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Sample records for hybrid sol-gel coat

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

    Science.gov (United States)

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

    2016-10-07

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

  2. Synthesis of hybrid sol-gel coatings for corrosion protection of we54-ae magnesium alloy

    Science.gov (United States)

    Hernández-Barrios, C. A.; Duarte, N. Z.; Hernández, L. M.; Peña, D. Y.; Coy, A. E.; Viejo, F.

    2013-11-01

    The present work shows some preliminary results related to the synthesis, characterization and corrosion evaluation of different hybrid sol-gel coatings applied on the WE54-AE magnesium alloy attending to the two experimental variables, i.e. the precursors ratio and the aging time, which may affect the quality and the electrochemical properties of the coatings resultant. The experimental results confirmed that, under some specific experimental conditions, it was possible to obtain homogeneous and uniform, porous coatings with good corrosion resistance that also permit to accommodate corrosion inhibitors.

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

    Science.gov (United States)

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

    2007-12-15

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

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

    Science.gov (United States)

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

    2011-02-01

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

  5. Hybrid Sol-Gel Coatings: Smart and Green Materials for Corrosion Mitigation

    Directory of Open Access Journals (Sweden)

    Rita B. Figueira

    2016-03-01

    Full Text Available Corrosion degradation of materials and metallic structures is one of the major issues that give rise to depreciation of assets, causing great financial outlays in their recovery and or prevention. Therefore, the development of active corrosion protection systems for metallic substrates is an issue of prime importance. The promising properties and wide application range of hybrid sol-gel-derived polymers have attracted significant attention over recent decades. The combination of organic polymers and inorganic materials in a single phase provides exceptional possibilities to tailor electrical, optical, anticorrosive, and mechanical properties for diverse applications. This unlimited design concept has led to the development of hybrid coatings for several applications, such as transparent plastics, glasses, and metals to prevent these substrates from permeation, mechanical abrasion, and corrosion, or even for decorative functions. Nevertheless, the development of new hybrid products requires a basic understanding of the fundamental chemistry, as well as of the parameters that influence the processing techniques, which will briefly be discussed. Additionally, this review will also summarize and discuss the most promising sol-gel coatings for corrosion protection of steel, aluminium, and their alloys conducted at an academic level.

  6. Sol-gel network silica/modified montmorillonite clay hybrid nanocomposites for hydrophobic surface coatings.

    Science.gov (United States)

    Meera, Kamal Mohamed Seeni; Sankar, Rajavelu Murali; Murali, Adhigan; Jaisankar, Sellamuthu N; Mandal, Asit Baran

    2012-02-01

    Sol-gel silica/nanoclay composites were prepared through sol-gel polymerization technique using tetraethylorthosilicate precursor and montmorillonite (MMT) clay in aqueous media. In this study, both montmorillonite-K(+) and organically modified MMT (OMMT) clays were used. The prepared composites were coated on glass substrate by making 1 wt% solution in ethyltrichlorosilane. The incorporation of nanoclay does not alter the intensity of characteristic Si-O-Si peak of silica network. Thermogravimetric studies show that increasing clay content increased the degradation temperature of the composites. Differential scanning calorimetry (DSC) results of organically modified MMT nanoclay incorporated composite show a shift in the melting behavior up to 38°C. From DSC thermograms, we observed that the ΔH value decreased with increasing clay loading. X-ray diffraction patterns prove the presence of nanoclay in the composite and increase in the concentration of organically modified nanoclay from 3 to 5 wt% increases the intensity of the peak at 2θ=8° corresponds to OMMT. Morphology of the control silica gel composite was greatly influenced by the incorporation of OMMT. The presence of nanoclay changed the surface of control silica gel composite into cleaved surface with brittle in nature. Contact angle measurements were done for the coatings to study their surface behavior. These hybrid coatings on glass substrate may have applications for hydrophobic coatings on leather substrate.

  7. Ceria nanoparticles vis-à-vis cerium nitrate as corrosion inhibitors for silica-alumina hybrid sol-gel coating

    Science.gov (United States)

    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.

