaction of Ni species and sol gel made alumina which lead to high nickel dispersion and small particle size.
Investigations on photolon-and porphyrin-doped sol-gel fiberoptic coatings for laser-assisted applications in medicine

NASA Astrophysics Data System (ADS)

Bindig, U.; Ulatowska-Jarza, A.; Kopaczynska, M.; Müller, G.; Podbielska, H.

2008-01-01

In view of laser-assisted medical applications, the construction of silica-based sol-gel fiberoptic sensors based on photolon (Ph) and protoporphyrin IX (PP IX) is discussed. Electron microscopy and AFM were used to characterize the silica sol-gel coatings. AFM measurements indicate a change in the surface porosity. The PP IX-based sensors were constructed as a one-layer optode as well as a multilayered structure. An additional hybrid sensor made up of alternate layers of PP IX-and Ph-doped sol-gel was also constructed and examined. Sol-gel matrices were prepared from silicate precursor tetraethylorthosilicate (TEOS) mixed with ethanol in acid-catalyzed hydrolysis. The carrier matrices of photosensitive dyes were produced with factor R = 20, where R denotes the ratio of solvent moles (ethanol) to the number of TEOS moles. A multilayered coating was built up using the reverse-dipping technique. The overall coating thickness was determined by electron microscopy. Doped sol-gels with different PP IX concentrations were used to produce fiberoptic coatings. The film optodes with a different number of layers were examined by fluorescence spectroscopy. It was found that photolon and protoporphyrin IX entrapped in sol-gel preserve their chemical reactivity and have contact with the external environment. The hybrid sensor demonstrated clear fluorescence and a reversible behavior in gaseous environments.
A neutral branched platinum-acetylide complex possessing a tetraphenylethylene core: preparation of a luminescent organometallic gelator and its unexpected spectroscopic behaviour during sol-to-gel transition.

PubMed

Ren, Yuan-Yuan; Wu, Nai-Wei; Huang, Junhai; Xu, Zheng; Sun, Dan-Dan; Wang, Cui-Hong; Xu, Lin

2015-10-21

A neutral branched platinum-acetylide complex TPA possessing a tetraphenylethylene core was successfully prepared, which was found to form luminescent organometallic gels in ethyl acetate. Stimulated by temperature or F(-), the reversible gel-sol transition was realized. More interestingly, TPA exhibited an unexpected blue shift of the emission during the sol-to-gel transition.
A new sol-gel processing routine without chelating agents for preparing highly transparent solutions and nanothin films: engineering the role of chemistry to design the process

NASA Astrophysics Data System (ADS)

Ashiri, Rouholah

2015-01-01

The great sensitivity of titanium alkoxides to hydrolysis makes their sol-gel transformation very fast and thus difficult to control. A method was proposed to alleviate this drawback. Preparation of highly transparent solutions and nanothin films is another objective of the present research. Employing nanoemulsion method and optimizing the processing conditions, a clear solution of well-dispersed nanosized particles was obtained. With the proposed process BaTiO3 precursor sols and nanothin films with enhanced optical transparency towards the visible were prepared. The optimal formulation of the sol consists of acetic acid, barium acetate, 2-propanol, TTIP and deionized water with 6:1:1:1:150 M ratios, respectively. It was found that the reduction of the temperature in the initial stage of mixing of precursors controls the size of the forming species and accordingly improves the stability and transparency of the sol. The results also showed that the applied modifications and optimizations significantly downsize the particles within the sol to the nanometric scale and accordingly result in a significant improvement in the optical response of the products.
Facile Synthesis of Smart Nanocontainers as Key Components for Construction of Self-Healing Coating with Superhydrophobic Surfaces.

PubMed

Liang, Yi; Wang, MingDong; Wang, Cheng; Feng, Jing; Li, JianSheng; Wang, LianJun; Fu, JiaJun

2016-12-01

SiO2-imidazoline nanocomposites (SiO2-IMI) owning high loading capacity of corrosion inhibitor, 1-hexadecyl-3-methylimidazolium bromide (HMID), and a special acid/alkali dual-stimuli-accelerated release property have been synthesized via a one-step modified Stöber method. SiO2-IMI were uniformly distributed into the hydrophobic SiO2 sol to construct "host"-"guest" feedback active coating with a superhydrophobic surface (SiO2-IMI@SHSC) on aluminium alloy, AA2024, by dip-coating technique. SiO2-IMI as "guest" components have good compatibility with "host" sol-gel coating, and more importantly, once localized corrosion occurs on the surface of AA2024, SiO2-IMI can simultaneously respond to the increase in environmental pH around corrosive micro-cathodic regions and decrease in pH near micro-anodic regions, promptly releasing HMID to form a compact molecular film on the damaged surface, inhibiting corrosion spread and executing a self-healing function. The scanning vibrating electrode technique (SVET) was applied to illustrate the suppression process of cathodic/anodic corrosion activities. Furthermore, benefiting from the superhydrophobic surface, SiO2-IMI@SHSC remained its protective ability after immersion in 0.5 M NaCl solution for 35 days, which is far superior to the conventional sol-gel coating with the same coating thickness. The facile fabrication method of SiO2-IMI simplifies the construction procedure of SiO2-IMI@SHSC, which have great potential to replace non-environmental chromate conversion coatings for practical use.

Forming foam structures with carbon foam substrates

DOEpatents

Landingham, Richard L.; Satcher, Jr., Joe H.; Coronado, Paul R.; Baumann, Theodore F.

2012-11-06

The invention provides foams of desired cell sizes formed from metal or ceramic materials that coat the surfaces of carbon foams which are subsequently removed. For example, metal is located over a sol-gel foam monolith. The metal is melted to produce a metal/sol-gel composition. The sol-gel foam monolith is removed, leaving a metal foam.
Accelerated weathering of wood surfaces coated with multifunctional allkoxysilanes by sol-gel deposition

Treesearch

Mandla A. Tshabalala; John E. Gangstad

2003-01-01

Accelerated weathering of wood surfaces coated with hexadecyltrimethoxysilane (HDTMOS) in the presence of methyltrimethoxysilane (MTMOS) by the sol-gel process was investigated. The sol-gel process allowed the deposition of a covalently bound thin layer of polysiloxane networks on the wood surface that was resistant to water sorption and water leaching. The rate of...
Synthesis and thermal stability of zirconia and yttria-stabilized zirconia microspheres.

PubMed

Leib, Elisabeth W; Vainio, Ulla; Pasquarelli, Robert M; Kus, Jonas; Czaschke, Christian; Walter, Nils; Janssen, Rolf; Müller, Martin; Schreyer, Andreas; Weller, Horst; Vossmeyer, Tobias

2015-06-15

Zirconia microparticles produced by sol-gel synthesis have great potential for photonic applications. To this end, identifying synthetic methods that yield reproducible control over size uniformity is important. Phase transformations during thermal cycling can disintegrate the particles. Therefore, understanding the parameters driving these transformations is essential for enabling high-temperature applications. Particle morphology is expected to influence particle processability and stability. Yttria-doping should improve the thermal stability of the particles, as it does in bulk zirconia. Zirconia and YSZ particles were synthesized by improved sol-gel approaches using fatty acid stabilizers. The particles were heated to 1500 °C, and structural and morphological changes were monitored by SEM, ex situ XRD and high-energy in situ XRD. Zirconia particles (0.4-4.3 μm in diameter, 5-10% standard deviation) synthesized according to the modified sol-gel approaches yielded significantly improved monodispersities. As-synthesized amorphous particles transformed to the tetragonal phase at ∼450 °C with a volume decrease of up to ∼75% and then to monoclinic after heating from ∼650 to 850 °C. Submicron particles disintegrated at ∼850 °C and microparticles at ∼1200 °C due to grain growth. In situ XRD revealed that the transition from the amorphous to tetragonal phase was accompanied by relief in microstrain and the transition from tetragonal to monoclinic was correlated with the tetragonal grain size. Early crystallization and smaller initial grain sizes, which depend on the precursors used for particle synthesis, coincided with higher stability. Yttria-doping reduced grain growth, stabilized the tetragonal phase, and significantly improved the thermal stability of the particles. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.
Luminescence properties of Lu2O3: Tb film prepared by Pechini sol-gel method

NASA Astrophysics Data System (ADS)

Shen, Siqing; Wang, Jian; Xu, Zhibin; Xie, Jianjun; Shi, Ying

2010-10-01

Uniform and crack free Tb3+ doped lutetium oxide (Lu2O3:Tb) films were prepared by Pechini sol-gel method combined with the spin-coating technique. The influence of the different substrate (monocrystalline silicon (111) and silica glass) and atmosphere (N2 and Air) on the luminescence properties of films was investigated. According to the emission spectra, we found that the luminous intensity was higher on silica glass substrate. Moreover, it was found that the luminous intensity calcined in N2 was higher almost twice as that calcined in air.
Luminescence properties of Lu2O3: Tb film prepared by Pechini sol-gel method

NASA Astrophysics Data System (ADS)

Shen, Siqing; Wang, Jian; Xu, Zhibin; Xie, Jianjun; Shi, Ying

2011-02-01

Uniform and crack free Tb3+ doped lutetium oxide (Lu2O3:Tb) films were prepared by Pechini sol-gel method combined with the spin-coating technique. The influence of the different substrate (monocrystalline silicon (111) and silica glass) and atmosphere (N2 and Air) on the luminescence properties of films was investigated. According to the emission spectra, we found that the luminous intensity was higher on silica glass substrate. Moreover, it was found that the luminous intensity calcined in N2 was higher almost twice as that calcined in air.
Sol Gel-Derived SBA-16 Mesoporous Material

PubMed Central

Rivera-Muñoz, Eric M.; Huirache-Acuña, Rafael

2010-01-01

The aim of this article is to review current knowledge related to the synthesis and characterization of sol gel-derived SBA-16 mesoporous silicas, as well as a review of the state of the art in this issue, to take stock of knowledge about current and future applications. The ease of the method of preparation, the orderly structure, size and shape of their pores and control, all these achievable through simple changes in the method of synthesis, makes SBA-16 a very versatile material, potentially applicable in many areas of science and molecular engineering of materials. PMID:20957080
The Preparation of TiO₂ Film by the Sol-Gel Method and Evaluation of Its Self-Cleaning Property.

PubMed

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.
Structural and physical property study of sol-gel synthesized CoFe2-xHoxO4 nano ferrites

NASA Astrophysics Data System (ADS)

Patankar, K. K.; Ghone, D. M.; Mathe, V. L.; Kaushik, S. D.

2018-05-01

CoFe2-xHoxO4 (x = 0.00, 0.05, 0.10, 0.15, 0.20) ferrites were prepared by the suitably modified Sol-Gel technique. X-ray diffraction (XRD) analysis revealed that the substituted samples show phase pure formation till 10% substitution, which is far higher phase pure than the earlier reports. Upon further substitution an inevitable secondary phase of HoFeO3 along with the spinel phase despite regulating synthesis parameters in the sol-gel reaction route. These results are further corroborated more convincingly by room temperature neutron diffraction. Morphological features of the ferrites were studied by Scanning Electron Microscopy (SEM). The magnetic parameters viz. the saturation magnetization (Ms), coercivity (Hc) and remanence (Mr) were determined from room temperature isothermal magnetization. These parameters were found to decrease with increase in Ho substitution. The decrease in magnetization is analyzed in the light of exchange interactions between rare earth and transition metal ions. Magnetostriction measurements revealed interesting results and the presence of a secondary phase was found to be responsible for decreased measu-red magnetostriction values. The solubility limit of Ho in CoFe2O4 lattice is also reflected from the X-ray and neutron diffraction analysis and magnetostriction studies.
Sol-gel encapsulation for controlled drug release and biosensing

NASA Astrophysics Data System (ADS)

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.
A copper ion-selective electrode with high selectivity prepared by sol-gel and coated wire techniques.

PubMed

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

PubMed

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.
Hybrid sol-gel optical materials

DOEpatents

Zeigler, J.M.

1993-04-20

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.
Hybrid sol-gel optical materials

DOEpatents

Zeigler, John M.

1993-01-01

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.
Hybrid sol-gel optical materials

DOEpatents

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

PubMed Central

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

2017-01-01

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. PMID:28703123
Amoeba-like self-oscillating polymeric fluids with autonomous sol-gel transition

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

PubMed

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.
Optical pH detector based on LTCC and sol-gel technologies

NASA Astrophysics Data System (ADS)

Tadaszak, R. J.; Łukowiak, A.; Golonka, L. J.

2013-01-01

This paper presents an investigation on using sol-gel thin film as a material for sensors application in LTCC (Low Temperature Co-fired Ceramics) technology. This material gives the opportunity to make new, low-cost highly integrated optoelectronic devices. Sensors with optical detection are a significant part of these applications. They can be used for quick and safe diagnostics of some parameters. Authors present a pH detector with the optical detection system made of the LTCC material. The main part of the device is a flow channel with the chamber and sol-gel active material. The silica sol-gel with bromocresol green indicator was used. As the absorbance of sol-gel layer changes with the pH value of a measured medium, the transmitted light power was measured. The pH detector was integrated with the electronic components on the LTCC substrate.
A simple and inexpensive on-column frit fabrication method for fused-silica capillaries for increased capacity and versatility in LC-MS/MS applications.

PubMed

Wang, Ling-Chi; Okitsu, Cindy Yen; Kochounian, Harold; Rodriguez, Anthony; Hsieh, Chih-Lin; Zandi, Ebrahim

2008-05-01

A modified sol-gel method for a one-step on-column frit preparation for fused-silica capillaries and its utility for peptide separation in LC-MS/MS is described. This method is inexpensive, reproducible, and does not require specialized equipments. Because the frit fabrication process does not damage polyimide coating, the frit-fabricated column can be tightly connected on-line for high pressure LC. These columns can replace any capillary liquid transfer tubing without any specialized connections up-stream of a spray tip column. Therefore multiple columns with different phases can be connected in series for one- or multiple-dimensional chromatography.
Surfactant-Templated Mesoporous Metal Oxide Nanowires

DOE PAGES

Luo, Hongmei; Lin, Qianglu; Baber, Stacy; ...

