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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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).

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.

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-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.

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.

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.

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.

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.

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

Sol-Gel Application for Consolidating Stone: An Example of Project-Based Learning in a Physical Chemistry Lab

ERIC Educational Resources Information Center

de los Santos, Desiree´ M.; Montes, Antonio; Sa´nchez-Coronilla, Antonio; Navas, Javier

2014-01-01

A Project Based Learning (PBL) methodology was used in the practical laboratories of the Advanced Physical Chemistry department. The project type proposed simulates "real research" focusing on sol-gel synthesis and the application of the obtained sol as a stone consolidant. Students were divided into small groups (2 to 3 students) to…

Graphene oxide-enhanced sol-gel transition sensitivity and drug release performance of an amphiphilic copolymer-based nanocomposite

PubMed Central

Hu, Huawen; Wang, Xiaowen; Lee, Ka I; Ma, Kaikai; Hu, Hong; Xin, John H.

2016-01-01

We report the fabrication of a highly sensitive amphiphilic copolymer-based nanocomposite incorporating with graphene oxide (GO), which exhibited a low-intensity UV light-triggered sol-gel transition. Non-cytotoxicity was observed for the composite gels after the GO incorporation. Of particular interest were the microchannels that were formed spontaneously within the GO-incorporated UV-gel, which expedited sustained drug release. Therefore, the present highly UV-sensitive, non-cytotoxic amphiphilic copolymer-based composites is expected to provide enhanced photothermal therapy and chemotherapy by means of GO’s unique photothermal properties, as well as through efficient passive targeting resulting from the sol-gel transition characteristic of the copolymer-based system with improved sensitivity, which thus promises the enhanced treatment of patients with cancer and other diseases. PMID:27539298

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.

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.

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.

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.

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.

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.

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.

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 niobia sorbent with a positively charged octadecyl ligand providing enhanced enrichment of nucleotides and organophosphorus pesticides in capillary microextraction for online HPLC analysis.

PubMed

Kesani, Sheshanka; Malik, Abdul

2018-04-01

A niobia-based sol-gel organic-inorganic hybrid sorbent carrying a positively charged C 18 ligand (Nb 2 O 5 -C 18 (+ve)) was synthesized to achieve enhanced enrichment capability in capillary microextraction of organophosphorus compounds (which include organophosphorus pesticides and nucleotides) before their online analysis by high-performance liquid chromatography. The sorbent was designed to simultaneously provide three different types of molecular level interactions: electrostatic, Lewis acid-base, and van der Waals interactions. To understand relative contributions of various molecular level analyte-sorbent interactions in the extraction process, two other sol-gel niobia sorbents were also created: (a) a purely inorganic sol-gel niobia sorbent (Nb 2 O 5 ) and (b) an organic-inorganic hybrid sol-gel niobia sorbent carrying an electrically neutral-bonded octadecyl ligand (Nb 2 O 5 -C 18 ). The extraction efficiency of the created sol-gel niobia sorbent (Nb 2 O 5 -C 18 (+ve)) was compared with that of analogously designed and synthesized titania-based sol-gel sorbent (TiO 2 -C 18 (+ve)), taking into consideration that titania-based sorbents present state-of-the-art extraction media for organophosphorus compounds. In capillary microextraction with high-performance liquid chromatography analysis, Nb 2 O 5 -C 18 (+ve) had shown 40-50% higher specific extraction values (a measure of extraction efficiency) over that of TiO 2 -C 18 (+ve). Compared to TiO 2 -C 18 (+ve), Nb 2 O 5 -C 18 (+ve) also provided superior analyte desorption efficiency (96 vs. 90%) during the online release of the extracted organophosphorus pesticides from the sorbent coating in the capillary microextraction capillary to the chromatographic column using reversed-phase high-performance liquid chromatography mobile phase. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-speed, Low Voltage, Miniature Electro-optic Modulators Based on Hybrid Photonic-Crystal/Polymer/Sol-Gel Technology

DTIC Science & Technology

2012-02-01

code) 01/02/2012 FINAL 15/11/2008 - 15/11/2011 High-speed, Low Voltage, Miniature Electro - optic Modulators Based on Hybrid Photonic-Crystal/Polymer... optic modulator, silicon photonics, integrated optics, electro - optic polymer, avionics, optical communications, sol-gel, nanotechnology U U U UU 25...2011 Program Manager: Dr. Charles Y-C Lee High-speed, Low Voltage, Miniature Electro - optic Modulators Based on Hybrid Photonic-Crystal/Polymer/Sol

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.

ELISA AND SOL-GEL BASED IMMUNOAFFINITY PURIFICATION OF THE PYRETHROID BIOALLETHRIN IN FOOD AND ENVIRONMENTAL SAMPLES

EPA Science Inventory

The peer-reviewed article describes the development of a new sol-gel based immunoaffinity purification procedure and an immunoassay for the pyrethroid bioallethrin. The immunoaffinity chromatography procedure was applied to food samples providing an efficient cleanup prior to im...

Characterization of SrCo1.5Ti1.5Fe9O19 hexagonal ferrite synthesized by sol-gel combustion and solid state route

NASA Astrophysics Data System (ADS)

Vinaykumar, R.; Mazumder, R.; Bera, J.

2017-05-01

Co-Ti co-substituted SrM hexagonal ferrite (SrCo1.5Ti1.5Fe9O19) was synthesized by sol-gel combustion and solid state route. The effects of sources of TiO2 raw materials; titanium tetra-isopropoxide (TTIP) and titanyl nitrate (TN) on the phase formation behavior and properties of the ferrite were studied. The thermal decomposition behavior of the gel was studied using TG-DSC. The phase formation behavior of the ferrite was studied by using X-ray powder diffraction and FTIR analysis. Phase formation was comparatively easier in the TN-based sol-gel process. The morphology of powder and sintered ferrite was investigated using scanning electron microscope. Magnetic properties like magnetization, coercivity, permeability, tan δμ and dielectric properties were investigated. The ferrite synthesized by sol-gel based chemical route showed higher saturation magnetization, permeability and permittivity compared to the ferrite synthesized by solid state route.

Sol-Gel-Based Titania-Silica Thin Film Overlay for Long Period Fiber Grating-Based Biosensors.

PubMed

Chiavaioli, Francesco; Biswas, Palas; Trono, Cosimo; Jana, Sunirmal; Bandyopadhyay, Somnath; Basumallick, Nandini; Giannetti, Ambra; Tombelli, Sara; Bera, Susanta; Mallick, Aparajita; Baldini, Francesco

2015-12-15

An evanescent wave optical fiber biosensor based on titania-silica-coated long period grating (LPG) is presented. The chemical overlay, which increases the refractive index (RI) sensitivity of the sensor, consists of a sol-gel-based titania-silica thin film, deposited along the sensing portion of the fiber by means of the dip-coating technique. Changing both the sol viscosity and the withdrawal speed during the dip-coating made it possible to adjust the thickness of the film overlay, which is a crucial parameter for the sensor performance. After the functionalization of the fiber surface using a methacrylic acid/methacrylate copolymer, an antibody/antigen (IgG/anti-IgG) assay was carried out to assess the performance of sol-gel based titania-silica-coated LPGs as biosensors. The analyte concentration was determined from the wavelength shift at the end of the binding process and from the initial binding rate. This is the first time that a sol-gel based titania-silica-coated LPG is proposed as an effective and feasible label-free biosensor. The specificity of the sensor was validated by performing the same model assay after spiking anti-IgG into human serum. With this structured LPG, detection limits of the order of tens of micrograms per liter (10(-11) M) are attained.

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.

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.

Sol-gel based optical sensor for determination of Fe (II): a novel probe for iron speciation.

PubMed

Samadi-Maybodi, Abdolraouf; Rezaei, Vida; Rastegarzadeh, Saadat

2015-02-05

A highly selective optical sensor for Fe (II) ions was developed based on entrapment of a sensitive reagent, 2,4,6-tri(2-pyridyl)-s-triazine (TPTZ), in a silica sol-gel thin film coated on a glass substrate. The thin films fabricated based on tetraethoxysilane (TEOS) as precursor, sol-gel pH∼3, water:alkoxyde ratio of 4:1 and TPTZ concentration of 0.112 mol L(-1). The influence of sol-gel parameters on sensing behavior of the fabricated sensor was also investigated. The fabricated sensor can be used for determination of Fe (II) ion with an outstanding high selectivity over a dynamic range of 5-115 ng mL(-1) and a detection limit of 1.68 ng mL(-1). It also showed reproducible results with relative standard deviation of 3.5% and 1.27% for 10 and 90 ng mL(-1) of Fe (II), respectively, along with a fast response time of ∼120 s. Total iron also was determined after reduction of Fe (III) to Fe (II) using ascorbic acid as reducing agent. Then, the concentration of Fe (III) was calculated by subtracting the concentration of Fe (II) from the total iron concentration. Interference studies showed a good selectivity for Fe (II) with trapping TPTZ into sol-gel matrix and appropriately adjusting the structure of doped sol-gel. The sensor was compared with other sensors and was applied to determine iron in different water samples with good results. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

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.

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.

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

PubMed

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

2001-07-01

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

Blue light emission from trivalent cerium doped in sol-gel silica glass

NASA Astrophysics Data System (ADS)

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

2017-02-01

Rare earths in glass matrices are promising for active optical devices as amplifiers and lasers. Emission originating from d-f transitions in sol-gel glass has not been studied very often, while those based on f-f transitions were widely utilized. However, d-f emission in rare earths is very important because of their strong oscillator strength and broad emission widths suitable for the application to scintillators and solid-state lasers. Co-doping of aluminum in sol-gel synthesis was known to be effective for the emission enhancement of trivalent terbium and europium. Recently, we applied aluminum co-doping to cerium and europium systems in sol-gel glass to succeed in the observation of strong blue light emission originating from d-f transitions. Glass samples were prepared with conventional sol-gel process where tetramethylorthosilicate was hydrolyzed in the mixture of water, ethanol and dimethylformamide with nitric acid catalyst. After adding cerium nitrate and aluminum nitrate, the solution experienced drying followed by calcination at 1,050°C under air environment. When molar ratio of cerium to silicon was adjusted at 0.1% and Al concentration was varied in 0.1 2.0%, transparent glass products showed bright and broad blue photoluminescence under UV illumination. The fluorescence lifetimes were found to be about 50 90 ns, indicating that the emission was due to d-f transitions. Considering the simplicity of the process, blue phosphors based on sol-gel glass will be very promising for future applications.

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

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.

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.

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.

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

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

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

PubMed

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

2014-11-28

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

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

PubMed Central

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

2014-01-01

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

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.

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.

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.

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.

Reagentless D-sorbitol biosensor based on D-sorbitol dehydrogenase immobilized in a sol-gel carbon nanotubes-poly(methylene green) composite.

PubMed

Wang, Zhijie; Etienne, Mathieu; Urbanova, Veronika; Kohring, Gert-Wieland; Walcarius, Alain

2013-04-01

A reagentless D-sorbitol biosensor based on NAD-dependent D-sorbitol dehydrogenase (DSDH) immobilized in a sol-gel carbon nanotubes-poly(methylene green) composite has been developed. It was prepared by durably immobilizing the NAD(+) cofactor with DSDH in a sol-gel thin film on the surface of carbon nanotubes functionalized with poly(methylene green). This device enables selective determination of D-sorbitol at 0.2 V with a sensitivity of 8.7 μA mmol(-1) L cm(-2) and a detection limit of 0.11 mmol L(-1). Moreover, this biosensor has excellent operational stability upon continuous use in hydrodynamic conditions.

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.

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.

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

NASA Technical Reports Server (NTRS)

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

1983-01-01

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

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.

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.

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.

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.

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.

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.

Mimicking nature: Self-strengthening properties in a dental adhesive.

PubMed

Song, Linyong; Ye, Qiang; Ge, Xueping; Misra, Anil; Spencer, Paulette

2016-04-15

Chemical and enzymatic hydrolysis provoke a cascade of events that undermine methacrylate-based adhesives and the bond formed at the tooth/composite interface. Infiltration of noxious agents, e.g. enzymes, bacteria, and so forth, into the spaces created by the defective bond will ultimately lead to failure of the composite restoration. This paper reports a novel, synthetic resin that provides enhanced hydrolytic stability as a result of intrinsic reinforcement of the polymer network. The behavior of this novel resin, which contains γ-methacryloxyproyl trimethoxysilane (MPS) as its Si-based compound, is reminiscent of self-strengthening properties found in nature. The efforts in this paper are focused on two essential aspects: the visible-light irradiation induced (photoacid-induced) sol-gel reaction and the mechanism leading to intrinsic self-strengthening. The FTIR band at 2840cm(-1) corresponding to CH3 symmetric stretch in -Si-O-CH3 was used to evaluate the sol-gel reaction. Results from the real-time FTIR indicated that the newly developed resin showed a limited sol-gel reaction (<5%) during visible-light irradiation, but after 48h dark storage, the reaction was over 65%. The condensation of methoxysilane mainly occurred under wet conditions. The storage moduli and glass transition temperature of the copolymers increased in wet conditions with the increasing MPS content. The cumulative amounts of leached species decreased significantly when the MPS-containing adhesive was used. The results suggest that the polymethacrylate-based network, which formed first as a result of free radical initiated polymerization, retarded the photoacid-induced sol-gel reaction. The sol-gel reaction provided a persistent, intrinsic reinforcement of the polymer network in both neutral and acidic conditions. This behavior led to enhanced mechanical properties of the dental adhesives under conditions that simulate the wet, oral environment. A self-strengthening dental adhesive system was developed through a dual curing process, which involves the free radical photopolymerization followed by slow hydrolysis and condensation (photoacid-induced sol-gel reaction) of alkoxylsilane groups. The concept of "living" photoacid-induced sol-gel reaction with visible-light irradiation was confirmed in the polymer. The sol-gel reaction was retarded by the polymethacrylate network, which was generated first; the network extended the life and retained the activity of silanol groups. The self-strengthening behavior was evaluated by monitoring the mechanical properties of the hybrid copolymers under wet conditions. The present research demonstrates the sol-gel reaction in highly crosslinked network as a potentially powerful strategy to prolong the functional lifetime of engineered biomaterials in wet environments. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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...

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.

Sol-gel preparation of hydrophobic silica antireflective coatings with low refractive index by base/acid two-step catalysis.

PubMed

Cai, Shuang; Zhang, Yulu; Zhang, Hongli; Yan, Hongwei; Lv, Haibing; Jiang, Bo

2014-07-23

Hydrophobic antireflective coatings with a low refractive index were prepared via a base/acid-catalyzed two-step sol-gel process using tetraethylorthosilicate (TEOS) and methyltriethoxysilane (MTES) as precursors, respectively. The base-catalyzed hydrolysis of TEOS leads to the formation of a sol with spherical silica particles in the first step. In the second step, the acid-catalyzed MTES hydrolysis and condensation occur at the surface of the initial base-catalyzed spherical silica particles, which enlarge the silica particle size from 12.9 to 35.0 nm. By a dip-coating process, this hybrid sol gives an antireflective coating with a refractive index of about 1.15. Moreover, the water contact angles of the resulted coatings increase from 22.4 to 108.7° with the increases of MTES content, which affords the coatings an excellent hydrophobicity. A "core-shell" particle growth mechanism of the hybrid sol was proposed and the relationship between the microstructure of silica sols and the properties of AR coatings was investigated.

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

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.

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.

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

Low temperature and UV curable sol-gel coatings for long lasting optical fiber biosensors

NASA Astrophysics Data System (ADS)

Otaduy, D.; Villar, A.; Gomez-Herrero, E.; Goitandia, A. M.; Gorritxategi, E.; Quintana, I.

2010-04-01

The use of optical fibers as sensing element is increasing in clinical, pharmaceutical and industrial applications. Excellent light delivery, long interaction length, low cost and ability not only to excite the target molecules but also to capture the emitted light from the targets are the hallmarks of optical fiber as biosensors. In biosensors based on fiber optics the interaction with the analyte can occur within an element of the optical fiber. One of the techniques for this kind of biosensors is to remove the fiber optic cladding and substitute it for biological coatings that will interact with the parameter to sensorize. The deposition of these layers can be made by sol-gel technology. The sol-gel technology is being increasingly used mainly due to the high versatility to tailor their optical features. Incorporation of suitable chemical and biochemical sensing agents have allowed determining pH, gases, and biochemical species, among others. Nonetheless, the relatively high processing temperatures and short lifetime values mean severe drawbacks for a successful exploitation of sol-gel based coated optical fibres. With regard to the latter, herein we present the design, preparation and characterization of novel sol-gel coated optical fibres. Low temperature and UV curable coating formulations were optimized to achieve a good adhesion and optical performance. The UV photopolymerizable formulation was comprised by glycidoxypropyltrimethoxysilane (GLYMO), Tetraethylorthosilicate (TEOS) and an initiator. While the thermoset coating was prepared by using 3-aminopropyltrimethoxysilane, GLYMO, and TEOS as main reagents. Both curable sol-gel coated fibres were analysed by FTIR, SEM and optical characterization. Furthermore, in the present work a new technique for silica cladding removal has been developed by ultra-short pulses laser processing, getting good dimensional accuracy and surface integrity.

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

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

PubMed

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

2016-10-07

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

Innovative Formulation Combining Al, Zr and Si Precursors to Obtain Anticorrosion Hybrid Sol-Gel Coating.

PubMed

Genet, Clément; Menu, Marie-Joëlle; Gavard, Olivier; Ansart, Florence; Gressier, Marie; Montpellaz, Robin

2018-05-10

The aim of our study is to improve the aluminium alloy corrosion resistance with Organic-Inorganic Hybrid (OIH) sol-gel coating. Coatings are obtained from unusual formulation with precursors mixing: glycidoxypropyltrimethoxysilane (GPTMS), zirconium (IV) propoxide (TPOZ) and aluminium tri-sec-butoxide (ASB). This formulation was characterized and compared with sol formulations GPTMS/TPOZ and GPTMS/ASB. In each formulation, a corrosion inhibitor, cerium (III) nitrate hexahydrate, is employed to improve the corrosion performance. Coatings obtained from sol based on GPTMS/TPOZ/ASB have good anti-corrosion performances with Natural Salt Spray (NSS) resistance of 500 h for a thickness lower than 4 µm. Contact angle measurement showed a coating hydrophobic behaviour. To understand these performances, nuclear magnetic resonance (NMR) analyses were performed, results make sol-gel coating condensation evident and are in very good agreement with previous results.

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.

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.

Resistive switching memory devices composed of binary transition metal oxides using sol-gel chemistry.

PubMed

Lee, Chanwoo; Kim, Inpyo; Choi, Wonsup; Shin, Hyunjung; Cho, Jinhan

2009-04-21

We describe a novel and versatile approach for preparing resistive switching memory devices based on binary transition metal oxides (TMOs). Titanium isopropoxide (TIPP) was spin-coated onto platinum (Pt)-coated silicon substrates using a sol-gel process. The sol-gel-derived layer was converted into a TiO2 film by thermal annealing. A top electrode (Ag electrode) was then coated onto the TiO2 films to complete device fabrication. When an external bias was applied to the devices, a switching phenomenon independent of the voltage polarity (i.e., unipolar switching) was observed at low operating voltages (about 0.6 VRESET and 1.4 VSET). In addition, it was confirmed that the electrical properties (i.e., retention time, cycling test and switching speed) of the sol-gel-derived devices were comparable to those of vacuum deposited devices. This approach can be extended to a variety of binary TMOs such as niobium oxides. The reported approach offers new opportunities for preparing the binary TMO-based resistive switching memory devices allowing a facile solution processing.

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

NASA Technical Reports Server (NTRS)

1982-01-01

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

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

Investigation of novel sol-gel hydrophobic surfaces for desorption electrospray ionization-mass spectrometry analysis.

PubMed

Penna, Andrea; Elviri, Lisa; Careri, Maria; Mangia, Alessandro; Predieri, Giovanni

2011-05-01

Sol-gel-based materials were synthesized, characterized and finally tested as solid supports for desorption electrospray ionization-mass spectrometry (DESI-MS) analysis of a mixture of compounds of different polarity. Films with thickness in the 2-4 μm range were obtained by a dip-coating process using tetraethoxysilane (TEOS) and octyltriethoxysilane (OTES) as sol-gel precursors. Three types of surface with different hydrophobic character were obtained by varying the TEOS/OTES ratio in the sol-gel mixture. Each coating was characterized by atomic force microscopy investigations, gaining insight into homogeneity, smoothness and thickness of the obtained films. To study hydrophobicity of each surface, surface free energy measurements were performed. Different DESI-MS responses were observed when different solvent mixture deposition procedures and solvent spray compositions were investigated. Results were finally compared to those obtained by using commercial polytetrafluoroethylene-coated slides. It was found that surface free energy plays an important role in the desorption/ionization process as a function of the polarity of analytes.

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.

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.

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.

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.

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

PubMed Central

2011-01-01

Two current technologies used in biosensor development are very promising: 1. The sol-gel process of making microporous glass at room temperature, and 2. Using a fluorescent compound that undergoes fluorescence quenching in response to a specific analyte. These technologies have been combined to produce an iron biosensor. To optimize the iron (II or III) specificity of an iron biosensor, pyoverdin (a fluorescent siderophore produced by Pseudomonas spp.) was immobilized in 3 formulations of porous sol-gel glass. The formulations, A, B, and C, varied in the amount of water added, resulting in respective R values (molar ratio of water:silicon) of 5.6, 8.2, and 10.8. Pyoverdin-doped sol-gel pellets were placed in a flow cell in a fluorometer and the fluorescence quenching was measured as pellets were exposed to 0.28 - 0.56 mM iron (II or III). After 10 minutes of exposure to iron, ferrous ion caused a small fluorescence quenching (89 - 97% of the initial fluorescence, over the range of iron tested) while ferric ion caused much greater quenching (65 - 88%). The most specific and linear response was observed for pyoverdin immobilized in sol-gel C. In contrast, a solution of pyoverdin (3.0 μM) exposed to iron (II or III) for 10 minutes showed an increase in fluorescence (101 - 114%) at low ferrous concentrations (0.45 - 2.18 μM) while exposure to all ferric ion concentrations (0.45 - 3.03 μM) caused quenching. In summary, the iron specificity of pyoverdin was improved by immobilizing it in sol-gel glass C. PMID:21554740

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

PubMed

Escobar, Sindy; Bernal, Claudia; Mesa, Monica

2015-01-01

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

Effects of inorganic acids and divalent hydrated metal cations (Mg(2+), Ca(2+), Co(2+), Ni(2+)) on γ-AlOOH sol-gel process.

PubMed

Zhang, Jian; Xia, Yuguo; Zhang, Li; Chen, Dairong; Jiao, Xiuling

2015-11-07

In-depth understanding of the sol-gel process plays an essential role in guiding the preparation of new materials. Herein, the effects of different inorganic acids (HCl, HNO3 and H2SO4) and divalent hydrated metal cations (Mg(2+), Ca(2+), Co(2+), Ni(2+)) on γ-AlOOH sol-gel process were studied based on experiments and density functional theory (DFT) calculations. In these experiments, the sol originating from the γ-AlOOH suspension was formed only with the addition of HCl and HNO3, but not with H2SO4. Furthermore, the DFT calculations showed that the strong adsorption of HSO4(-) on the surface of the γ-AlOOH particles, and the hydrogen in HSO4(-) pointing towards the solvent lead to an unstable configuration of electric double layer (EDL). In the experiment, the gelation time sequence of γ-AlOOH sol obtained by adding metal ions changed when the ionic strength was equal to or greater than 0.198 mol kg(-1). The DFT calculations demonstrated that the adsorption energy of hydrated metal ions on the γ-AlOOH surface can actually make a difference in the sol-gel process.

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

PubMed

Kapusuz, Derya; Durucan, Caner

2017-07-01

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

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.

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.

Fabrication of highly uniform and porous MgF2 anti-reflective coatings by polymer-based sol-gel processing on large-area glass substrates.

PubMed

Raut, Hemant Kumar; Dinachali, Saman Safari; Ansah-Antwi, Kwadwo Konadu; Ganesh, V Anand; Ramakrishna, Seeram

2013-12-20

Despite recent progress in the fabrication of magnesium fluoride (MgF2) anti-reflective coatings (ARCs), simple, effective and scalable sol-gel fabrication of MgF2 ARCs for large-area glass substrates has prospective application in various optoelectronic devices. In this paper, a polymer-based sol-gel route was devised to fabricate highly uniform and porous MgF2 ARCs on large-area glass substrates. A sol-gel precursor made of polyvinyl acetate and magnesium trifluoroacetate assisted in the formation of uniformly mesoporous MgF2 ARCs on glass substrates, leading to the attainment of a refractive index of ~1.23. Systematic optimization of the thickness of the ARC in the sub-wavelength regime led to achieving ~99.4% transmittance in the case of the porous MgF2 ARC glass. Precise control of the thickness of porous MgF2 ARC glass also resulted in a mere ~0.1% reflection, virtually eliminating reflection off the glass surface at the target wavelength. Further manipulation of the thickness of the ARC on either side of the glass substrate led to the fabrication of relatively broadband, porous MgF2 ARC glass.