  8. Nano rods for coloured glasses obtained by hybrid sol-gel coating.

    Science.gov (United States)

    Veron, Olivier; Blondeau, Jean-Philippe; Moineau, Johanne; Aubert, Pierre-Henri; Vignolle, Caroline Andreazza; Banet, Philippe; Allam, Lévi

    2011-09-01

    Many new materials are now allowing new properties thanks to nanotechnology because this domain of physics gives possibilities to optimize targeted properties even if these materials react in very various influential parameters. Architectural, automotive, bone pathologies, environment, display applications are some concerned domains. The sol-gel process is a method allowing the realisation of coats at ambiant temperature, thus it is possible to realize Liquid Crystal Display (LCD), water-repellent coatings on privacy glass, antireflective coatings, hydrophobic or hydrophilic surfaces, bone tissue regeneration. In this study, the purpose is to show the thermal influence on a covered glass with a complex hybrid sol-gel solution. This coated glass is going to change color from red to orange under the heat influence. This color change effect comes from the evolution of various compounds organizations then/or from their loss during the degassing sequence. We show in spite of the complexity of the process that the responsible is mainly the organic dye. Thus the structure of the heated glass at 250 degrees C looks radically different than the heated one at 350 degrees C. SEM measurement allows to identify the surface compositions and to determine the elementary composition along the sample's cross section. TGA is used to justify a mass loss when samples are annealed. UV/Visible measurement is realized by two methods: in-line transmission to evaluate luminous flux and thus give colorimetric dot in the normalized CIE diagram and diffuse transmission to observe the size influence of the pigments. Infrared Reflectivity allows to evaluate the influence of species on the structure and to better target the nature of the lost compounds during annealing. TEM measurement proves that the obtained iron particles are nano rods for both samples.

  9. Biocompatibility improvement of titanium implants by coating with hybrid materials synthesized by sol-gel technique.

    Science.gov (United States)

    Catauro, M; Bollino, F; Papale, F

    2014-12-01

    Organic-inorganic hybrid materials based on zirconia and polyethylene glycol (PEG) have been synthesized via sol-gel method in the present study. Those materials, still in the sol phase, have been used to coat a titanium grade 4 (Ti-4) substrate to improve its biological properties. Dip-coating technique has been used to obtain thin films. PEG, a biocompatible polymer, used as the organic phase, has been incorporated with different percentages in an inorganic zirconium-based matrix. Those hybrids have been characterized by Fourier transform infrared spectroscopy (FTIR) to detect interactions between the two phases. The films have been examined using SEM to detect morphological changes with PEG percentages. The potential applications of the hybrid coatings in biomedical field have been evaluated by bioactivity and cytotoxicity tests. The coated titanium was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated, as that feature can be used as an index of bone-bonding capability. SEM equipped with energy dispersive spectrometer (EDS) was used to examine hydroxyapatite formation. NIH 3T3 mouse embryonic fibroblast cells were seeded on specimens to evaluate cells-materials interactions and cell vitality was inspected using WST-8 Assay.

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

    Science.gov (United States)

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

    2016-02-17

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

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

    Institute of Scientific and Technical Information of China (English)

    Hamed Rahimi; Reza Mozaffarinia; Akbar Hojjati Najafabadi

    2013-01-01

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

  12. Corrosion resistance of multilayer hybrid sol-gel coatings deposited on the AISI 316L austenitic stainless steel

    Science.gov (United States)

    Caballero, Y. T.; Rondón, E. A.; Rueda, L.; Hernández Barrios, C. A.; Coy, A.; Viejo, F.

    2016-02-01

    In the present work multilayer hybrid sol-gel coatings were synthesized on the AISI 316L austenitic stainless steel employed in the fabrication of orthopaedic implants. Hybrid sols were obtained from a mixture of inorganic precursor, TEOS, and organic, GPTMS, using ethanol as solvent, and acetic acid as catalyst. The characterization of the sols was performed using pH measurements, rheological tests and infrared spectroscopy (FTIR) for different ageing times. On the other hand, the coatings were characterized by scanning electron microscopy (SEM), while the corrosion resistance was evaluated using anodic potentiodynamic polarization in SBF solution at 37±2°C. The results confirmed that sol-gel synthesis employing TEOS-GPTMS systems produces uniform and homogeneous coatings, which enhanced the corrosion resistance with regard to the parent alloy. Moreover, corrosion performance was retained after applying more than one layer (multilayer coatings).