2010-01-01

We demore » monstrate two approaches to prepare mesoporous metal oxide nanowires by surfactant assembly and nanoconfinement via sol-gel or electrochemical deposition. For example, mesoporous Ta 2 O 5 and zeolite nanowires are prepared by block copolymer Pluronic 123-templated sol-gel method, and mesoporous ZnO nanowires are prepared by electrodeposition in presence of anionic surfactant sodium dodecyl sulfate (SDS) surfactant, in porous membranes. The morphologies of porous nanowires are studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analyses.« less

Induced conductivity in sol-gel ZnO films by passivation or elimination of Zn vacancies

NASA Astrophysics Data System (ADS)

Winarski, D. J.; Anwand, W.; Wagner, A.; Saadatkia, P.; Selim, F. A.; Allen, M.; Wenner, B.; Leedy, K.; Allen, J.; Tetlak, S.; Look, D. C.

2016-09-01

Undoped and Ga- and Al- doped ZnO films were synthesized using sol-gel and spin coating methods and characterized by X-ray diffraction, high-resolution scanning electron microscopy (SEM), optical spectroscopy and Hall-effect measurements. SEM measurements reveal an average grain size of 20 nm and distinct individual layer structure. Measurable conductivity was not detected in the unprocessed films; however, annealing in hydrogen or zinc environment induced significant conductivity (˜10-2 Ω .cm) in most films. Positron annihilation spectroscopy measurements provided strong evidence that the significant enhancement in conductivity was due to hydrogen passivation of Zn vacancy related defects or elimination of Zn vacancies by Zn interstitials which suppress their role as deep acceptors. Hydrogen passivation of cation vacancies is shown to play an important role in tuning the electrical conductivity of ZnO, similar to its role in passivation of defects at the Si/SiO2 interface that has been essential for the successful development of complementary metal-oxide-semiconductor (CMOS) devices. By comparison with hydrogen effect on other oxides, we suggest that hydrogen may play a universal role in oxides passivating cation vacancies and modifying their electronic properties.
Structural, magnetic and hyperfine characterization of ZnxFe3-xO4 nanoparticles prepared by sol-gel approach via inorganic precursors

NASA Astrophysics Data System (ADS)

Kotsikau, Dzmitry; Pankov, Vladimir; Petrova, Elena; Natarov, Valentin; Filimonov, Dmitry; Pokholok, Konstantin

2018-03-01

Structural characteristics and magnetic properties of ZnxFe3-xO4 (where x = 0; 0.09; 0.18; 0.45; 1) nanoparticles were studied with X-ray diffraction (XRD), transmission electron microscopy (TEM), infrared spectroscopy (IR) and vibrating sample magnetometry (VSM). Oxidation of Fe2+ ions, redistribution of Zn2+ and Fe3+ ions between octahedral and tetrahedral sites, and the formation of cation vacancies in spinel-type cubic structure of the obtained ZnxFe3-x-y□yO4 substitutional solid solutions were revealed by 57Fe Mössbauer spectroscopy. The nanoparticles synthesized via a modified sol-gel method using inorganic precursors have a size of 4-10 nm, single-phase composition, superparamagnetic behavior at room temperature (300 K) and a relatively hydrophilic surface to form stable aqueous suspensions. The maximum magnetization of 59 emu/g at 300 K corresponds to Zn0.18Fe2.82O4 composition. The listed features make the materials promising candidates for various biological and medical applications such as contrast-enhanced magnetic resonance imaging, hyperthermia of pathological tissues, controlled drug release, and separation of nucleic acids.
Catalytic activity of calcium-based mixed metal oxides nanocatalysts in transesterification reaction of palm oil

NASA Astrophysics Data System (ADS)

Hassan, Noraakinah; Ismail, Kamariah Noor; Hamid, Ku Halim Ku; Hadi, Abdul

2017-12-01

Nowadays, biodiesel has become the forefront development as an alternative diesel fuel derived from biological sources such as oils of plant and fats. Presently, the conventional transesterification of vegetable oil to biodiesel gives rise to some technological problem. In this sense, heterogeneous nanocatalysts of calcium-based mixed metal oxides were synthesized through sol-gel method. It was found that significant increase of biodiesel yield, 91.75 % was obtained catalyzed by CaO-NbO2 from palm oil compared to pure CaO of 53.99 % under transesterification conditions (methanol/oil ratio 10:1, reaction time 3 h, catalyst concentration 4 wt%, reaction temperature 60 °C, and mixing speed of 600 rpm). The phase structure and crystallinity as well as the texture properties of the prepared catalysts were characterized by X-ray Diffraction (XRD) and the textural properties were characterized by N2 adsorption-desorption analysis. Sol-gel method has been known as versatile method in controlling the structural and chemical properties of the catalyst. Calcium-based mixed oxide synthesized from sol-gel method was found to exist as smaller crystallite size with high surface area.
Asymmetric bioreduction of acetophenones by Baker's yeast and its cell-free extract encapsulated in sol-gel silica materials

NASA Astrophysics Data System (ADS)

Kato, Katsuya; Nakamura, Hitomi; Nakanishi, Kazuma

2014-02-01

Baker's yeast (BY) encapsulated in silica materials was synthesized using a yeast cell suspension and its cell-free extract during a sol-gel reaction of tetramethoxysilane with nitric acid as a catalyst. The synthesized samples were fully characterized using various methods, such as scanning electron microscopy, nitrogen adsorption-desorption, Fourier transform infrared spectroscopy, thermogravimetry, and differential thermal analysis. The BY cells were easily encapsulated inside silica-gel networks, and the ratio of the cells in the silica gel was approximately 75 wt%, which indicated that a large volume of BY was trapped with a small amount of silica. The enzyme activity (asymmetric reduction of prochiral ketones) of BY and its cell-free extract encapsulated in silica gel was investigated in detail. The activities and enantioselectivities of free and encapsulated BY were similar to those of acetophenone and its fluorine derivatives, which indicated that the conformation structure of BY enzymes inside silica-gel networks did not change. In addition, the encapsulated BY exhibited considerably better solvent (methanol) stability and recyclability compared to free BY solution. We expect that the development of BY encapsulated in sol-gel silica materials will significantly impact the industrial-scale advancement of high-efficiency and low-cost biocatalysts for the synthesis of valuable chiral alcohols.
Y3Fe5O12 nanoparticulate garnet ferrites: Comprehensive study on the synthesis and characterization fabricated by various routes

NASA Astrophysics Data System (ADS)

Niaz Akhtar, Majid; Azhar Khan, Muhammad; Ahmad, Mukhtar; Murtaza, G.; Raza, Rizwan; Shaukat, S. F.; Asif, M. H.; Nasir, Nadeem; Abbas, Ghazanfar; Nazir, M. S.; Raza, M. R.

2014-11-01

The effects of synthesis methods such as sol-gel (SG), self combustion (SC) and modified conventional mixed oxide (MCMO) on the structure, morphology and magnetic properties of the (Y3Fe5O12) garnet ferrites have been studied in the present work. The samples of Y3Fe5O12 were sintered at 950 °C and 1150 °C (by SG and SC methods). For MCMO route the sintering was done at 1350 °C for 6 h. Synthesized samples prepared by various routes were investigated using X-ray diffraction (XRD) analysis, Field emission scanning electron microscopy (FESEM), Impedance network analyzer and transmission electron microscopy (TEM). The structural analysis reveals that the samples are of single phase structure and shows variations in the particle sizes and cells volumes, prepared by various routes. FESEM and TEM images depict that grain size increases with the increase of sintering temperature from 40 nm to 100 nm.Magnetic measurements reveal that garnet ferrite synthesized by sol gel method has high initial permeability (60.22) and low magnetic loss (0.0004) as compared to other garnet ferrite samples, which were synthesized by self combustion and MCMO methods. The M-H loops exhibit very low coercivity which enables the use of these materials in relays and switching devices fabrications. Thus, the garnet nanoferrites with low magnetic loss prepared by different methods may open new horizon for electronic industry for their use in high frequency applications.
Synthesis of Copper-Based Nanostructured Catalysts on SiO2-Al2O3, SiO2-TiO2, and SiO2-ZrO2 Supports for NO Reduction.

PubMed

Namkhang, Pornpan; Kongkachuichay, Paisan

2015-07-01

The selective catalytic reduction of NO over a series of Cu-based catalysts supported on modified silica including SiO2-Al2O3, SiO2-TiO2, and SiO2-ZrO2 prepared via a sol-gel process and a flame spray pyrolysis (FSP) was studied. The prepared catalysts were characterized by means of TEM, XRD, XRF, TPR, and nitrogen physisorption measurement techniques, to determine particle diameter, morphology, crystallinity, phase composition, copper reducibility, surface area, and pore size of catalysts. The particles obtained from sol-gel method were almost spherical while the particles obtained from the FSP were clearly spherical and non-porous nanosized particles. The effects of Si:Al, Si:Ti, and Si:Zr molar ratio of precursor were identified as the domain for different crystalline phase of materials. It was clearly seen that a high SiO2 content inhibited the crystallization of materials. The BET surface area of catalysts obtained from sol-gel method was higher than that from the FSP and it shows that surface area increased with increasing SiO2 molar ratio due to high surface area from SiO2. The catalyst performances were tested for the selective catalytic reduction of NO with H2. It was found that the catalyst prepared over 7 wt% Cu on Si02-Al2O3 support was the most active compared with the others which converted NO as more than 70%. Moreover, the excess copper decreased the performance of NO reduction, due to the formation of CuO agglomeration covered on the porous silica as well as the alumina surface, preventing the direct contact of CO2 and AL2O3.
Liposomes as protective capsules for active silica sol-gel biocomposite synthesis.

PubMed

Li, Ye; Yip, Wai Tak

2005-09-21

Using liposome to shield an enzyme from hostile chemical environments during the sol-gel formation process has resulted in a novel approach to synthesizing silica sol-gel biocomposite materials. By reporting the encapsulation of horseradish peroxidase and firefly luciferase, we demonstrate that this new protocol can produce silica biocomposites that are more active than trapping the enzymes directly into hydrogels.
Weathering characteristics and moisture uptake properties of wood coated with water-borne sol-gel thin films

Treesearch

M. A. Tshabalala; C. Starr; N. R. Sutherland

2010-01-01

In this study, wood specimens were coated with water-borne silsesquioxane oligomers by an in situ sol-gel deposition process. The effect of these water-borne sol-gel thin films on weathering characteristics and moisture-uptake properties of the wood specimens were investigated. The weathering characteristics were investigated by exposure of the specimens to artificial...
Radiation hardening of sol gel-derived silica fiber preforms through fictive temperature reduction.

PubMed

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

2016-09-20

The impact of fictive temperature (T_f) 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.
Renewable Decyl-alcohol Templated Synthesis of Si-Cu Core-Shell Nanocomposite

NASA Astrophysics Data System (ADS)

Salim, M. A.; >H Misran, S. Z.; Shah, N. N. H.; Razak, N. A. A.; >A Manap,
2013-06-01

Monodispersed silica spheres with particles size of ca. 450 nm were successfully synthesized using a modified Stöber method. The synthesized monodispersed silica spheres were successfully coated with copper using modified sol-gel method employing nonsurfactant surface modifiers and catalyst. A renewable palm oil based decyl-alcohol (C10) as nonsurfactant surface modifiers and catalyst were used to modify the silica surfaces prior to coating with copper. The X-ray diffraction patterns of Si-Cu core-shell exhibited a broad peak corresponding to amorphous silica networks and monoclinic CuO phase. It was found that samples modified in the presence of 1 ml catalyst exhibited homogeneous deposition. The surface area of core materials (SiO2) was at ca. 7.04 m2/g and Si-Cu core-shell was at ca. 8.21 m2/g. The band gap of samples prepared with and without catalyst was calculated to be ca. 2.45 eV and ca. 3.90 eV respectively based on the UV-vis absorption spectrum of the product.
Down- and up-conversion luminescent carbon dot fluid: inkjet printing and gel glass fabrication

NASA Astrophysics Data System (ADS)

Wang, Fu; Xie, Zheng; Zhang, Bing; Liu, Yun; Yang, Wendong; Liu, Chun-Yan

2014-03-01

Room temperature liquid-like nanoparticles have emerged as an exciting new research and development area, because their properties could be tailored over a broad range by manipulating geometric and chemical characteristics of the inorganic core and organic canopy. However, related applications are rarely reported due to the multi-step synthesis process and potential toxicity of cadmium based nanomaterials. In this study, we prepared inexpensive and eco-friendly carbon dot fluid by the direct thermal decomposition method. The carbon dot fluid can be excited from UV to near infrared light, and can be prepared as highly concentrated luminescent ink or incorporated into sol-gel derived organically modified silicate glass, suggesting that it has great application potential in the field of printable electronics, solid state lighting and so on.Room temperature liquid-like nanoparticles have emerged as an exciting new research and development area, because their properties could be tailored over a broad range by manipulating geometric and chemical characteristics of the inorganic core and organic canopy. However, related applications are rarely reported due to the multi-step synthesis process and potential toxicity of cadmium based nanomaterials. In this study, we prepared inexpensive and eco-friendly carbon dot fluid by the direct thermal decomposition method. The carbon dot fluid can be excited from UV to near infrared light, and can be prepared as highly concentrated luminescent ink or incorporated into sol-gel derived organically modified silicate glass, suggesting that it has great application potential in the field of printable electronics, solid state lighting and so on. Electronic supplementary information (ESI) available: Details of FTIR, XRD and DLS of CDF, optical properties of CDF, TEM images of other obtained products, luminescent spectra of CDF at different temperatures, and the optical photographs of CDF inks and silica glasses with different concentrations under normal, UV and 800 nm light. See DOI: 10.1039/c3nr05869g
Investigation of optical properties of anthocyanin doped into sol-gel based matrix

NASA Astrophysics Data System (ADS)

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

2012-06-01

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

PubMed

Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Marcé, Rosa Maria; Fontanals, Núria

2018-05-01

A novel sample preparation technique named capsule phase microextraction (CPME) is presented here. The technique utilizes a miniaturized microextraction capsule (MEC) as the extraction medium. The MEC consists of two conjoined porous tubular polypropylene membranes, one of which encapsulates the sorbent through sol-gel technology, while the other encapsulates a magnetic metal rod. As such, MEC integrates both the extraction and stirring mechanisms into a single device. The aim of this article is to demonstrate the application potential of CPME as sample preparation technique for the extraction of a group of personal care products (PCPs) from water matrices. Among the different sol-gel sorbent materials (UCON ® , poly(caprolactone-dimethylsiloxane-caprolactone) (PCAP-DMS-CAP) and Carbowax 20M (CW-20M)) evaluated, CW-20M MEC demonstrated the best extraction performance for the selected PCPs. The extraction conditions for sol-gel CW-20M MEC were optimized, including sample pH, stirring speed, addition of salt, extraction time, sample volume, liquid desorption solvent, and time. Under the optimal conditions, sol-gel CW-20M MEC provided recoveries, ranging between 47 and 90% for all analytes, except for ethylparaben, which showed a recovery of 26%. The method based on CPME with sol-gel CW-20M followed by liquid chromatography-tandem mass spectrometry was developed and validated for the extraction of PCPs from river water and effluent wastewater samples. When analyzing different environmental samples, some analytes such as 2,4-dihydroxybenzophenone, 2,2-dihydroxy-4-4 methoxybenzophenone and 3-benzophenone were found at low ng L -1 .
Synthesis of microspheres of triuranium octaoxide by simultaneous water and nitrate extraction from ascorbate-uranyl sols.