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.

Mimicking Nature: Self-strengthening Properties in a Dental Adhesive

PubMed Central

Song, Linyong; Ye, Qiang; Ge, Xueping; Misra, Anil; Spencer, Paulette

2016-01-01

Chemical and enzymatic hydrolysis provoke a cascade of events that undermine methacrylate-based adhesives and the bond formed at the tooth/composite interface. Infiltration of noxious agents, e.g. enzymes, bacteria, and so forth, into the spaces created by the defective bond will ultimately lead to failure of the composite restoration. This paper reports a novel, synthetic resin that provides enhanced hydrolytic stability as a result of intrinsic reinforcement of the polymer network. The behavior of this novel resin, which contains γ-methacryloxyproyl trimethoxysilane (MPS) as its Si-based compound, is reminiscent of self-strengthening properties found in nature. The efforts in this paper are focused on two essential aspects: the visible-light irradiation induced (photoacid-induced) sol-gel reaction and the mechanism leading to intrinsic self-strengthening. The FTIR band at 2840 cm−1 corresponding to CH3 symmetric stretch in −Si−O−CH3 was used to evaluate the sol-gel reaction. Results from the real-time FTIR indicated that the newly developed resin showed a limited sol-gel reaction (<5%) during visible-light irradiation, but after 48h dark storage, the reaction was over 65%. The condensation of methoxysilane mainly occurred under wet conditions. The storage moduli and glass transition temperature of the copolymers increased in wet conditions with the increasing MPS content. The cumulative amounts of leached species decreased significantly when the MPS-containing adhesive was used. The results suggest that the polymethacrylate-based network, which formed first as a result of free radical initiated polymerization, retarded the photoacid-induced sol-gel reaction. The sol-gel reaction provided a persistent, intrinsic reinforcement of the polymer network in both neutral and acidic conditions. This behavior led to enhanced mechanical properties of the dental adhesives under conditions that simulate the wet, oral environment. PMID:26883773

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.

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.

Rational construction of gel-based supramolecular logic gates by using a functional gelator with multiple-stimuli responsive properties.

PubMed

Fan, Kaiqi; Yang, Jun; Wang, Xiaobo; Song, Jian

2014-11-07

A gelator containing a sorbitol moiety and a naphthalene-based salicylideneaniline group exhibits macroscopic gel-sol behavior in response to four complementary input stimuli: temperature, UV light, OH(-), and Cu(2+). On the basis of its multiple-stimuli responsive properties, we constructed a rational gel-based supramolecular logic gate that performed OR and INH types of reversible stimulus responsive gel-sol transition in the presence of various combinations of the four stimuli when the gel state was defined as an output. Moreover, a combination two-output logic gate was obtained, owing to the existence of the naked eye as an additional output. Hence, gelator 1 could construct not only a basic logic gate, but also a two-input-two-output logic gate because of its response to multiple chemical stimuli and multiple output signals, in which one input could erase the effect of another input.

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.

Thermosensitive In Situ Gel Based on Solid Dispersion for Rectal Delivery of Ibuprofen.

PubMed

Liu, Yangdan; Wang, Xin; Liu, Youping; Di, Xin

2018-01-01

The objective of this study was to develop a thermosensitive in situ gel based on solid dispersions (SDs) for rectal delivery of ibuprofen (IBU). Thermosensitive (poloxamer 407) and mucoadhesive (hydroxypropylmethyl cellulose E5 and sodium alginate) polymers were used to prepare the in situ gel and the sol-gel transition temperature (T sol-gel ) and gel strength were optimized. The in vitro release performance and in vivo pharmacokinetic properties of the in situ gel after their rectal administration to rabbits were investigated. Compared with the solid suppository, the cumulative release of the IBU SDs loaded in situ gel was significantly increased. The in vivo pharmacokinetics indicated that in situ gel had a higher peak plasma concentration (C max ) and area under the curve (AUC (0-∞) ) in plasma than the solid suppositories. Histopathology results showed that the IBU in situ gel given at a dose of 15 mg/kg did not produce any irritation. In conclusion, this study suggested that the in situ gel could be an effective rectal formulation for IBU.

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...

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 © 2016 Elsevier B.V. All rights reserved.

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.

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.

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.

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

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.

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.

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.

A proton-exchange membrane prepared by the radiation grafting of styrene and silica into polytetrafluoroethylene films

NASA Astrophysics Data System (ADS)

Yu, Hongyan; Shi, Jianheng; Zeng, Xinmiao; Bao, Mao; Zhao, Xinqing

2009-07-01

A polytetrafluoroethylene (PTFE) based organic-inorganic hybrid proton-exchange membrane was prepared from simultaneous radiation grafting of styrene (St) into porous PTFE membrane with the in situ sol-gel reaction of tetraethoxysilane (TEOS) followed by sulfonation in fuming sulfonic acid. The effect of radiation on the sol-gel reaction was studied. The results show that radiation promotes the sol-gel reaction with the help of St at room temperature. Incorporated silica gel helps to produce higher degree of grafting (DOG). SEM analysis was conducted to confirm that the inorganic silicon oxide was introduced to produce hybrid membrane in this work. The proton conductivity of membrane evaluated using electrochemical impedance spectroscopy is much higher (14.3×10 -2 S cm -1) than that of Nafion ® 117 at temperature of 80 °C with acceptable water uptake 51 wt%.

[pH sensors based on rubbery ormosils preparation and their spectrum studies].

PubMed

Chen, Xi; Dai, Yuan-jing; Li, Wei; Zhuang, Zhi-xia; Wang, Xiao-ru

2002-02-01

A new type of methyl substituted ormosils as a matrix for bromophenol blue (BPhB) and bromocresol green (BCG) is described. The new ormosils combine features of classical TEOS sol-gel material such as solvability in organic solvent and those of sol-gel glasses such as transparent and a porous structure, the ormosils also make a good mechanical stability. The influence of the conditions during the polymerisation process on the photochemical properties of BPhB and BCG has been studied. This sol-gel material was wed to immobilize pH-sensitive absorption dyes, bromothymol blue and bromocresol green, to prepare pH sensing films. The several aspects of the sensing films, including the leaching of the dye from gel, response time to different pH buffer solution, absorption spectra and the improvement of the immobilization of the dyes to filmo, were also discussed.

Synthesis of hybrid cellulose nanocomposite bonded with dopamine SiO2/TiO2 and its antimicrobial activity

NASA Astrophysics Data System (ADS)

Ramesh, Sivalingam; Kim, Gwang-Hoon; Kim, Jaehwan; Kim, Joo-Hyung

2015-04-01

Organic-inorganic hybrid material based cellulose was synthesized by the sol-gel approach. The explosion of activity in this area in the past decade has made tremendous progress in industry or academic both fundamental understanding of sol-gel process and applications of new functionalized hybrid materials. In this present research work, we focused on cellulose-dopamine functionalized SiO2/TiO2 hybrid nanocomposite by sol-gel process. The cellulose-dopamine hybrid nanocomposite was synthesized via γ-aminopropyltriethoxysilane (γ-APTES) coupling agent by in-situ sol-gel process. The chemical structure of cellulose-amine functionalized dopamine bonding to cellulose structure with covalent cross linking hybrids was confirmed by FTIR spectral analysis. The morphological analysis of cellulose-dopamine nanoSiO2/TiO2 hybrid nanocomposite materials was characterized by XRD, SEM and TEM. From this different analysis results indicate that the optical transparency, thermal stability, control morphology of cellulose-dopamine-SiO2/TiO2 hybrid nanocomposite. Furthermore cellulose-dopamine-SiO2/TiO2 hybrid nanocomposite was tested against pathogenic bacteria for antimicrobial activity.

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.

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.

Organization versus frustration: low temperature transitions in a gelatine-based gel

NASA Astrophysics Data System (ADS)

Philipp, M.; Müller, U.; Sanctuary, R.; Baller, J.; Krüger, J. K.

2008-09-01

A commercial physical gel composed of gelatine, water and glycerol shows a sol-gel transition which has been resolved by optical rotation measurements by step-wise heating the gel. This transition is not observable in the longitudinal acoustic mode measured at hypersonic frequencies with Brillouin spectroscopy. Depending on the thermal treatment of the investigated material during the sol-gel transition and within the gel state, Brillouin spectroscopy reflects tremendously different hypersonic dynamics. These distinct dynamics are responsible for the formation of different glassy states at low temperatures including that of a glass-ceramic. The large variety of super-cooled and glassy states is attributed to distinct distributions of the gel's constituents within the samples. Surprisingly, the same gel state can be produced either by annealing the gel over months or by the non-equilibrium effect of thermo-diffusion (Soret effect) in the course of some minutes.

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.

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

NASA Astrophysics Data System (ADS)

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

2014-08-01

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

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.

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.

Chitosan-based thermosensitive hydrogel as a promising ocular drug delivery system: preparation, characterization, and in vivo evaluation.

PubMed

Chen, Xingwei; Li, Xinru; Zhou, Yanxia; Wang, Xiaoning; Zhang, Yanhui; Fan, Yating; Huang, Yanqing; Liu, Yan

2012-11-01

The purpose of this study was to evaluate the feasibility of in situ thermosensitive hydrogel based on chitosan in combination with disodium α-d-Glucose 1-phosphate (DGP) for ocular drug delivery system. Aqueous solution of chitosan/DGP underwent sol-gel transition as temperature increased which was flowing sol at room temperature and then turned into non-flowing hydrogel at physiological temperature. The properties of gels were characterized regarding gelation time, gelation temperature, and morphology. The sol-to-gel phase transition behaviors were affected by the concentrations of chitosan, DGP and the model drug levocetirizine dihydrochloride (LD). The developed hydrogel presented a characteristic of a rapid release at the initial period followed by a sustained release and remarkably enhanced the cornea penetration of LD. The results of ocular irritation demonstrated the excellent ocular tolerance of the hydrogel. The ocular residence time for the hydrogel was significantly prolonged compared with eye drops. The drug-loaded hydrogel produced more effective anti-allergic conjunctivitis effects compared with LD aqueous solution. These results showed that the chitosan/DGP thermosensitive hydrogel could be used as an ideal ocular drug delivery system in terms of the suitable sol-gel transition temperature, mild pH environment in the hydrogel as well as the organic solvent free.

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…

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.

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.

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.

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.

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.

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

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.

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 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.

Direct nanopatterning of 100 nm metal oxide periodic structures by Deep-UV immersion lithography.

PubMed

Stehlin, Fabrice; Bourgin, Yannick; Spangenberg, Arnaud; Jourlin, Yves; Parriaux, Olivier; Reynaud, Stéphanie; Wieder, Fernand; Soppera, Olivier

2012-11-15

Deep-UV lithography using high-efficiency phase mask has been developed to print 100 nm period grating on sol-gel based thin layer. High efficiency phase mask has been designed to produce a high-contrast interferogram (periodic fringes) under water immersion conditions for 244 nm laser. The demonstration has been applied to a new developed immersion-compatible sol-gel layer. A sol-gel photoresist prepared from zirconium alkoxides caped with methacrylic acids was developed to achieve 50 nm resolution in a single step exposure. The nanostructures can be thermally annealed into ZrO(2). Such route considerably simplifies the process for elaborating nanopatterned surfaces of transition metal oxides, and opens new routes for integrating materials of interest for applications in the field of photocatalysis, photovoltaic, optics, photonics or microelectronics.

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.

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

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.

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.

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.

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...

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 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.

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.

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.

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.

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.

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

Meeting the Challenge of Environmental Regulations in Europe and North America

DTIC Science & Technology

2011-02-08

salts • Electrolytic • Trivalent chromium • Rare earth salts • Sol Gel Socomor Finishing Technologies 24 Ce document et les informations qu’il contient...l’autorisation préalable et écrite de Safran. ASETS DEFENSE 2011 CHROMATE C.C. REPLACEMENT (3) TRIVALENT CHROMIUM • SUITABLE ONLY TO 1000, 3000, 5000...REPLACEMENT(4) ) - TRIVALENT CHROMIUM + TOP COAT - TRIVALENT CHROMIUM + INHIBITORS - OTHER CHEMISTRY BASED - SOL GEL Socomor Finishing Technologies

Ring-Resonator/Sol-Gel Interferometric Immunosensor

NASA Technical Reports Server (NTRS)

Bearman, Gregory; Cohen, David

2007-01-01

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

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.

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.

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

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.

Integrated optical devices based on sol – gel waveguides using the temperature dependence of the effective refractive index

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

Pavlov, S V; Trofimov, N S; Chekhlova, T K

2014-07-31

A possibility of designing optical waveguide devices based on sol – gel SiO{sub 2} – TiO{sub 2} films using the temperature dependence of the effective refractive index is shown. The dependences of the device characteristics on the parameters of the film and opticalsystem elements are analysed. The operation of a temperature recorder and a temperature limiter with a resolution of 0.6 K mm{sup -1} is demonstrated. The film and output-prism parameters are optimised. (fibreoptic and nonlinear-optic devices)

Chemistry and Processing of Nanostructured Materials

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

Fox, G A; Baumann, T F; Hope-Weeks, L J

2002-01-18

Nanostructured materials can be formed through the sol-gel polymerization of inorganic or organic monomer systems. For example, a two step polymerization of tetramethoxysilane (TMOS) was developed such that silica aerogels with densities as low as 3 kg/m{sup 3} ({approx} two times the density of air) could be achieved. Organic aerogels based upon resorcinol-formaldehyde and melamine-formaldehyde can also be prepared using the sol-gel process. Materials of this type have received significant attention at LLNL due to their ultrafine cell sizes, continuous porosity, high surface area and low mass density. For both types of aerogels, sol-gel polymerization depends upon the transformation ofmore » these monomers into nanometer-sized clusters followed by cross-linking into a 3-dimensional gel network. While sol-gel chemistry provides the opportunity to synthesize new material compositions, it suffers from the inability to separate the process of cluster formation from gelation. This limitation results in structural deficiencies in the gel that impact the physical properties of the aerogel, xerogel or nanocomposite. In order to control the properties of the resultant gel, one should be able to regulate the formation of the clusters and their subsequent cross-linking. Towards this goal, we are utilizing dendrimer chemistry to separate the cluster formation from the gelation so that new nanostructured materials can be produced. Dendrimers are three-dimensional, highly branched macromolecules that are prepared in such a way that their size, shape and surface functionality are readily controlled. The dendrimers will be used as pre-formed clusters of known size that can be cross-linked to form an ordered gel network.« less

Aptamer entrapment in microfluidic channel using one-step sol-gel process, in view of the integration of a new selective extraction phase for lab-on-a-chip.

PubMed

Perréard, Camille; d'Orlyé, Fanny; Griveau, Sophie; Liu, Baohong; Bedioui, Fethi; Varenne, Anne

2017-10-01

There is a great demand for integrating sample treatment into μTASs. In this context, we developed a new sol-gel phase for extraction of trace compounds in complex matrices. For this purpose, the incorporation of aptamers in silica-based gel within PDMS/glass microfluidic channels was performed for the first time by a one-step sol-gel process. The effective gel attachment onto microchannel walls and aptamer incorporation in the polymerized gel were evaluated using fluorescence microscopy. A good gel stability and aptamer incorporation inside the microchannel was demonstrated upon rinsing and over storage time. The ability of gel-encapsulated aptamers to interact with its specific target (either sulforhodamine B as model fluorescent target, or diclofenac, a pain killer drug) was assessed too. The binding capacity of entrapped aptamers was quantified (in the micromolar range) and the selectivity of the interaction was evidenced. Preservation of aptamers binding affinity to target molecules was therefore demonstrated. Dissociation constant of the aptamer-target complex and interaction selectivity were evaluated similar to those in bulk solution. This opens the way to new selective on-chip SPE techniques for sample pretreatment. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

Anti-adhesive effect of poloxamer-based thermo-sensitive sol-gel in rabbit laminectomy model.

PubMed

Shin, Sung Joon; Lee, Jae Hyup; So, Jungwon; Min, Kyungdan

2016-11-01

Poloxamer-based thermo-sensitive sol-gel has been developed to reduce the incidence of postoperative scar formation at the laminectomy site. The purpose of this study was to evaluate the anti-adhesive effect of poloxamer based thermo-sensitive sol-gel compared to hyaluronate based solution after laminectomy, using a rabbit model. A thermo-sensitive anti-adhesive with a property of sol-gel transition was manufactured by a physical mixture of Poloxamer188/407, Chitosan and Gelatin. The viscosity in different temperatures was assessed. 72 adult New Zealand rabbits underwent lumbar laminectomy and were randomly divided into experimental (treated with the newly developed agent), positive (treated with hyaluronate based solution), and negative control groups. Each group was subdivided into 1 and 4-week subgroups. Gross and histological evaluations were performed to assess the extent of epidural adhesion. The experimental group showed significantly higher viscosity compared to the positive control group and showed a significant increase of viscosity as the temperature increased. Gross evaluation showed no statistically significant differences between the 1- and 4-week subgroups. However, histologic evaluation showed significant differences both in 1- and 4-week subgroups. Although the 4-week histologic results of the experimental and the positive control subgroups showed no significant difference, both subgroups revealed higher value compared to the negative control subgroup with regard to the ratio of adhesion less than 50 %. The new poloxamer based thermo-sensitive agent showed superior efficacy over the hyaluronate based agent at 1 week postoperatively. At 4 weeks postoperatively, there were no statistically significant differences between the two agents, although both showed efficacy over the sham group.

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

NASA Astrophysics Data System (ADS)

Yadav, Reeta

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

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.

Sol-Gel Deposited Double Layer TiO₂ and Al₂O₃ Anti-Reflection Coating for Silicon Solar Cell.

PubMed

Jung, Jinsu; Jannat, Azmira; Akhtar, M Shaheer; Yang, O-Bong

2018-02-01

In this work, the deposition of double layer ARC on p-type Si solar cells was carried out by simple spin coating using sol-gel derived Al2O3 and TiO2 precursors for the fabrication of crystalline Si solar cells. The first ARC layer was created by freshly prepared sol-gel derived Al2O3 precursor using spin coating technique and then second ARC layer of TiO2 was deposited with sol-gel derived TiO2 precursor, which was finally annealed at 400 °C. The double layer Al2O3/TiO2 ARC on Si wafer exhibited the low average reflectance of 4.74% in the wavelength range of 400 and 1000 nm. The fabricated solar cells based on double TiO2/Al2O3 ARC attained the conversion efficiency of ~13.95% with short circuit current (JSC) of 35.27 mA/cm2, open circuit voltage (VOC) of 593.35 mV and fill factor (FF) of 66.67%. Moreover, the fabricated solar cells presented relatively low series resistance (Rs) as compared to single layer ARCs, resulting in the high VOC and FF.

The Effect of Poly (Glycerol Sebacate) Incorporation within Hybrid Chitin-Lignin Sol-Gel Nanofibrous Scaffolds.

PubMed

Abudula, Tuerdimaimaiti; Gzara, Lassaad; Simonetti, Giovanna; Alshahrie, Ahmed; Salah, Numan; Morganti, Pierfrancesco; Chianese, Angelo; Fallahi, Afsoon; Tamayol, Ali; Bencherif, Sidi A; Memic, Adnan

2018-03-19

Chitin and lignin primarily accumulate as bio-waste resulting from byproducts of crustacean crusts and plant biomass. Recently, their use has been proposed for diverse and unique bioengineering applications, amongst others. However, their weak mechanical properties need to be improved in order to facilitate their industrial utilization. In this paper, we fabricated hybrid fibers composed of a chitin-lignin (CL)-based sol-gel mixture and elastomeric poly (glycerol sebacate) (PGS) using a standard electrospinning approach. Obtained results showed that PGS could be coherently blended with the sol-gel mixture to form a nanofibrous scaffold exhibiting remarkable mechanical performance and improved antibacterial and antifungal activity. The developed hybrid fibers showed promising potential in advanced biomedical applications such as wound care products. Ultimately, recycling these sustainable biopolymers and other bio-wastes alike could propel a "greener" economy.

Sol-Gel Thin Films for Plasmonic Gas Sensors

PubMed Central

Della Gaspera, Enrico; Martucci, Alessandro

2015-01-01

Plasmonic gas sensors are optical sensors that use localized surface plasmons or extended surface plasmons as transducing platform. Surface plasmons are very sensitive to dielectric variations of the environment or to electron exchange, and these effects have been exploited for the realization of sensitive gas sensors. In this paper, we review our research work of the last few years on the synthesis and the gas sensing properties of sol-gel based nanomaterials for plasmonic sensors. PMID:26184216

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.

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.

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.

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.

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.

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

PubMed Central

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

2017-01-01

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

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

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

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.

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.

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.

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%.

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.

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 .

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.

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.

Self-organized micro-holes on titania based sol-gel films under continuous direct writing with a continuous wave ultraviolet laser

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

Bakhti, S.; Destouches, N.; Gamet, E.

The microstructuring of titania based sol-gel films is investigated by direct writing with a continuous wave ultraviolet laser beam emitting at 244 nm. Depending on the exposure conditions, the films exhibit a volume expansion, a volume shrinkage, a self-shaped delamination, or are damaged. This paper is mainly focused on the regime where spontaneous local delamination occurs, which corresponds to a narrow range of laser irradiances and writing speeds. In this regime, self-organized round-shape micro-holes opened on the substrate are generated.

Luminescent and scintillation properties of composites based on sol-gel SiO2 matrices and organic scintillators

NASA Astrophysics Data System (ADS)

Vyagin, O. G.; Bespalova, I. I.; Masalov, A. A.; Zelenskaya, O. V.; Tarasov, V. A.; Malyukin, Yu. V.

2014-11-01

Luminescent composites based on SiO2 matrices synthesized using the sol-gel method and organic scintillators PPO and o-POPOP are produced, and their optical, luminescent, and scintillation characteristics are studied. It is shown that these composites generate an intense photoluminescence signal, possess a nanosecond decay time, and have a transparency in the range of 400-700 nm of no less than 70%. The absolute light output during excitation by α radiation with an energy of 5.46 MeV is 4400-5100 photon/MeV, and the amplitude resolution is 27-32%.

Investigation of the surface morphology of biocompatible chitosan-based hydrogels and xerogels

NASA Astrophysics Data System (ADS)

Zhuravleva, Yulia Yu.; Malinkina, Olga N.; Shipovskaya, Anna B.

2018-04-01

Our biocompatible hydrogel systems obtained by the sol-gel technqiue and based on chitosan and silicon polyolates are promising for medical and biological applications. The surface microrelief of these sol-gel materials (hydrogels and xerogels) based on chitosan and silicon tetraglycerolate was explored by AFM and SEM. A significant influence of the component ratio in the mixed system on the morphology and surface profile of the hydrogels and xerogels prepared therefrom was established. An increased content of the structure-forming component (chitosan) in the system was shown to increase the roughness scale of the hydrogel surface and to promote the porosity of the xerogel structure.

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

Reversible sol-to-gel transformation of uracil gelators: specific colorimetric and fluorimetric sensor for fluoride ions.

PubMed

Xing, Ling-Bao; Yang, Bing; Wang, Xiao-Jun; Wang, Jiu-Ju; Chen, Bin; Wu, Qianhong; Peng, Hui-Xing; Zhang, Li-Ping; Tung, Chen-Ho; Wu, Li-Zhu

2013-03-05

A new type of anthracene organogelator based on uracil was obtained using organic aromatic solvents, cyclohexane, DMSO, ethanol, and ethyl acetate. It was further characterized by field-emission scanning electron microscopy and transmission electron microscopy. Specifically, the resulting organogels were demonstrated to be promising colorimetric and fluorescent sensors toward fluoride ions with high sensitivity and selectivity, accompanying the disruption of the gelators. Spectroscopic study and (1)H NMR titration experiment revealed that the deprotonation of the hydrogen atom on the N position of uracil moiety by fluoride ions is responsible for the recognition events, evidenced by immediate transformation from the sol phase to the gel state upon adding a small amount of a proton solvent, methanol. The process is reversible, with zero loss in sensing activity and sol-to-gel transformation ability even after five runs.

Sol-gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

NASA Astrophysics Data System (ADS)

Kareiva, Simonas; Klimavicius, Vytautas; Momot, Aleksandr; Kausteklis, Jonas; Prichodko, Aleksandra; Dagys, Laurynas; Ivanauskas, Feliksas; Sakirzanovas, Simas; Balevicius, Vytautas; Kareiva, Aivaras

2016-09-01

Aqueous sol-gel chemistry route based on ammonium-hydrogen phosphate as the phosphorus precursor, calcium acetate monohydrate as source of calcium ions, and 1,2-ethylendiaminetetraacetic acid (EDTA), or 1,2-diaminocyclohexanetetracetic acid (DCTA), or tartaric acid (TA), or ethylene glycol (EG), or glycerol (GL) as complexing agents have been used to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, CHAp). The phase transformations, composition, and structural changes in the polycrystalline samples were studied by infrared spectroscopy (FTIR), X-ray powder diffraction analysis (XRD), and scanning electron microscopy (SEM). The local short-range (nano- and mezo-) scale effects in CHAp were studied using solid-state NMR spectroscopy. The spatial 3D data from the SEM images of CHAp samples obtained by TA, EG and GL sol-gel routes were recovered for the first time to our knowledge.