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

    Directory of Open Access Journals (Sweden)

    Rita B. Figueira

    2015-04-01

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

  14. Epoxy Sol-Gel Hybrid Thermosets

    Directory of Open Access Journals (Sweden)

    Angels Serra

    2016-02-01

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

  15. Applications of sol gel ceramic coatings

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-12-31

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

  16. Sol-gel antireflective coating on plastics

    Science.gov (United States)

    Ashley, Carol S.; Reed, Scott T.

    1990-01-01

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

  17. A bioactive coating of a silica xerogel/chitosan hybrid on titanium by a room temperature sol-gel process.

    Science.gov (United States)

    Jun, Shin-Hee; Lee, Eun-Jung; Yook, Se-Won; Kim, Hyoun-Ee; Kim, Hae-Won; Koh, Young-Hag

    2010-01-01

    A bioactive coating consisting of a silica xerogel/chitosan hybrid was applied to Ti at room temperature as a novel surface treatment for metallic implants. A crack-free thin layer (coated on Ti with a chitosan content of >30 vol.% through a sol-gel process. The coating layer became more hydrophilic with increasing silica xerogel content, as assessed by contact angle measurement. The hybrid coatings afforded excellent bone bioactivity by inducing the rapid precipitation of apatite on their surface when immersed in a simulated body fluid (SBF). Osteoblastic cells cultured on the hybrid coatings were more viable than those on a pure chitosan coating. Furthermore, the alkaline phosphate activity of the cells was significantly higher on the hybrid coatings than on a pure chitosan coating, with the highest level being achieved on the hybrid coating containing 30% chitosan. These results indicate that silica xerogel/chitosan hybrids are potentially useful as room temperature bioactive coating materials on titanium-based medical implants.

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

    Science.gov (United States)

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

    2015-07-01

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

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

    Science.gov (United States)

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

    2006-03-10

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

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

    Science.gov (United States)

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

    2015-10-01

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

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

    Science.gov (United States)

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

    2016-10-14

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

  2. Sol-Gel Derived Hafnia Coatings

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    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.

  3. An antibacterial coating based on a polymer/sol-gel hybrid matrix loaded with silver nanoparticles

    Directory of Open Access Journals (Sweden)

    Rivero Pedro

    2011-01-01

    Full Text Available Abstract In this work a novel antibacterial surface composed of an organic-inorganic hybrid matrix of tetraorthosilicate and a polyelectrolyte is presented. A precursor solution of tetraethoxysilane (TEOS and poly(acrylic acid sodium salt (PAA was prepared and subsequently thin films were fabricated by the dip-coating technique using glass slides as substrates. This hybrid matrix coating is further loaded with silver nanoparticles using an in situ synthesis route. The morphology and composition of the coatings have been studied using UV-VIS spectroscopy and atomic force microscopy (AFM. Energy dispersive X-ray (EDX was also used to confirm the presence of the resulting silver nanoparticles within the thin films. Finally the coatings have been tested in bacterial cultures of genus Lactobacillus plantarum to observe their antibacterial properties. It has been experimentally demonstrated that these silver loaded organic-inorganic hybrid films have a very good antimicrobial behavior against this type of bacteria.

  4. An antibacterial coating based on a polymer/sol-gel hybrid matrix loaded with silver nanoparticles

    Science.gov (United States)

    Rivero, Pedro José; Urrutia, Aitor; Goicoechea, Javier; Zamarreño, Carlos Ruiz; Arregui, Francisco Javier; Matías, Ignacio Raúl

    2011-12-01

    In this work a novel antibacterial surface composed of an organic-inorganic hybrid matrix of tetraorthosilicate and a polyelectrolyte is presented. A precursor solution of tetraethoxysilane (TEOS) and poly(acrylic acid sodium salt) (PAA) was prepared and subsequently thin films were fabricated by the dip-coating technique using glass slides as substrates. This hybrid matrix coating is further loaded with silver nanoparticles using an in situ synthesis route. The morphology and composition of the coatings have been studied using UV-VIS spectroscopy and atomic force microscopy (AFM). Energy dispersive X-ray (EDX) was also used to confirm the presence of the resulting silver nanoparticles within the thin films. Finally the coatings have been tested in bacterial cultures of genus Lactobacillus plantarum to observe their antibacterial properties. It has been experimentally demonstrated that these silver loaded organic-inorganic hybrid films have a very good antimicrobial behavior against this type of bacteria.

  5. Hybrid sol-gel optical materials

    Science.gov (United States)

    Zeigler, John M.

    1992-01-01

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

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

    Science.gov (United States)

    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.