PubMed

Brykala, M; Deptula, A; Rogowski, M; Lada, W; Olczak, T; Wawszczak, D; Smolinski, T; Wojtowicz, P; Modolo, G

A new method for synthesis of uranium oxide microspheres (diameter <100 μm) has been developed. It is a variant of our patented Complex Sol-Gel Process, which has been used to synthesize high-quality powders of a wide variety of complex oxides. Starting uranyl-nitrate-ascorbate sols were prepared by addition of ascorbic acid to uranyl nitrate hexahydrate solution and alkalizing by aqueous ammonium hydroxide and then emulsified in 2-ethylhexanol-1 containing 1v/o SPAN-80. Drops of emulsion were firstly gelled by extraction of water by the solvent. Destruction of the microspheres during thermal treatment, owing to highly reactive components in the gels, requires modification of the gelation step by Double Extraction Process-simultaneously extraction of water and nitrates using Primene JMT, which completely eliminates these problem. Final step was calcination in air of obtained microspheres of gels to triuranium octaoxide.
Wet powder processing of sol-gel derived mesoporous silica-hydroxyapatite hybrid powders.

PubMed

Andersson, Jenny; Johannessen, Espen; Areva, Sami; Järn, Mikael; Lindén, Mika

2006-08-01

This paper describes a method by which a porous silica coating layer can be obtained on different apatite particles through a simple sol-gel synthesis route. Sol-gel derived powders of hydroxyapatite (HAP) and beta tricalciumphosphate (beta-TCP) were coated with a mesoporous silica using C16TAB (hexadecyltrimethylammonium bromide) as a template in order to induce mesophase formation. Further calcination of the material removes the template from the mesophase and leaves a highly ordered hexagonal arranged mesoporous silica structure with a core of HAP/beta-TCP. The phase purity of the SiO2/apatite composites has been thoroughly investigated by the means of FT-IR, XRD, and solid state 31P MAS NMR. The phase purity of these materials is shown to be dependent on the solubility properties of the used apatites. The hybrid materials are suitable as a multifunctional biomaterial where osteoconductive properties can be combined with drug delivery.
Optical properties of rhodamine 6G-doped TiO2 sol-gel films

NASA Astrophysics Data System (ADS)

Tomás, S. A.; Stolik, S.; Palomino, R.; Lozada, R.; Persson, C.; Ahuja, R.; Pepe, I.; Ferreira da Silva, A.

2005-06-01

The optical properties of titania (TiO2) thin films prepared by the sol-gel process and doped with rhodamine 6G were studied by Photoacoustic Spectroscopy. Rhodamine 6G-doping was achieved by adding 0.01%, 0.02%, 0.05% y 0.1% mol rhodamine to a solution that contained titanium isopropoxide as precursor. Two absorption regions were distinguished in the absorption spectrum of a typical rhodamine 6G-doped TiO2 film. A shift of these bands occured as a function of rhodamine 6G-doping concentration. In addition, the optical absorption and band gap energy for rutile-phase TiO2 films were calculated employing the full-potential linearized augmented plane wave method. A comparison of these calculations with experimental data of TiO2 films prepared by sol-gel at room temperature was performed.
Chemistry of surface nanostructures in lead precursor-rich PbZr0.52Ti0.48O3 sol-gel films

NASA Astrophysics Data System (ADS)

Gueye, I.; Le Rhun, G.; Gergaud, P.; Renault, O.; Defay, E.; Barrett, N.

2016-02-01

We present a study of the chemistry of the nanostructured phase at the surface of lead zirconium titanate PbZr0.52Ti0.48O3 (PZT) films synthesized by sol-gel method. In sol-gel synthesis, excess lead precursor is used to maintain the target stoichiometry. Surface nanostructures appear at 10% excess whereas 30% excess inhibits their formation. Using the surface-sensitive, quantitative X-ray photoelectron spectroscopy and glancing angle X-ray diffraction we have shown that the chemical composition of the nanostructures is ZrO1.82-1.89 rather than pyrochlore often described in the literature. The presence of a possibly discontinuous layer of wide band gap ZrO1.82-1.89 could be of importance in determining the electrical properties of PZT-based metal-insulator-metal heterostructures.
Nonhydrolytic sol-gel approach to facile creation of surface-bonded zirconia organic-inorganic hybrid coatings for sample preparation. Ι. Capillary microextraction of catecholamine neurotransmitters.

PubMed

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.
Optical Sensors for Biomolecules Using Nanoporous Sol-Gel Materials

NASA Technical Reports Server (NTRS)

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
Preparation of Composite Coating on AZ91D Magnesium Alloy by Silica Sol-Micro Oxidation

NASA Astrophysics Data System (ADS)

Shao, Zhongcai; Zhang, Feifei; Zhao, Ruiqiang; Shen, Xiaoyi

2016-03-01

Composite coating was prepared on AZ91D magnesium alloy with a new method which combined silica sol with micro-arc oxidation (MAO). The MAO coating was prepared on the basis of MAO solution, and then coated by sol-gel process. The composite coating was obtained after second MAO treatment. Scanning electron microscopy coupled with X-ray diffraction (XRD), energy spectrum analysis and electrochemical testing was applied to characterize the properties of MAO coating and composite coating. The experimental test results indicated that the Si element derived from SiO2 gel particle embedded into the MAO coating by second MAO treatment. The surface of composite coating became dense and the holes were smaller with silica sol sealing process. The corrosion resistance of composite coating was improved than the MAO coating.

Metal-doped organic gels and method thereof

DOEpatents

Satcher, Jr., Joe H.; Baumann, Theodore F.

2003-09-02

Disclosed herein is a sol-gel polymerization process for synthesizing metal-doped organic gels. The process polymerizes metal salts of hydroxylated benzenes or hydroxylated benzene derivatives with alkyl or aryl aldehydes to form metal-doped, wet, organic gels. The gels can then be dried by supercritical solvent extraction to form metal-doped aerogels or by evaporation to form metal-doped xerogels. The aerogels and xerogels can then be pyrolyzed.
Metal-doped organic gels and method thereof

DOEpatents

Satcher, Jr., Joe H.; Baumann, Theodore F.

2007-10-23

Disclosed herein is a sol-gel polymerization process for synthesizing metal-doped organic gels. The process polymerizes metal salts of hydroxylated benzenes or hydroxylated benzene derivatives with alkyl or aryl aldehydes to form metal-doped, wet, organic gels. The gels can then be dried by supercritical solvent extraction to form metal-doped aerogels or by evaporation to form metal-doped xerogels. The aerogels and xerogels can then be pyrolyzed.
Sol-gel thin-film based mesoporous silica and carbon nanotubes for the determination of dopamine, uric acid and paracetamol in urine.

PubMed

Canevari, Thiago C; Raymundo-Pereira, Paulo A; Landers, Richard; Benvenutti, Edilson V; Machado, Sérgio A S

2013-11-15

This work describes the preparation, characterization and application of a hybrid material composed of disordered mesoporous silica (SiO2) modified with multiwalled carbon nanotubes (MWCNTs), obtained by the sol-gel process using HF as the catalyst. This hybrid material was characterized by N2 adsorption-desorption isotherms, X-ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission microscopy (HR-TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). This new hybrid material was used for the construction of a thin film on a glassy carbon electrode. The modified electrode using this material was designated SiO2/MWCNT/GCE. The electrocatalytic properties of the electrode toward dopamine, uric acid and paracetamol oxidation were studied by differential pulse voltammetry. Well-defined and separated oxidation peaks were observed in phosphate buffer solution at pH 7.0, in contrast with the ill-defined peaks observed with unmodified glassy carbon electrodes. The electrode had high sensitivity for the determination of dopamine, uric acid and paracetamol, with the limits of detection obtained using statistical methods, at 0.014, 0.068 and 0.098 µmol L(-1), respectively. The electrode presented some important advantages, including enhanced physical rigidity, surface renewability by polishing and high sensitivity, allowing the simultaneous determination of these three analytes in a human urine sample. Crown Copyright © 2013 Published by Elsevier B.V. All rights reserved.
The Sol-Gel-Xerogel Transition

DTIC Science & Technology

1993-11-01

basic pH. Bioactive sol-gel glasses obtained by a surface adsorption of trypsin to a readymade xerogel were also completley * L...presence of siloxane chains and hydrophobic methyl groups an easy film deposition on glass sheets can be obtained. Rhodamine 6G and Coumarin 4 were...Research Proposal was prepared (early 1989) have witnessed a tremendous, almost explosive, progress in the field of organically doped sol-gel glasses
Sol-gel chemistry by ring-opening polymerization

DOE Office of Scientific and Technical Information (OSTI.GOV)

RAHIMIAN,KAMYAR; LOY,DOUGLAS A.

2000-02-07

Sol-gel processing of materials is plagued by shrinkage during polymerization of the alkoxide monomers and processing (aging and drying) of the resulting gels. The authors have developed a new class of hybrid organic-inorganic materials based on the solventless ring-opening polymerization (ROP) of monomers bearing the 2,2,5,5-tetramethyl-2,5-disilaoxacyclopentyl group, which permits them to drastically reduce shrinkage in sol-gel processed materials. Because the monomers are polymerized through a chain growth mechanism catalyzed by base rather than the step growth mechanism normally used in sol-gel systems, hydrolysis and condensation products are entirely eliminated. Furthermore, since water is not required for hydrolysis, an alcohol solventmore » is not necessary. Monomers with two disilaoxacyclopentyl groups, separated by a rigid phenylene group or a more flexible alkylene group, were prepared through disilylation of the corresponding diacetylenes, followed by ring closure and hydrogenation. Anionic polymerization of these materials, either neat or with 2,2,5,5-tetramethyl-2,5-disila-1-oxacyclopentane as a copolymer, affords thermally stable transparent gels with no visible shrinkage. These materials provide an easy route to the introduction of sol-gel type materials in encapsulation of microelectronics, which they have successfully demonstrated.« less
Piezoelectric Sol-Gel Composite Film Fabrication by Stencil Printing.

PubMed

Kaneko, Tsukasa; Iwata, Kazuki; Kobayashi, Makiko

2015-09-01

Piezoelectric films using sol-gel composites could be useful as ultrasonic transducers in various industrial fields. For sol-gel composite film fabrication, the spray coating technique has been used often because of its adaptability for various substrates. However, the spray technique requires multiple spray coating processes and heating processes and this is an issue of concern, especially for on-site fabrication in controlled areas. Stencil printing has been developed to solve this issue because this method can be used to fabricate thick sol-gel composite films with one coating process. In this study, PbTiO3 (PT)/Pb(Zr,Ti)O3 (PZT) films, PZT/PZT films, and Bi4Ti3O12 (BiT)/PZT films were fabricated by stencil printing, and PT/ PZT films were also fabricated using the spray technique. After fabrication, a thermal cycle test was performed for the samples to compare their ultrasonic performance. The sensitivity and signal-to-noise-ratio (SNR) of the ultrasonic response of PT/PZT fabricated by stencil printing were equivalent to those of PT/PZT fabricated by the spray technique, and better than those of other samples between room temperature and 300°C. Therefore, PT/PZT films fabricated by stencil printing could be a good candidate for nondestructive testing (NDT) ultrasonic transducers from room temperature to 300°C.
Microstructural changes in NiFe{sub 2}O{sub 4} ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chauhan, Lalita, E-mail: chauhan.lalita5@gmail.com; Sreenivas, K.; Bokolia, Renuka

2016-05-23

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

PubMed

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.
Novel Materials through Non-Hydrolytic Sol-Gel Processing: Negative Thermal Expansion Oxides and Beyond

PubMed Central

Lind, Cora; Gates, Stacy D.; Pedoussaut, Nathalie M.; Baiz, Tamam I.

2010-01-01

Low temperature methods have been applied to the synthesis of many advanced materials. Non-hydrolytic sol-gel (NHSG) processes offer an elegant route to stable and metastable phases at low temperatures. Excellent atomic level homogeneity gives access to polymorphs that are difficult or impossible to obtain by other methods. The NHSG approach is most commonly applied to the preparation of metal oxides, but can be easily extended to metal sulfides. Exploration of experimental variables allows control over product stoichiometry and crystal structure. This paper reviews the application of NHSG chemistry to the synthesis of negative thermal expansion oxides and selected metal sulfides.
Surface and catalytic properties of acid metal carbons prepared by the sol gel method

NASA Astrophysics Data System (ADS)

Aguado-Serrano, J.; Rojas-Cervantes, M. L.; Martín-Aranda, R. M.; López-Peinado, A. J.; Gómez-Serrano, V.

2006-06-01

The sol-gel method has been applied for the synthesis of a series of acid metal-carbon xerogels (with M = V, Cr, Mo and Ni) by polymerisation of resorcinol with formaldehyde in the presence of metallic precursors. A blank sample was also prepared without any metal addition. The xerogels were heated in nitrogen at 1000 °C to obtain the pyrolysed products. The samples were characterised by different techniques such as thermal-mass spectrometry analysis, gas physisorption, and mercury porosimetry. In addition, the acid character of the pyrolysed products was tested by the Claisen-Schmidt condensation between benzaldehyde and acetophenone for the formation of chalcones.
Sol-gel syntheses of pentaborate β-LaB5O9 and the photoluminescence by doping with Eu3+, Tb3+, Ce3+, Sm3+, and Dy3+

NASA Astrophysics Data System (ADS)

Yang, Ruirui; Sun, Xiaorui; Jiang, Pengfei; Gao, Wenliang; Cong, Rihong; Yang, Tao

2018-02-01

Rare earth (RE) borates have been extensively studied as good photoluminescent materials, however, the target hosts were limited to "RE3BO6", REBO3, and REB3O6 in the RE2O3-B2O3 phase diagram until the recent discovery of rare earth pentaborate. For the first time, the sol-gel method was employed to synthesize β-LaB5O9 doped with Eu3+, Tb3+, Ce3+, Sm3+, Dy3+. In comparison to the previous synthetic methods, the sol-gel method possesses superiorities including easily-controllable doping concentration, high yield and emission efficiency. Solid solutions of phosphors were prepared and carefully analyzed by powder X-ray diffraction. Concentration quenching or saturation was observed in Eu3+, Tb3+ and Ce3+ doped phosphors at round 10 at%. Eu3+, Tb3+, Sm3+, and Dy3+ emit red, green, orange, and close-to-white light, respectively. The absolute emission efficiency of Ce3+ is high and in the UV range, suggesting the function of being sensitizer once combined with other activators.
Tertiary-amine-containing thermo- and pH-sensitive hydrophilic ABA triblock copolymers: effect of different tertiary amines on thermally induced sol-gel transitions.