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.

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 sol–gel deposition or by plasma-enhanced chemical vapor deposition. This paper describes in situ sol–gel deposition of hybrid inorganic/organic thin films on wood substrates using...

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%.

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.

Spatiotemporal control of synergistic gel disintegration consisting of boroxole- and glyco-based polymers via photoinduced proton transfer.

PubMed

Kotsuchibashi, Yohei; Ebara, Mitsuhiro; Sato, Takeshi; Wang, Yinan; Rajender, Rajender; Hall, Dennis G; Narain, Ravin; Aoyagi, Takao

2015-02-12

We demonstrate here a local- and remote-control of gel disintegration by using photoinduced proton transfer chemistry of photoacid generator (PAG). The gels were prepared by simply mixing two polymers, poly(N-isopropylacrylamide-co-5-methacrylamido-1,2-benzoxaborole) (P(NIPAAm-co-MAAmBO)) and poly(3-gluconamidopropyl methacrylamide) (PGAPMA) via the synergistic interaction of benzoxaborole and diol groups. The o-nitrobenzaldehyde (o-NBA) was then loaded into the gel as a PAG. The benzoxaborole-diol interaction was successfully disintegrated upon UV irradiation due to the local pH decrease inside the gel. When the gel was irradiated to a specific gel region, the synergistic interactions were disintegrated only at the exposed region. Of special interest is that the whole material eventually transitioned from gel to sol state, as the generated protons diffused gradually toward the nonilluminated region. The ability of the proposed gel-sol transition system via photoinduced proton diffusion may be beneficial for not only prompt pH changes within the gel but also the design of predictive and programmable devices for drug delivery.

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

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.

Molecularly imprinted sol-gel nanofibers based solid phase microextraction coupled on-line with high performance liquid chromatography for selective determination of acesulfame.

PubMed

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

2015-03-01

Sol-gel based molecularly imprinted polymer (MIP) nanofiber was successfully fabricated by electrospinning technique on the surface of a stainless steel bar. The manufactured tool was applied for on-line selective solid phase microextraction (SPME) and determination of acesulfame (ACF) as an artificial sweetener with high performance liquid chromatography (HPLC). The selective ability of method for the extraction of ACF was investigated in the presence of some selected sweeteners such as saccharine (SCH), aspartame (ASP) and caffeine (CAF). Electrospinning of MIP sol-gel solution on the stainless steel bar provided an unbreakable sorbent with high thermal, mechanical, and chemical stability. Moreover, application of the MIP-SPME tool revealed a unique approach for the selective microextraction of the analyte in beverage samples. In this work, 3-(triethoxysilyl)-propylamine (TMSPA) was chosen as a precursor due to its ability to imprint the analyte by hydrogen bonding, Van der Walls, and dipole-dipole interactions. Nylon 6 was also added as a backbone and support for the precursor in which sol could greatly growth during the sol-gel process and makes the solution electrospinable. Various effective parameters in the extraction efficiency of the MIP-SPME tool such as loading time, flow rate, desorption time, selectivity, and the sample volume were evaluated. The linearity for the ACF in beverage sample was in the range of 0.78-100.5 ng mL(-1). Limit of detection (LOD) and quantification (LOQ) were 0.23 and 0.78 ng mL(-1) respectively. The RSD values (n=5) were all below 3.5%at the 20 ng mL(-1) level. Copyright © 2014 Elsevier B.V. All rights reserved.

Poly(aniline) nanowires in sol-gel coated ITO: A pH-responsive substrate for planar supported lipid bilayers

PubMed Central

Ge, Chenhao; Orosz, Kristina S.; Armstrong, Neal R.; Saavedra, S. Scott

2011-01-01

Facilitated ion transport across an artificial lipid bilayer coupled to a solid substrate is a function common to several types of bioelectronic devices based on supported membranes, including biomimetic fuel cells and ion channel biosensors. Described here is fabrication of a pH-sensitive transducer composed of a porous sol-gel layer derivatized with poly(aniline) (PANI) nanowires grown from an underlying planar indium-tin oxide (ITO) electrode. The upper sol-gel surface is hydrophilic, smooth, and compatible with deposition of a planar supported lipid bilayer (PSLB) formed via vesicle fusion. Conducting tip AFM was used to show that the PANI wires are connected to the ITO, which convert this electrode into a potentiometric pH sensor. The response to changes in the pH of the buffer contacting the PANI nanowire/sol-gel/ITO electrode is blocked by the very low ion permeability of the overlying, fluid PSLB. The feasibility of using this assembly to monitor facilitated proton transport across the PSLB was demonstrated by doping the membrane with lipophilic ionophores that respond to a transmembrane pH gradient, which produced an apparent proton permeability several orders of magnitude greater than values measured for undoped lipid bilayers. PMID:21707069

Amperometric detector for gas chromatography based on a silica sol-gel solid electrolyte.

PubMed

Steinecker, William H; Miecznikowski, Krzysztof; Kulesza, Pawel J; Sandlin, Zechariah D; Cox, James A

2017-11-01

An electrochemical cell comprising a silica sol-gel solid electrolyte, a working electrode that protrudes into a gas phase, and reference and counter electrodes that contact the solid electrolyte comprises an amperometric detector for gas chromatography. Under potentiostatic conditions, a current related to the concentration of an analyte in the gas phase is produced by its oxidation at the three-phase boundary among the sol-gel, working electrode, and the gas phase. The sol-gel is processed to contain an electrolyte that also serves as a humidistat to maintain a constant water activity even in the presence the gas chromatographic mobile phase. Response was demonstrated toward a diverse set of analytes, namely hydrogen, 1,2-ethandithiol, phenol, p-cresol, and thioanisole. Using flow injection amperometry of hydrogen with He as the carrier gas, 90% of the steady-state current was achieved in < 1s at a flow rate of 20mLmin -1 . A separation of 1,2-ethandithiol, phenol, p-cresol, and thioanisole at a 2.2mLmin -1 flow rate was achieved with respective detection limits (k = 3 criterion) of 4, 1, 3, and 70 ppmv when the working electrode potential was 800mV. Copyright © 2017 Elsevier B.V. All rights reserved.

Surface and biological evaluation of hydroxyapatite-based coatings on titanium deposited by different techniques.

PubMed

Massaro, C; Baker, M A; Cosentino, F; Ramires, P A; Klose, S; Milella, E

2001-01-01

Hydroxyapatite coatings have been deposited on titanium cp by plasma spray, sol-gel, and sputtering techniques for dental implant applications. The latter two techniques are of current interest, as they allow coatings of micrometer dimensions to be deposited. Coating morphology, composition, and structure have been investigated by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). All coatings were homogeneous and exhibited a rough morphology suitable for implant applications. The sputtered (after annealing), plasma spray, and sol-gel coatings all showed diffraction peaks corresponding to hydroxyapatite. The surface contaminants were observed to be different for the different coating types. The sputtered coatings were found to have a composition most similar to hydroxyapatite; the sol-gel deposits also showed a high concentration of hydroxyl ions. A discrepancy in the Ca/P ratio was observed for the plasma spray coatings, and a small concentration of carbonate ions was found in the sputter-deposited coatings. The in vitro cell-culture studies using MG63 osteoblast-like cells demonstrated the ability of cells to proliferate on the materials tested. The sol-gel coating promotes higher cell growth, greater alkaline phosphatase activity, and greater osteocalcin production compared to the sputtered and plasma-sprayed coatings. Copyright 2001 John Wiley & Sons, Inc.

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.

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.

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).

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.

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.

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.

Molecular interactions in high conductive gel electrolytes based on low molecular weight gelator.

PubMed

Bielejewski, Michał; Łapiński, Andrzej; Demchuk, Oleg

2017-03-15

Organic ionic gel (OIG) electrolytes, also known as gel electrolytes or ionogels are one example of modern functional materials with the potential to use in wide range of electrochemical applications. The functionality of OIGs arises from the thermally reversible solidification of electrolytes or ionic liquids and their superior ionic conductivity. To understand and to predict the properties of these systems it is important to get the knowledge about the interactions on molecular level between the solid gelator matrix and the electrolyte solution. This paper reports the spectroscopic studies (FT-IR, UV-Vis and Raman) of the gel electrolyte based on low molecular weight gelator methyl-4,6-O-(p-nitrobenzylidene)-α-d-glucopyranoside and solution of quaternary ammonium salt, tetramethylammonium bromide. The solidification process was based on sol-gel technique. Below characteristic temperature, defined as gel to sol phase transition temperature, T gs , the samples were solid-like and showed high conductivity values of the same order as observed for pure liquid electrolytes. The investigations were performed for a OIGs in a wide range of molar concentrations of the electrolyte solution. Copyright © 2016 Elsevier Inc. All rights reserved.

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.

Dual controlled release, in situ gelling periodontal sol of metronidazole benzoate and serratiopeptidase: statistical optimization and mechanistic evaluation.

PubMed

Kumari, Neeraj; Pathak, Kamla

2012-01-01

In situ gelling syringeable periodontal sol capable of dual controlled delivery of metronidazole benzoate and serratiopeptidase was designed based on 2(3) factorial design with drug, poloxamer 407 and aerosil as independent variables and sol gel transition characteristics, %CDR(48h) and palatability as responses. The sols had agreeable taste, were mucoadhesive, syringeable and inverted into gels at periodontal cavity temperature. F8 with optimal drug release was identified as the best formulation. The dispersion characteristics of poloxamer significantly affected the pharmacotechnical properties of the in situ gelling systems. Extra design checkpoint generated using Design Expert software 8.02 (Stat-Ease, USA) validated the experimental design. Thus a thermoreversible, in situ gelling and syringeable periodontal sol with acceptable taste characteristics that offered controlled release of metronidazole benzoate and serratiopeptidase was developed for application into the periodontal pocket. The developed optimized sol was satisfactory in terms of taste, syringeability, palatability and incorporation of serratiopeptidase as anti-inflammatory agent, has the potential of developing a therapeutically efficacious system for treatment of periodontal inflammatory anaerobic infections.

Rheological study of physical cross-linked quaternized cellulose hydrogels induced by β-glycerophosphate.

PubMed

You, Jun; Zhou, Jinping; Li, Qian; Zhang, Lina

2012-03-20

As a weak base, β-glycerophosphate (β-GP) was used to spontaneously initiate gelation of quaternized cellulose (QC) solutions at body temperature. The QC/β-GP solutions are flowable below or at room temperature but gel rapidly under physiological conditions. In order to clarify the sol-gel transition process of the QC/β-GP systems, the complex was investigated by dynamic viscoelastic measurements. The shear storage modulus (G') and loss modulus (G″) as a function of (1) concentration of β-GP (c(β-GP)), (2) concentration of QC (c(QC)), (3) degree of substitution (DS; i.e., the average number of substituted hydroxyl groups in the anhydroglucose unit) of QC, (4) viscosity-average molecular weight (M(η)) of QC, and (5) solvent medium were studied by the oscillatory rheology. The sol-gel transition temperature of QC/β-GP solutions decreased with an increase of c(QC) and c(β-GP), the M(η) of QC, and a decrease of the DS of QC and pH of the solvent. The sol-gel transition temperature and time could be easily controlled by adjusting the concentrations of QC and β-GP, M(η) and DS of QC, and the solvent medium. Gels formed after heating were irreversible; i.e., after cooling to lower temperature they could not be dissolved to become liquid again. The aggregation and entanglement of QC chains, electrostatic interaction, and hydrogen bonding between QC and β-GP were the main factors responsible for the irreversible sol-gel transition behavior of QC/β-GP systems.

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

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

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)).

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.

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.

Photonic devices based on patterning by two photon induced polymerization techniques

NASA Astrophysics Data System (ADS)

Fortunati, I.; Dainese, T.; Signorini, R.; Bozio, R.; Tagliazucca, V.; Dirè, S.; Lemercier, G.; Mulatier, J.-C.; Andraud, C.; Schiavuta, P.; Rinaldi, A.; Licoccia, S.; Bottazzo, J.; Franco Perez, A.; Guglielmi, M.; Brusatin, G.

2008-04-01

Two and three dimensional structures with micron and submicron resolution have been achieved in commercial resists, polymeric materials and sol-gel materials by several lithographic techniques. In this context, silicon-based sol-gel materials are particularly interesting because of their versatility, chemical and thermal stability, amount of embeddable active compounds. Compared with other micro- and nano-fabrication schemes, the Two Photon Induced Polymerization is unique in its 3D processing capability. The photopolymerization is performed with laser beam in the near-IR region, where samples show less absorption and less scattering, giving rise to a deeper penetration of the light. The use of ultrashort laser pulses allows the starting of nonlinear processes like multiphoton absorption at relatively low average power without thermally damaging the samples. In this work we report results on the photopolymerization process in hybrid organic-inorganic films based photopolymerizable methacrylate-containing Si-nanobuilding blocks. Films, obtained through sol-gel synthesis, are doped with a photo-initiator allowing a radical polymerization of methacrylic groups. The photo-initiator is activated by femtosecond laser source, at different input energies. The development of the unexposed regions is performed with a suitable solvent and the photopolymerized structures are characterized by microscopy techniques.

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.

Evaluation of cost-effective sol-gel-based sensor for monitoring of formaldehyde in workplace environment and cancer risk assessment.

PubMed

Bunkoed, Opas; Thavarungkul, Panote; Thammakhet, Chongdee; Kanatharana, Proespichaya

2013-01-01

Formaldehyde was monitored in the workplace environment of an adhesive manufacturer producing formaldehyde and urea-formaldehyde resin using a cost-effective sol-gel-based sensor. The sensor was first evaluated by comparing its performance to the conventional 2,4-dinitrophynylhydrazine-devivatization method (2,4-DNPH) followed by high-performance liquid chromatography coupled to a UV detector. The formaldehyde concentrations obtained by both techniques were not significantly different. The cost-effective sol-gel-based sensor was then used for monitoring formaldehyde levels in the laboratories, production areas and storage room. Formaldehyde concentrations in this adhesive manufacturer workplace environment were lower than the limit value of, 0.75 ppm for an 8-h time weight average and 2 ppm for a short-term exposure (15 min). However, the cancer risk for employees who worked in the laboratories, (1.7±0.7)×10(-4)-(5±2)×10(-4), were higher than the acceptable cancer risk recommended by the US EPA (10(-6)). Therefore, some precaution should be taken to reduce the risk, such as an increase of ventilation to dilute the levels of formaldehyde and use air cleaners to remove formaldehyde.

Sol-gel antireflective coating on plastics

DOEpatents

Ashley, C.S.; Reed, S.T.

1988-01-26

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

Effect of ethanol variation on the internal environment of sol-gel bulk and thin films with aging.

PubMed

Gupta, R; Mozumdar, S; Chaudhury, N K

2005-10-15

Sol-gel derived bulk and thin films were prepared from different compositions at low pH ( approximately 2.0) containing varying concentrations of ethanol from 15 to 60% at constant water (H(2)O)/tetraethyl-orthosilicate (TEOS) ratio (R=4). The fluorescence microscopic and spectroscopic measurements on fluorescent probe, Hoechst 33258 (H258) entrapped in these compositions were carried out at different days of storage to monitor the effects of concentration of ethanol on the internal environment of sol-gel materials. Fluorescence microscopic observations on sol-gel thin films, prepared by dip coating technique depicted uniform and cracked surface at withdrawal speed 1cm/min (high speed) and 0.1cm/min (low speed) respectively, which did not change during aging. Fluorescence spectral measurements showed emission maximum of H258 at approximately 535 nm in fresh sols at all concentrations of ethanol which depicted slight blue shift to 512 nm during aging in bulk. No such spectral shift has been observed in sol-gel thin films coated at high speed whereas thin films coated at low speed clearly showed an additional band at approximately 404 nm at 45 and 60% concentration of ethanol after about one month of storage. Analysis of the fluorescence lifetime data indicated single exponential decay (1.6-1.8 ns) in fresh sol and from third day onwards, invariably double exponential decay with a short (tau(1)) and a long (tau(2)) component were observed in sol-gel bulk with a dominant tau(1) at approximately 1.2 ns at all concentrations of ethanol. A double exponential decay consisting of a short component (tau(1)) at approximately 0.2 ns and a long component (tau(2)) at approximately 3.5 ns were observed at all ethanol concentrations in both fresh and aged sol-gel thin films. Further, distribution analysis of lifetimes of H258 showed two mean lifetimes with increased width in aged bulk and thin films. These results are likely to have strong implications in designing the internal environment for applications in biosensors.

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.

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

THE MECHANISM OF THE INFLAMMATORY PROCESS : III. ELECTROPHORETIC MIGRATION OF INERT PARTICLES AND BLOOD CELLS IN GELATIN SOLS AND GELS WITH REFERENCE TO LEUCOCYTE EMIGRATION THROUGH THE CAPILLARY WALL.

PubMed

Abramson, H A

1928-07-20

1. Quartz particles and certain other particles move cataphoretically in certain soft gelatin gels, with the same velocity as in the sol. The speed is a function of the true viscosity of the sol or gel, and it is See PDF for Structure apparently not altered in these soft gels by the presence of gel structure. It is proportional to the applied difference of potential. 2. This finding is compatible with the fact that certain sols undergo gelation with no increase of the true viscosity although a marked change in the apparent viscosity takes place. 3. Red cells in soft gelatin-serum gels show a distinct difference in behavior. They migrate through the sol or gel with a speed that is about twice as great as the leucocytes and quartz particles, which latter particles migrate with the same velocity. This ratio has been found to hold for serum and plasma. The absolute velocities are comparatively slightly decreased by the presence of the gel. 4. In more concentrated or stiffer gels, leucocytes, red cells and quartz particles all move at first with the same velocity. By producing mechanical softening of these gels (shearing from cataphoretic movement of the micells within the cell) the red cells presently resume their previous property of independent migration through the gel. 5. The movements of particles in gelatin gels produced by a magnetic force or the force of gravity are of a different nature than those movements produced by cataphoresis. 6. The mechanical nature of obstruction to the cataphoretic migration of leucocytes and red cells in fibrin gels is briefly described. 7. The correlation of cataphoresis of microscopic particles in gels with the order of magnitude and nature of the potential differences in the capillary wall, lends additional evidence to the theory that polymorphonuclear leucocyte emigration and migration are dependent upon these potential differences.

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

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

PubMed Central

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

2016-01-01

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. PMID:28773848

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.

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

PubMed

Alqasaimeh, Muawia Salameh; Heng, Lee Yook; Ahmad, Musa

2007-10-11

An optical urea biosensor was fabricated by stacking several layers of sol-gelfilms. The stacking of the sol-gel films allowed the immobilization of a Nile Bluechromoionophore (ETH 5294) and urease enzyme separately without the need of anychemical attachment procedure. The absorbance response of the biosensor was monitoredat 550 nm, i.e. the deprotonation of the chromoionophore. This multi-layer sol-gel filmformat enabled higher enzyme loading in the biosensor to be achieved. The urea opticalbiosensor constructed from three layers of sol-gel films that contained urease demonstrateda much wider linear response range of up to 100 mM urea when compared with biosensorsthat constructed from 1-2 layers of films. Analysis of urea in urine samples with thisoptical urea biosensor yielded results similar to that determined by a spectrophotometricmethod using the reagent p-dimethylaminobenzaldehyde (R² = 0.982, n = 6). The averagerecovery of urea from urine samples using this urea biosensor is approximately 103%.

Sol-gel antireflective coating on plastics

DOEpatents

Ashley, Carol S.; Reed, Scott T.

1990-01-01

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

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.

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.

Synthesis of superhydrophobic alumina membrane: Effects of sol-gel coating, steam impingement and water treatment

NASA Astrophysics Data System (ADS)

Ahmad, N. A.; Leo, C. P.; Ahmad, A. L.

2013-11-01

Ceramic membranes possess natural hydrophilicity thus tending to absorb water droplets. The absorption of water molecules on membrane surface reduces their application in filtration, membrane distillation, osmotic evaporation and membrane gas absorption. Fluoroalkylsilane (FAS) grafting allows the conversion of hydrophilic ceramic membranes into superhydrophobic thin layer, but it usually introduces a great increment of mass transfer resistance. In this study, superhydrophobic alumina membranes were synthesized by dip coating alumina support into sol-gel and grafted with the fluoroalkylsilane (FAS) named (heptadecafluoro-1,1,2,2-tetra hydrodecyl) triethoxysilane. Steam impingement and water treatment acted as additional steps to generate surface roughness on sol-gel and most importantly to reduce mass transfer resistance. Superhydrophobic alumina membrane with high water contact angle (158.4°) and low resistance (139.5 ± 24.9 G m-1) was successfully formed when the alumina membrane was dip coated into sol-gel for 7 s, treated with steam impingement for 1 min and immersed in hot water at 100 °C. However, the mass transfer resistance was greatly induced to 535.6 ± 23.5 G m-1 when the dip coating time was increased to 60 s. Long dip coating time contributes more on the blockage of porous structure rather than creates a thin film on the top of membrane surface. Reducing the pore size and porosity significantly due to increase of coating molecules deposited on the membrane. Steam impingement for 1 min promoted the formation of cones and valleys on the sol-gel, but the macro-roughness was destroyed when the steam impingement duration was extended to more than 3 min. The immersions of membranes into hot water at temperatures higher than 60 °C encouraged the formation of boehmite which enhances the formation of additional roughness and enlarges pore size greatly. Thus, this work showed that the formation of superhydrophobic alumina membrane with low resistance is influenced by three factors; sol-gel dip coating time, steam impingement time and temperature of water treatment. The optimum dip coating time could promote appropriate thickness of the sol-gel layer on the membrane support. The highest surface roughness and porosity could be created when the sol-gel layer was further treated with optimum steam impingement duration and immersed in hot water at 100 °C. The presence of appropriate sol-gel thickness can reduce the penetration of FAS during the grafting and reduce the membrane resistance.

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.

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.

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.

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.

A Comparative Study of Phosphoric Acid-doped m-PBI Membranes

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

Perry, Kelly A; More, Karren Leslie; Payzant, E Andrew

2014-01-01

Phosphoric acid (PA)-doped m-polybenzimidazole (PBI) membranes used in high temperature fuel cells and hydrogen pumps were prepared by a conventional imbibing process and a sol-gel fabrication process. A comparative study was conducted to investigate the critical properties of PA doping levels, ionic conductivities, mechanical properties, and molecular ordering. This systematic study found that sol-gel PA-doped m-PBI membranes were able to absorb higher acid doping levels and to achieve higher ionic conductivities than conventionally imbibed membranes when treated in an equivalent manner. Even at similar acid loadings, the sol-gel membranes exhibited higher ionic conductivities. Heat treatment of conventionally imbibed membranes withmore » 29wt% solids caused a significant reduction in mechanical properties; conversely, sol-gel membranes exhibited an enhancement in mechanical properties. From X-ray structural studies and atomistic simulations, both conventionally imbibed and sol-gel membranes exhibited d-spacings of 3.5 and 4.6 , which were tentatively attributed to parallel ring stacking and staggered side-to-side packing, respectively, of the imidazole rings in these aromatic hetercyclic polymers. An anisotropic staggered side-to-side chain packing present in the conventional membranes may be root to the reduction in mechanical properties.« less

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.

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

PubMed

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

2017-12-19

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

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.

Sol-gel immobilization as a suitable technique for enhancement of α-amylase activity of Aspergillus oryzae PP.

PubMed

Evstatieva, Yana; Yordanova, Mariya; Chernev, Georgi; Ruseva, Yanislava; Nikolova, Dilyana

2014-07-04

Bioencapsulation of microbial cells in silica-based matrices has proved to be a good strategy to enhance the biosynthetic capabilities and viability of bioproducers. In the present study, mycelium and pellet cultures of strain Aspergillus oryzae PP were successfully immobilized in sol-gel hybrid matrices composed of tetraethylorthosilicate as an inorganic precursor, 5% (w/v) starch and 10 or 15% (w/v) polyethylene oxide, or 10% (w/v) calcium alginate as organic compounds. Biosynthetic activity of immobilized cultures was investigated by batch and fed-batch cultivation and the obtained results of 3042.04 IU cm -3 were comparable with the enzyme activity of the free cell culture. Immobilized cultures retained their viability and biosynthetic capabilities up to the 744th h during fed-batch fermentation processes. Consequently, sol-gel encapsulation in hybrid matrices could be considered as a promising technique for immobilization of Aspergillus oryzae PP in order to increase the α-amylase production.