  7. Response of SAOS-2 cells to simulated microgravity and effect of biocompatible sol-gel hybrid coatings

    Science.gov (United States)

    Catauro, M.; Bollino, F.; Papale, F.

    2016-05-01

    The health of astronauts, during space flight, is threatened by bone loss induced by microgravity, mainly attributed to an imbalance in the bone remodeling process. In the present work, the response to the microgravity of bone cells has been studied using the SAOS-2 cell line grown under the condition of weightlessness, simulated by means of a Random Positioning Machine (RPM). Cell viability after 72 h of rotation has been evaluated by means of WST-8 assay and compared to that of control cells. Although no significant difference between the two cell groups has been observed in terms of viability, F-actin staining showed that microgravity environment induces cell apoptosis and altered F-actin organization. To investigate the possibility of hindering the trend of the cells towards the death, after 72 h of rotation the cells have been seeded onto biocompatible ZrO2/PCL hybrid coatings, previously obtained using a sol-gel dip coating procedure. WST-8 assay, carried out after 24 h, showed that the materials are able to inhibit the pro-apoptotic effect of microgravity on cells.

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

    Science.gov (United States)

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

    2005-01-07

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2015-02-01

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

  11. Self-Healing Corrosion Protective Sol-Gel Coatings

    NARCIS (Netherlands)

    Abdolah Zadeh, M.

    2016-01-01

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

  12. Self-Healing Corrosion Protective Sol-Gel Coatings

    NARCIS (Netherlands)

    Abdolah Zadeh, M.

    2016-01-01

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

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

    OpenAIRE

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

    1997-01-01

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

  14. Influence of PCL on mechanical properties and bioactivity of ZrO2-based hybrid coatings synthesized by sol-gel dip coating technique.

    Science.gov (United States)

    Catauro, Michelina; Bollino, Flavia; Veronesi, Paolo; Lamanna, Giuseppe

    2014-06-01

    The biological properties of medical implants can be enhanced through surface modifications such as to provide a firm attachment of the implant. In this study, organic-inorganic hybrid coatings have been synthesized via sol-gel dip coating. They consist of an inorganic ZrO2 matrix in which different amounts of poly(ε-caprolactone) have been entrapped to improve the mechanical properties of the films. The influence of the PCL amount on the microstructural, biological and mechanical properties of the coating has been investigated. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses have shown that the hybrids used for the coating are homogenous and totally amorphous materials; Fourier transform infrared spectroscopy (FT-IR) has demonstrated that hydrogen bonds arise between the organic and inorganic phases. SEM and atomic force microscopy (AFM) have highlighted the nanostructured nature of the film. SEM and EDS analyses, after soaking the samples in a simulated body fluid (SBF), have pointed out the apatite formation on the coating surface, which proves the bone-bonding ability of the nanocomposite bioactive films. Scratch and nano-indentation tests have shown that the coating hardness, stiffness and Young's modulus decrease in the presence of large amounts of the organic phase.

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

    Science.gov (United States)

    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.

  16. Sol-gel deposited electrochromic coatings

    Energy Technology Data Exchange (ETDEWEB)

    Ozer, N.; Lampert, C.M.

    1995-06-01

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

  17. Self-Healing Corrosion Protective Sol-Gel Coatings

    OpenAIRE

    Abdolah Zadeh, M.

    2016-01-01

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

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

    Science.gov (United States)

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

    2010-10-01

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

  19. Sol-gel derived contamination resistant antireflective coatings

    Science.gov (United States)

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

    2011-02-01

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

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

    OpenAIRE

    2012-01-01

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

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

    Science.gov (United States)

    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.

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

    OpenAIRE

    1990-01-01

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

  3. Effect of surface fluorination of TiO2 particles on photocatalitytic activity of a hybrid multilayer coating obtained by sol-gel method.