PubMed

Henn, Daniel M; Wright, Roger A E; Woodcock, Jeremiah W; Hu, Bin; Zhao, Bin

2014-03-11

This Article reports on the synthesis of a series of well-defined, tertiary-amine-containing ABA triblock copolymers, composed of a poly(ethylene oxide) (PEO) central block and thermo- and pH-sensitive outer blocks, and the study of the effect of different tertiary amines on thermally induced sol-gel transition temperatures (T(sol-gel)) of their 10 wt % aqueous solutions. The doubly responsive ABA triblock copolymers were prepared from a difunctional PEO macroinitiator by atom transfer radical polymerization of methoxydi(ethylene glycol) methacrylate and ethoxydi(ethylene glycol) methacrylate at a feed molar ratio of 30:70 with ∼5 mol % of either N,N-diethylaminoethyl methacrylate (DEAEMA), N,N-diisopropylaminoethyl methacrylate, or N,N-di(n-butyl)aminoethyl methacrylate. The chain lengths of thermosensitive outer blocks and the molar contents of tertiary amines were very similar for all copolymers. Using rheological measurements, we determined the pH dependences of T(sol-gel) of 10 wt % aqueous solutions of these copolymers in a phosphate buffer. The T(sol-gel) versus pH curves of all polymers exhibited a sigmoidal shape. The T(sol-gel) increased with decreasing pH; the changes were small on both high and low pH sides. At a specific pH, the T(sol-gel) decreased with increasing the hydrophobicity of the tertiary amine, and upon decreasing pH the onset pH value for the T(sol-gel) to begin to increase noticeably was lower for the more hydrophobic tertiary amine-containing copolymer. In addition, we studied the effect of different tertiary amines on the release behavior of FITC-dextran from 10 wt % micellar gels in an acidic medium at 37 and 27 °C. The release profiles for three studied hydrogels at 37 °C were essentially the same, suggesting that the release was dominated by the diffusion of FITC-dextran. At 27 °C, the release was significantly faster for the DEAEMA-containing copolymer, indicating that both diffusion and gel dissolution contributed to the release at this temperature.
Structural properties and gas sensing behavior of sol-gel grown nanostructured zinc oxide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rajyaguru, Bhargav; Gadani, Keval; Kansara, S. B.

2016-05-06

In this communication, we report the results of the studies on structural properties and gas sensing behavior of nanostructured ZnO grown using acetone precursor based modified sol-gel technique. Final product of ZnO was sintered at different temperatures to vary the crystallite size while their structural properties have been studied using X-ray diffraction (XRD) measurement performed at room temperature. XRD results suggest the single phasic nature of all the samples and crystallite size increases from 11.53 to 20.96 nm with increase in sintering temperature. Gas sensing behavior has been studied for acetone gas which indicates that lower sintered samples are moremore » capable to sense the acetone gas and related mechanism has been discussed in the light of crystallite size, crystal boundary density, defect mechanism and possible chemical reaction between gas traces and various oxygen species.« less
Effects of ion irradiation on the mechanical properties of SiNa wO xC yH z sol-gel derived thin films

NASA Astrophysics Data System (ADS)

Lucca, D. A.; Qi, Y.; Harriman, T. A.; Prenzel, T.; Wang, Y. Q.; Nastasi, M.; Dong, J.; Mehner, A.

2010-10-01

A study of the effects of ion irradiation of hybrid organic/inorganic modified silicate thin films on their mechanical properties is presented. NaOH catalyzed SiNa wO xC yH z thin films were synthesized by sol-gel processing from tetraethylorthosilicate (TEOS) and methyltriethoxysilane (MTES) precursors and spin-coated onto Si substrates. After drying at 300 °C, the films were irradiated with 125 keV H + or 250 keV N 2+ at fluences ranging from 1 × 10 14 to 2.5 × 10 16 ions/cm 2. Nanoindentation was used to characterize the films. Changes in hardness and reduced elastic modulus were examined as a function of ion fluence and irradiating species. The resulting increases in hardness and reduced elastic modulus are compared to similarly processed acid catalyzed silicate thin films.
Titanium modified with layer-by-layer sol-gel tantalum oxide and an organodiphosphonic acid: a coating for hydroxyapatite growth.

PubMed

Arnould, C; Volcke, C; Lamarque, C; Thiry, P A; Delhalle, J; Mekhalif, Z

2009-08-15

Titanium and its alloys are widely used in surgical implants due to their appropriate properties like corrosion resistance, biocompatibility, and load bearing. Unfortunately when metals are used for orthopedic and dental implants there is the possibility of loosening over a long period of time. Surface modification is a good way to counter this problem. A thin tantalum oxide layer obtained by layer-by-layer (LBL) sol-gel deposition on top of a titanium surface is expected to improve biocorrosion resistance in the body fluid, biocompatibility, and radio-opacity. This elaboration step is followed by a modification of the tantalum oxide surface with an organodiphosphonic acid self-assembled monolayer, capable of chemically binding to the oxide surface, and also improving hydroxyapatite growth. The different steps of this proposed process are characterized by surfaces techniques like contact angle, X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM).
Fabrication of a novel nanocomposite based on sol-gel process for hollow fiber-solid phase microextraction of aflatoxins: B1 and B2, in cereals combined with high performane liquid chromatography-diode array detection.

PubMed

Es'haghi, Zarrin; Sorayaei, Hoda; Samadi, Fateme; Masrournia, Mahboubeh; Bakherad, Zohreh

2011-10-15

The new pre-concentration technique, hollow fiber-solid phase microextraction based on carbon nanotube reinforced sol-gel and liquid chromatography-photodiode array detection was applied to determination of aflatoxins B(1), B(2) (AFB(1), AFB(2)) in rice, peanut and wheat samples. This research provides an overview of trends related to synthesis of solid phase microextraction (SPME) sorbnents that improves the assay of aflatoxins as the semi-polar compounds in several real samples. It mainly includes summary and a list of the results for a simple carbon nanotube reinforced sol-gel in-fiber device. This device was used for extraction, pre-concentration and determination of aflatoxins B1, B2 in real samples. In this technique carbon nanotube reinforced sol was prepared by the sol-gel method via the reaction of phenyl trimethoxysilane (PTMS) with a basic catalyst (tris hydroxymethyl aminomethan). The influences of microextraction parameters such as pH, ageing time, carbon nanotube contents, desorption conditions, desorption solvent and agitation speed were investigated. Optimal HPLC conditions were: C(18) reversed phase column for separation, water-acetonitril-methanol (35:10:55) as the mobile phase and maximum wavelength for detection was 370 nm. The method was evaluated statistically and under optimized conditions, the detection limits for the analytes were 0.074 and 0.061 ng/mL for B1 and B2 respectively. Limit of quantification for B1 and B2 was 0.1 ng/mL too (n=7). The precisions were in the range of 2.829-2.976% (n=3), and linear ranges were within 0.1 and 400 ng/mL. The method was successfully applied to the analysis of cereals (peanut, wheat, rice) with the relative recoveries from 47.43% to 106.83%. Copyright © 2011 Elsevier B.V. All rights reserved.
A thermosensitive hydrogel based on biodegradable amphiphilic poly(ethylene glycol) polycaprolactone poly(ethylene glycol) block copolymers

NASA Astrophysics Data System (ADS)

Gong, Chang Yang; Qian, Zhi Yong; Liu, Cai Bing; Juan Huang, Mei; Gu, Ying Chun; Wen, Yan Jun; Kan, Bing; Wang, Ke; Dai, Mei; Li, Xing Yi; Gou, Ma Ling; Tu, Ming Jing; Wei, Yu Quan

2007-06-01

A series of low molecular weight poly(ethylene glycol)-polycaprolactone-poly(ethylene glycol) (PEG-PCL-PEG) biodegradable block copolymers were successfully synthesized using isophorone diisocyanate (IPDI) as the coupling agent, and were characterized using 1H NMR and Fourier transform infrared spectroscopy. The aqueous solutions of the PEG-PCL-PEG copolymers displayed a special thermosensitive gel-sol transition when the concentration was above the corresponding critical gel concentration. Gel-sol phase diagrams were recorded using the test-tube-inversion method; they depended on the hydrophilic/hydrophobic balance in the macromolecular structure, as well as some other factors, including the heating history, volume, and the ageing time of the copolymer aqueous solutions and dissolution temperature of the copolymers. As a result, the gel-sol transition temperature range could be altered, which might be very useful for application in injectable drug delivery systems. This work was financially supported by the Chinese Key Basic Research Program (2004CB518800 and 2004CB518807), and the Sichuan Key Project of Science and Technology (06(05SG022-021-02)).
Plasmon mediated cathodic photocurrent generation in sol-gel synthesized doped SrTiO{sub 3} nanofilms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sugavaneshwar, Ramu Pasupathi, E-mail: r.p.sugavaneshwar@nims.go.jp, E-mail: NAGAO.Tadaaki@nims.go.jp; Chen, Kai; Lakshminarayana, Gandham

2015-11-01

Thin films of SrTiO{sub 3} (STO) and Rh-doped SrTiO{sub 3} (Rh-STO) were synthesized by sol-gel method and loaded with Ag nanoparticles. Pristine STO films exhibited anodic photocurrent while Rh-STO exhibited cathodic photocurrent. An enhancement in the overall cathodic photocurrent is observed with Ag nanoparticle loading and an additional enhancement in the visible light range is seen from the incident photon-to-current efficiency spectrum due to synergetic effect of Rh doping and Ag loading in STO.
Sol-gel-derived double-layered nanocrystal memory

NASA Astrophysics Data System (ADS)

Ko, Fu-Hsiang; You, Hsin-Chiang; Lei, Tan-Fu

2006-12-01

The authors have used the sol-gel spin-coating method to fabricate a coexisting hafnium silicate and zirconium silicate double-layered nanocrystal (NC) memories. From transmission electron microscopic and x-ray photoelectron spectroscopic analyses, the authors determined that the hafnium silicate and zirconium silicate NCs formed after annealing at 900°C for 1min. When using channel hot electron injection for charging and band-to-band tunneling-induced hot hole injection for discharging, the NC memories exhibited superior Vth shifting because of the higher probability for trapping the charge carrier.
Fabrication of transparent ceramics using nanoparticles

DOEpatents

Cherepy, Nerine J; Tillotson, Thomas M; Kuntz, Joshua D; Payne, Stephen A

2012-09-18

A method of fabrication of a transparent ceramic using nanoparticles synthesized via organic acid complexation-combustion includes providing metal salts, dissolving said metal salts to produce an aqueous salt solution, adding an organic chelating agent to produce a complexed-metal sol, heating said complexed-metal sol to produce a gel, drying said gel to produce a powder, combusting said powder to produce nano-particles, calcining said nano-particles to produce oxide nano-particles, forming said oxide nano-particles into a green body, and sintering said green body to produce the transparent ceramic.

Green synthesis and characterization of size tunable silica-capped gold core-shell nanoparticles

NASA Astrophysics Data System (ADS)

Wangoo, Nishima; Shekhawat, Gajendra; Wu, Jin-Song; Bhasin, Aman K. K.; Suri, C. R.; Bhasin, K. K.; Dravid, Vinayak

2012-08-01

Silica-coated gold nanoparticles (Au@SiO2) with controlled silica-shell thickness were prepared by a modified Stober's method using 10-nm gold nanoparticles (AuNPs) as seeds. The AuNPs were silica-coated with a sol-gel reaction using tetraethylorthosilicate (TEOS) as a silica source and ammonia as a catalyst. An increase in TEOS concentration resulted in an increase in shell thickness. The NPs were characterized by transmission electron microscopy, selected area electron diffraction, energy-dispersive X-ray spectroscopy, scanning near-field ultrasound holography and scanning transmission electron microscopy. The method required no surface modification and the synthesized core shell nanoparticles can be used for various types of biological applications.
Production of monodisperse cerium oxide microspheres with diameters near 100 µm by internal-gelation sol–gel methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

Cerium dioxide microspheres with uniform diameters between 65 – 211 µm were fabricated using internal gelation sol-gel methods. Although uniform microspheres are produced for nuclear fuel applications with diameters above 300 µm, sol-gel microspheres with diameters of 50 - 200 µm have historically been made by emulsion techniques and had poor size uniformity [1, 2]. An internal gelation, sol-gel apparatus was designed and constructed to accommodate the production of small, uniform microspheres whereby cerium-containing solutions were dispersed into flowing silicone oil and heated in a gelation column to initiate solidification [3, 4]. Problems with premature feed gelation and microsphere coalescencemore » were overcome by equipment modifications unique among known internal gelation setups. Microspheres were fabricated and sized in batches as a function of dispersing needle diameter and silicone oil flow rate in the two-fluid nozzle in order to determine the range of sizes possible and corresponding degree of monodispersity. Initial experiments with poor size uniformity were linked to microsphere coalescence in the gelation column prior to solidification as well as excessive flow rates for the cerium feed solution. Average diameter standard deviations as low as 2.23% were observed after optimization of flow rates and minimization of coalescence reactions.« less
Development of flame retardant cotton fabric based on ionic liquids via sol-gel technique.

NASA Astrophysics Data System (ADS)

Bentis, A.; Boukhriss, A.; Boyer, D.; Gmouh, S.