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.

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.

Hybrid sol-gel planar optics for astronomy.

PubMed

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

2009-02-02

Hybrid sol-gel planar optics devices for astronomy are produced for the first time. This material system can operate from the visible (0.5 microm) up to the edge of astronomical J-band (1.4 microm). The design, fabrication and characterization results of a coaxial three beam combiner are given as an example. Fringe contrasts above 94% are obtained with a source with spectral bandwidth of 50 nm. These results demonstrate that hybrid sol-gel technology can produce devices with high quality, opening the possibility of rapid prototyping of new designs and concepts for astronomical applications.

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

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.

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

PubMed

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

2012-12-18

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

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.

Preparation and Characterisation of Hydroxyapatite Coatings on Nanotubular TiO2 Surface Obtained by Sol-Gel Process.

PubMed

Shin, Jin-Ho; Kim, Jung-Hwa; Koh, Jeong-Tae; Lim, Hyun-Pil; Oh, Gye-Jeong; Lee, Seok-Woo; Lee, Kwang-Min; Yun, Kwi-Dug; Park, Sang-Won

2015-08-01

Hydroxyapatite (HA) coating on titanium dioxide (TiO2) nanotubular surface has been developed to complement the defects of both TiO2 and HA. A sol-gel processing technique was used to coat HA on TiO2 nanotubular surface. All the titanium discs were blasted with resorbable blast media (RBM). RBM-blasted Ti surface, anodized Ti surface, and sol-gel HA coating on the anodized Ti surface were prepared. The characteristics of samples were observed using scanning electron microscopy and X-ray photoemission spectroscopy. Biologic responses were evaluated with human osteosarcoma MG63 cells in vitro. The top of the TiO2 nanotubes was not completely covered by HA particles when the coating time was less than 60 sec. It was demonstrated the sol-gel derived HA film was well-crystallized and this enhanced biologic responses in early stage cell response.

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.

Controlled Sol-Gel Transitions of a Thermoresponsive Polymer in a Photoswitchable Azobenzene Ionic Liquid as a Molecular Trigger.

PubMed

Wang, Caihong; Hashimoto, Kei; Tamate, Ryota; Kokubo, Hisashi; Watanabe, Masayoshi

2018-01-02

Producing ionic liquids (ILs) that function as molecular trigger for macroscopic change is a challenging issue. Photoisomerization of an azobenzene IL at the molecular level evokes a macroscopic response (light-controlled mechanical sol-gel transitions) for ABA triblock copolymer solutions. The A endblocks, poly(2-phenylethyl methacrylate), show a lower critical solution temperature in the IL mixture containing azobenzene, while the B midblock, poly(methyl methacrylate), is compatible with the mixture. In a concentrated polymer solution, different gelation temperatures were observed in it under dark and UV conditions. Light-controlled sol-gel transitions were achieved by a photoresponsive solubility change of the A endblocks upon photoisomerization of the azobenzene IL. Therefore, an azobenzene IL as a molecular switch can tune the self-assembly of a thermoresponsive polymer, leading to macroscopic light-controlled sol-gel transitions. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Luminescence of Eu(3+) doped SiO2 Thin Films and Glass Prepared by Sol-gel Technology

NASA Technical Reports Server (NTRS)

Castro, Lymari; Jia, Weiyi; Wang, Yanyun; Santiago, Miguel; Liu, Huimin

1998-01-01

Trivalent europium ions are an important luminophore for lighting and display. The emission of (5)D0 to (7)F2 transition exhibits a red color at about 610 nm, which is very attractive and fulfills the requirement for most red-emitting phosphors including lamp and cathode ray phosphorescence materials. Various EU(3+) doped phosphors have been developed, and luminescence properties have been extensively studied. On the other hand, sol-gel technology has been well developed by chemists. In recent years, applications of this technology to optical materials have drawn a great attention. Sol-gel technology provides a unique way to obtain homogeneous composition distribution and uniform doping, and the processing temperature can be very low. In this work, EU(3+) doped SiO2 thin films and glasses were prepared by sol-gel technology and their spectroscopic properties were investigated.

Tantalum-tungsten oxide thermite composites prepared by sol-gel synthesis and spark plasma sintering

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

Kuntz, Joshua D.; Gash, Alexander E.; Cervantes, Octavio G.

2010-08-15

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

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

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

Cervantes, O; Kuntz, J; Gash, A

2009-02-13

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

L-Phenylalanine functionalized silver nanoparticles: Photocatalytic and nonlinear optical applications

NASA Astrophysics Data System (ADS)

Nidya, M.; Umadevi, M.; Sankar, Pranitha; Philip, Reji; Rajkumar, Beulah J. M.

2015-04-01

An extensive study on the behavior of L-Phenylalanine capped silver nanoparticles (Phe-Ag NPs) in the aqueous phase and in a sol-gel thin film showed different UV/Vis, Transmission Electron Microscope (TEM), Dynamic Light Scattering and Zeta potential profiles. Scanning Electron Microscope (SEM) images of the samples in the sol gel film showed Ag embedded in the SiO2 matrix. Surface Enhanced Raman Spectra (SERS) confirmed that both in the aqueous media and in the sol gel film, the attachment of Phe to the Ag NP surface was through the benzene ring, with the sol-gel film showing a better enhancement. Photocatalytic degradation of crystal violet was measured spectrophotometrically using Phe-Ag NPs as a nanocatalyst under visible light illumination. Intensity-dependent nonlinear optical absorption of Phe-Ag measured using the open aperture Z-scan technique revealed that the material is an efficient optical limiter with potential applications.

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.

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.

The effect of high temperature sol-gel polymerization parameters on the microstructure and properties of hydrophobic phenol-formaldehyde/silica hybrid aerogels.

PubMed

Seraji, Mohamad Mehdi; Sameri, Ghasem; Davarpanah, Jamal; Bahramian, Ahmad Reza

2017-05-01

Phenol-formaldehyde/silica hybrid aerogels with different degree of hydrophobicity were successfully synthesized via high temperature sol-gel polymerization. Tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES) were used as precursor and co-precursor of the hydrophobic silica-based phase, respectively. The hydrolysis step of silica based sols were conducted by acid catalyzed reactions and HCl was used as hydrolysis catalyst. The chemical structure of prepared hybrid aerogels was characterized by Fourier Transform Infrared spectroscopy (FT-IR). The effect of MTES/TEOS proportion and catalyst content on the morphology and microstructure of samples were investigated by FE-SEM and C, Si mapping analysis. The acid catalyzed hydrolysis of TEOS and MTES sols leads to formation of a sol with primarily silica particles in the organic-inorganic hybrid sol and varying colloid growth mechanisms were occurred with change in MTES and HCl molar ratio. With the increasing of MTES content, the microstructure of samples changed from uniform colloidal network, core-shell structure to polymeric structure with a huge phase separation. The increasing of HCl mole fraction leads to smaller particle size. Moreover, the shrinkage of samples was decreased and water contact angles of the resulted aerogels were increased from 40 to 156.8° with the increases of MTES content. Copyright © 2017 Elsevier Inc. All rights reserved.

ZnO-based transparent conductive thin films via sonicated-assisted sol-gel technique

NASA Astrophysics Data System (ADS)

Malek, M. F.; Mamat, M. H.; Ismail, A. S.; Yusoff, M. M.; Mohamed, R.; Rusop, M.

2018-05-01

We report on the growth of Al-doped ZnO (AZO) thin films onto Corning 7740 glass substrates via sonicated-assisted sol-gel technique. The influence of Al dopant on crystallisation behavior, optical and electrical properties of AZO films has been systematically investigated. All films are polycrystalline with a hexagonal wurtzite structure with a preferential orientation according to the direction <002>. All films exhibit a transmittance above than 80-90 % along the visible range up to 800 nm and a sharp absorption onset below 400 nm corresponding to the fundamental absorption edge of ZnO.

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

NASA Astrophysics Data System (ADS)

Yasakau, Kiryl

A industria aeronautica utiliza ligas de aluminio de alta resistencia para o fabrico dos elementos estruturais dos avioes. As ligas usadas possuem excelentes propriedades mecanicas mas apresentam simultaneamente uma grande tendencia para a corrosao. Por esta razao essas ligas necessitam de proteccao anticorrosiva eficaz para poderem ser utilizadas com seguranca. Ate a data, os sistemas anticorrosivos mais eficazes para ligas de aluminio contem cromio hexavalente na sua composicao, sejam pre-tratamentos, camadas de conversao ou pigmentos anticorrosivos. O reconhecimento dos efeitos carcinogenicos do cromio hexavalente levou ao aparecimento de legislacao banindo o uso desta forma de cromio pela industria. Esta decisao trouxe a necessidade de encontrar alternativas ambientalmente inocuas mas igualmente eficazes. O principal objectivo do presente trabalho e o desenvolvimento de pretratamentos anticorrosivos activos para a liga de aluminio 2024, baseados em revestimentos hibridos produzidos pelo metodo sol-gel. Estes revestimentos deverao possuir boa aderencia ao substrato metalico, boas propriedades barreira e capacidade anticorrosiva activa. A proteccao activa pode ser alcancada atraves da incorporacao de inibidores anticorrosivos no pretratamento. O objectivo foi atingido atraves de uma sucessao de etapas. Primeiro investigou-se em detalhe a corrosao localizada (por picada) da liga de aluminio 2024. Os resultados obtidos permitiram uma melhor compreensao da susceptibilidade desta liga a processos de corrosao localizada. Estudaram-se tambem varios possiveis inibidores de corrosao usando tecnicas electroquimicas e microestruturais. Numa segunda etapa desenvolveram-se revestimentos anticorrosivos hibridos organico-inorganico baseados no metodo sol-gel. Compostos derivados de titania e zirconia foram combinados com siloxanos organofuncionais a fim de obter-se boa aderencia entre o revestimento e o substrato metalico assim como boas propriedades barreira. Testes industriais mostraram que estes novos revestimentos sao compativeis com os esquemas de pintura convencionais actualmente em uso. A estabilidade e o prazo de validade das formulacoes foram optimizados modificando a temperatura de armazenamento e a quantidade de agua usada durante a sintese. As formulacoes sol-gel foram dopadas com os inibidores seleccionados durante a primeira etapa e as propriedades anticorrosivas passivas e activas dos revestimentos obtidos foram estudadas numa terceira etapa do trabalho. Os resultados comprovam a influencia dos inibidores nas propriedades anticorrosivas dos revestimentos sol-gel. Em alguns casos a accao activa dos inibidores combinou-se com a proteccao passiva dada pelo revestimento mas noutros casos tera ocorrido interaccao quimica entre o inibidor e a matriz de sol-gel, de onde resultou a perda de propriedades protectoras do sistema combinado. Atendendo aos problemas provocados pela adicao directa dos inibidores na formulacao sol-gel procurou-se, numa quarta etapa, formas alternativas de incorporacao. Na primeira, produziu-se uma camada de titania nanoporosa na superficie da liga metalica que serviu de reservatorio para os inibidores. O revestimento sol-gel foi aplicado por cima da camada nanoporosa. Os inibidores armazenados nos poros actuam quando o substrato fica exposto ao ambiente agressivo. Numa segunda, os inibidores foram armazenados em nano-reservatorios de silica ou em nanoargilas (halloysite), os quais foram revestidos por polielectrolitos montados camada a camada. A terceira alternativa consistiu no uso de nano-fios de molibdato de cerio amorfo como inibidores anticorrosivos nanoparticulados. Os nano-reservatorios foram incorporados durante a sintese do sol-gel. Qualquer das abordagens permitiu eliminar o efeito negativo do inibidor sobre a estabilidade da matriz do sol-gel. Os revestimentos sol-gel desenvolvidos neste trabalho apresentaram proteccao anticorrosiva activa e capacidade de auto-reparacao. Os resultados obtidos mostraram o elevado potencial destes revestimentos para a proteccao anticorrosiva da liga de aluminio 2024.

The in vivo behaviour of a sol-gel glass and a glass-ceramic during critical diaphyseal bone defects healing.

PubMed

Gil-Albarova, Jorge; Salinas, Antonio J; Bueno-Lozano, Antonio L; Román, Jesus; Aldini-Nicolo, Nicolo; García-Barea, Agustina; Giavaresi, Gianluca; Fini, Milena; Giardino, Roberto; Vallet-Regí, Maria

2005-07-01

The in vivo evaluation, in New Zealand rabbits, of a sol-gel glass 70% CaO-30% SiO2 (in mol%) and a glass-ceramic obtained from thermal treatment of the glass, both bioactive in Kokubo's simulated body fluid (SBF), is presented. Femoral bone diaphyseal critical defects were filled with: (i) sol-gel glass cylinders, (ii) glass-ceramic cylinders, or (iii) no material (control group). Osteosynthesis was done by means of anterior screwed plates with an associate intramedullar Kirschner wire. Each group included 10 mature rabbits, 9 months old. Follow-up was 6 months. After sacrifice, macroscopic study showed healing of bone defects, with bone coating over the cylinders, but without evidence of satisfactory repair in control group. Radiographic study showed good implant stability and periosteal growth and bone remodelling around and over the filled bone defect. The morphometric study showed minimum evidences of degradation or resorption in glass-ceramic cylinders, maintaining its original shape, but sol-gel glass cylinders showed abundant fragmentation and surface resorption. An intimate union of the new-formed bone to both materials was observed. Mechanical study showed the higher results in the glass-ceramic group, whereas sol-gel glass and control group showed no differences. The minimum degradation of glass-ceramic cylinders suggests their application in critical bone defects locations of transmission forces or load bearing. The performance of sol-gel glass cylinders suggests their usefulness in locations where a quick resorption should be preferable, considering the possibility of serving as drug or cells vehicle for both of them.

Molecular Level Understanding of Sodium Dodecyl Sulfate (SDS) Induced Sol-Gel Transition of Pluronic F127 Using Fisetin as a Fluorescent Molecular Probe.

PubMed

Mishra, Jhili; Swain, Jitendriya; Mishra, Ashok Kumar

2018-01-11

The thermoreversible sol-gel transition of pluronic F127 is markedly altered even with addition of submicellar concentration of sodium dodecyl sulfate (SDS) surfactant. Multiple fluorescence parameters like fluorescence intensity, fluorescence anisotropy and fluorescence lifetime of both the prototropic forms (anion (A - *) and phototautomer FT*) of the photoprototropic fluorescent probe fisetin has been efficiently used to understand the molecular level properties like polarity and microviscosity of the PF127-SDS system as a function of temperature. The SDS-induced increase in the interfacial hydrophobicity level is seen to affect the sol-gel phase transition of PF127 (21-18 °C). The E T (30) polarity parameter value of anionic emission of fisetin suggests that there is a considerable decrease in the polarity of the PF127 medium with increase in temperature and with the addition of SDS. The microviscosity progressively increases from ∼5 mPa s (sol state, 10 °C) to ∼22.01 mPa s (gel state 35 °C) in aqueous solution of PF127. The variation in microviscosity with addition of SDS in PF127-SDS mixed system is significant in sol phase whereas in gel phase this variation is significantly less. Temperature dependent fluorescence lifetime of FT* indicates that there is heterogeneity in distribution of fisetin molecules at different domains of PF127. This work also show-cases the sensitivity of fisetin toward change in polarity and change in sol-gel transition temperature of copolymer PF127 with variation in temperature (both forward and reverse directions) and SDS.

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.

Effect of Parainfluenza-3 Neuraminidase on Bovine Nasal Secretion

PubMed Central

Morein, Bror; Bergman, Rune

1972-01-01

Three samples of bovine nasal secretion were each separated into a sol phase and a surface gel phase. In all samples, the gel phase contained an approximately four times greater amount of bound N-acetylneuraminic acid (NANA) than the sol phase. From the gel phase, bound NANA could be released by exposure to parainfluenza-3 virus neuraminidase. The surface gel appears to be a natural substrate for this enzyme. PMID:4347547

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

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

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

2009-02-01

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

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.

A micro oxygen sensor based on a nano sol-gel TiO2 thin film.

PubMed

Wang, Hairong; Chen, Lei; Wang, Jiaxin; Sun, Quantao; Zhao, Yulong

2014-09-03

An oxygen gas microsensor based on nanostructured sol-gel TiO2 thin films with a buried Pd layer was developed on a silicon substrate. The nanostructured titania thin films for O2 sensors were prepared by the sol-gel process and became anatase after heat treatment. A sandwich TiO2 square board with an area of 350 μm × 350 μm was defined by both wet etching and dry etching processes and the wet one was applied in the final process due to its advantages of easy control for the final structure. A pair of 150 nm Pt micro interdigitated electrodes with 50 nm Ti buffer layer was fabricated on the board by a lift-off process. The sensor chip was tested in a furnace with changing the O2 concentration from 1.0% to 20% by monitoring its electrical resistance. Results showed that after several testing cycles the sensor's output becomes stable, and its sensitivity is 0.054 with deviation 2.65 × 10(-4) and hysteresis is 8.5%. Due to its simple fabrication process, the sensor has potential for application in environmental monitoring, where lower power consumption and small size are required.

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.

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.

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

PubMed

Rashti, Ali; Yahyaei, Hossein; Firoozi, Saman; Ramezani, Sara; Rahiminejad, Ali; Karimi, Roya; Farzaneh, Khadijeh; Mohseni, Mohsen; Ghanbari, Hossein

2016-12-01

Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Anti-reflective and anti-soiling coatings with self-cleaning properties

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

Nair, Vinod; Brophy, Brenor L.

Disclosed herein is a coated glass element including a glass component and a coating adhered to the glass component through siloxane linkages, the coating having at least one of an anti-reflective property, a high abrasion resistance property and a hydrophobic property, wherein the coating comprises a dried gel formed from at least one hydrolyzed alkoxysilane-based sol and at least one hydrolyzed organosilane-based sol.

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.

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.

Porous Silica Sol-Gel Glasses Containing Reactive V2O5 Groups

NASA Technical Reports Server (NTRS)

Stiegman, Albert E.

1995-01-01

Porous silica sol-gel glasses into which reactive vanadium oxide functional groups incorporated exhibit number of unique characteristics. Because they bind molecules of some species both reversibly and selectively, useful as chemical sensors or indicators or as scrubbers to remove toxic or hazardous contaminants. Materials also oxidize methane gas photochemically: suggests they're useful as catalysts for conversion of methane to alcohol and for oxidation of hydrocarbons in general. By incorporating various amounts of other metals into silica sol-gel glasses, possible to synthesize new materials with broad range of new characteristics.

Ion-irradiation-induced densification of zirconia sol-gel thin films

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

Levine, T.E.; Giannelis, E.P.; Kodali, P.

1994-02-01

We have investigated the densification behavior of sol-gel zirconia films resulting from ion irradiation. Three sets of films were implanted with neon, krypton, or xenon. The ion energies were chosen to yield approximately constant energy loss through the film and the doses were chosen to yield similar nuclear energy deposition. Ion irradiation of the sol-gel films resulted in carbon and hydrogen loss as indicated by Rutherford backscattering spectrometry and forward recoil energy spectroscopy. Although the densification was hypothesized to result from target atom displacement, the observed densification exhibits a stronger dependence on electronic energy deposition.

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.

Ternary Phase-Separation Investigation of Sol-Gel Derived Silica from Ethyl Silicate 40

PubMed Central

Wang, Shengnan; Wang, David K.; Smart, Simon; Diniz da Costa, João C.

2015-01-01

A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification. PMID:26411484

Foldable and Cytocompatible Sol-gel TiO2 Photonics

NASA Astrophysics Data System (ADS)

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

2015-09-01

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

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.

Foldable and Cytocompatible Sol-gel TiO2 Photonics

PubMed Central

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

2015-01-01

Integrated photonics provides a miniaturized and potentially implantable platform to manipulate and enhance the interactions between light and biological molecules or tissues in in-vitro and in-vivo settings, and is thus being increasingly adopted in a wide cross-section of biomedical applications ranging from disease diagnosis to optogenetic neuromodulation. However, the mechanical rigidity of substrates traditionally used for photonic integration is fundamentally incompatible with soft biological tissues. Cytotoxicity of materials and chemicals used in photonic device processing imposes another constraint towards these biophotonic applications. Here we present thin film TiO2 as a viable material for biocompatible and flexible integrated photonics. Amorphous TiO2 films were deposited using a low temperature (<250 °C) sol-gel process fully compatible with monolithic integration on plastic substrates. High-index-contrast flexible optical waveguides and resonators were fabricated using the sol-gel TiO2 material, and resonator quality factors up to 20,000 were measured. Following a multi-neutral-axis mechanical design, these devices exhibit remarkable mechanical flexibility, and can sustain repeated folding without compromising their optical performance. Finally, we validated the low cytotoxicity of the sol-gel TiO2 devices through in-vitro cell culture tests. These results demonstrate the potential of sol-gel TiO2 as a promising material platform for novel biophotonic devices. PMID:26344823

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.

Foldable and Cytocompatible Sol-gel TiO2 Photonics.

PubMed

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

2015-09-07

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

Anisotropic growth and formation mechanism investigation of 1D ZnO nanorods in spin-coating sol-gel process.

PubMed

Song, Yijian; Zheng, Maojun; Ma, Li; Shen, Wenzhong

2010-01-01

ZnO nanorods are fabricated on glass substrate by spin-coating sol-gel process using non-basic aged solution and annealing. Sample solutions reserved in room temperature for different time (one day, one month, two months and four months) are prepared for the experiment. The morphology study indicates that the aging time has direct influence on the final products. This is verified by the Transmission Electron Microscopy and Photon Correlation Spectroscopy study. Small crystalline nanoparticles would gradually nucleate and aggregate in the sol during the aging process. They act as nucleation site for the secondary crystal growth into nanorods during anneal. Both the size of crystalline particles in the sol and the size of nanorods will grow bigger as the aging time increases. The products' structure and optical property are further studied by X-ray diffraction spectroscopy, Photoluminescence and Raman spectroscopy. This work also helps to further clarify the formation mechanism of ZnO nanorods by solution-based method.

Effect of silica coating on fracture strength of glass-infiltrated alumina ceramic cemented to dentin.

PubMed

Xie, Haifeng; Zhu, Ye; Chen, Chen; Gu, Ning; Zhang, Feimin

2011-10-01

To examine the availability of sol-gel processed silica coating for alumina-based ceramic bonding, and determine which silica sol concentration was appropriate for silica coating. Sixty disks of In-Ceram alumina ceramic were fabricated and randomly divided into 5 main groups. The disks received 5 different surface conditioning treatments: Group Al, sandblasted; Group AlC, sandblasted + silane coupling agent applied; Groups Al20C, Al30C, and Al40C, sandblasted, silica coating via sol-gel process prepared using 20 wt%, 30 wt%, and 40 wt% silica sols, and then silane coupling agent applied. Before bonding, one-step adhesives were applied on pre-prepared ceramic surfaces of all groups. Then, 60 dentin specimens were prepared and conditioned with phosphoric acid and one-step adhesive. Ceramic disks of all groups were cemented to dentin specimens with dual-curing resin cements. Fracture strength was determined at 24 h and after 20 days of storage in water. Groups Al20C, Al30C, and Al40C revealed significantly higher fracture strength than groups Al and AlC. No statistically significant difference in fracture strength was found between groups Al and AlC, or among groups Al20C, Al30C, and Al40C. Fracture strength values of all the groups did not change after 20 days of water storage. Sol-gel processed silica coating can enhance fracture strength of In-Ceram alumina ceramic after bonding to dentin, and different silica sol concentrations produced the same effects. Twenty days of water storage did not decrease the fracture strength.

Domain Engineered Magnetoelectric Thin Films for High Sensitivity Resonant Magnetic Field Sensors

DTIC Science & Technology

2012-02-28

texture E analysis w cated by poo re accounted n measurem 8 sol-gel samp d PZT sol-g as utilized t r fit between in the mo ent spot). les shown i el...nsformer str nted by aero ure. ure 34: Un were grow as varied in D) as show texturing in . D pattern of the films d ucture. Figu sol jet depo ipoled PZT ...the detailed characterization was the development of prediction models for texturing of PZT sol-gel thin films, an understanding of the analytical

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.

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.

The sol-gel template synthesis of porous TiO2 for a high performance humidity sensor

NASA Astrophysics Data System (ADS)

Wang, Zhuyi; Shi, Liyi; Wu, Fengqing; Yuan, Shuai; Zhao, Yin; Zhang, Meihong

2011-07-01

This research develops a simple template assisted sol-gel process for preparing porous TiO2 for a high performance humidity sensor. Tetraethyl orthosilicate (TEOS) as a template was directly introduced into TiO2 sol formed by the hydrolysis and condensation of titanium alkoxide; the following calcination led to the formation of TiO2-SiO2 composite, and the selective removal of SiO2 by dilute HF solution led to the formation of porous structure in TiO2. The resulting porous TiO2-based sensor exhibits high sensitivity and linear response in the wide relative humidity (RH) range of 11%-95%, with an impedance variation of four orders of magnitude to humidity change. Moreover, it exhibits a rapid and highly reversible response characterized by a very small hysteresis of < 1% RH and a short response-recovery time (5 s for adsorption and 8 s for desorption), and a 30-day stability test also confirms its long-term stability. Compared with pure TiO2 prepared by the conventional sol-gel method, our product shows remarkably improved performance and good prospect for a high performance humidity sensor. The complex impedance spectra were used to elucidate its humidity sensing mechanism in detail.