    Science.gov (United States)

    Zhu, Yunfeng; Piscitelli, Filomena; Buonocore, Giovanna G; Lavorgna, Marino; Amendola, Eugenio; Ambrosio, Luigi

    2012-01-01

    A multilayer photoactive coating containing surface fluorinated TiO(2) nanoparticles and hybrid matrices by sol gel approach based on renewable chitosan was applied on poly(lactic acid) (PLA) film by a step wise spin-coating method. The upper photoactive layer contains nano-sized functionalized TiO(2) particles dispersed in a siloxane based matrix. For the purpose of improving TiO(2) dispersion at the air interface coating surface, TiO(2) nanoparticles were modified by silane coupling agent 1H,1H,2H,2H-perfluorooctyltriethoxysilane (FTS) with fluoro-organic side chains. An additional hybrid material consisting of chitosan (CS) cross-linked with 3-glycidyloxypropyl trimethoxy silane (GOTMS) was applied as interlayer between the PLA substrate and the upper photoactive coating to increase the adhesion and reciprocal affinity. The multilayer TiO(2)/CS-GOTMS coatings on PLA films showed a thickness of ~4-6 μm and resulted highly transparent. Their structure was exhaustively characterized by SEM, optical microscope, UV-vis spectroscopy and contact angle measurements. The photocatalytic activity of the multilayer coatings were investigated using methyl orange (MeO) as a target pollutant; the results showed that PLA films coated with surface fluorinated particles exhibit higher activity than films with neat particles, because of a better dispersion of TiO(2) particles. The mechanical properties of PLA and films coated with fluorinated particles, irradiated by UV light were also investigated; the results showed that the degradation of PLA substrate was markedly suppressed because of the UV adsorptive action of the multilayer coating.

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

    Science.gov (United States)

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

    2009-09-01

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

  5. Alumina Coating on Carbon Fibers by Sol-Gel Method

    OpenAIRE

    2006-01-01

    Alumina precursor film was coated on carbon fibers by a sol-gel method using aluminum alkoxide solution. The optimum coating condition for the concentration of alumina alkoxide and silane coupling agent was determined to uniformly coat alumina precursor on carbon fibers. Alumina precursor converted to alumina ceramics by heating at 750℃. SEM and EPMA showed that alumina ceramics was uniformly coated on carbon fibers. The thickness of alumina layer increased with increasing coating times. The ...

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

    OpenAIRE

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

    2014-01-01

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

  7. Tough ceramic coatings: Carbon nanotube reinforced silica sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, A.J., E-mail: antoniojulio.lopez@urjc.es [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain); Rico, A.; Rodriguez, J.; Rams, J. [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain)

    2010-08-15

    Silica coatings reinforced with carbon nanotubes were produced via sol-gel route using two mixing techniques of the sol-gel precursors, mechanical and ultrasonic mixing, and dip-coating as deposition process on magnesium alloy substrates. Effective incorporation and distribution of 0.1 wt.% of carbon nanotubes in the amorphous silica matrix of the coatings were achieved using both techniques. Fabrication procedure determines the morphological aspects of the coating. Only mechanical mixing process produced coatings dense and free of defects. Nanoindentation technique was used to examine the influence of the fabrication process in the mechanical features of the final coatings, i.e. indentation fracture toughness, Young's modulus and hardness. A maximum toughening effect of about 24% was achieved in silica coatings reinforced with carbon nanotubes produced by the mechanical mixing route. Scanning electron microscopy investigation revealed that the toughening of these reinforced coatings was mainly due to bridging effect of the reinforcement.

  8. COMPARISON OF SOL-GEL SILICATE COATINGS ON Ti SUBSTRATE

    OpenAIRE

    2012-01-01

    The objective of the submitted work was to prepare and to characterize two types of silicate coatings prepared by the sol-gel method using the dip-coating technique on a titanium substrate. Efforts have been made to use mechanical properties of bio-inert titanium and bioactive properties of a silicate layer enriched with an admixture of compounds identified below. The first group consisted of silicate coatings containing silver, brushite and monetite. The other group of silicate coatings cont...

  9. Analyses of laser and furnace treated sol-gel coatings

    NARCIS (Netherlands)

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

    1998-01-01

    Here we explore a new method that allows thin films to be made with almost any composition and degree of porosity by means of a combination of sol-gel and laser technology. Results are presented for furnace and laser treated TEOTI-(tetraethylorthotitanate as sol precursor) coated silicon samples.

  10. Analyses of laser and furnace treated sol-gel coatings

    NARCIS (Netherlands)

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

    1998-01-01

    Here we explore a new method that allows thin films to be made with almost any composition and degree of porosity by means of a combination of sol-gel and laser technology. Results are presented for furnace and laser treated TEOTI-(tetraethylorthotitanate as sol precursor) coated silicon samples. Fr

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

    Science.gov (United States)

    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.