2017-10-01

In this study, flame retardant cotton fabrics were developed by the sol-gel method, in order to enhance their flame retardant proprieties. For this aim, seven sols were prepared using tetraethylorthosilicate (TEOS) and different ionic liquids (ILs) consist on pyridinium and Methylimidazolium cations with different anions such as: PF6-, CH3COO-, and Br-. Those sols were applied separately to the cotton fabrics by a pad-dry-cure process. The flame retardant properties of functionalized cotton fabrics before and after washing were determined by the vertical flame tests according to ISO6940:2004(F) standard. The effects of anions have been thoroughly investigated, aiming at the optimization of the targeted properties. Thermogravimetric and mechanical according to NF EN ISO 13934-1:2013standard, analyses have been also investigated. The results showed that flame retardancy, thermal stability and mechanical properties of treated fabrics were enhanced by using ionic liquids.
Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

NASA Astrophysics Data System (ADS)

He, Feng

The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single phase and heterogeneous diphasic mullite gels from same starting chemicals. Amorphous powders were obtained after optimized calcinations. Their different crystallization routes and sintering behavior were investigated and correlated with the different homogeneities of precursor gels. Structurally stable open, porous ceramics (up to 80% porosity) were produced from the single-phase gel derived powder, where gases exsolved during calcination caused foaming coincident with sintering. Translucent, dense glass ceramic was made from the calcined diphasic gel by hot-pressing.
Thickening compositions containing xanthomonas gum and hydroxyalkyl ether of guar gum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jordan, W.A.

1973-07-24

Natural and synthetic gums have been used as thickeners for foods, coatings, paints, dyes, explosive slurries, oil-well fluids, and many other applications. Thickening compositions are described which consist of xanthomonas gum and hydroxyalkyl ether of guar gum and are suitable for use in explosive slurries. Aqueous sols of xanthomonas gum are plastic in nature and exhibit higher gel strengths than sols of other gums. Aqueous sols of hydroxyalkyl ether of guar are almost Newtonian and exhibit little or no gel strength. Aqueous sols of the thickening compositions of the present invention are plastic in character. At certain concentrations of themore » thickening compositions in aqueous sols, the sols have higher gel strengths than can be obtained from xanthomonas gum alone. At certain concentrations, the aqueous sols containing the thickening compositions exhibit greater viscosity differentials than do sols containing xanthomonas gum alone. In addition, the aqueous sols exhibit a greater drop in viscosity as the thickening composition concentration is reduced than do aqueous sols of xanthomonas gum alone.(5 claims)« less
Chemical sensing of copper phthalocyanine sol-gel glass through organic vapors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ridhi, R.; Gawri, Isha; Abbas, Saeed J.

2015-05-15

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

NASA Astrophysics Data System (ADS)

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

2016-03-01

New approaches for β-cyclodextrin-containing silicas synthesis were demonstrated. Materials with hexagonally ordered mesoporous structure were prepared by postsynthesis grafting and by co-condensation methods. β-Cyclodextrin activated by a N, N'-carbonyldiimidazole was employed for postsynthesis treatment of 3-aminopropyl-modified MCM-41 support as well as for sol-gel synthesis with β-cyclodextrin-containing organosilane and tetraethyl orthosilicate participation in the presence of cetyltrimethylammonium bromide. The successful incorporation of cyclic oligosaccharide moieties in silica surface layer was verified by means of FT-IR spectroscopy and chemical analysis. Obtained β-cyclodextrin-containing materials were characterized by X-ray diffraction, transmission electron microscopy, and low-temperature adsorption-desorption of nitrogen. In spite of commensurable loading of β-cyclodextrin groups attained by both proposed approaches (up to 0.028 μmol · m-2), it was found that co-condensation procedure provides uniform distribution of β-cyclodextrin functionalities in silica framework, whereas postsynthesis grafting results in modification of external surface of silica surface. Adsorption of benzene from aqueous solutions onto the surface of β-cyclodextrin-containing materials prepared by co-condensation method was studied as the function of time and equilibrium concentration. Langmuir and Freundlich models were used to evaluate adsorption processes and parameters. Adsorption experiments showed that β-cyclodextrin-containing silicas could be promising for the trace amount removal of aromatics from water.
Optical sensors for application in intelligent food-packaging technology

NASA Astrophysics Data System (ADS)

McEvoy, Aisling K.; Von Bueltzingsloewen, Christoph; McDonagh, Colette M.; MacCraith, Brian D.; Klimant, Ingo; Wolfbeis, Otto S.

2003-03-01

Modified Atmosphere Packaged (MAP) food employs a protective gas mixture, which normally contains selected amounts of carbon dioxide (CO2) and oxygen (O2), in order to extend the shelf life of food. Conventional MAP analysis of package integrity involves destructive sampling of packages followed by carbon dioxide and oxygen detection. For quality control reasons, as well as to enhance food safety, the concept of optical on-pack sensors for monitoring the gas composition of the MAP package at different stages of the distribution process is very attractive. The objective of this work was to develop printable formulations of oxygen and carbon dioxide sensors for use in food packaging. Oxygen sensing is achieved by detecting the degree of quenching of a fluorescent ruthenium complex entrapped in a sol-gel matrix. In particular, a measurement technique based on the quenching of the fluorescence decay time, phase fluorometric detection, is employed. A scheme for detecting CO2 has been developed which is compatible with the oxygen detection scheme. It is fluorescence-based and uses the pH-sensitive 8-hydroxypyrene-1,3,6-trisulfonic acid (HPTS) indicator dye encapsulated in an organically modified silica (ORMOSIL) glass matrix. Dual Luminophore Referencing (DLR) has been employed as an internal referencing scheme, which provides many of the advantages of lifetime-based fluorometric methods. Oxygen cross-sensitivity was minimised by encapsulating the reference luminophore in dense sol-gel microspheres. The sensor performance compared well with standard methods for both oxygen and carbon dioxide detection. The results of preliminary on-pack print trials are presented and a preliminary design of an integrated dual gas optical read-out device is discussed.
Synthesis of a colloid solution of silica-coated gold nanoparticles for X-ray imaging applications

NASA Astrophysics Data System (ADS)

Kobayashi, Yoshio; Nagasu, Ryoko; Shibuya, Kyosuke; Nakagawa, Tomohiko; Kubota, Yohsuke; Gonda, Kohsuke; Ohuchi, Noriaki

2014-08-01

This work proposes a method for fabricating silica-coated gold (Au) nanoparticles, surface modified with poly(ethylene glycol) (PEG) (Au/SiO2/PEG), with a particle size of 54.8 nm. X-ray imaging of a mouse is performed with the colloid solution. A colloid solution of 17.9 nm Au nanoparticles was prepared by reducing Au ions (III) with sodium citrate in water at 80 °C. The method used for silica-coating the Au nanoparticles was composed of surface-modification of the Au nanoparticles with (3-aminopropyl)-trimethoxysilane (APMS) and a sol-gel process. The sol-gel process was performed in the presence of the surface-modified Au nanoparticles using tetraethylorthosilicate, APMS, water, and sodium hydroxide, in which the formation of silica shells and the introduction of amino groups to the silica-coated particles took place simultaneously (Au/SiO2-NH2). Surface modification of the Au/SiO2-NH2 particles with PEG, or PEGylation of the particle surface, was performed by adding PEG with a functional group that reacted with an amino group in the Au/SiO2-NH2 particle colloid solution. A computed tomography (CT) value of the aqueous colloid solution of Au/SiO2/PEG particles with an actual Au concentration of 0.112 M was as high as 922 ± 12 Hounsfield units, which was higher than that of a commercial X-ray contrast agent with the same iodine concentration. Injecting the aqueous colloid solution of Au/SiO2/PEG particles into a mouse increased the light contrast of tissues. A CT value of the heart rose immediately after the injection, and this rise was confirmed for up to 6 h.
[Study on surface modification and biocompatibility of NiTi alloy intravascular stents].

PubMed

Shen, Yang; Wang, Gui-xue; Quan, Xue-jun; Yu, Qing-song

2006-01-01

This paper introduces the surface modification of NiTi alloy intravascular stents for roughness by chemical erosion and plasma deposition technology. The stent which had been granulated with chemical erosion was treated with TiO2 film prepared with Gel-sol. The study on the biocompatibility of the modified stent by the above two ways shows that the modified stent is rougher, and its anticoagulation and hydrophilicity are improved. However, the capability of erosion resistance is not enhanced significantly.
Grafting the sol-gel based sorbents by diazonium salts: a novel approach toward unbreakable capillary microextraction.

PubMed

Bagheri, Habib; Bayat, Parisa; Piri-Moghadam, Hamed

2013-11-29

The present work deals with a novel approach for grafting a sol-gel based sorbent, using diazonium salts for preparation of an unbreakable capillary microextraction (CME) device in on-line combination with high performance liquid chromatography (HPLC). The use of diazonium salts modifier allowed all types of metallic and non-metallic substrates to be used without any limitation. Substrates including copper, brass, stainless steel and polytetrafluoroethylene (PTFE) were chosen to be functionalized by chemical or electrochemical reduction of 4-amino phenyl acetic acid. Then, 3-(trimethoxysilyl)propylamine (3TMSPA) was selected as the precursor and the only reagent for preparation of the desired surface chemical bonded sorbent. The presence of chemical bond between substrate, diazonium salts and 3TMSPA is more probably responsible for thermal and solvent stability and long lifetime of the prepared sorbent. Characterization of the aryl group formation on the various substrates along with the prepared sorbents was thoroughly investigated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and thermogravimetry analysis (TGA). Typically, one of the prepared sorbents, deposited on the inner surface of the copper tube, was selected for assessing the developed method. The CME device was used for on-line extraction of atrazine, ametryn and terbutryn, as model compounds, from the aquatic media. After extraction, the HPLC mobile phase was used for on-line desorption and elution of the extracted analytes from the CME loop, containing the grafted sol-gel based sorbent, through the HPLC column. Figures of merit of the developed method were also obtained in which the linearity for the analytes was in the range of 30-1000μgL(-1). The value of LOD (S/N=3) for all analytes was 10μgL(-1) and the RSD% values (n=5) were all below 9.4% at the 500μgL(-1) level. Applicability of the developed method was examined by analyzing some real water samples in which the relative recovery percentage ranged from 75 to 95%. Copyright © 2013 Elsevier B.V. All rights reserved.
Development of novel sol-gel coatings by chemically bonded ionic liquids for stir bar sorptive extraction--application for the determination of NSAIDS in real samples.

PubMed

Fan, Wenying; Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

2014-11-01

In this work, a novel ionic liquid (IL) chemically bonded sol-gel coating was prepared for stir bar sorptive extraction (SBSE) of nonsteroidal anti-inflammatory drugs (NSAIDs) followed by high-performance liquid chromatography-ultraviolet detection (HPLC-UV). By using γ-(methacryloxypropyl)trimethoxysilane (KH-570) as a bridging agent, 1-allylimidazolium tetrafluoroborate ([AIM][BF4]) was chemically bonded onto the bare stir bar, and the prepared IL-bonded sol-gel stir bar coating showed higher extraction efficiency and better adsorption/desorption kinetics for target NSAIDs over other polydimethylsiloxane (PDMS)-based or monolithic stir bar coatings. The mechanical strength and durability (chemical/thermal stability) of the prepared IL-bonded sol-gel coating were excellent. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent, and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limits of detection (LODs) of the proposed method for three NSAIDs were in the range of 0.23-0.31 μg L(-1), and the enrichment factors (EFs) were in the range of 51.6-56.3 (theoretical enrichment factor was 100). The reproducibility was also investigated at concentrations of 5, 20, and 100 μg L(-1), and the relative standard deviations (RSDs) were found to be less than 9.5, 7.5, and 7.6 %, respectively. The proposed method was successfully applied for the determination of NSAIDs in environmental water, urine, and milk samples.
Chitosan-doped-hybrid/TiO2 nanocomposite based sol-gel coating for the corrosion resistance of aluminum metal in 3.5% NaCl medium.

PubMed

J, Balaji; M G, Sethuraman

2017-11-01

The study outlines the role of chitosan, a biopolymer on corrosion behavior of Hy/nano-TiO 2 based sol-gel coating over aluminum metal. In this study organic-inorganic hybrid sols were synthesized through hydrolysis and condensation of 3-glycidoxypropyltrimethoxy silane (GPTMS), tetraethoxysilane (TEOS) and titanium (IV) isopropoxide (TIP) in acidic solution. Chitosan was doped into sol-gel matrix and self-assembled over aluminum substrate. The resultant chitosan-doped-Hy/nano-TiO 2 sol-gel coating was characterized by Fourier Transform Infrared (FT-IR) spectra, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and Energy-Dispersive X-ray Spectroscopy (EDX) analyses. The as-tailored aluminum substrate was evaluated for corrosion resistance in neutral medium. The protection ability of these coatings was evaluated by electrochemical impedance studies (EIS) and potentiodynamic polarization (PP) measurements in 3.5% NaCl medium. The EIS and PP results showed that chitosan-doped- Hy/nano-TiO 2 sol-gel coating exhibited better protection from corrosion than the undoped Hy/TiO 2 nanocomposite coating. Copyright © 2017 Elsevier B.V. All rights reserved.
Fabrication of mesoporous silica nanoparticles by sol gel method followed various hydrothermal temperature

NASA Astrophysics Data System (ADS)

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.
Surface modification of wood by alkoxysilane sol-gel deposition to create anti-mold and anti-fungal characteristics

Treesearch

Mandla A. Tshabalala; Vina Yang; Ryan Libert

2009-01-01

Hybrid inorganic/organic thin films deposited on wood substrates have been shown to lower the rate of moisture sorption of the wood. Deposition of such thin films can be accomplished by solâgel deposition or by plasma-enhanced chemical vapor deposition. This paper describes in situ solâgel deposition of hybrid inorganic/organic thin films on wood substrates using...
Adjustable rheology of fumed silica dispersion in urethane prepolymers: Composition-dependent sol and gel behaviors and energy-mediated shear responses

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 shearmore » 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.« less
Photo-Definable Self Assembled Maerials

DOEpatents

DOSHI, DHAVAL; [et al

2004-10-26

The present invention provides a mesoporous material comprising at least one region of mesoporous material patterned at a lithographic scale. The present invention also provides a a method for forming a patterned mesoporous material comprising: coating a sol on a substrate to form a film, the sol comprising: a templating molecule, a photoactivator generator, a material capable of being sol-gel processed, water, and a solvent; and exposing the film to light to form a patterned mesoporous material.
Synthesis of Silver-Strontium Titanate Hybrid Nanoparticles by Sol-Gel-Hydrothermal Method.