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.

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

PubMed

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

2017-06-01

Pullulanase was sol-gel encapsulated in the presence of magnetic chitosan/Fe 3 O 4 nanoparticles. The resulting immobilized pullulanase was characterized by scanning electron microscopy, vibrating sample magnetometry, Fourier transform infrared spectroscopy and thermogravimetric analysis. The results showed that the addition of pullulanase created a more regular surface on the sol-gel matrix and an enhanced magnetic response to an applied magnetic field. The maximal activity retention (83.9%) and specific activity (291.7 U/mg) of the immobilized pullulanase were observed under optimized conditions including an octyltriethoxysilane:tetraethoxysilane (OTES:TEOS) ratio of 1:2 and enzyme concentration of 0.484 mg/mL sol. The immobilized enzyme exhibited good thermal stability. When the temperature was above 60 °C, the immobilized pullulanase showed significantly higher activity than the free enzyme (p < 0.01); enzyme immobilized by simple sol-gel encapsulation and co-immobilized by crosslinking-encapsulation retained 52 and 69% of their initial activity after 5 h at 62 °C, respectively, compared to 11% for the free enzyme. Moreover, the stability of the pullulanase was improved by crosslinking-encapsulation, as the enzyme retained more than 85 and 81% of its original activity after 5 and 6 consecutive reuses, respectively, compared to 80 and 72% of its original activity for simple sol-gel encapsulated enzymes. This indicated the leakage of enzyme molecules through the pores of the gel was substantially abated by cross-linking. Such immobilized pullulanase provides high stability and ease of enzyme recovery, characteristics that are advantageous for applications in the food industry that involve continuous starch processing.

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 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.

First report of charge-transfer induced heat-set hydrogel. Structural insights and remarkable properties

NASA Astrophysics Data System (ADS)

Bhattacharjee, Subham; Maiti, Bappa; Bhattacharya, Santanu

2016-05-01

The remarkable ability of a charge-transfer (CT) complex prepared from a pyrene-based donor (Py-D) and a naphthalenediimide-based acceptor (NDI-A) led to the formation of a deep-violet in color, transparent hydrogel at room temperature (RT-gel). Simultaneously, the RT-gel was diluted beyond its critical gelator concentration (CGC) to obtain a transparent sol. Very interestingly, the resultant sol, on heating above 70 °C, transformed into a heat-set gel instantaneously with a hitherto unknown CGC value. Detailed studies revealed the smaller globular aggregates of the RT-gels fuse to form giant globules upon heating, which, in turn, resulted in heat-set gelation through further aggregation. The thermoresponsive property of Py-D alone and 1 : 1 Py-D : NDI-A CT complex was investigated in detail which revealed the hydrophobic collapse of the oxyethylene chains of the CT complex upon heating was mainly responsible for heat-set gelation. Thixotropy, injectability, as well as stimuli responsiveness of the RT-gels were also addressed. In contrast, heat-set gel did not show thixotropic behavior. The X-ray diffraction (XRD) patterns of the xerogel depicted lamellar packing of the CT stacks in the gel phase. Single crystal XRD studies further evidenced the 1 : 1 mixed CT stack formation in the lamellae and also ruled out orthogonal hydrogen bonding possibilities among the hydrazide unit in the CT gel although such interaction was observed in a single crystal of NDI-A alone. In addition, a Ag+-ion triggered metallogelation of NDI-A and nematic liquid-crystalline property of Py-D were also observed.The remarkable ability of a charge-transfer (CT) complex prepared from a pyrene-based donor (Py-D) and a naphthalenediimide-based acceptor (NDI-A) led to the formation of a deep-violet in color, transparent hydrogel at room temperature (RT-gel). Simultaneously, the RT-gel was diluted beyond its critical gelator concentration (CGC) to obtain a transparent sol. Very interestingly, the resultant sol, on heating above 70 °C, transformed into a heat-set gel instantaneously with a hitherto unknown CGC value. Detailed studies revealed the smaller globular aggregates of the RT-gels fuse to form giant globules upon heating, which, in turn, resulted in heat-set gelation through further aggregation. The thermoresponsive property of Py-D alone and 1 : 1 Py-D : NDI-A CT complex was investigated in detail which revealed the hydrophobic collapse of the oxyethylene chains of the CT complex upon heating was mainly responsible for heat-set gelation. Thixotropy, injectability, as well as stimuli responsiveness of the RT-gels were also addressed. In contrast, heat-set gel did not show thixotropic behavior. The X-ray diffraction (XRD) patterns of the xerogel depicted lamellar packing of the CT stacks in the gel phase. Single crystal XRD studies further evidenced the 1 : 1 mixed CT stack formation in the lamellae and also ruled out orthogonal hydrogen bonding possibilities among the hydrazide unit in the CT gel although such interaction was observed in a single crystal of NDI-A alone. In addition, a Ag+-ion triggered metallogelation of NDI-A and nematic liquid-crystalline property of Py-D were also observed. Electronic supplementary information (ESI) available: General experimental section, synthesis and characterization, single crystal X-ray data including CIF files and additional experimental results. See DOI: 10.1039/c6nr01128d

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

PubMed

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

2013-06-07

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

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

PubMed

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

2015-02-07

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

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.

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.

Influence of Gd3+ concentration on luminescence properties of Eu3+ ions in sol-gel materials

NASA Astrophysics Data System (ADS)

Szpikowska-Sroka, Barbara; Pawlik, Natalia; Pisarski, Wojciech A.

2016-12-01

The sol-gel powders doubly-doped with Gd3+/Eu3+ ions with different concentration of Gd3+ have been successfully obtained. The spectroscopic characterization of prepared samples was conducted based on excitation and emission spectra as well as luminescence decay analysis. Upon direct excitation of Eu3+ active ions, the characteristic 5D0 → 7F1 (orange) and 5D0 → 7F2 (red) emission bands were observed. The energy transfer from Gd3+ to Eu3+ ions was registered upon λexc = 273 nm excitation. An efficient conversion of ultraviolet radiation (UV) into visible luminescence was successfully observed. The energy transfer process from Gd3+ to Eu3+ led to longer luminescence decay from the 5D0 state in comparison to that obtained under direct excitation of Eu3+ ions (λexc = 393 nm). Generally, obtained results clearly indicated the beneficial influence of increasing concentration of Gd3+ ions on luminescence properties of Eu3+ in studied silica sol-gel phosphors.

Chemical Processing of Nanostructured Coatings

DTIC Science & Technology

2000-01-01

increasing particle loading in sol-gel process (8-10). This approach involved dispersing large ceramic powders in sol-gel solution, and the mixture...the high loading of ceramic powders. One way to prepare thicker coatings is to add powders into the sol. This helps to reduce the capillary stresses...thickness that range between 2 and 4 microns. In order to investigate the nature and origin of the textured region of the coatings, GIXS was used to

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.

Antioxidant Sol-Gel Improves Cutaneous Wound Healing in Streptozotocin-Induced Diabetic Rats

PubMed Central

Lee, Yen-Hsien; Chang, Jung-Jhih; Chien, Chiang-Ting; Yang, Ming-Chien; Chien, Hsiung-Fei

2012-01-01

We examined the effects of vitamin C in Pluronic F127 on diabetic wound healing. Full-thickness excision skin wounds were made in normal and diabetic Wistar rats to evaluate the effect of saline, saline plus vitamin C (antioxidant sol), Pluronic F127, or Pluronic F127 plus vitamin C (antioxidant sol-gel). The rate of wound contraction, the levels of epidermal and dermal maturation, collagen synthesis, and apoptosis production in the wound tissue were determined. In vitro data showed that after 6 hours of air exposure, the order of the scavenging abilities for HOCl, H2O2, and O2  − was antioxidant sol-gel > antioxidant saline > Pluronic F127 = saline. After 7 and 14 days of wound injury, the antioxidant sol-gel improved wound healing significantly by accelerated epidermal and dermal maturation, an increase in collagen content, and a decrease in apoptosis formation. However, the wounds of all treatments healed mostly at 3 weeks. Vitamin C in Pluronic F127 hastened cutaneous wound healing by its antioxidant and antiapoptotic mechanisms through a good drug delivery system. This study showed that Pluronic F127 plus vitamin C could potentially be employed as a novel wound-healing enhancer. PMID:22919368

Antioxidant sol-gel improves cutaneous wound healing in streptozotocin-induced diabetic rats.

PubMed

Lee, Yen-Hsien; Chang, Jung-Jhih; Chien, Chiang-Ting; Yang, Ming-Chien; Chien, Hsiung-Fei

2012-01-01

We examined the effects of vitamin C in Pluronic F127 on diabetic wound healing. Full-thickness excision skin wounds were made in normal and diabetic Wistar rats to evaluate the effect of saline, saline plus vitamin C (antioxidant sol), Pluronic F127, or Pluronic F127 plus vitamin C (antioxidant sol-gel). The rate of wound contraction, the levels of epidermal and dermal maturation, collagen synthesis, and apoptosis production in the wound tissue were determined. In vitro data showed that after 6 hours of air exposure, the order of the scavenging abilities for HOCl, H(2)O(2), and O(2) (-) was antioxidant sol-gel > antioxidant saline > Pluronic F127 = saline. After 7 and 14 days of wound injury, the antioxidant sol-gel improved wound healing significantly by accelerated epidermal and dermal maturation, an increase in collagen content, and a decrease in apoptosis formation. However, the wounds of all treatments healed mostly at 3 weeks. Vitamin C in Pluronic F127 hastened cutaneous wound healing by its antioxidant and antiapoptotic mechanisms through a good drug delivery system. This study showed that Pluronic F127 plus vitamin C could potentially be employed as a novel wound-healing enhancer.

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 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.

Nanocrystal/sol-gel nanocomposites

DOEpatents

Klimov, Victor L.; Petruska, Melissa A.

2010-05-25

The present invention is directed to a process for preparing a solid composite having colloidal nanocrystals dispersed within a sol-gel matrix, the process including admixing colloidal nanocrystals with an amphiphilic polymer including hydrophilic groups selected from the group consisting of --COOH, --OH, --SO.sub.3H, --NH.sub.2, and --PO.sub.3H.sub.2 within a solvent to form an alcohol-soluble colloidal nanocrystal-polymer complex, admixing the alcohol-soluble colloidal nanocrystal-polymer complex and a sol-gel precursor material, and, forming the solid composite from the admixture. The present invention is also directed to the resultant solid composites and to the alcohol-soluble colloidal nanocrystal-polymer complexes.

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.

ARSENIC REMOVAL USING SOL-GEL SYNTHESIZED TITANIUM DIOXIDE NANOPARTICLES

EPA Science Inventory

In this study, the effectiveness of TiO₂ nanoparticles in arsenic adsorption was examined. TiO₂ particles (LS) were synthesized via sol-gel techniques and characterized for their crystallinity, surface area and pore volume. Batch adsorption studies were perf...

Sol-gel transition of organogels observed by terahertz spectroscopy

NASA Astrophysics Data System (ADS)

Hoshina, Hiromichi; Ozaki, Atsumi; Itagaki, Yusuke; Yajima, Setsuko; Suzuki, Hal; Ishii, Shinya; Ishida, Misaki; Uchiyama, Tetsuji; Kimura, Keiichi; Otani, Chiko

2014-07-01

Terahertz (THz) absorption spectra of organogels consisting of (1R,2R)-1,2-bis(dodecanoylamino)cyclohexane/2-nitrophenyl octyl ether (RR-BDC/NPOE) and RR-BDC/n-dodecane were measured by Fourier-transform far-infrared (FT-FIR) spectroscopy. The vibrational peaks of the gels were observed at the same frequencies as those of the pure gelator, suggesting that the intermolecular structure around the Nsbnd H⋯Odbnd C hydrogen bond is maintained in the gel phase. Temperature-dependent spectroscopy showed a drastic spectral change at the sol-gel transition temperature, in which the vibrational peak at 3.5 THz disappears and a new peak appears at 2.9 THz. The change in THz vibrational frequency is indicative of the structural collapse of the hydrogen-bonded fibrous architecture in the sol phase.

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

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.

A needle extraction utilizing a molecularly imprinted-sol-gel xerogel for on-line microextraction of the lung cancer biomarker bilirubin from plasma and urine samples.

PubMed

Moein, Mohammad Mahdi; Jabbar, Dunia; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-10-31

In the present work, a needle trap utilizing a molecularly imprinted sol-gel xerogel was prepared for the on-line microextraction of bilirubin from plasma and urine samples. Each prepared needle could be used for approximately one hundred extractions before it was discarded. Imprinted and non-imprinted sol-gel xerogel were applied for the extraction of bilirubin from plasma and urine samples. The produced molecularly imprinted sol-gel xerogel polymer showed high binding capacity and fast adsorption/desorption kinetics for bilirubin in plasma and urine samples. The adsorption capacity of molecularly imprinted sol-gel xerogel polymer was approximately 60% higher than that of non-imprinted polymer. The effect of the conditioning, washing and elution solvents, pH, extraction time, adsorption capacity and imprinting factor were investigated. The limit of detection and the lower limit of quantification were set to 1.6 and 5nmolL(-1), respectively using plasma or urine samples. The standard calibration curves were obtained within the concentration range of 5-1000nmolL(-1) in both plasma and urine samples. The coefficients of determination values (R(2)) were ≥0.998 for all runs. The extraction recovery was approximately 80% for BR in the human plasma and urine samples. Copyright © 2014 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%.

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.

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.

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.

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.

Improvement of Adhesion Properties and Corrosion Resistance of Sol-Gel Coating on Zinc.

PubMed

Savignac, Pauline; Menu, Marie-Joëlle; Gressier, Marie; Denat, Bastien; Khadir, Yacine El; Manov, Stephan; Ansart, Florence

2018-05-03

Corrosion is a major problem for durability of many metals and alloys. Among the efficient classical surface treatments, chromate-based treatments must be banished from industrial use due to their toxicity. At the same time, sol-gel routes have demonstrated high potential to develop an efficient barrier effect against aggressive environments. By this process, the anti-corrosion property can be also associated to others in the case of the development of multi-functional hybrid coatings. In this paper, the main goal is precisely to improve both the corrosion resistance and the adhesion properties of phosphated zinc substrates by the deposition of a hybrid (organic-inorganic) sol-gel layer. To reach this double objective, a choice between two formulations 3-glycidoxypropyltrimethoxysilane (GPTMS)/aluminum-tri-sec-butoxide (ASB) and 3-(trimethoxysilyl)propylmethacrylate (MAP)/tetraethylorthosilicate (TEOS) was firstly made based on the results obtained by microstructural characterizations using SEM, optical analysis, and mechanical characterization such as shock and/or scratch tests (coupled to climatic chamber and salt spray exposure). Several investigations were performed in this study, and the best formulation and performances of the system were obtained by adding a new precursor (1-[3-(trimethoxysilyl)propyl]ureido-UPS) under controlled conditions, as detailed in this paper.

A Micro Oxygen Sensor Based on a Nano Sol-Gel TiO2 Thin Film

PubMed Central

Wang, Hairong; Chen, Lei; Wang, Jiaxin; Sun, Quantao; Zhao, Yulong

2014-01-01

An oxygen gas microsensor based on nanostructured sol-gel TiO2 thin films with a buried Pd layer was developed on a silicon substrate. The nanostructured titania thin films for O2 sensors were prepared by the sol-gel process and became anatase after heat treatment. A sandwich TiO2 square board with an area of 350 μm × 350 μm was defined by both wet etching and dry etching processes and the wet one was applied in the final process due to its advantages of easy control for the final structure. A pair of 150 nm Pt micro interdigitated electrodes with 50 nm Ti buffer layer was fabricated on the board by a lift-off process. The sensor chip was tested in a furnace with changing the O2 concentration from 1.0% to 20% by monitoring its electrical resistance. Results showed that after several testing cycles the sensor's output becomes stable, and its sensitivity is 0.054 with deviation 2.65 × 10−4 and hysteresis is 8.5%. Due to its simple fabrication process, the sensor has potential for application in environmental monitoring, where lower power consumption and small size are required. PMID:25192312

Process of forming a sol-gel/metal hydride composite

DOEpatents

Congdon, James W [Aiken, SC

2009-03-17

An external gelation process is described which produces granules of metal hydride particles contained within a sol-gel matrix. The resulting granules are dimensionally stable and are useful for applications such as hydrogen separation and hydrogen purification. An additional coating technique for strengthening the granules is also provided.

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.

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

Synthesis of PEG-rich PLGA-PEG-PLGA for the PLGA-PEG-PLGA/laponite hydrogels with thermoresponsive sol-gel transitions

NASA Astrophysics Data System (ADS)

Tanimoto, Keishi; Maeda, Tomoki; Hotta, Atsushi

Poly (D,L-lactide-co-glycolide)-b-poly (ethylene glycol)-b-poly (D,L-lactide-co-glycolide) (PLGA-PEG-PLGA) possesses moderate biocompatibility originating from the relatively shorter PEG block in its polymeric molecule. For the maximum utilization of the highly biocompatible PEG block, the PEG block should be relatively longer, and thus the PEG/PLGA ratio, the molecular weight ratio of PEG and PLGA, should be higher. In addition, for the wider use of PLGA-PEG-PLGA in the biological fields, the aqueous PLGA-PEG-PLGA solution should transfer from sol to gel states in response to the increase in temperature. It was reported, however, through the previous researches, that the PLGA-PEG-PLGA solution with a high PEG/PLGA ratio (above 0.5) would not exhibit thermoresponsive sol-gel transitions. In this work, PLGA-PEG-PLGAs with higher PEG/PLGA ratios were synthesized and the laponite, an inorganic nanoparticle, was added to the solutions to realize the thermoresponsive sol-gel transition. It was found that the PLGA-PEG-PLGA with the high PEG/PLGA ratio of 3.0 could exhibit the thermoresponsive sol-gel transition by adding laponite at 1.25 weight percent. The physical characteristics of the gel were also studied by the dynamic mechanical analysis (DMA) This work was supported by a Grant-in-Aid for Scientific Research (A) (No. 15H02298 to A.H.) and a Grant-in-Aid for Research Activity Start-up (No.15H06586 to T.M.) from JSPS: KAKENHI\\x9D.

A pH- and temperature-responsive bioresorbable injectable hydrogel based on polypeptide block copolymers for the sustained delivery of proteins in vivo.

PubMed

Turabee, Md Hasan; Thambi, Thavasyappan; Duong, Huu Thuy Trang; Jeong, Ji Hoon; Lee, Doo Sung

2018-02-27

Sustained delivery of protein therapeutics is limited owing to the fragile nature of proteins. Despite its great potential, delivery of proteins without any loss of bioactivity remains a challenge in the use of protein therapeutics in the clinic. To surmount this shortcoming, we report a pH- and temperature-responsive in situ-forming injectable hydrogel based on comb-type polypeptide block copolymers for the controlled delivery of proteins. Polypeptide block copolymers, composed of hydrophilic polyethylene glycol (PEG), temperature-responsive poly(γ-benzyl-l-glutamate) (PBLG), and pH-responsive oligo(sulfamethazine) (OSM), exhibit pH- and temperature-induced sol-to-gel transition behavior in aqueous solutions. Polypeptide block copolymers were synthesized by combining N-carboxyanhydride-based ring-opening polymerization and post-functionalization of the chain-end using N-hydroxy succinimide ester activated OSM. The physical properties of polypeptide-based hydrogels were tuned by varying the composition of temperature- and pH-responsive PBLG and OSM in block copolymers. Polypeptide block copolymers were non-toxic to human embryonic kidney cells at high concentrations (2000 μg mL -1 ). Subcutaneous administration of polypeptide block copolymer sols formed viscoelastic gel instantly at the back of Sprague-Dawley (SD) rats. The in vivo gels exhibited sustained degradation and were found to be bioresorbable in 6 weeks without any noticeable inflammation at the injection site. Anionic characteristics of hydrogels allow efficient loading of a cationic model protein, lysozyme, through electrostatic interaction. Lysozyme-loaded polypeptide block copolymer sols readily formed a viscoelastic gel in vivo and sustained lysozyme release for at least a week. Overall, the results demonstrate an elegant approach to control the release of certain charged proteins and open a myriad of therapeutic possibilities in protein therapeutics.

Synthesis of Ba 0.6K 0.4BiO 3 and BaPb 0.75Bi 0.25O 3 superconductors by sol-gel process

NASA Astrophysics Data System (ADS)

Rao, G. V. Rama; Varadaraju, U. V.; Mannan, S. L.

1994-12-01

We have synthesised Ba 0.6K 0.4BiO 3 (BKB) and BaPb 1-xBi xO 3-y compounds by sol-gel process. IR spectra of gels indicated the bridging type of bonding between metal carboxylates leading to the formation of homogeneous gels. BKB and BaPb 0.75Bi 0.25O 3 compounds exhibited sharp superconducting transitions from R-T and χ-T measurements indicating excellent homogeneity of the samples

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.

Transparent Glass-Ceramics Produced by Sol-Gel: A Suitable Alternative for Photonic Materials.

PubMed

Gorni, Giulio; Velázquez, Jose J; Mosa, Jadra; Balda, Rolindes; Fernández, Joaquin; Durán, Alicia; Castro, Yolanda

2018-01-30

Transparent glass-ceramics have shown interesting optical properties for several photonic applications. In particular, compositions based on oxide glass matrices with fluoride crystals embedded inside, known as oxyfluoride glass-ceramics, have gained increasing interest in the last few decades. Melt-quenching is still the most used method to prepare these materials but sol-gel has been indicated as a suitable alternative. Many papers have been published since the end of the 1990s, when these materials were prepared by sol-gel for the first time, thus a review of the achievements obtained so far is necessary. In the first part of this paper, a review of transparent sol-gel glass-ceramics is made focusing mainly on oxyfluoride compositions. Many interesting optical results have been obtained but very little innovation of synthesis and processing is found with respect to pioneering papers published 20 years ago. In the second part we describe the improvements in synthesis and processing obtained by the authors during the last five years. The main achievements are the preparation of oxyfluoride glass-ceramics with a much higher fluoride crystal fraction, at least double that reported up to now, and the first synthesis of NaGdF₄ glass-ceramics. Moreover, a new SiO₂ precursor was introduced in the synthesis, allowing for a reduction in the treatment temperature and favoring hydroxyl group removal. Interesting optical properties demonstrated the incorporation of dopant ions in the fluoride crystals, thus obtaining crystal-like spectra along with higher efficiencies with respect to xerogels, and hence demonstrating that these materials are a suitable alternative for photonic applications.

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

PubMed

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

2006-10-06

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

[In vitro evaluation of the gels properties prepared thermosensitive polymers as vehicles for administration substance by injection].

PubMed

Karolewicz, Bozena; Owczarek, Artur; Pluta, Janusz

2011-01-01

The aim of this study was to prepare a thermoresponsive formulations, which are a carrier for substance administered directly into site of action and which obtain sol-gel transitions at physiological ranges of temperature. The investigated formulations of liquid consistency at room temperature were obtained in sterile conditions on the basis of nonionic polymers Pluronic F-127, Pluronic F-68 and anionic polymer hyaluronic acid in different concentrations. The sol-gel transition temperature of the formulations was investigated and their physicochemical properties such as pH, density, osmotic pressure, sol-gel transition temperature, texture and release of vancomycin hydrochloride were studied. In vitro release experiments indicated that the optimised platform was able to prolong vancomycin hydrochloride release and their physico-chemical properties allow for application by injection form.

Cellulose-silica/gold nanomaterials for electronic applications.

PubMed

Kim, Gwang-Hoon; Ramesh, Sivalingam; Kim, Joo-Hyung; Jung, Dongsoo; Kim, Heung Soo

2014-10-01

Cellulose and one dimensional nano-material composite has been investigated for various industrial applications due to their optical, mechanical and electrical properties. In present investigation, cellulose/silica and silica-gold hybrid biomaterials were prepared by sol-gel covalent cross-linking process. The tetraethoxysiliane (TEOS) and gold precursors and γ-aminopropyltriethoxysilane (γ-APTES) as coupling agent were used for sol-gel cross-linking process. The chemical and morphological properties of cellulose/silica and cellulose/silica-gold nano-materials via covalent cross-linking hybrids were confirmed by FTIR, XRD, SEM, and TEM analysis. In the sol-gel process, the inorganic particles were dispersed in the cellulose host matrix at the nanometer scale, bonding to the cellulose through the covalent bonds.

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.

CO2 Responsive Imidazolium-Type Poly(Ionic Liquid) Gels.