PubMed

Ueno, Shintaro; Nakashima, Kouichi; Sakamoto, Yasunao; Wada, Satoshi

2015-03-24

Silver (Ag) nanoparticle-loaded strontium titanate (SrTiO₃) nanoparticles were attempted to be synthesized by a sol-gel-hydrothermal method. We prepared the titanium oxide precursor gels incorporated with Ag⁺ and Sr 2+ ions with various molar ratios, and they were successfully converted into the Ag-SrTiO₃ hybrid nanoparticles by the hydrothermal treatment at 230 °C in strontium hydroxide aqueous solutions. The morphology of the SrTiO₃ nanoparticles is dendritic in the presence and absence of Ag⁺ ions. The precursor gels, which act as the high reactive precursor, give rise to high nucleation and growth rates under the hydrothermal conditions, and the resultant diffusion-limited aggregation phenomena facilitate the dendritic growth of SrTiO₃. From the field-emission transmission electron microscope observation of these Ag-SrTiO₃ hybrid nanoparticles, the Ag nanoparticles with a size of a few tens of nanometers are distributed without severe agglomeration, owing to the competitive formation reactions of Ag and SrTiO₃.
Synthesis and characterization of nanoporous silica aerogel beads using cheap industrial grade sodium silacte precursor

NASA Astrophysics Data System (ADS)

Khan, Tasneem M. A.; Khan, Asiya; Sarawade, Pradip B.

2018-05-01

We report a method to synthesize low-density transparent mesoporous silica aerogel beads by ambient pressure drying (APD). The beads were prepared by acid-base sol-gel polymerization of sodium silicate in via the ball dropping method (BDM). To minimize shrinkage during drying, wet silica beads were initially prepared; their surfaces were then modified using trimethylchlorosilane (TMCS) via simultaneous solvent exchange and surface modification. The specific surface area and cumulative pore volume of the silica aerogel beads increased with an increase in the %V of TMCS. Silica aerogel beads with low packing bed density, high surface area, and large cumulative pore volume was obtained when TMCS was used. Properties of the final product were examined by BET, and TG-DT analyses. The hydrophobic silica aerogel beads were thermally stable up to 350°C. We discuss our results and compare our findings for modified versus unmodified silica beads.
Ionogel Electrolytes through Sol-Gel Processing

NASA Astrophysics Data System (ADS)

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 morphologies. The IL identity is shown to have an impact on the apparent strength of the acid catalyst, leading to significant shifts in gelation time. Delayed casting is proven to be an optimal technique for avoiding pore blockage when combining ionogels with high surface area electrodes for supercapacitor applications. Finally, a simple recycling process is proposed, establishing that ILs can be easily reclaimed from silica-supported ionogels and reused, thereby validating the reputation of ILs as "green" materials.

Study of Wrinkle Resistant, Breathable, Anti-Uv Nanocoated Woven Polyester Fabric

NASA Astrophysics Data System (ADS)

Memon, Hafeezullah; Yasin, Sohail; Khoso, Nazakat Ali; Memon, Samiulah

2016-02-01

The multifunctional textiles are interesting areas to be researched on. In this paper, the effect of the fiber nanocoating on the wrinkle recovery, air permeability and anti-Ultraviolet (UV) property of different woven fabrics using sol-gel method has been studied. The sol-gel method has various advantages over other methods. Along with these properties, no change in visual appearance has also been discussed in this paper. The dispersion of nanoparticles of titanium was obtained into silica sol. The characterization of nanocoating was done using Field emission scanning electron micrograph (FESEM) and Fourier transform infrared spectroscopy (FTIR) studies. The fabric wrinkle recovery properties, air permeability and anti-UV performance were analyzed using three different immersion timings into the nanosol. The results revealed that both wrinkle recovery properties and anti-UV performance have increased with respect to immersing time of the nanocoating although a slight decrease in air permeability and whiteness index of the fabric was also observed.
Influence of Operating Parameters on Surface Properties of RF Glow Discharge Oxygen Plasma Treated TiO2/PET Film for Biomedical Application

EPA Science Inventory

Thin transparent titania (TiO2) films were coated on the surface of flexible poly (ethylene terephthalate) (PET) surface using standard sol gel techniques. The TiO2/PET thin film surfaces were further modified by exposing the films to a RF glow discharge oxygen plasma. The exposu...
An improved soft-chemistry approach to the preparation of spinel powders

NASA Astrophysics Data System (ADS)

Cook, Ronald

2007-04-01

Spinel powders for the production of transparent polycrystalline ceramic windows have been produced using a number of traditional ceramic and sol-gel methods. We have demonstrated that magnesium aluminate spinel powders produced from the reaction of organo-magnesium compounds with surface modified boehmite precursors can be used to produce high quality transparent spinel parts. In previous work, the spinel powders were prepared by the reaction of surface-modified boehmite nanoparticles with magnesium acetylacetonate. While the magnesium acetylacetonate can produce small quantities of high quality spinel powders, it use for large scale production of spinel powders is problematic. Through a thermodynamic analysis we have identified a new high-purity, low-cost, low-toxicity organomagnesium compound that reacts the with surface modified boehmite nanoparticles to produce a spinel precursor. The magnesium doped precursor readily transforms into pure phase spinel at temperature between 900°C and 1200°C.
Optical detection of parasitic protozoa in sol-gel matrices

NASA Astrophysics Data System (ADS)

Livage, Jacques; Barreau, J. Y.; Da Costa, J. M.; Desportes, I.

1994-10-01

Whole cell parasitic protozoa have been entrapped within sol-gel porous silica matrices. Stationary phase promastigote cells of Leishmania donovani infantum are mixed with a silica sol before gelation occurs. They remain trapped within the growing oxide network and their cellular organization appears to be well preserved. Moreover protozoa retain their antigenic properties in the porous gel. They are still able to detect parasite specific antibodies in serum samples from infected patients via an enzyme linked immunosorbent assay (ELISA). Antigen- antibody associations occurring in the gel are optically detected via the reactions of a peroxidase conjugate with ortho-phenylenediamine leading to the formation of a yellow coloration. A clear-cut difference in optical density is measured between positive and negative sera. Such an entrapment of antigenic species into porous sol-gel matrices avoids the main problems due to non specific binding and could be advantageously used in diagnostic kits.
Electrochemical determination of L-phenylalanine at polyaniline modified carbon electrode based on β-cyclodextrin incorporated carbon nanotube composite material and imprinted sol-gel film.

PubMed

Hu, Yu-fang; Zhang, Zhao-hui; Zhang, Hua-bin; Luo, Li-juan; Yao, Shou-zhuo

2011-04-15

A sensitive and selective electrochemical sensor based on a polyaniline modified carbon electrode for the determination of L-phenylalanine has been proposed by utilizing β-cyclodextrin (β-CD) incorporated multi-walled carbon nanotube (MWNT) and imprinted sol-gel film. The electrochemical behavior of the sensor towards L-phenylalanine was investigated by cyclic voltammetry (CV), differential pulse voltammetry (DPV), and amperometric i-t curve. The surface morphologies of layer-by-layer assembly electrodes were displayed by scanning electron microscope (SEM). The response mechanism of the imprinted sensor for L-phenylalanine was based on the inclusion interaction of β-CD and molecular recognition capacity of the imprinted film for L-phenylalanine. A linear calibration plot was obtained covering the concentration range from 5.0 × 10(-7) to 1.0 × 10(-4) mol L(-1) with a detection limit of 1.0 × 10(-9) mol L(-1). With excellent sensitivity, selectivity, stability, reproducibility and recovery, the electrochemical imprinted sensor was used to detect L-phenylalanine in blood plasma samples successfully. Copyright © 2011 Elsevier B.V. All rights reserved.
Correlation of the oxidation state of cerium in sol-gel glasses as a function of thermal treatment via optical spectroscopy and XANES studies.

PubMed

Assefa, Zerihun; Haire, R G; Caulder, D L; Shuh, D K

2004-07-01

Sol-gel glass matrices containing lanthanides have numerous technological applications and their formation involves several chemical facets. In the case of cerium, its ability to exist in two different oxidation states or in mixed valence state provides additional complexities for the sol-gel process. The oxidation state of cerium present during different facets of preparation of sol-gel glasses, and also as a function of the starting oxidation state of cerium added, were studied both by optical spectroscopy and X-ray absorption near-edge structures (XANES). The findings acquired by each approach were compared. The primary focus was on the redox chemistries associated with sample preparation, gelation, and thermal treatment. When Ce3+ is introduced into the starting sols, the trivalent state normally prevails in the wet and room temperature-dried gels. Heating in air at >100 degrees C can generate a light yellow coloration with partial oxidation to the tetravalent state. Above 200 degrees C and up to approximately 1000 degrees C, cerium is oxidized to its tetravalent state. In contrast, when tetravalent cerium is introduced into the sol, both the wet and room temperature-dried gels lose the yellow-brown color of the initial ceric ammonium nitrate solution. When the sol-gel is heated to 110 degrees C it turns yellowish as the cerium tends to be re-oxidized. The yellow color is believed to represent the effect of oxidation and oligomerization of the cerium-silanol units in the matrix. The luminescence properties are also affected by these changes, the details of which are reported herein.
Ultra-high-stability, pH-resistant sol-gel titania poly(tetrahydrofuran) coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

PubMed

Segro, Scott S; Cabezas, Yaniel; Malik, Abdul

2009-05-15

A sol-gel titania poly(tetrahydrofuran) (poly-THF) coating was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). Poly-THF was covalently bonded to the sol-gel titania network which, in turn, became chemically anchored to the inner surface of a 0.25mm I.D. fused silica capillary. For sample preconcentration, a 38-cm segment of the sol-gel titania poly-THF coated capillary was installed on an HPLC injection port as a sampling loop. Aqueous samples containing a variety of analytes were passed through the capillary and, during this process, the analytes were extracted by the sol-gel titania poly-THF coating on the inner surface of the capillary. Using isocratic and gradient elution with acetonitrile/water mobile phases, the extracted analytes were desorbed into the on-line coupled HPLC column for separation and UV detection. The sol-gel titania poly-THF coating was especially efficient in extracting polar analytes, such as underivatized phenols, alcohols, amines, and aromatic carboxylic acids. In addition, this coating was capable of extracting moderately polar and nonpolar analytes, such as ketones and polycyclic aromatic hydrocarbons. The sol-gel titania poly-THF coated capillary was also able to extract polypeptides at pH values near their respective isoelectric points. Extraction of these compounds can be important for environmental and biomedical applications. The observed extraction behavior can be attributed to the polar and nonpolar moieties in the poly-THF structure. This coating was found to be stable under extremely low and high pH conditions-even after 18h of exposure to 1M HCl (pH approximately 0.0) and 1M NaOH (pH approximately 14.0).
Percutaneous external fixator pins with bactericidal micron-thin sol-gel films for the prevention of pin tract infection.

PubMed

Qu, Haibo; Knabe, Christine; Radin, Shula; Garino, Jonathan; Ducheyne, Paul

2015-09-01

Risk of infection is considerable in open fractures, especially when fracture fixation devices are used to stabilize the fractured bones. Overall deep infection rates of 16.2% have been reported. The infection rate is even greater, up to 32.2%, with external fixation of femoral fractures. The use of percutaneous implants for certain clinical applications, such as percutaneous implants for external fracture fixation, still represents a challenge today. Currently, bone infections are very difficult to treat. Very potent antibiotics are needed, which creates the risk of irreversible damage to other organs, when the antibiotics are administered systemically. As such, controlled, local release is being pursued, but no such treatments are in clinical use. Herein, the use of bactericidal micron-thin sol-gel films on metallic fracture fixation pins is reported. The data demonstrates that triclosan (2,4,4'-trichloro-2'-hydroxydiphenylether), an antimicrobial agent, can be successfully incorporated into micron-thin sol-gel films deposited on percutaneous pins. The sol-gel films continuously release triclosan in vitro for durations exceeding 8 weeks (longest measured time point). The bactericidal effect of the micron-thin sol-gel films follows from both in vitro and in vivo studies. Inserting percutaneous pins in distal rabbit tibiae, there were no signs of infection around implants coated with a micron-thin sol-gel/triclosan film. Healing had progressed normally, bone tissue growth was normal and there was no epithelial downgrowth. This result was in contrast with the results in rabbits that received control, uncoated percutaneous pins, in which abundant signs of infection and epithelial downgrowth were observed. Thus, well-adherent, micron-thin sol-gel films laden with a bactericidal molecule successfully prevented pin tract infection. Copyright © 2015 Elsevier Ltd. All rights reserved.
Synthesis and Characterization of BaFe12O19 Thin Films Using Suspension of Nano Powders

NASA Astrophysics Data System (ADS)

Salemizadeh, Saman; Seyyed Ebrahimi, S. A.

BaM thin films have been synthesized by dispersing the dried gel nano powders prepared by Sol-Gel method. The solution was made by dissolving iron nitrate Fe(NO3).9H2O, barium nitrate Ba(NO3)2 and citric acid in deyonized water and methanol. This sol was slowly evaporated until a dried gel was formed. This dried gel was then added to ethylene glycol. The final solution was vigorously shaken and mixed in ultrasonic cleaner for 30 min to disperse particles sufficiently. Then the prepared solution spin coated on Si(110) substrate. The obtained thin films were dried at 120 °C and then calcined at 900 °C for 1 h. The films were characterized using X-ray diffraction (XRD) and vibrating sample magnetometer (VSM).
Anomalously large bend elastic constant and faster electro-optic response in anisotropic gels formed by a dipeptide

NASA Astrophysics Data System (ADS)

Bhargavi, R.; Nair, Geetha G.; Prasad, S. Krishna; Prabhu, Rashmi; Yelamaggad, C. V.

2011-04-01

We report rheological, static, and dynamic Freedericksz transformation measurements on an anisotropic thermoreversible gel formed by gelation of a nematic liquid crystal (NLC) with a monodisperse dipeptide. The storage and loss modulii obtained from a low strain oscillatory shear experiment display that the material forms a weak anisotropic gel, and undergoes a sharp thermal transition to an anisotropic sol state. Freedericksz transformation studies employing an electric field for the reorientation of the molecules present a surprising result: the gel possesses a very large Frank bend elastic constant value, which is orders of magnitude higher than that for the high temperature sol state as well as that for the neat NLC used. On the other hand, the splay elastic constant shows relatively a small increase. Further, these elastic constants show systematic but nonlinear variation with the concentration of the gelator. Attractive features of the electro-optic switching when the sol transforms to the gel state are the vanishing of the undesirable backflow effect, and nearly an order of magnitude decrease in the switching speed. In both the gel and sol states the extracted rotational viscosities are comparable to the values of the neat NLC at corresponding temperatures. In contrast, the bulk dynamic viscosity is more than three orders of magnitude higher in the gel. The studies also demonstrate that the anisotropic gel to anisotropic sol transition seen in this weak gel can be tracked by simply monitoring the static or the dynamic Freedericksz transformation.
Use of CdSe/ZnS luminescent quantum dots incorporated within sol-gel matrix for urea detection.

PubMed

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

PubMed

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

PubMed

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

NASA Astrophysics Data System (ADS)

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

2011-03-01

Sol-gel routes are often investigated and adapted to prepare, by suitable chemical modifications, submicronic powders and derived materials with controlled morphology, which cannot be obtained by conventional solid state chemistry paths. Wet chemistry methods provide attractive alternative routes because mixing of species occurs at the atomic scale. In this paper, ultrafine powders were prepared by a novel synthesis method based on the sol-gel process and were dispersed into suspensions before processing. This paper presents new developments for the preparation of functional materials like yttria-stabilized-zirconia (YSZ, 8% Y2O3) used as electrolyte for solid oxide fuel cells. YSZ thick films were coated onto porous Ni-YSZ substrates using a suspension with an optimized formulation deposited by either a dip-coating or a spin-coating process. The suspension composition is based on YSZ particles encapsulated by a zirconium alkoxide which was added with an alkoxide derived colloidal sol. The in situ growth of these colloids increases significantly the layer density after an appropriated heat treatment. The derived films were continuous, homogeneous and around 20 μm thick. The possible up-scaling of this process has been also considered and the suitable processing parameters were defined in order to obtain, at an industrial scale, homogeneous, crack-free, thick and adherent films after heat treatment at 1400 °C.
Seed-mediated photodeposition route to Ag-decorated SiO2@TiO2 microspheres with ideal core-shell structure and enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Ma, Jianqi; Guo, Xiaohua; Ge, Hongguang; Tian, Guanghui; Zhang, Qiang

2018-03-01

Ag-decorated SiO2@TiO2 microspheres (SiO2@TiO2-Ag) with ideal core-shell structure and enhanced photocatalytic activity were successfully fabricated by combining both coating anatase TiO2 on the surface of SiO2 spheres and subsequent depositing face-centered cubic Ag nanoparticles (NPs) on the coated TiO2 surface via novel sol-gel method and Ag-seed-mediated photodeposition (PD) route, respectively. The morphology, structure, composition and optical properties of the resulting composites were characterized in detail. The results reveal that the monodisperse SiO2 spheres of ∼260 nm were covered uniformly and perfectly by the TiO2 nanoparticle coating layer with the thickness of ca. 55 nm by the novel sol-gel method. Further, homogeneously and highly dispersed Ag NPs with an average size of 8 ± 1.5 nm were strongly anchored onto the TiO2 surface in SiO2@TiO2 core-shell spheres by the modified PD process (Ag-seed-mediated PD route), whereas polydispersed Ag aggregates and detached Ag NPs were irregularly deposited over the TiO2 surface in previous works, which is the inherent problem and has not been effectively solved for depositing noble metal NPs such as Au, Ag, Pt, Pd on TiO2 surface by conventional PD method. The formation mechanism of small and uniformly dispersed Ag NPs with narrow size distribution via the modified PD method is tentatively explained by both nucleation kinetics and growth kinetics. The key reason is that the pre-deposited seeds firmly tethered on SiO2@TiO2 spheres served as nucleation sites and anchoring points for the further nucleation and subsequent growth of Ag via photoreduction of Ag+.
Structural, optical, and electrical properties of Ni-doped ZnO nanorod arrays prepared via sonicated sol-gel immersion method

NASA Astrophysics Data System (ADS)

Ismail, A. S.; Mamat, M. H.; Malek, M. F.; Saidi, S. A.; Yusoff, M. M.; Mohamed, R.; Sin, N. D. Md; Suriani, A. B.; Rusop, M.

2018-05-01

Nickel (Ni)-doped zinc oxide (ZnO) nanorod array films were synthesised using sonicated sol-gel immersion method. The FESEM images showed that the Ni-doped ZnO nanorod arrays possess hexagonal shape with average diameter about 120 nm and thickness about 1.10 µm. The Ni-doped ZnO nanorod arrays possess better transmittance properties with 3.27 eV of optical band gap energy and 40 meV of urbach energy. The current-voltage (I-V) measurement indicated that the conductivity of ZnO film slightly improved with Ni-doping. The doped film displayed good humidity sensing performance with sensitivity of 1.21.
Nano sized La2Co2O6 double perovskite synthesized by sol gel method

NASA Astrophysics Data System (ADS)

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.
Structure and magnetic properties of Fe-doped ZnO prepared by the sol-gel method.

PubMed

Liu, Huilian; Yang, Jinghai; Zhang, Yongjun; Yang, Lili; Wei, Maobin; Ding, Xue

2009-04-08

Zn(0.97)Fe(0.03)O nanoparticles were synthesized by the sol-gel method. X-ray diffraction (XRD) and transmission electron microscope (TEM) analysis revealed that the samples had pure ZnO wurtzite structure and Fe ions were well incorporated into the ZnO crystal lattice. X-ray photoelectron spectroscopy (XPS) showed that both Fe(2+) and Fe(3+) existed in Zn(0.97)Fe(0.03)O. The result of x-ray absorption near-edge structure (XANES) further testified that Fe ions took the place of Zn sites in our samples. Magnetic measurements indicated that Zn(0.97)Fe(0.03)O was ferromagnetic at room temperature.
Synthesis of galium nitride thin films using sol-gel dip coating method

NASA Astrophysics Data System (ADS)

Hamid, Maizatul Akmam Ab; Ng, Sha Shiong

2017-12-01

In this research, gallium nitride (GaN) thin film were grown on silicon (Si) substrate by a low-cost sol-gel dip coating deposition method. The GaN precursor solution was prepared using gallium (III) nitrate hydrate powder, ethanol and diethanolamine as a starting material, solvent and surfactant respectively. The structural, morphological and optical characteristics of the deposited GaN thin film were investigated. Field-emission scanning electron microscopy observations showed that crack free and dense grains GaN thin films were formed. Energy dispersive X-ray analysis confirmed that the oxygen content in the deposited films was low. X-ray diffraction results revealed that deposited GaN thin films have hexagonal wurtzite structure.
Synthesis of Bi0.9Nd0.1FeO3 multiferroic nanoceramic by sol-gel method and its structural, surface morphology and dielectric analysis

NASA Astrophysics Data System (ADS)

Das, S.; Bera, K. P.; Nath, T. K.

2017-05-01

Synthesis of Nd-doped BFO multiferroic nanoceramic by the conventional sol-gel method has been carried out. HRXRD and FESEM have been used for the structural analysis to confirm the triclinic structure and to obtain the surface morphology showing agglomeration and to find out the size of the nanoparticles. A high precision LCR meter has been used to record the dielectric constants at various temperatures. Several anomalies are observed whose physical explanations have been given. Space charge polarization effect and magnetoelectric coupling have been confirmed in the synthesized Bi0.9Nd0.1FeO3 nanoceramic sample.

Synthesis and characterization of NiO nanopowder by sol-gel process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ningsih, Sherly Kasuma Warda

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 weremore » 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.« less
Solid-phase microextraction of methadone in urine samples by electrochemically co-deposited sol-gel/Cu nanocomposite fiber.

PubMed

Mohammadiazar, Sirwan; Hasanli, Fateme; Maham, Mehdi; Payami Samarin, Somayeh

2017-08-01

Electrochemically co-deposited sol-gel/Cu nanocomposites have been introduced as a novel, simple and single-step technique for preparation of solid-phase microextraction (SPME) coating to extract methadone (MDN) (a synthetic opioid) in urine samples. The porous surface structure of the sol-gel/Cu nanocomposite coating was revealed by scanning electron microscopy. Direct immersion SPME followed by HPLC-UV determination was employed. The factors influencing the SPME procedure, such as the salt content, desorption solvent type, pH and equilibration time, were optimized. The best conditions were obtained with no salt content, acetonitrile as desorption solvent type, pH 9 and 10 min equilibration time. The calibration graphs for urine samples showed good linearity. The detection limit was about 0.2 ng mL -1 . Also, the novel method for preparation of nanocomposite fiber was compared with previously reported techniques for MDN determination. The results show that the novel nanocomposite fiber has relatively high extraction efficiency. Copyright © 2016 John Wiley & Sons, Ltd.
Structure and intense UV up-conversion emissions in RE3+-doped sol-gel glass-ceramics containing KYF4 nanocrystals

NASA Astrophysics Data System (ADS)

Yanes, A. C.; Santana-Alonso, A.; Méndez-Ramos, J.; del-Castillo, J.

2013-12-01

Transparent nano-glass-ceramics containing KYF4 nanocrystals were successfully obtained by the sol-gel method, doped with Eu3+ and co-doped with Yb3+ and Tm3+ ions. Precipitation of cubic KYF4 nanocrystals was confirmed by X-ray diffraction and high-resolution transmission electron microscope images. Excitation and emission spectra let us to discern between ions into KYF4 nanocrystals and those remaining in a glassy environment, supplemented with time-resolved photoluminescence decays, that also clearly reveal differences between local environments. Unusual high-energy up-conversion emissions in the UV range were obtained in Yb3+-Tm3+ co-doped samples, and involved mechanisms were discussed. The intensity of these high-energy emissions was analyzed as a function of Yb3+ concentration, heat treatment temperature of precursor sol-gel glasses and pump power, determining the optimum values for potential optical applications as highly efficient UV up-conversion materials in UV solid-state lasers.
Holographic sol-gel monoliths: optical properties and application for humidity sensing

NASA Astrophysics Data System (ADS)

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

PubMed

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

2016-03-02

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

PubMed

Liu, Wenmin; Wang, Hanwen; Guan, Yafeng

2004-08-06

A sol-gel coating method for the preparation of extractive phase on bars used in sorptive microextraction is described. The extraction phase of poly(dimethylsiloxane) is partially crosslinked with the sol-gel network, and the most part is physically incorporated in the network. Three aging steps at different temperatures are applied to complete the crosslinking process. Thirty-micrometer-thick coating layer is obtained by one coating process. The improved coating shows good thermal stability up to 300 degrees C. Spiked aqueous samples containing n-alkanes, polycyclic aromatic hydrocarbons and organophosphorus pesticides were analyzed by using the sorptive bars and GC. The results demonstrate that it is suitable for both aploar and polar analytes. The detection limit for chrysene is 7.44 ng/L, 0.74 ng/L for C19 and 0.9 ng/L for phorate. The extraction equilibration can be reached in less than 15 min by supersonic extraction with the bars of 30 microm coating layer.
Investigation of phase evolution of CaCu3Ti4O12 (CCTO) by in situ synchrotron high-temperature powder diffraction

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

2014-03-01

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu3Ti4O12 (CCTO) precursors prepared via solid-state and sol-gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol-gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol-gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study.
Enhance the pyroelectricity of polyvinylidene fluoride by graphene-oxide doping.

PubMed

Hu, Yuh-Chung; Hsu, Wei-Li; Wang, Yi-Ta; Ho, Cheng-Tao; Chang, Pei-Zen

2014-04-16

The high quality properties and benefits of graphene-oxide have generated an active area of research where many investigations have shown potential applications in various technological fields. This paper proposes a methodology for enhancing the pyro-electricity of PVDF by graphene-oxide doping. The PVDF film with graphene-oxide is prepared by the sol-gel method. Firstly, PVDF and graphene-oxide powders are dispersed into dimethylformamide as solvent to form a sol solution. Secondly, the sol solution is deposited on a flexible ITO/PET substrate by spin-coating. Thirdly, the particles in the sol solution are polymerized through baking off the solvent to produce a gel in a state of a continuous network of PVDF and graphene-oxide. The final annealing process pyrolyzes the gel and form a β-phase PVDF film with graphene-oxide doping. A complete study on the process of the graphene oxide doping of PVDF is accomplished. Some key points about the process are addressed based on experiments. The solutions to some key issues are found in this work, such as the porosity of film, the annealing temperature limitation by the use of flexible PET substrate, and the concentrations of PVDF and graphene-oxide.
Effect of Synthesis Method of La1 - x Sr x MnO3 Manganite Nanoparticles on Their Properties

NASA Astrophysics Data System (ADS)

Shlapa, Yulia; Solopan, Sergii; Belous, Anatolii; Tovstolytkin, Alexandr

2018-01-01

Nanoparticles of lanthanum-strontium manganite were synthesized via different methods, namely, sol-gel method, precipitation from non-aqueous solution, and precipitation from reversal microemulsions. It was shown that the use of organic compounds and non-aqueous media allowed significantly decreasing of the crystallization temperature of nanoparticles, and the single-phased crystalline product was formed in one stage. Morphology and properties of nanoparticles depended on the method and conditions of the synthesis. The heating efficiency directly depended on the change in the magnetic parameters of nanoparticles, especially on the magnetization. Performed studies showed that each of these methods of synthesis can be used to obtain weakly agglomerated manganite nanoparticles; however, particles synthesized via sol-gel method are more promising for use as hyperthermia inducers. PACS: 61.46.Df 75.75.Cd 81.20. Fw
Antibacterial modification of an injectable, biodegradable, non-cytotoxic block copolymer-based physical gel with body temperature-stimulated sol-gel transition and controlled drug release.

PubMed

Wang, Xiaowen; Hu, Huawen; Wang, Wenyi; Lee, Ka I; Gao, Chang; He, Liang; Wang, Yuanfeng; Lai, Chuilin; Fei, Bin; Xin, John H

2016-07-01

Biomaterials are being extensively used in various biomedical fields; however, they are readily infected with microorganisms, thus posing a serious threat to the public health care. We herein presented a facile route to the antibacterial modification of an important A-B-A type biomaterial using poly (ethylene glycol) methyl ether (mPEG)- poly(ε-caprolactone) (PCL)-mPEG as a typical model. Inexpensive, commercial bis(2-hydroxyethyl) methylammonium chloride (DMA) was adopted as an antibacterial unit. The effective synthesis of the antibacterial copolymer mPEG-PCL-∼∼∼-PCL-mPEG (where ∼∼∼ denotes the segment with DMA units) was well confirmed by FTIR and (1)H NMR spectra. At an appropriate modification extent, the DMA unit could render the copolymer mPEG-PCL-∼∼∼-PCL-mPEG highly antibacterial, but did not largely alter its fascinating intrinsic properties including the thermosensitivity (e.g., the body temperature-induced sol-gel transition), non-cytotoxicity, and controlled drug release. A detailed study on the sol-gel-sol transition behavior of different copolymers showed that an appropriate extent of modification with DMA retained a sol-gel-sol transition, despite the fact that a too high extent caused a loss of sol-gel-sol transition. The hydrophilic and hydrophobic balance between mPEG and PCL was most likely broken upon a high extent of quaternization due to a large disturbance effect of DMA units at a large quantity (as evidenced by the heavily depressed PCL segment crystallinity), and thus the micelle aggregation mechanism for the gel formation could not work anymore, along with the loss of the thermosensitivity. The work presented here is highly expected to be generalized for synthesis of various block copolymers with immunity to microorganisms. Light may also be shed on understanding the phase transition behavior of various multiblock copolymers. Copyright © 2016 Elsevier B.V. All rights reserved.
Optimizing Metalloporphyrin-Catalyzed Reduction Reactions for In Situ Remediation of DOE Contaminants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schlautman, Mark A.