PubMed

Zhang, Jing; Xu, Dan; Guo, Jiangna; Sun, Zhe; Qian, Wenjing; Zhang, Ye; Yan, Feng

2016-07-01

Poly(ionic liquid) (PIL) gels with CO2 stimulus responsiveness have been synthesized through the copolymerization of an imidazolium-type ionic liquid monomer with 2-(dimethyl amino) ethyl methacrylate. Upon bubbling with CO2 gas, the prepared PIL solution is converted to a transparent and stable gel, which can be turned back to the initial solution state after N2 bubbling. The reversible sol-gel phase transition behavior is proved by the reversible values of viscosity and ionic conductivity. The possible mechanism for such a reversible sol-gel phase transition is demonstrated by NMR, conductivity, and rheological measurements. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Two-dimensional porous anodic alumina for optoelectronics and photocatalytic application

NASA Astrophysics Data System (ADS)

Khoroshko, L. S.

2015-11-01

Fabrication of porous anodic alumina film structures using anodizing, sol-gel synthesis and photolithography is reported. The structures receive interest as planar waveguides due to strong photoluminescence of the embedded trivalent lanthanides. Mesoporous structures comprising sol-gel derived titania in porous anodic alumina play a role of effective catalyst for water purification.

Surface chemistry and moisture sorption properties of wood coated with multifunctional alkoxysilanes by sol-gel process

Treesearch

Mandla A. Tshabalala; Peter Kingshott; Mark R. VanLandingham; David Plackett

2003-01-01

Sol-gel surface deposition of a hydrophobic polysiloxane coating on wood was accomplished by using a mixture of a low molecular weight multifunctional alkoxysilane, methyltrimethoxysilane (MTMOS), and a high molecular weight multifunctional alkoxysilane, hexadecyltrimethoxysilane (HDTMOS). Investigation of the surface chemistry and morphology of the wood specimens by...

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.

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.

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.

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.

Protection of enzymes from photodegradation by entrapment within alumina.

PubMed

Shapovalova, Olga E; Levy, David; Avnir, David; Vinogradov, Vladimir V

2016-10-01

Most enzymes are highly sensitive to UV-light in all of its ranges and their activity can irreversibly drop even after a short time of exposure. Here we report a solution of this problem by using sol-gel matrices as effective protectors against this route of enzyme inactivation and denaturation. The concept presented here utilizes several modes of action: First, the entrapment within the rigid ceramic sol-gel matrix, inhibits denaturation motions, and the hydration shell around the entrapped protein provides extra protection. Second, the matrix itself - alumina in this report - absorbs UV light. And third, sol-gel materials have been shown to be quite universal in their ability to entrap small molecules, and so co-entrapment with well documented sun-screening molecules (2-hydroxybenzophenone, 2,2'-dihydroxybenzophenone, and 2,2'-dihydroxy-4-methoxybenzophenone) is an additional key protective tool. Three different enzymes as models were chosen for the experiments: carbonic anhydrase, acid phosphatase and horseradish peroxidase. All showed greatly enhanced UV (regions UV-A, UV-B, and UV-C) stabilization after entrapment within the doped sol-gel alumina matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Graphene-supported zinc oxide solid-phase microextraction coating with enhanced selectivity and sensitivity for the determination of sulfur volatiles in Allium species.

PubMed

Zhang, Suling; Du, Zhuo; Li, Gongke

2012-10-19

A graphene-supported zinc oxide (ZnO) solid-phase microextraction (SPME) fiber was prepared via a sol-gel approach. Graphite oxide (GO), with rich oxygen-containing groups, was selected as the starting material to anchor ZnO on its nucleation center. After being deoxidized by hydrazine, the Zn(OH)2/GO coating was dehydrated at high temperature to give the ZnO/graphene coating. Sol-gel technology could efficiently incorporate ZnO/graphene composites into the sol-gel network and provided strong chemical bonding between sol-gel polymeric SPME coating and silica fiber surface, which enhanced the durability of the fiber and allowed more than 200 replicate extractions. Results indicated that pure ZnO coated fiber did not show adsorption selectivity toward sulfur compounds, which might because the ZnO nanoparticles were enwrapped in the sol-gel network, and the strong coordination action between Zn ion and S ion was therefore blocked. The incorporation of graphene into ZnO based sol-gel network greatly enlarged the BET surface area from 1.2 m2/g to 169.4 m2/g and further increased the adsorption sites. Combining the superior properties of extraordinary surface area of graphene and the strong coordination action of ZnO to sulfur compounds, the ZnO/graphene SPME fiber showed much higher adsorption affinity to 1-octanethiol (enrichment factor, EF, 1087) than other aliphatic compounds without sulfur-containing groups (EFs<200). Also, it showed higher extraction selectivity and sensitivity toward sulfur compounds than commercial polydimethylsiloxane (PDMS) and polydimethylsiloxane/divinylbenzene (PDMS/DVB) SPME fibers. Several most abundant sulfur volatiles in Chinese chive and garlic sprout were analyzed using the ZnO/graphene SPME fiber in combination with gas chromatography-mass spectrometry (GC-MS). Their limits of detection were 0.1-0.7 μg/L. The relative standard deviation (RSD) using one fiber ranged from 3.6% to 9.1%. The fiber-to-fiber reproducibility for three parallel prepared fibers was 4.8-10.8%. The contents were in the range of 1.0-46.4 μg/g with recoveries of 80.1-91.6% for four main sulfides in Chinese chive and 17.1-122.6 μg/g with recoveries of 73.2-80.6% for three main sulfides in garlic sprout. Copyright © 2012 Elsevier B.V. All rights reserved.

Additive Manufacturing of Transparent Silica Glass from Solutions.

PubMed

Cooperstein, Ido; Shukrun, Efrat; Press, Ofir; Kamyshny, Alexander; Magdassi, Shlomo

2018-06-06

A sol, aqueous solution-based ink is presented for fabrication of 3D transparent silica glass objects with complex geometries, by a simple 3D printing process conducted at room temperature. The ink combines a hybrid ceramic precursor that can undergo both the photopolymerization reaction and a sol-gel process, both in the solution form, without any particles. The printing is conducted by localized photopolymerization with the use of a low-cost 3D printer. Following printing, upon aging and densifying, the resulting objects convert from a gel to a xerogel and then to a fused silica. The printed objects, which are composed of fused silica, are transparent and have tunable density and refractive indices.

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

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

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

PubMed

Jillani, Shehzada Muhammad Sajid; Alhooshani, Khalid

2018-03-30

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

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

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.

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).

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.

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

Development and Characterization of Titanium Dioxide Gel with Encapsulated Bacteriorhodopsin for Hydrogen Production.

PubMed

Johnson, Kaitlin E; Gakhar, Sukriti; Risbud, Subhash H; Longo, Marjorie L

2018-06-06

We study bacteriorhodopsin (BR) in its native purple membrane encapsulated within amorphous titanium dioxide, or titania, gels and in the presence of titania sol-particles to explore this system for hydrogen production. Förster resonance energy transfer between BR and titanium dioxide sol particles was used to conclude that there is nanometer-scale proximity of bacteriorhodopsin to the titanium dioxide. The detection of BR-titania sol aggregates by fluorescence anisotropy and particle sizing indicated the affinity amorphous titania has for BR without the use of additional cross-linkers. UV-Visible spectroscopy of BR-titania gels show that methanol addition did not denature BR at a 25 mM concentration presence as a sacrificial electron donor. Additionally, confinement of BR in the gels significantly limited protein denaturation at higher concentration of added methanol or ethanol. Subsequently, titania gels fabricated through the sol-gel process using a titanium ethoxide precursor, water and the addition of 25 mM methanol were used to encapsulate BR and a platinum reduction catalyst for the production of hydrogen gas under white light irradiation. The inclusion of 5 µM bacteriorhodopsin resulted in a hydrogen production rate of about 3.8 µmole hydrogen mL -1 hr -1 , an increase of 52% compared to gels containing no protein. Electron transfer and proton pumping by BR in close proximity to the titania gel surface are feasible explanations for the enhanced production of hydrogen without the need to crosslink BR to the titania gel. This work sets the stage for further developments of amorphous, rather than crystalline, titania-encapsulated bacteriorhodopsin for solar-driven hydrogen production through water-splitting.

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.

Sol-gel TiO2 colloidal suspensions and nanostructured thin films: structural and biological assessments.

PubMed

Procopio, Elsa Quartapelle; Colombo, Valentina; Santo, Nadia; Sironi, Angelo; Lenardi, Cristina; Maggioni, Daniela

2018-02-02

The role of substrate topography in phenotype expression of in vitro cultured cells has been widely assessed. However, the production of the nanostructured interface via the deposition of sol-gel synthesized nanoparticles (NPs) has not yet been fully exploited. This is also evidenced by the limited number of studies correlating the morphological, structural and chemical properties of the grown thin films with those of the sol-gel 'brick' within the framework of the bottom-up approach. Our work intends to go beyond this drawback presenting an accurate investigation of sol-gel TiO 2 NPs shaped as spheres and rods. They have been fully characterized by complementary analytical techniques both suspended in apolar solvents, by dynamic light scattering (DLS) and nuclear magnetic resonance (NMR) and after deposition on substrates (solid state configuration) by transmission electron microscopy (TEM) and powder x-ray diffraction (PXRD). In the case of suspended anisotropic rods, the experimental DLS data, analyzed by the Tirado-Garcia de la Torre model, present the following ranges of dimensions: 4-5 nm diameter (∅) and 11-15 nm length (L). These results are in good agreement with that obtained by the two solid state techniques, namely 3.8(9) nm ∅ and 13.8(2.5) nm L from TEM and 5.6(1) ∅ and 13.3(1) nm L from PXRD data. To prove the suitability of the supported sol-gel NPs for biological issues, spheres and rods have been separately deposited on coverslips. The cell response has been ascertained by evaluating the adhesion of the epithelial cell line Madin-Darby canine kidney. The cellular analysis showed that titania films promote cell adhesion as well clustering organization, which is a distinguishing feature of this type of cell line. Thus, the use of nanostructured substrates via sol-gel could be considered a good candidate for cell culture with the further advantages of likely scalability and interfaceability with many different materials usable as supports.

Sol-gel TiO2 colloidal suspensions and nanostructured thin films: structural and biological assessments

NASA Astrophysics Data System (ADS)

Quartapelle Procopio, Elsa; Colombo, Valentina; Santo, Nadia; Sironi, Angelo; Lenardi, Cristina; Maggioni, Daniela

2018-02-01

The role of substrate topography in phenotype expression of in vitro cultured cells has been widely assessed. However, the production of the nanostructured interface via the deposition of sol-gel synthesized nanoparticles (NPs) has not yet been fully exploited. This is also evidenced by the limited number of studies correlating the morphological, structural and chemical properties of the grown thin films with those of the sol-gel ‘brick’ within the framework of the bottom-up approach. Our work intends to go beyond this drawback presenting an accurate investigation of sol-gel TiO2 NPs shaped as spheres and rods. They have been fully characterized by complementary analytical techniques both suspended in apolar solvents, by dynamic light scattering (DLS) and nuclear magnetic resonance (NMR) and after deposition on substrates (solid state configuration) by transmission electron microscopy (TEM) and powder x-ray diffraction (PXRD). In the case of suspended anisotropic rods, the experimental DLS data, analyzed by the Tirado-Garcia de la Torre model, present the following ranges of dimensions: 4-5 nm diameter (∅) and 11-15 nm length (L). These results are in good agreement with that obtained by the two solid state techniques, namely 3.8(9) nm ∅ and 13.8(2.5) nm L from TEM and 5.6(1) ∅ and 13.3(1) nm L from PXRD data. To prove the suitability of the supported sol-gel NPs for biological issues, spheres and rods have been separately deposited on coverslips. The cell response has been ascertained by evaluating the adhesion of the epithelial cell line Madin-Darby canine kidney. The cellular analysis showed that titania films promote cell adhesion as well clustering organization, which is a distinguishing feature of this type of cell line. Thus, the use of nanostructured substrates via sol-gel could be considered a good candidate for cell culture with the further advantages of likely scalability and interfaceability with many different materials usable as supports.

Effects of sol-gel processed silica coating on bond strength of resin cements to glass-infiltrated alumina ceramic.

PubMed

Xie, Haifeng; Wang, Xiaozu; Wang, Yu; Zhang, Feimin; Chen, Chen; Xia, Yang

2009-02-01

The aim of this study was to verify the effects of sol-gel processed silica coating on the bond strength between resin cement and glass-infiltrated aluminum oxide ceramic. Silica coatings were prepared on glass-infiltrated aluminum oxide ceramic surface via the sol-gel process. Atomic Force Microscope (AFM), Fourier Transmission Infrared spectrum (FTIR), and Energy Dispersive X-ray Spectroscopy (EDS) were used for coating characterization. Forty-eight blocks of glass-infiltrated aluminum oxide ceramic were fabricated. The ceramic surfaces were polished following sandblasting. Three groups of specimens (16 for each group) with different surface treatment were prepared. Group P: no treatment; group PO: treated with silane solution; group PTO: silica coating via sol-gel process, followed by silane application. Composite cylinders were luted with resin cement to the test specimens. Half of the specimens in each group were stored in distilled water for 24 h and the other half were stored in distilled water for 30 days before shear loading in a universal testing machine until failure. Selected ceramic surfaces were analyzed to identify the failure mode using a scanning electron microscopy (SEM). Nanostructured silica coatings were prepared on glass-infiltrated aluminum oxide ceramic surfaces by the sol-gel process. The silicon element on the ceramic surface increased significantly after the coating process. The mean shear bond strength values (standard deviation) before artificial aging were: group P: 1.882 +/- 0.156 MPa; group PO: 2.177 +/- 0.226 MPa; group PTO: 3.574 +/- 0.671 MPa. Statistically significant differences existed between group PTO and group P, and group PTO and groups PO. The failure mode for group P and group PO was adhesive, while group PTO was mixed. The mean shear bond strength values (standard deviation) after artificial aging were: group P: 1.594 +/- 0.111 MPa; group PO: 2.120 +/- 0.339 MPa; group PTO: 2.955 +/- 0.113 MPa. Statistically significant differences existed between each two groups after artificial aging, group P had the lowest bond durability, and group PTO had the highest bond durability. The sol-gel process is an effective way to prepare silica coating on dental glass-infiltrated alumina ceramic. Sol-gel processed silica coating can improve the resin bond strength of glass-infiltrated alumina ceramic.

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.

Development of a fiber coating based on molecular sol-gel imprinting technology for selective solid-phase micro extraction of caffeine from human serum and determination by gas chromatography/mass spectrometry.

PubMed

Rajabi Khorrami, Afshin; Rashidpur, Amene

2012-05-21

In this work, a molecular sol-gel imprinting approach has been introduced to produce a fiber coating for selective direct immersion solid-phase microextraction (SPME) of caffeine. The polymerization mixture was composed of vinyl trimethoxysilane and methacrylic acid as vinyl sol-gel precursor and functional monomer, respectively. Caffeine was used as template molecule during polymerization process. The prepared fibers could be coupled directly to gas chromatography/mass spectrometry (GC/MS) and used for trace analysis of caffeine in a complex sample such as human serum. The parameters influencing SPME such as time, temperature and stirring speed were optimized. The prepared coating showed good selectivity towards caffeine in the presence of some structurally related compounds. Also, it offered high imprinting capability in comparison to bare fiber and non-imprinted coating. Linear range for caffeine detection was 1-80 μg mL(-1) and the limit of detection was 0.1 μg mL(-1). The intra-day and inter-day precisions of the peak areas for five replicates were 10 and 16%, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis of nano-scale fast ion conducting cubic Li7La3Zr2O12.

PubMed

Sakamoto, Jeff; Rangasamy, Ezhiylmurugan; Kim, Hyunjoung; Kim, Yunsung; Wolfenstine, Jeff

2013-10-25

A solution-based process was investigated for synthesizing cubic Li7La3Zr2O12 (LLZO), which is known to exhibit the unprecedented combination of fast ionic conductivity, and stability in air and against Li. Sol-gel chemistry was developed to prepare solid metal-oxide networks consisting of 10 nm cross-links that formed the cubic LLZO phase at 600 ° C. Sol-gel LLZO powders were sintered into 96% dense pellets using an induction hot press that applied pressure while heating. After sintering, the average LLZO grain size was 260 nm, which is 13 times smaller compared to LLZO prepared using a solid-state technique. The total ionic conductivity was 0.4 mS cm(-1) at 298 K, which is the same as solid-state synthesized LLZO. Interestingly, despite the same room temperature conductivity, the sol-gel LLZO total activation energy is 0.41 eV, which 1.6 times higher than that observed in solid-state LLZO (0.26 eV). We believe the nano-scale grain boundaries give rise to unique transport phenomena that are more sensitive to temperature when compared to the conventional solid-state LLZO.

Natamycin based sol-gel antimicrobial coatings on polylactic acid films for food packaging.

PubMed

Lantano, Claudia; Alfieri, Ilaria; Cavazza, Antonella; Corradini, Claudio; Lorenzi, Andrea; Zucchetto, Nicola; Montenero, Angelo

2014-12-15

In this work a comprehensive study on a new active packaging obtained by a hybrid organic-inorganic coating with antimicrobial properties was carried out. The packaging system based on polylactic acid was realised by sol-gel processing, employing tetraethoxysilane as a precursor of the inorganic phase and polyvinyl alcohol as the organic component, and incorporating natamycin as the active agent. Films with different organic-inorganic ratios (in a range between 1:19 and 1:4) were prepared, and the amount of antimycotic entrapped was found to be modulated by the sol composition, and was between 0.18 and 0.25mg/dm(2). FTIR microspectroscopic measurements were used to characterise the prepared coatings. The antifungal properties of the films were investigated against mould growth on the surface of commercial semi-soft cheese. The release of natamycin from the films to ethanol 50% (v/v) was studied by means of HPLC UV-DAD. The maximal level released was about 0.105 mg/dm(2), which is far below the value allowed by legislation. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Powers, Kevin William

1998-12-01

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

The gelation influence on diffusion and conductivity enhancement effect in renewable ionic gels based on a LMWG.

PubMed

Bielejewski, M; Rachocki, A; Kaszyńska, J; Tritt-Goc, J

2018-02-21

This paper reports the interdisciplinary study on molecular dynamics, ionic interactions and electrical conductivity in a quaternary ammonium salt (TMABr) ionogel based on a low molecular weight gelator (LMWG) in a wide range of electrolyte molar concentrations. The thermal scanning conductometry (TSC) was used to investigate the electric properties of the ionogels. The prepared TMABr/H 2 O/LMWG ionogel exhibits better ion transport properties than the dissociated TMA + cation in solution. The enhanced ionic conductivity effect (EICE) was observed in the concentration range of the TMABr salt up to 1 M. To investigate the transport properties of the TMA + cation and solvent molecules in the gel and sol phase, the NMR diffusiometry method was used. The field-cycling relaxometry method (FFC NMR) was applied to study the local motions of the electrolyte at the surface of the gelator matrix. On the basis of the obtained data, the higher ionic conductivity observed in the gel phase has been related to the microstructure of the gel matrix. The possible explanation for the origin of this effect has been given. The investigated system is a thermally reversible physical gel, all registered data were reproducible upon transforming the sample from gel to sol and back to the gel state, confirming the enhancement effect as a permanent property of the investigated ionogels. Therefore, the EICE has been proposed to be used as an internal sensor to monitor the condition of the ionogel phase, thus making them smart materials.

Improvement of Sol-Gel Derived PbZrxTi1-xO3 Film Properties Using Thermal Press Treatment

NASA Astrophysics Data System (ADS)

Kaneda, Toshihiko; Kim, Joo-Nam; Tokumitsu, Eisuke; Shimoda, Tatsuya

2010-09-01

A thermal press treatment was introduced in the sol-gel process of PbZrxTi1-xO3 (PZT) thin films for the first time and the crystalline and electrical characteristics of the PZT films were investigated. The thermal press treatment was applied to the amorphous PZT gel film before crystallization annealing. It is found that the crystalline orientation and grain size of the PZT film fabricated with the thermal press treatment are different from those of the film fabricated by the conventional sol-gel process without the thermal press treatment, even though the crystallization conditions are exactly the same. It is demonstrated that the electrical properties, especially leakage current density and breakdown field, are significantly improved for the PZT film fabricated with the thermal press treatment. Furthermore, we also demonstrate that the fatigue property is improved by introducing the thermal press treatment.

Sol-Gel Processing Science Using a Sol-Gel Optics Research Facility (SGORF)

DTIC Science & Technology

1989-09-10

Malaysia , Hong-Kong) where labor rates are perhaps one-tenth those of the U.S.. Figure 1 presents the trends of imports and exports of all optical... ACerS Annual Meeting, Washington, DC, May 1972. 2. W. A. Plummer, "Differential Dilatometry--A Powerful Tool," Corning Gla 33 Works, Corning, NY 14830

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.

THE ROLE OF CATALYST PROPERTIES ON METHANOL OXIDATION OVER V2O5-TIO2 USING OZONE

EPA Science Inventory

Oxidation of methanol over V₂O₅ catalysts supported on anatase TiO₂ that were prepared using sol-gel formation and impregnation procedures were investigated. The effects of incorporating Mg in sol-gel to influence the properties of the catalyst w...

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.

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.

Straight single-crystalline germanium nanowires and their patterns grown on sol gel prepared gold/silica substrates

NASA Astrophysics Data System (ADS)

Pan, Zheng Wei; Dai, Sheng; Lowndes, Douglas H.

2005-04-01

Straight single-crystalline Ge nanowires with a uniform diameter distribution of 50-80 nm and lengths up to tens of micrometers were grown in a high yield on sol-gel prepared gold/silica substrates by using Ge powder as the Ge source. Detailed electron microscopy analyses show that the nanowires grow through a vapor-liquid-solid growth mechanism with gold nanoparticles located at the nanowire tips. By using transmission electron microscope grids as the shadow mask, the sol-gel technique can be readily adapted to prepare patterned film-like gold/silica substrates, so that regular micropatterns of Ge nanowires were obtained, which could facilitate the integration of Ge nanowires for characterization and devices.

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.

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

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.

Hybrid Silicon-Based Organic/Inorganic Block Copolymers with Sol-Gel Active Moieties: Synthetic Advances, Self-Assembly and Applications in Biomedicine and Materials Science.

PubMed

Czarnecki, Sebastian; Bertin, Annabelle

2018-03-07

Hybrid silicon-based organic/inorganic (multi)block copolymers are promising polymeric precursors to create robust nano-objects and nanomaterials due to their sol-gel active moieties via self-assembly in solution or in bulk. Such nano-objects and nanomaterials have great potential in biomedicine as nanocarriers or scaffolds for bone regeneration as well as in materials science as Pickering emulsifiers, photonic crystals or coatings/films with antibiofouling, antibacterial or water- and oil-repellent properties. Thus, this Review outlines recent synthetic efforts in the preparation of these hybrid inorganic/organic block copolymers, gives an overview of their self-assembled structures and finally presents recent examples of their use in the biomedical field and material science. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Sol-gel-processed yttrium-doped NiO as hole transport layer in inverted perovskite solar cells for enhanced performance

NASA Astrophysics Data System (ADS)

Hu, Zijun; Chen, Da; Yang, Pan; Yang, Lijun; Qin, Laishun; Huang, Yuexiang; Zhao, Xiaochong

2018-05-01

In this work, high-performance inverted planar perovskite solar cells (PSCs) using sol-gel processed Y-doped NiO thin films as hole transport layer (HTL) were demonstrated. Y-doped NiO thin films containing different Y doping concentrations were successfully prepared through a simple sol-gel process. The Y doping could significantly improve the electrical conductivity of NiO thin film, and the photovoltaic performance of Y-doped NiO HTL-based PSC devices outperformed that of the pristine NiO HTL-based device. Notably, the PSC using a 5%Y-NiO HTL exhibited the champion performance with an open-circuit voltage (Voc) of 1.00 V, a short circuit current density (Jsc) of 23.82 mA cm-2, a fill factor (FF) of 68% and a power conversion efficiency (PCE) of 16.31%, resulting in a 27.62% enhancement in PCE in comparison with the NiO device. The enhanced performance of the Y-doped NiO device could be attributed to the improved hole mobility, the high quality compact active layer morphology, the more efficient charge extraction from perovskite absorber as well as the lower recombination probability of charge carriers. Thus, this work provides a simple and effective approach to improve the electrical conductivity of p-type NiO thin films for use as a promising HTL in high performance PSCs.

Nanocrystalline mesoporous SMO thin films prepared by sol gel process for MEMS-based hydrogen sensor

NASA Astrophysics Data System (ADS)

Gong, Jianwei; Fei, Weifeng; Seal, Sudipta; Chen, Quanfang

2004-01-01

MEMS based SnO2 gas sensor with sol gel synthesized mesoporous nanocrystalline (<10 nm) semiconductor thin (100~150 nm) film has been recently developed. The SnO2 nano film is fabricated with the combination of polymeric sol gel chemistry with block copolymers used for structure directing agents. The novel hydrogen sensor has a fast response time (1s) and quick recovery time (3s), as well as good sensitivity (about 90%), comparing to other hydrogen sensors developed. The improved capabilities are credited to the large surface to volume ratio of gas sensing thin film with nano sized porous surface topology, which can greatly increase the sensitivity even at relatively low working temperature. The gas sensing film is deposited onto a thin dielectric membrane of low thermal conductivity, which provides good thermal isolation between substrate and the gas-sensitive heated area on the membrane. In this way the power consumption can be kept very low. Since the fabrication process is completely compatible with IC industry, it makes mass production possible and greatly reduces the cost. The working temperature of the new sensor can be reduced as low as 100°C. The low working temperature posse advantages such as lower power consumption, lower thermal induced signal shift as well as safe detection in certain environments where temperature is strictly limited.

Sol-gel-graphene-based fabric-phase sorptive extraction for cow and human breast milk sample cleanup for screening bisphenol A and residual dental restorative material before analysis by HPLC with diode array detection.

PubMed

Samanidou, Victoria; Filippou, Olga; Marinou, Eirini; Kabir, Abuzar; Furton, Kenneth G

2017-06-01

Fabric-phase sorptive extraction has already been recognized as a simple and green alternative to the conventional sorbent-based sorptive microextraction techniques, using hybrid organic-inorganic sorbent coatings chemically bonded to a flexible fabric surface. Herein, we have investigated the synergistic combination of the advanced material properties offered by sol-gel graphene sorbent and the simplicity of Fabric phase sorptive extraction approach in selectively extracting bisphenol A and residual monomers including bisphenol A glycerolatedimethacrylate, urethane dimethacrylate, and triethylene glycol dimethacrylate derived dental restorative materials from cow and human breast milk samples. Different coatings were evaluated. Final method development employed sol-gel graphene coated media. The main experimental parameters influencing extraction of the compounds, such as sorbent chemistry used, sample loading conditions, elution solvent, sorption stirring time, elution time, impact of protein precipitation, amount of sample, and matrix effect, were investigated and optimized. Absolute recovery values from standard solutions were 50% for bisphenol A, 78% for T triethylene glycol dimethacrylate, 110% for urethane dimethacrylate, and 103% for bisphenol A glycerolatedimethacrylate, while respective absolute recovery values from milk were 30, 52, 104, and 42%. Method validation was performed according to European Decision 657/2002/EC in terms of selectivity, sensitivity, linearity, accuracy, and precision. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-Quality Solution-Processed Silicon Oxide Gate Dielectric Applied on Indium Oxide Based Thin-Film Transistors.

PubMed

Jaehnike, Felix; Pham, Duy Vu; Anselmann, Ralf; Bock, Claudia; Kunze, Ulrich

2015-07-01

A silicon oxide gate dielectric was synthesized by a facile sol-gel reaction and applied to solution-processed indium oxide based thin-film transistors (TFTs). The SiOx sol-gel was spin-coated on highly doped silicon substrates and converted to a dense dielectric film with a smooth surface at a maximum processing temperature of T = 350 °C. The synthesis was systematically improved, so that the solution-processed silicon oxide finally achieved comparable break downfield strength (7 MV/cm) and leakage current densities (<10 nA/cm(2) at 1 MV/cm) to thermally grown silicon dioxide (SiO2). The good quality of the dielectric layer was successfully proven in bottom-gate, bottom-contact metal oxide TFTs and compared to reference TFTs with thermally grown SiO2. Both transistor types have field-effect mobility values as high as 28 cm(2)/(Vs) with an on/off current ratio of 10(8), subthreshold swings of 0.30 and 0.37 V/dec, respectively, and a threshold voltage close to zero. The good device performance could be attributed to the smooth dielectric/semiconductor interface and low interface trap density. Thus, the sol-gel-derived SiO2 is a promising candidate for a high-quality dielectric layer on many substrates and high-performance large-area applications.

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.

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.

Novel route for rapid sol-gel synthesis of hydroxyapatite, avoiding ageing and using fast drying with a 50-fold to 200-fold reduction in process time.

PubMed

Ben-Arfa, Basam A E; Salvado, Isabel M Miranda; Ferreira, José M F; Pullar, Robert C

2017-01-01

We have developed an innovative, rapid sol-gel method of producing hydroxyapatite nanopowders that avoids the conventional lengthy ageing and drying processes (over a week), being 200 times quicker in comparison to conventional aqueous sol-gel preparation, and 50 times quicker than ethanol based sol-gel synthesis. Two different sets of experimental conditions, in terms of pH value (5.5 and 7.5), synthesis temperature (45 and 90°C), drying temperature (60 and 80°C) and calcination temperature (400 and 700°C) were explored. The products were characterised by X-ray diffraction (XRD) Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and specific surface area (SSA) measurements. Pure hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 , HAp) was obtained for the powders synthesised at pH7.5 and calcined at 400°C, while biphasic mixtures of HAp/β-tricalcium phosphate (β-Ca 3 (PO 4 ) 2 , TCP) were produced at pH5.5 and (pH7.5 at elevated temperature). The novel rapid drying was up to 200 times faster than conventional drying, only needing 1h with no prior ageing step, and favoured the formation of smaller/finer nanopowders, while producing pure HAp or phase mixtures virtually identical to those obtained from the slow conventional drying method, despite the absence of a slow ageing process. The products of this novel rapid process were actually shown to have smaller crystallite sizes and larger SSA, which should result in increased bioactivity. Copyright © 2016 Elsevier B.V. All rights reserved.

Transparent Glass-Ceramics Produced by Sol-Gel: A Suitable Alternative for Photonic Materials

PubMed Central

Gorni, Giulio; Mosa, Jadra; Balda, Rolindes; Fernández, Joaquin; Durán, Alicia; Castro, Yolanda

2018-01-01

Transparent glass-ceramics have shown interesting optical properties for several photonic applications. In particular, compositions based on oxide glass matrices with fluoride crystals embedded inside, known as oxyfluoride glass-ceramics, have gained increasing interest in the last few decades. Melt-quenching is still the most used method to prepare these materials but sol-gel has been indicated as a suitable alternative. Many papers have been published since the end of the 1990s, when these materials were prepared by sol-gel for the first time, thus a review of the achievements obtained so far is necessary. In the first part of this paper, a review of transparent sol-gel glass-ceramics is made focusing mainly on oxyfluoride compositions. Many interesting optical results have been obtained but very little innovation of synthesis and processing is found with respect to pioneering papers published 20 years ago. In the second part we describe the improvements in synthesis and processing obtained by the authors during the last five years. The main achievements are the preparation of oxyfluoride glass-ceramics with a much higher fluoride crystal fraction, at least double that reported up to now, and the first synthesis of NaGdF4 glass-ceramics. Moreover, a new SiO2 precursor was introduced in the synthesis, allowing for a reduction in the treatment temperature and favoring hydroxyl group removal. Interesting optical properties demonstrated the incorporation of dopant ions in the fluoride crystals, thus obtaining crystal-like spectra along with higher efficiencies with respect to xerogels, and hence demonstrating that these materials are a suitable alternative for photonic applications. PMID:29385706

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

NASA Technical Reports Server (NTRS)

Mukherjee, S. P.

1980-01-01

The alkali-borosilicate system was selected as the glass system for the preparation of ultrapure low loss glasses suitable for optical communication. The effect of different oxide contents on the absorption loss was critically reviewed. One composition was chosen to develop the gel preparation procedure in the alkali-borosilicate system. In addition, several procedures for the preparation of gels based on two different approaches were developed. The influence of different preparation parameters were investigated qualitatively. Several conclusions are drawn from the results.

Spherical LDH-Ag°-montmorillonite heterocoagulated system with a pH-dependent sol-gel structure for controlled accessibility of AgNPs immobilized on the clay lamellae.

PubMed

Deák, Ágota; Janovák, László; Tallósy, Szabolcs Péter; Bitó, Tamás; Sebők, Dániel; Buzás, Norbert; Pálinkó, István; Dékány, Imre

2015-02-17

Aqueous suspensions of spherical ZnMgAl-layered double hydroxides [LDH(sph)] and antibacterial silver nanoparticles (AgNPs) deposited on the lamellae of montmorillonite were used for the synthesis of composites, which behave like coherent gels at low pH (≲4.5) and incoherent sols at higher pH (≳4.5). The composition of the composite was chosen as LDH(sph)/Ag°-montm. = 25:75 wt % in order to ensure a sol-gel transition that can also be characterized by viscometry. This pH-sensitive heterocoagulated system consisting of oppositely charged colloid particles was suitable for the release of antimicrobial AgNPs immobilized on the clay lamellae via a pH-controlled gel-sol transition. The heterocoagulation process was also characterized by surface charge titration measurements. Spherical LDH/Ag°-montmorillonite composite samples were identified by X-ray diffraction (XRD) measurements. The morphological properties of the composites were studied, and the presence of the heterocoagulated structure was confirmed by scanning electron microscopy (SEM). The nanoscale structure of the LDH(sph)-Ag°-montmorillonite composite obtained was also verified by small-angle X-ray scattering (SAXS), and the rheological characteristics were studied at various pH values. The viscosity and yield value of the composite decreased by an order of magnitude upon increasing the pH from 3.0 to 5.5. The sol-gel transition of the composite suspension was reversible in the previously mentioned pH range.

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.

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.

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

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.

Sol-gel-Derived nano-sized double layer anti-reflection coatings (SiO2/TiO2) for low-cost solar cell fabrication.

PubMed

Lee, Seung Jun; Hur, Man Gyu; Yoon, Dae Ho

2013-11-01

We investigate nano-sized double layer anti-reflection coatings (ARCs) using a TiO2 and SiO2 sol-gel solution process for mono-crystalline silicon solar cells. The process can be easily adapted for spraying sol-gel coatings to reduce manufacturing cost. The spray-coated SiO2/TiO2 nano-sized double layer ARCs were deposited on mono-crystalline silicon solar cells, and they showed good optical properties. The spray coating process is a lower-cost fabrication process for large-scale coating than vacuum deposition processes such as PECVD. The measured average optical reflectance (300-1200 nm) was about approximately 8% for SiO2/TiO2 nano-sized double layer ARCs. The electrical parameters of a mono-crystalline silicon solar cell and reflection losses show that the SiO2/TiO2 stacks can improve cell efficiency by 0.2% compared to a non-coated mono-crystalline silicon solar cell. In the results, good correlation between theoretical and experimental data was obtained. We expect that the sol-gel spray-coated mono-crystalline silicon solar cells have high potential for low-cost solar cell fabrication.

[Effect of silicon coating on bonding strength of ceramics and titanium].

PubMed

Zhou, Shu; Wang, Yu; Zhang, Fei-Min; Guang, Han-Bing

2009-06-01

This study investigated the effect of silicon coating (SiO2) by solution-gelatin (Sol-Gel) technology on bonding strength of titanium and ceramics. Sixteen pure titanium specimens with the size of 25 mm x 3 mm x 0.5 mm were divided into two groups (n=8), test group was silicon coated by Sol-Gel technology, the other one was control group. The middle area of the samples were veneered with Vita Titankeramik system, the phase composition of two specimens were characterized by X-ray diffraction (XRD). The bonding strength of titanium/porcelain was evaluated using three-point bending test. The interface of titanium and porcelain and fractured titanium surface were investigated by scanning electron microscope (SEM) with energy depressive spectrum (EDS). Contents of surface silicon increased after modification with silicon coated by Sol-Gel technology. The mean bonding strength of test group and control group were (37.768 +/- 0.777) MPa and (29.483 +/- 1.007) MPa. There was a statistically significant difference (P=0.000) between them. The bonded ceramic boundary of test group was wider than control group. Silicon coating by Sol-Gel technology was significant in improving bonding strength of titanium/Vita Titankeramik system.

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.

Microwave sintering of sol-gel derived abrasive grain

DOEpatents

Plovnick, Ross; Celikkaya, Ahmet; Blake, Rodger D.

1997-01-01

A method is provided for making microwave-sintered, free flowing alpha alumina-based ceramic abrasive grain, under conditions effective to couple microwaves with calcined alpha alumina-based abrasive gain precursor and sinter it at a temperature of at least about 1150.degree. C.

Encapsulation of nanoclusters in dried gel materials via an inverse micelle/sol gel synthesis

DOEpatents

Martino, Anthony; Yamanaka, Stacey A.; Kawola, Jeffrey S.; Showalter, Steven K.; Loy, Douglas A.

1998-01-01

A dried gel material sterically entrapping nanoclusters of a catalytically active material and a process to make the material via an inverse micelle/sol-gel synthesis. A surfactant is mixed with an apolar solvent to form an inverse micelle solution. A salt of a catalytically active material, such as gold chloride, is added along with a silica gel precursor to the solution to form a mixture. To the mixture are then added a reducing agent for the purpose of reducing the gold in the gold chloride to atomic gold to form the nanoclusters and a condensing agent to form the gel which sterically entraps the nanoclusters. The nanoclusters are normally in the average size range of from 5-10 nm in diameter with a monodisperse size distribution.

Optical Constants of Crystallized TiO2 Coatings Prepared by Sol-Gel Process

PubMed Central

Wang, Xiaodong; Wu, Guangming; Zhou, Bin; Shen, Jun

2013-01-01

Titanium oxide coatings have been deposited by the sol-gel dip-coating method. Crystallization of titanium oxide coatings was then achieved through thermal annealing at temperatures above 400 °C. The structural properties and surface morphology of the crystallized coatings were studied by micro-Raman spectroscopy and atomic force microscopy, respectively. Characterization technique, based on least-square fitting to the measured reflectance and transmittance spectra, is used to determine the refractive indices of the crystallized TiO2 coatings. The stability of the synthesized sol was also investigated by dynamic light scattering particle size analyzer. The influence of the thermal annealing on the optical properties was then discussed. The increase in refractive index with high temperature thermal annealing process was observed, obtaining refractive index values from 1.98 to 2.57 at He-Ne laser wavelength of 633 nm. The Raman spectroscopy and atomic force microscopy studies indicate that the index variation is due to the changes in crystalline phase, density, and morphology during thermal annealing. PMID:28811410

Optical Constants of Crystallized TiO₂ Coatings Prepared by Sol-Gel Process.

PubMed

Wang, Xiaodong; Wu, Guangming; Zhou, Bin; Shen, Jun

2013-07-12

Titanium oxide coatings have been deposited by the sol-gel dip-coating method. Crystallization of titanium oxide coatings was then achieved through thermal annealing at temperatures above 400 °C. The structural properties and surface morphology of the crystallized coatings were studied by micro-Raman spectroscopy and atomic force microscopy, respectively. Characterization technique, based on least-square fitting to the measured reflectance and transmittance spectra, is used to determine the refractive indices of the crystallized TiO₂ coatings. The stability of the synthesized sol was also investigated by dynamic light scattering particle size analyzer. The influence of the thermal annealing on the optical properties was then discussed. The increase in refractive index with high temperature thermal annealing process was observed, obtaining refractive index values from 1.98 to 2.57 at He-Ne laser wavelength of 633 nm. The Raman spectroscopy and atomic force microscopy studies indicate that the index variation is due to the changes in crystalline phase, density, and morphology during thermal annealing.

s-Triazine and tri-s-triazine based organic-inorganic hybrid gels prepared from chlorosilanes by exchange reactions.

PubMed

El-Gamel, Nadia E A; Schwarz, Marcus; Brendler, Erica; Kroke, Edwin

2006-12-07

Hybrid polymers [(DeltaO3)4Si3]n and [(DeltaO3)SiMe]n (where Delta = C6N7 or C3N3) have been prepared by a novel sol-gel process based on exchange reactions of MeSiCl3 or SiCl4 with C6N7(OSiMe3)3 and C3N3(OSiMe3)3.

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.

Sol-gel synthesis and adsorption properties of mesoporous manganese oxide

NASA Astrophysics Data System (ADS)

Ivanets, A. I.; Kuznetsova, T. F.; Prozorovich, V. G.

2015-03-01

Sol-gel synthesis of mesoporous xerogels of manganese oxide with different phase compositions has been performed. The manganese oxide sols were obtained by redox reactions of potassium permanganate with hydrogen peroxide or manganese(II) chloride in aqueous solutions. The isotherms of the low-temperature adsorption-desorption of nitrogen with manganese oxide xerogels treated at 80, 200, 400, and 600°C were measured. The samples were studied by electron microscopy and thermal and XRD analysis. The phase transformation and the changes in the adsorption and capillary-condensation properties of manganese oxide were shown to depend on the sol synthesis conditions and the temperature of the thermal treatment of the gel. The X-ray amorphous samples heated at 80°C were shown to have low values of the specific surface; at higher temperatures, the xerogel crystallized into mixed phases with various compositions and its surface area increased at 200-400°C and decreased at 600°C.

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.

Transparent organic/inorganic hybrid sol-gel materials based on perfluorinated polymers and silica

NASA Astrophysics Data System (ADS)

Wojcik, Anna B.; Klein, Lisa C.

1996-01-01

Two types of hybrid gels based on silica and perfluorinated polymers have been prepared. The first type involves a perfluorinated polymer containing acrylate groups. Perfluoropolyether diol diacrylate (PFDA) was functionalized by reacting it with (3-mercapto-propyl) trimethoxysilane by a Michael addition. The resulting silyl derivative (PFDAS) was able to copolymerize with a silica precursor, tetraethylorthosilicate (TEOS), resulting in perfluorinated polymer/silica hybrid gels. For the second type, perfluoroalkylsilane (FAS), vinyltriethoxysilane (VTES), and TEOS were polymerized in one step. In both cases, the gels were transparent, crack-free and water repellent. Since the inorganic and organic components are covalently bonded to each other, these materials can be classified as organic/inorganic copolymers.

Sol-gel dip coating of yttria-stabilized tetragonal zirconia dental ceramic by aluminosilicate nanocomposite as a novel technique to improve the bonding of veneering porcelain.

PubMed

Madani, Azamsadat; Nakhaei, Mohammadreza; Karami, Parisa; Rajabzadeh, Ghadir; Salehi, Sahar; Bagheri, Hossein

2016-01-01

The aim of this in vitro study was to evaluate the effect of silica and aluminosilicate nanocomposite coating of zirconia-based dental ceramic by a sol-gel dip-coating technique on the bond strength of veneering porcelain to the yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) in vitro. Thirty Y-TZP blocks (10 mm ×10 mm ×3 mm) were prepared and were assigned to four experimental groups (n=10/group): C, without any further surface treatment as the control group; S, sandblasted using 110 μm alumina powder; Si, silica sol dip coating + calcination; and Si/Al, aluminosilicate sol dip coating + calcination. After preparing Y-TZP samples, a 3 mm thick layer of the recommended porcelain was fired on the coated Y-TZP surface. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray analysis were used to characterize the coating and the nature of the bonding between the coating and zirconia. To examine the zirconia-porcelain bond strength, a microtensile bond strength (μTBS) approach was chosen. FT-IR study showed the formation of silica and aluminosilicate materials. XRD pattern showed the formation of new phases consisting of Si, Al, and Zr in coated samples. SEM showed the formation of a uniform coating on Y-TZP samples. Maximum μTBS values were obtained in aluminosilicate samples, which were significantly increased compared to control and sandblasted groups (P=0.013 and P<0.001, respectively). This study showed that aluminosilicate sol-gel dip coating can be considered as a convenient, less expensive reliable method for improving the bond strength between dental Y-TZP ceramics and veneering porcelain.

[Surface modification of dental alumina ceramic with silica coating].

PubMed

Xie, Hai-Feng; Zhang, Fei-Min; Wang, Xiao-Zu; Xia, Yang

2006-12-01

To make silica coating through sol-gel process, and to evaluate the wettability of dental alumina ceramic with or without coating. Silica coating was prepared with colloidal silica sol on In-Ceram alumina ceramic surface which had been treated with air particle abrasion. Coating gel after heat treatment was observed with atomic force microscope (AFM), and was analyzed by infrared spectrum (IR) with gel without sintered as control. Contact angles of oleic acid to be finished, sandblasted and coated ceramic surface of were measured. AFM pictures showed that some parts of nano-particles in coating gel conglomerated after heat treatment. It can be seen from the IR picture that bending vibration absorption kurtosis of Si-OH also vanished after heat treatment. Among contact angles of three treated surface, the ones on polished surface were the biggest (P = 0.000, P = 0.000), and sandblasting+silica coating surface the smallest (P = 0.000, P = 0.003). Silica coating can be made with sol-gel process successfully. Heat treatment may reinforce Si-O-Si net structure of coating gel. Wettability of dental alumina ceramic with silica coating is higher than with sandblasting and polishing.

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

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.

Characterization of the Sol-Gel Transition for Zirconia-Toughened Alumina Precursors

NASA Technical Reports Server (NTRS)

Moeti, I.; Karikari, E.; Chen, J.

1998-01-01

High purity ZTA ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and theological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. In all experimental cases a-alumina and tetragonal zirconia phases were confirmed even in the absence of yttria.

High-mobility low-temperature ZnO transistors with low-voltage operation

NASA Astrophysics Data System (ADS)

Bong, Hyojin; Lee, Wi Hyoung; Lee, Dong Yun; Kim, Beom Joon; Cho, Jeong Ho; Cho, Kilwon

2010-05-01

Low voltage high mobility n-type thin film transistors (TFTs) based on sol-gel processed zinc oxide (ZnO) were fabricated using a high capacitance ion gel gate dielectric. The ion gel gated solution-processed ZnO TFTs were found to exhibit excellent electrical properties. TFT carrier mobilities were 13 cm2/V s, ON/OFF current ratios were 105, regardless of the sintering temperature used for the preparation of the ZnO thin films. Ion gel gated ZnO TFTs are successfully demonstrated on plastic substrates for the large area flexible electronics.

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.

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.

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.

Nano-scale optical circuits and self-organized lightwave network (SOLNET) fabricated using sol-gel materials with photo-induced refractive index increase

NASA Astrophysics Data System (ADS)

Ono, Shigeru; Yoshimura, Tetsuzo; Sato, Tetsuo; Oshima, Juro

2009-02-01

Recently, Nissan Chemical Industries, LTD, developed the photo-induced refractive index variation sol-gel materials, in which the refractive index increases from 1.65 to 1.85 by ultra-violet (UV) light exposure and baking. The materials enable us to fabricate high-index-contract waveguides without developing/etching processes and strong-lightconfinement self-organized lightwave network (SOLNET). Therefore, the materials are expected promising for nanoscale optical circuits with self-alignment capability. Nano-scale optical circuits with core thickness of ~230 nm and core width of ~1 μm were fabricated. Propagation loss was 1.86 dB/cm for TE mode and 1.89 dB/cm for TM mode at 633 nm in wavelength, indicating that there were small polarization dependences. Spot sizes of guided beams along core width direction and along core thickness direction were respectively 0.6 μm and 0.3 μm for both TE and TM mode. Bending loss of S-bending waveguides was reduced from 0.44 dB to 0.24 dB for TE mode with increasing the bending curvature radius from 5 μm to 60 μm. Difference in bending loss between TM and TE mode was less than 10%. Branching loss of Y-branching waveguides was reduced from 1.33 dB to 0.08 dB for TE mode, and from 1.34 dB to 0.12 dB for TM mode with decreasing the branching angle from 80° to 20°. These results indicate that the photoinduced refractive index variation sol-gel materials can realize miniaturized optical circuits with sizes of several tens μm and guided beam confinement within a cross-section area less than 1.0 μm2 with small polarization dependences, suggesting potential applications to intra-chip optical interconnects. In addtion, we fabricated self-organized lightwave network (SOLNET) using the photo-induced refractive index variation sol-gel materials. When write beams of 405 nm in wavelength were introduced into the sol-gel thin film under baking at 200°C, self-focusing was induced, and SOLNET was formed. SOLNET fabricated by low write beam intensity exhibited strong light confinement. Furthermore, SOLNET was found to be drawn automatically to reflective portion such as a defect and a silver paste droplet in the sol-gel thin film during SOLNET formation, indicating that reflective SOLNET is formed. The results suggest that the photo-induced refractive index variation sol-gel materials can provide self-alignment capability to the nano-scale optical circuits.

Photostability and moisture uptake properties of wood veneers coated with a combination of thin sol-gel films and light stabilizers

Treesearch

Mandla A. Tshabalala; Ryan Libert; Christian M. Schaller

2011-01-01

In recent years, there has been increased interest in the use of inorganic UV blocking nanoparticles for photostabilization of wood surfaces. Photostability and moisture uptake properties of wood veneers coated with a combination of hybrid inorganic-organic thin sol-gel films and organic light stabilizers was investigated. The light stabilizers were applied by brushing...

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.

Recent advances in preparation and application of hybrid organic-silica monolithic capillary columns.