2013-07-14

Past activities have resulted in a legacy of contaminated soil and groundwater at Department of Energy facilities nationwide. Uranium and chromium are among the most frequently encountered and highest-priority metal and radionuclide contaminants at DOE installations. Abiotic chemical reduction of uranium and chromium at contaminated DOE sites can be beneficial because the reduced metal species are less soluble in water, less mobile in the environment, and less toxic to humans and ecosystems. Although direct biological reduction has been reported for U(VI) and Cr(VI) in laboratory studies and at some field sites, the reactions can sometimes be slow or even inhibitedmore » due to unfavorable environmental conditions. One promising approach for the in-situ remediation of DOE contaminants is to develop electron shuttle catalysts that can be delivered precisely to the specific subsurface locations where contaminants reside. Previous research has shown that reduction of oxidized organic and inorganic contaminants often can be catalyzed by electron shuttle systems. Metalloporphyrins and their derivatives are well known electron shuttles for many biogeochemical systems, and thus were selected to study their catalytic capabilities for the reduction of chromium and uranium in the presence of reducing agents. Zero valent iron (ZVI) was chosen as the primary electron donor in most experimental systems. Research proceeded in three phases and the key findings of each phase are reported here. Phase I examined Cr(VI) reduction and utilized micro- and nano-sized ZVI as the electron donors. Electron shuttle catalysts tested were cobalt- and iron-containing metalloporphyrins and Vitamin B12. To aid in the recycle and reuse of the nano-sized ZVI and soluble catalysts, sol-gels and calcium-alginate gel beads were tested as immobilization/support matrices. Although the nano-sized ZVI could be incorporated within the alginate gel beads, preliminary attempts to trap it in sol-gels were not successful. Conversely, the water-soluble catalysts could be trapped within sol-gel matrices but they tended to leach out of the alginate gel beads during use. In general, immobilization of the nano-sized ZVI in gel beads and of the catalysts in sol-gels tended to result in slower rates of Cr(VI) reduction, but these effects could be overcome to some extent by using higher reactant/catalyst concentrations. In addition, the lowering of their effectiveness would likely be offset by the benefits obtained when recycling and reusing the materials because they were immobilized. Addition of the catalytic electron shuttles will be most useful when the micro-sized or nano-sized ZVI becomes less reactive with reaction time. Continued work in Phase II in the area of nano-sized ZVI immobilization led to procedures that were successful in incorporating the iron particles in sol-gel matrices. The water-soluble reductants sodium dithionite and L-ascorbic acid were also tested, but their use appeared to lead to formation of complexes with the uranyl cation which limited their effectiveness. Also, although the sol-gel supported nano-sized ZVI showed some promise at reducing uranium, the fluoride used in the sol-gel synthesis protocol appeared to lead to formation of uranyl-fluoride complexes that were less reactive. Because hexavalent chromium is an anion which does not form complexes with fluoride, it was used to demonstrate the intrinsic reactivity of the sol-gel immobilized nano-sized ZVI. Consistent with our observations in Phase I, the sol-gel matrix once again slowed down the reduction reaction but the expected benefits of recycle/reuse should outweigh this adverse effect. The major emphasis in Phase III of this study was to simultaneously incorporate nano-sized ZVI and water-soluble catalysts in the same sol-gel matrix. The catalysts utilized were cobalt complexes of uroporphyrin and protoporphyrin and Cr(VI) reduction was used to test the efficacy of the combined "catalyst + reductant" sol-gel matrix. When enough catalyst was added to the sol-gels, enhancement of the Cr(VI) reduction reaction was observed. At the lowest levels of catalyst addition, however, the rates of Cr(VI) reduction were similar to those systems which only used sol-gel immobilized nano-sized ZVI without any catalyst present. These findings suggest future areas of research that should be pursued to further optimize abiotic reduction reactions of metals with combined "catalyst + reductant" matrices.« less
Soft nanoimprint lithography on SiO2 sol-gel to elaborate sensitive substrates for SERS detection

NASA Astrophysics Data System (ADS)

Hamouda, Frédéric; Bryche, Jean-François; Aassime, Abdelhanin; Maillart, Emmanuel; Gâté, Valentin; Zanettini, Silvia; Ruscica, Jérémy; Turover, Daniel; Bartenlian, Bernard

2017-12-01

This paper presents a new alternative fabrication of biochemical sensor based on surface enhanced Raman scattering (SERS) by soft nanoimprint lithography (S-NIL) on SiO2 sol-gel. Stabilization of the sol-gel film is obtained by annealing which simplifies the manufacturing of these biosensors and is compatible with mass production at low cost. This detector relies on a specific pattern of gold nanodisks on a thin gold film to obtain a better sensitivity of molecules' detection. Characterizations of SERS devices were performed on a confocal Raman microspectrophotometer after a chemical functionalization. We report a lateral collapse effect on poly(diméthylsiloxane) (PDMS) stamp for specific nanostructure dimensions. This unintentional effect is used to evaluate S-NIL resolution in SiO2 sol-gel.
Electronic nose screening of ethanol release during sol-gel encapsulation. A novel non-invasive method to test silica polymerisation.

PubMed

Lovino, Magalí; Cardinal, M Fernanda; Zubiri, Diana B V; Bernik, Delia L

2005-12-15

Porous silica matrices prepared by sol-gel process yield biocompatible materials adequate for encapsulation of biomolecules or drugs. The procedure is simple and fast, but when alkoxyde precursors like tetraethoxysilane (TEOS) are used the polymerisation reaction leads to the formation of alcohol as a by-product, which can produce undesirable effects on the activity of entrapped enzymes or modify a drug release kinetic. Therefore, it is critical to determine that no remnant ethanol is left prior using or storing the obtained biomaterial. In this regard, the technique used in the alcohol determination should be non-invasive and non-destructive to preserve the encapsulation device intact and ready to use. In this work we have successfully used a portable electronic nose (e-nose) for the screening of silica polymerisation process during theophylline encapsulation. TEOS reaction was "smelt" since precursor pre-hydrolysis until the end of ethanol release, sensed directly at the headspace of matrices slabs. Measurements showed that ethanol was negligible since 10th day in polymeric slabs of 10 mm width and 2 cm diameter. This first use of e-nose following a polymerisation reaction opens a wide number of putative applications in pharmaceutical and biochemical fields.
Sol-gel processing of bioactive glass nanoparticles: A review.

PubMed

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.
Synthesis of a fluorine-free polymeric water-repellent agent for creation of superhydrophobic fabrics

NASA Astrophysics Data System (ADS)

Shen, Keke; Yu, Miao; Li, Qianqian; Sun, Wei; Zhang, Xiting; Quan, Miao; Liu, Zhengtang; Shi, Suqing; Gong, Yongkuan

2017-12-01

A non-fluorinated polymeric alkylsilane, poly(isobutyl methacrylate-co-3-methacryloxypropyltrimethoxysilane) (PIT), is designed and synthesized to replace the commercial long-chain perfluoroalkylsilane (FAS) water-repellent agent. The superhydrophobic polyester fabrics are prepared by anchoring sol-gel derived silica nanoparticles onto alkali-treated polyester fabric surfaces and subsequently hydrophobilizing with PIT, using FAS as control. The surface chemical composition, surface morphology, wetting behavior and durability of the modified polyester fabrics are characterized by scanning electron microscopy (SEM), X-ray photoelectron spectrophotometer (XPS) and video-based contact angle goniometer, respectively. The results show that a porous silica layer could be successfully fabricated onto the surface of polyester fabric through base-catalyzed sol-gel process with tetraethoxysilane (TEOS) as precursor, incorporating additional nanostructured roughness essential for superhydrophobicity. At the same time, such a silica primer layer could provide both secondary reactive moieties (-Si - OH) for the subsequent surface hydrophobization and acceptable adhesion at the silica-polyester fabric interface. When silica modified polyester fabric (SiO2@ fabric) is hydrophobized by PIT solution (10 mg/mL), excellent water-repellency could be obtained. The water contact angle is up to 154° and the sliding angle is about 5°. Compared with small molecule water-repellent agent FAS, PIT modified SiO2@ fabric exhibits greatly improved solvent resistance under ultra-sonication, abrasion and simulated laundering durability. The anti-stain property of PIT-modified SiO2@ fabric is also evaluated by using different aqueous colored solutions.
Use of sol-gels as solid matrixes for simultaneous multielement determination by radio frequency glow discharge optical emission spectrometry: determinations of suspended particulate matter.

PubMed

Davis, W Clay; Knippel, Brad C; Cooper, Julia E; Spraul, Bryan K; Rice, Jeanette K; Smith, Dennis W; Marcus, R Kenneth

2003-05-15

A new approach for the analysis of particulate matter by radio frequency glow discharge optical emission spectrometry (rf-GD-OES) is described. Dispersion of the particles in a sol-gel sample matrix provides a convenient means of generating a thin film suitable for sputter-sampling into the discharge. Acid-catalyzed sol-gel glasses synthesized from tetramethyl orthosilicate were prepared and spun-cast on glass substrates. The resultant thin films on glass substrates were analyzed to determine the discharge operating conditions and resultant sputtering characteristics while a number of optical emission lines of the film components were monitored. Slurries of powdered standard reference materials NIST SRM 1884a (Portland Cement) and NIST SRM 2690 (Coal Fly Ash) dispersed in the sols were cast into films in the same manner. Use of the sol-gels as sample matrixes allows for background subtraction through the use of analytical blanks and may facilitate the generation of calibration curves via readily synthesized, matrix-matched analytical standards in solids analysis. Detection limits were determined for minor elements via the RSDB method to be in the range of 1-10 microg/g in Portland Cement and Coal Fly Ash samples for the elements Al, Fe, Mg, S, and Si. Values for Ca were in the range of 15-35 microg/g. This preliminary study demonstrates the possibility of incorporating various insoluble species, including ceramics and geological specimens in powder form, into a solid matrix for further analysis by either rf-GD-OES or MS.
Development of an extended-range fiber optic pH sensor using evanescent wave absorption of sol-gel-entrapped pH indicators

NASA Astrophysics Data System (ADS)

Butler, Thomas M.; MacCraith, Brian D.; McDonagh, Colette M.

1995-09-01

The sol-gel process has been used to entrap pH indicators in porous glass coatings for sensor applications. This sensor is based on evanescent wave absorption using an unclad optical fiber dipcoated with the pH sensitive coating. The entrapped pH indicators show a broadening of the pH range with respect to the behavior in solution giving accurate measurement over three pH units when one indicator is used (bromophenol blue) and over six pH units (pH 3-9) when two indicators are used (bromophenol blue and bromocresol purple). The response of the pH sensor was monitored by measuring absorption at 590 nm referenced against a nonabsorbing region of the spectrum. This enabled the use of LED sources together with low cost photodiodes. The sensor displayed short response time and good repeatability. The thickness and stability of the pH sensitive coatings can be influenced by modifying the composition of the starting sol mixture. The evanescent absorption, and hence the sensitivity of the sensor, can be increased by selectively launching higher order modes in the fiber. These issues together with a full sensor characterization will be reported.
Method for net-shaping using aerogels

DOEpatents

Brinker, C. Jeffrey; Ashey, Carol S.; Reed, Scott T.; Sriram, Chunangad S.; Harris, Thomas M.

2001-01-01

A method of net-shaping using aerogel materials is provided by first forming a sol, aging the sol to form a gel, with the gel having a fluid component and having been formed into a medium selected from the group consisting of a powder, bulk material, or granular aerobeads, derivatizing the surface of the gel to render the surface unreactive toward further condensation, removing a portion of the fluid component of the final shaped gel to form a partially dried medium, placing the medium into a cavity, wherein the volume of said medium is less that the volume of the cavity, and removing a portion of the fluid component of the medium. The removal, such as by heating at a temperature of approximately less than 50.degree. C., applying a vacuum, or both, causes the volume of the medium to increase and to form a solid aerogel. The material can be easily removed by exposing the material to a solvent, thereby reducing the volume of the material. In another embodiment, the gel is derivatized and then formed into a shaped medium, where subsequent drying reduces the volume of the shaped medium, forming a net-shaping material. Upon further drying, the material increases in volume to fill a cavity. The present invention is both a method of net-shaping and the material produced by the method.
High Refractive Organic–Inorganic Hybrid Films Prepared by Low Water Sol-Gel and UV-Irradiation Processes

PubMed Central

Ma, Hsiao-Yuan; Wang, Tzong-Liu; Chang, Pei-Yu; Yang, Chien-Hsin

2016-01-01

Organic-inorganic hybrid sols (Ti–O–Si precursor) were first synthesized by the sol-gel method at low addition of water, and were then employed to prepare a highly refractive hybrid optical film. This film was obtained by blending the Ti–O–Si precursor with 2-phenylphenoxyethyl acrylate (OPPEA) to perform photo-polymerization by ultraviolet (UV) irradiation. Results show that the film transparency of poly(Ti–O–Si precursor-co-OPPEA) film is higher than that of a pure poly(Ti–O–Si precursor) film, and that this poly(Ti–O–Si precursor-co-OPPEA) hybrid film exhibits a high transparency of ~93.7% coupled with a high refractive index (n) of 1.83 corresponding to a thickness of 2.59 μm. PMID:28344303
Solid materials for removing metals and fabrication method

DOEpatents

Coronado, Paul R.; Reynolds, John G.; Coleman, Sabre J.

2004-10-19

Solid materials have been developed to remove contaminating metals and organic compounds from aqueous media. The contaminants are removed by passing the aqueous phase through the solid materials which can be in molded, granular, or powder form. The solid materials adsorb the metals and the organics leaving a purified aqueous stream. The materials are sol-gel and or sol-gel and granulated activated carbon (GAC) mixtures. The species-specific adsorption occurs through specific chemical modifications of the solids tailored towards the contaminant(s). The contaminated solid materials can then be disposed of or the contaminant can be removed and the solids recycled.

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