PubMed

Ou, Junjie; Lin, Hui; Zhang, Zhenbin; Huang, Guang; Dong, Jing; Zou, Hanfa

2013-01-01

Hybrid organic-silica monolithic columns, regarded as a second generation of silica-based monoliths, have received much interest due to their unique properties over the pure silica-based monoliths. This review mainly focuses on development in the fields of preparation of hybrid monolithic columns in a capillary and their application for CEC and capillary liquid chromatography separation, as well as for sample pretreatment of solid-phase microextraction and immobilized enzyme reactor since July 2010. The preparation approaches are comprehensively summarized with three routes: (i) general sol-gel process using trialkoxysilanes and tetraalkoxysilanes as coprecursors; (ii) "one-pot" process of alkoxysilanes and organic monomers concomitantly proceeding sol-gel chemistry and free radical polymerization; and (iii) other polymerization approaches of organic monomers containing silanes. The modification of hybrid monoliths containing reactive groups to acquire the desired surface functionality is also described. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrochemical Study and Characterization of an Amperometric Biosensor Based on the Immobilization of Laccase in a Nanostructure of TiO₂ Synthesized by the Sol-Gel Method.

PubMed

Romero-Arcos, Mariana; Garnica-Romo, Ma Guadalupe; Martínez-Flores, Héctor Eduardo

2016-07-07

Laccase amperometric biosensors were developed to detect the catechol compound. The laccase enzyme (LAC) immobilization was performed on nanostructures of (a) titania (TiO₂); (b) titania/Nafion (TiO₂/NAF) (both immobilized by the sol-gel method) and a third nanostructure, which consisted of a single biosensor composite of Nafion and laccase enzyme denoted as NAF/LAC. The Nafion was deposited on a graphite electrode and used to avoid "cracking" on the matrix. The TiO₂ particle size was an average of 66 nm. FTIR spectroscopy vibration modes of different composites were determined. The electrochemical behavior of the biosensor was studied using electrochemical spectroscopy (EIS) and cyclic voltammetry (CV). The biosensor based on TiO₂/NAF/LAC presented the best electro-chemical properties with regard to sensitivity, stability and detection limit after a period of 22 days.

A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

PubMed

Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

2010-01-01

A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

“Beating speckles” via electrically-induced vibrations of Au nanorods embedded in sol-gel

PubMed Central

Ritenberg, Margarita; Beilis, Edith; Ilovitsh, Asaf; Barkai, Zehava; Shahmoon, Asaf; Richter, Shachar; Zalevsky, Zeev; Jelinek, Raz

2014-01-01

Generation of macroscopic phenomena through manipulating nano-scale properties of materials is among the most fundamental goals of nanotechnology research. We demonstrate cooperative “speckle beats” induced through electric-field modulation of gold (Au) nanorods embedded in a transparent sol-gel host. Specifically, we show that placing the Au nanorod/sol-gel matrix in an alternating current (AC) field gives rise to dramatic modulation of incident light scattered from the material. The speckle light patterns take form of “beats”, for which the amplitude and frequency are directly correlated with the voltage and frequency, respectively, of the applied AC field. The data indicate that the speckle beats arise from localized vibrations of the gel-embedded Au nanorods, induced through the interactions between the AC field and the electrostatically-charged nanorods. This phenomenon opens the way for new means of investigating nanoparticles in constrained environments. Applications in electro-optical devices, such as optical modulators, movable lenses, and others are also envisaged. PMID:24413086

Ultrafast Sol-Gel Synthesis of Graphene Aerogel Materials

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

Lim, Mathew; Hu, Matthew; Manandhar, Sandeep

2015-12-01

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

Gelatin/nano-hydroxyapatite hydrogel scaffold prepared by sol-gel technology as filler to repair bone defects.

PubMed

Raucci, Maria Grazia; Demitri, Christian; Soriente, Alessandra; Fasolino, Ines; Sannino, Alessandro; Ambrosio, Luigi

2018-03-25

This study reports on the development of a scaffold with a gradient of bioactive solid signal embedded in the biodegradable polymer matrix by combining a sol-gel approach and freeze-drying technology. The chemical approach based on the sol-gel transition of calcium phosphates ensures the particles dispersion into the gelatin matrix and a direct control of interaction among COOH gelatin /Ca 2+ ions. Morphological analysis demonstrated that on the basis of the amount of inorganic component and by using specific process conditions, it is possible to control the spatial distribution of nanoparticles around the gelatin helix. In fact, methodology and formulations were able to discriminate between the different hydroxyapatite concentrations and their respective morphology. The good biological response represented by good cell attachment, proliferation and increased levels of alkaline phosphatase as an indicator of osteoblastic differentiation of human mesenchymal stem cells toward the osteogenic lineage, demonstrating the effect of bioactive solid signals on cellular behavior. Furthermore, the inhibition of reactive oxygen species production by composite materials predicted potential anti-inflammatory properties of scaffolds thus confirming their biocompatibility. Indeed, these interesting biological results suggest good potential application of this scaffold as filler to repair bone defects. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part A, 2018. © 2018 Wiley Periodicals, Inc.

Low- and high-index sol-gel films for planar and channel-doped waveguides

NASA Astrophysics Data System (ADS)

Canva, Michael; Chaput, Frederic; Lahlil, Khalid; Rachet, Vincent; Goudket, Helene; Boilot, Jean-Pierre; Levy, Yves

2001-11-01

In view of realizing integrated optic components based on effects such as electro-optic, chi(2):chi(2) cascading, stimulated emission,... one has to first synthesize materials with the proper functionality; this may be achieved by doping solid state matrices by the appropriate organic chromophores. Second, and as important, these materials have to be properly structured into the final optical guiding structures. We shall report on issues related to the realization of chromophore-doped planar waveguides as well as channel waveguides. These structures were realized by either photo-transformation such as photo- chromism and photo-bleaching or reactive ion etching technique, starting with chromophore doped sol-gel materials at high loading contents for which optical index may be controlled via the local dopant concentration. With these materials and techniques, waveguides and components characterized by propagation losses of the order of a cm-1, measured off the edge of the absorption band of the doping species, were fabricated. In order to be also able to study and use waveguide functionalized with low concentration of chromophore species, we developed new sol-gel materials of high optical index, yet low temperature processed. These new films are under study to evaluate their potential as host for organic doped waveguides devices.

Encapsulation of nanoclusters in dried gel materials via an inverse micelle/sol gel synthesis

DOEpatents

Martino, A.; Yamanaka, S.A.; Kawola, J.S.; Showalter, S.K.; Loy, D.A.

1998-09-29

A dried gel material sterically entrapping nanoclusters of a catalytically active material and a process to make the material via an inverse micelle/sol-gel synthesis are disclosed. A surfactant is mixed with an apolar solvent to form an inverse micelle solution. A salt of a catalytically active material, such as gold chloride, is added along with a silica gel precursor to the solution to form a mixture. To the mixture are then added a reducing agent for the purpose of reducing the gold in the gold chloride to atomic gold to form the nanoclusters and a condensing agent to form the gel which sterically entraps the nanoclusters. The nanoclusters are normally in the average size range of from 5--10 nm in diameter with a monodisperse size distribution. 1 fig.

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.

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

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.

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.

Chitosan-silane sol-gel hybrid thin films with controllable layer thickness and morphology.

PubMed

Spirk, Stefan; Findenig, Gerald; Doliska, Ales; Reichel, Victoria E; Swanson, Nicole L; Kargl, Rupert; Ribitsch, Volker; Stana-Kleinschek, Karin

2013-03-01

The preparation of thin films of chitosan-silane hybrid materials by combining sol-gel processing and spin coating is reported. A variety of silanes can be used as starting materials for the preparation of such thin films, namely tetraethoxysilane, tri-tert-butoxysilanol, trimethylethoxysilane, p-trifluoromethyltetra-fluorophenyltriethoxysilane, trivinylmethoxysilane, (methoxymethyl)trimethyl-silane, and hexamethoxydisilane. These silanes are subjected to a sol-gel process before they are added to acidic chitosan solutions. The chitosan:silane ratio is kept constant at 6:1 (w/w) and dilutions with ethanol are prepared and spin coated. Depending on the degree of dilution, film thickness can be controlled in a range between 5 and 70 nm. For the determination of additional surface properties, static water contact angle measurements and atomic force microscopy have been employed. Copyright © 2012 Elsevier Ltd. All rights reserved.

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.

Preparation and characterization of polydimethylsiloxane/poly(vinylalcohol) coated solid phase microextraction fibers using sol-gel technology.

PubMed

Lopes, Alexandre Leite; Augusto, Fabio

2004-11-12

The applicability of a composite composed of polydimethylsiloxane (PDMS) and poly(vinyl alcohol) (PDMS/PVA) as coating sorbent for SPME fibers is demonstrated here. Fused silica (FS) fibers were coated with PDMS/PVA composite through a sol-gel process, using methyltrimethoxysilane as reticulating agent. The chemical and physical properties of the sol-gel PDMS/PVA composite were determined by infrared spectroscopy and thermogravimetric analysis. Electron scanning microscopy of the prepared fibers, showed that the coating obtained was highly microporous, having a thickness of approximately 5 microm. The fibers were tested for the headspace extraction of several organic compounds (o-xylene, naphthalene, ethyl caprate, p-chlorotoluene and PCB) prior to gas chromatographic analysis. The extractive capacity of the PDMS/PVA coating was found to be superior to that of pure conventional PDMS fibers.

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.

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.

Morphology of one-time coated palladium-alumina composite membrane prepared by sol-gel process and electroless plating technique

NASA Astrophysics Data System (ADS)

Sari, R.; Dewi, R.; Pardi; Hakim, L.; Diana, S.

2018-03-01

Palladium coated porous alumina ceramic membrane tube was obtained using a combination of sol-gel process and electroless plating technique. The thickness, structure and composition of palladium-alumina composite membrane were analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM). Palladium particle size was 6.18 to 7.64 nm. Palladium membrane with thickness of approximately 301.5 to 815.1 nm was formed at the outer surface of the alumina layer. EDX data confirmed the formation of palladium-alumina membrane containing 45% of palladium. From this research it shows the combination of sol-gel process and electroless plating technique with one-time coating can produce a homogeneous and smoother palladium nano layer film on alumina substrate.

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.

Enhanced optical band-gap of ZnO thin films by sol-gel technique

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

Raghu, P., E-mail: dpr3270@gmail.com; Naveen, C. S.; Shailaja, J.

2016-05-06

Transparent ZnO thin films were prepared using different molar concentration (0.1 M, 0.2 M & 0.8 M) of zinc acetate on soda lime glass substrates by the sol-gel spin coating technique. The optical properties revealed that the transmittance found to decrease with increase in molar concentration. Absorption edge showed that the higher concentration film has increasingly red shifted. An increased band gap energy of the thin films was found to be direct allowed transition of ∼3.9 eV exhibiting their relevance for photovoltaic applications. The extinction coefficient analysis revealed maximum transmittance with negligible absorption coefficient in the respective wavelengths. The resultsmore » of ZnO thin film prepared by sol-gel technique reveal its suitability for optoelectronics and as a window layer in solar cell applications.« less

Bioactivity of gel-glass powders in the CaO-SiO2 system: a comparison with ternary (CaO-P2O5-SiO2) and quaternary glasses (SiO2-CaO-P2O5-Na2O).

PubMed

Saravanapavan, Priya; Jones, Julian R; Pryce, Russell S; Hench, Larry L

2003-07-01

Bioactive glasses react chemically with body fluids in a manner that is compatible with the repair processes of the tissues. This results in the formation of an interfacial bond between the glasses and living tissue. Bioactive glasses also stimulate bone-cell proliferation. This behavior is dependent on the chemical composition as well as the surface texture of the glasses. It has been recently reported that gel-derived monolith specimens in the binary SiO2 - CaO are bioactive over a similar molar range of SiO2 content as the previously studied ternary CaO-P2O5-SiO2 system. In this report, the preparation and bioactivity of the binary gel-glass powder with 70 mol % SiO2 is discussed and its bioactivity is compared with the melt-derived 45S5 (quaternary) Bioglass and sol-gel-derived 58S (ternary) bioactive gel-glass compositions. Dissolution kinetic parameters K(1) and K(2) were also computed based on the silicon release for all glass powders. It was shown that the simple two-component SiO2-CaO gel-glass powder is bioactive with comparable dissolution rates as the clinically used melt-derived 45S5 Bioglass powder and extensively studied sol-gel-derived 58S gel-glass powder. Copyright 2003 Wiley Periodicals, Inc.

Organic/inorganic hybrid coatings for anticorrosion

NASA Astrophysics Data System (ADS)

He, Zhouying

Compared to organic coatings, organic-inorganic hybrid coatings can potentially improve the anticorrosion performance. The organic phase provides the excellent mechaincal and barrier properties while the inorganic phase acts as an adhesion promoter and corrosion inhibitor. Despite that many studies on alkoxylsilane-based hybrid coatings have been developed and studied, their weatherability and anticorrosion performance has been rarely evaluated. On the other hand, organic-inorganic hybrid coatings based on mixed sol-gel precursors have received much less attention compared to alkoxylsilane-based hybrid coatings. In the first part, polyurethane hybrid coatings with a unique hybrid crosslinked structure as an improved unicoat were successfully prepared. The effect of polyesters on physical properties of the hybrid coatings was studied. Polyurethane coatings derived from cycloaliphatic polyester show comparable properties than those derived from the commercially viable aromatic polyester. Introducing the polysiloxane part into the polyurethane coatings enhanced the crosslinking density, Tg, mechanical properties, and general coating properties. The increased adhesion between the hybrid coating and the substrate make the hybrid coating a good candidate for anticorrosion application, which is shown by electrochemical impedance spectroscopy (EIS). The degradation mechanism of the polyurethane/polysiloxane hybrid coatings under various weathering conditions was shown to be the scission of the urethane and ester groups in the organic phase along with reorganizing and rearranging of the inorganic phase. The anticorrosion performance of the cycloaliphatic hybrid was much better than that of aromatic based hybrid under outdoor weathering based on visual observation and EIS analysis. Acid undercutting is an issue for TEOS based hybrid coating. In the second part, design of experiments (DOEs) was used to statistically investigate on the effect of sol-gel precursors. The synergistic effect of the mixed sol-gel precursors was shown to enhance the overall properties and was also observed structurally by SAXS and SEM. The improved resistance to the acid undercutting was observed for mixed sol-gel precursors based hybrids. The application of hybrids provides excellent anticorrosive properties as observed in salt spray and EIS study. The formation of Al2O3 protective layer as well as M-O-Al covalent bond provided the basis for excellent corrosion protection on Al substrate. However, the generation of Fe ions as corrosion product caused the accumulation of electrolyte, which resulted in the delamination of the coating on steel substrate. In this way, the corrosion of steel substrate is much faster than that of Al substrate. The maintenance of high impedance and corresponding resistance and capacitance based on EIS results further confirmed the great anticorrosion performance of hybrids on both Al and steel substrate.

Dynamic light-scattering study of gelatin and aggregation of gastric mucin

NASA Astrophysics Data System (ADS)

Bansil, Rama; Cao, Xingxiang; Bhaskar, K. Ramakrishnan; LaMont, Jeffrey T.

1997-05-01

Dynamic light scattering studies show that concentration and pH play important roles in determining pig gastric mucin's (PGM) ability to aggregate and gel. At low concentrations, PGM macromolecules exist in solution predominantly in the form of monomers. At high concentrations, PGM macromolecules aggregate to form supra-macromolecular clusters. When the pH of the high concentration PGM solution is changed from 7.0 to 2.0, the system undergoes a sol-gel transition: from a solution of polydisperse aggregates to a gel. This pH and concentration dependent sol-gel transition of PGM solution may provide a mechanism for the mammalian stomach to protect itself against being digested by the gastric juice.

[In vitro evaluation of the gels properties prepared on Pluronic F-127 as vehicles for administration prolactin by injection].

PubMed

Karolewicz, Bozena; Pawlik-Gałczyńska, Anna; Pluta, Janusz; Ryszka, Florian

2011-01-01

The aim of this study was to prepare a thermoresponsive formulations, which are a carrier for proteins--prolactin administered directly into solid tumor and which obtain sol-gel transitions at physiological ranges of temperature. Prolactin (PRL) is a hormone that in vivo and in vitro exhibits antiangiogenic properties. Application of this protein in the proposed formulations can be particularly advantageous because of its relatively low stability and limited ability to transmembrane penetration. The paper prepared thermoresponsive carriers, based on nonionic polymer Pluronic F-127 with selected excipients such as dextran 7000, PEG 400, Tween 20 and Tween 80. The sol-gel transition temperature of the formulations was investigated and their physicochemical properties such as pH, density, osmotic pressure were studied. In the remainder of the work carried out tests of prolactin release from the proposed media. The results obtained indicate that a significant influence on the theological parameters obtained carriers and the availability of pharmaceutical composition of prolactin was developed formulation.

Well-aligned Vertically Oriented ZnO Nanorod Arrays and their Application in Inverted Small Molecule Solar Cells.

PubMed

Lin, Ming-Yi; Wu, Shang-Hsuan; Hsiao, Li-Jen; Budiawan, Widhya; Chen, Shih-Lun; Tu, Wei-Chen; Lee, Chia-Yen; Chang, Yia-Chung; Chu, Chih-Wei

2018-04-25

This manuscript describes how to design and fabricate efficient inverted solar cells, which are based on a two-dimensional conjugated small molecule (SMPV1) and [6,6]-phenyl-C71-butyric acid methyl ester (PC71BM), by utilizing ZnO nanorods (NRs) grown on a high quality Al-doped ZnO (AZO) seed layer. The inverted SMPV1:PC71BM solar cells with ZnO NRs that grew on both a sputtered and sol-gel processed AZO seed layer are fabricated. Compared with the AZO thin film prepared by the sol-gel method, the sputtered AZO thin film exhibits better crystallization and lower surface roughness, according to X-ray diffraction (XRD) and atomic force microscope (AFM) measurements. The orientation of the ZnO NRs grown on a sputtered AZO seed layer shows better vertical alignment, which is beneficial for the deposition of the subsequent active layer, forming better surface morphologies. Generally, the surface morphology of the active layer mainly dominates the fill factor (FF) of the devices. Consequently, the well-aligned ZnO NRs can be used to improve the carrier collection of the active layer and to increase the FF of the solar cells. Moreover, as an anti-reflection structure, it can also be utilized to enhance the light harvesting of the absorption layer, with the power conversion efficiency (PCE) of solar cells reaching 6.01%, higher than the sol-gel based solar cells with an efficiency of 4.74%.

Quasi-distributed sol-gel coated fiber optic oxygen sensing probe

NASA Astrophysics Data System (ADS)

Zolkapli, Maizatul; Saharudin, Suhairi; Herman, Sukreen Hana; Abdullah, Wan Fazlida Hanim

2018-03-01

In the field of aquaculture, optical sensor technology is beginning to provide alternatives to the conventional electrical sensor. Hence, the development and characterization of a multipoint quasi-distributed optical fiber sensor for oxygen measurement is reported. The system is based on 1 mm core diameter plastic optical fiber where sections of cladding have been removed and replaced with three metal complexes sol-gel films to form sensing points. The sensing locations utilize luminophores that have emission peaks at 385 nm, 405 nm and 465 nm which associated with each of the sensing points. Interrogation of the optical sensor system is through a fiber optic spectrometer incorporating narrow bandpass emission optical filter. The sensors showed comparable sensitivity and repeatability, as well as fast response and recovery towards oxygen.

Stability Improvements of DNA Photonic Devices

DTIC Science & Technology

2008-12-20

possible in such areas as photonics, separation process or biomedical materials . Recent research results on DNA-lipid complexes have shown various...onto Teflon- coated glass plate to obtain films by irradiating UV light to cause crosslinking reactions of the Adeka sol-gel materials Clear and...into sol-gel materials or synthetic polymers so that water permeation is prevented by glass or synthetic polymers to stabilize and to keep the optical

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.

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 Material-Enabled Electro-Optic Polymer Modulators

PubMed Central

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

2015-01-01

Sol-gels are an important material class, as they provide easy modification of material properties, good processability and are easy to synthesize. In general, an electro-optic (EO) modulator transforms an electrical signal into an optical signal. The incoming electrical signal is most commonly information encoded in a voltage change. This voltage change is then transformed into either a phase change or an intensity change in the light signal. The less voltage needed to drive the modulator and the lower the optical loss, the higher the link gain and, therefore, the better the performance of the modulator. In this review, we will show how sol-gels can be used to enhance the performance of electro-optic modulators by allowing for designs with low optical loss, increased poling efficiency and manipulation of the electric field used for driving the modulator. The optical loss is influenced by the propagation loss in the device, as well as the losses occurring during fiber coupling in and out of the device. In both cases, the use of sol-gel materials can be beneficial due to the wide range of available refractive indices and low optical attenuation. The influence of material properties and synthesis conditions on the device performance will be discussed. PMID:26225971

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.

Low cost sol-gel derived SiC-SiO2 nanocomposite as anti reflection layer for enhanced performance of crystalline silicon solar cells

NASA Astrophysics Data System (ADS)

Jannat, Azmira; Lee, Woojin; Akhtar, M. Shaheer; Li, Zhen Yu; Yang, O.-Bong

2016-04-01

This paper describes the preparation, characterizations and the antireflection (AR) coating application in crystalline silicon solar cells of sol-gel derived SiC-SiO2 nanocomposite. The prepared SiC-SiO2 nanocomposite was effectively applied as AR layer on p-type Si-wafer via two step processes, where the sol-gel of precursor solution was first coated on p-type Si-wafer using spin coating at 2000 rpm and then subjected to annealing at 450 °C for 1 h. The crystalline, and structural observations revealed the existence of SiC and SiO2 phases, which noticeably confirmed the formation of SiC-SiO2 nanocomposite. The SiC-SiO2 layer on Si solar cells was found to be an excellent AR coating, exhibiting the low reflectance of 7.08% at wavelengths ranging from 400 to 1000 nm. The fabricated crystalline Si solar cell with SiC-SiO2 nanocomposite AR coating showed comparable power conversion efficiency of 16.99% to the conventional SixNx AR coated Si solar cell. New and effective sol-gel derived SiC-SiO2 AR layer would offer a promising technique to produce high performance Si solar cells with low-cost.

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

Biodegradable and adjustable sol-gel glass based hybrid scaffolds from multi-armed oligomeric building blocks.

PubMed

Kascholke, Christian; Hendrikx, Stephan; Flath, Tobias; Kuzmenka, Dzmitry; Dörfler, Hans-Martin; Schumann, Dirk; Gressenbuch, Mathias; Schulze, F Peter; Schulz-Siegmund, Michaela; Hacker, Michael C

2017-11-01

Biodegradability is a crucial characteristic to improve the clinical potential of sol-gel-derived glass materials. To this end, a set of degradable organic/inorganic class II hybrids from a tetraethoxysilane(TEOS)-derived silica sol and oligovalent cross-linker oligomers containing oligo(d,l-lactide) domains was developed and characterized. A series of 18 oligomers (Mn: 1100-3200Da) with different degrees of ethoxylation and varying length of oligoester units was established and chemical composition was determined. Applicability of an established indirect rapid prototyping method enabled fabrication of a total of 85 different hybrid scaffold formulations from 3-isocyanatopropyltriethoxysilane-functionalized macromers. In vitro degradation was analyzed over 12months and a continuous linear weight loss (0.2-0.5wt%/d) combined with only moderate material swelling was detected which was controlled by oligo(lactide) content and matrix hydrophilicity. Compressive strength (2-30MPa) and compressive modulus (44-716MPa) were determined and total content, oligo(ethylene oxide) content, oligo(lactide) content and molecular weight of the oligomeric cross-linkers as well as material porosity were identified as the main factors determining hybrid mechanics. Cytocompatibility was assessed by cell culture experiments with human adipose tissue-derived stem cells (hASC). Cell migration into the entire scaffold pore network was indicated and continuous proliferation over 14days was found. ALP activity linearly increased over 2weeks indicating osteogenic differentiation. The presented glass-based hybrid concept with precisely adjustable material properties holds promise for regenerative purposes. Adaption of degradation kinetics toward physiological relevance is still an unmet challenge of (bio-)glass engineering. We therefore present a glass-derived hybrid material with adjustable degradation. A flexible design concept based on degradable multi-armed oligomers was combined with an established indirect rapid prototyping method to produce a systematic set of porous sol-gel-derived class II hybrid scaffolds. Mechanical properties in the range of cancellous bone were narrowly controlled by hybrid composition. The oligoester introduction resulted in significantly increased compressive moduli. Cytocompatible hybrids degraded in physiologically relevant time frames and a promising linear and controllable weight loss profile was found. To our knowledge, our degradation study represents the most extensive long-term investigation of sol-gel-derived class II hybrids. Due to the broad adjustability of material properties, our concept offers potential for engineering of biodegradable hybrid materials for versatile applications. Copyright © 2017. Published by Elsevier Ltd.