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

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

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

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

    Science.gov (United States)

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

    2009-09-04

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

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

    Science.gov (United States)

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

    2014-02-18

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

  15. Modified sol-gel coatings for biotechnological applications

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-12-15

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

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

    Science.gov (United States)

    Seyyal, Emre; Malik, Abdul

    2017-04-29

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

  17. Composite sol-gel coatings on steel for tribological applications

    OpenAIRE

    Hermange, Kurt

    2016-01-01

    This thesis focuses on the elaboration and the characterization of composite sol-gel coatings “CSG” on austenitic stainless steelAISI 304. The aim of the thesis is to develop the process and to study the mechanical properties and tribological behavior of thecoatings. The first experimental part presents the optimization of the synthesis conditions of a stable alumina sol and the influence of the thermal treatment of the gel on the physic-chemical and thermostructural properties. The studied p...

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

    OpenAIRE

    2011-01-01

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

  19. Luminescent hybrid porphyrinosilica obtained by sol gel chemistry

    Directory of Open Access Journals (Sweden)

    Neri Cláudio Roberto

    2003-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Erika Kiele

    2015-06-01

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

  1. Multifunctional bioinspired sol-gel coatings for architectural glasses

    Energy Technology Data Exchange (ETDEWEB)

    Cannavale, Alessandro; Fiorito, Francesco; Tortorici, Giovanni [Politecnico di Bari, Dipartimento di Architettura e Urbanistica, Via E. Orabona, 4, 70126, Bari (Italy); Manca, Michele; Cingolani, Roberto; Gigli, Giuseppe [Center for Biomolecular Nanotechnologies (CBN) of the Italian Institute of Technology (IIT), Via Barsanti 1, 73010, Arnesano (LECCE) (Italy)

    2010-05-15

    Although several multinational companies have recently released products incorporating bioinspired functional coatings, their practical integration in building envelopes is still an open issue. High production costs associated to the existing vacuum deposition technologies, as well as the difficulties in extending the number of functions achievable by a single coating, represent to date the main limitations to their diffusion on a large scale. This review summarizes the key topics in the field of functional coatings for architectural glasses, focusing in particular on the potential applications of sol-gel based antireflective and self-cleaning coatings, that have received a tremendous attention in the last years. It provides an overview of the recent research efforts aimed to improve their properties and to extend their range of applicability. The bioinspired principles, upon which such coatings are based, are also described and are related to the chemical and morphological properties of such surfaces. (author)

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

    Science.gov (United States)

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

    2016-02-01

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

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

    Science.gov (United States)

    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.

  4. Novel hybrid sol-gel materials for smart sensor windows

    Science.gov (United States)

    Wencel, Dorota; Higgins, Clare; Guckian, Adrian; McDonagh, Colette; MacCraith, Brian D.

    2005-06-01

    Current sensor trends, such as multianalyte capability, miniaturisation and patternability are important drivers for materials requirements in optical chemical sensors. In particular, issues such as enhanced sensitivity and printablity are key in developing optimised sensor materials for smart windows for bioprocessing applications. This study focuses on combining novel sol-gel-based hybrid matrices with engineered luminescent complexes to produce stable luminescence-based optical sensors with enhanced sensitivity for a range of analytes including oxygen, pH and carbon dioxide. As well as optimising sensor performance, issues such as surface modification of the plastic substrate and compatibility with different deposition techniques were addressed. Hybrid sol-gel matrices were developed using a range of precursors including tetraethoxysilane (TEOS), methyltriethoxysilane (MTEOS), ethyltriethoxysilane (ETEOS), n-propyltriethoxysilane (PTEOS), phenyltriethoxysilane (PhTEOS), and n-octyltriethoxysilane (C8TEOS). Oxygen sensing, based on luminescence quenching of ruthenium phenanthroline complexes, has been realised with each of these hybrid materials. Furthermore, the possibility of immobilising pH-indicators for pH and carbon dioxide sensing has been investigated with some success. In the context of in-situ monitoring of bioprocesses, issues such as humidity interference as well as the chemical robustness of the multianalyte platform, were addressed.

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

    Science.gov (United States)

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

    2007-12-07

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

  6. COMPARISON OF SOL-GEL SILICATE COATINGS ON Ti SUBSTRATE

    Directory of Open Access Journals (Sweden)

    DIANA HORKAVCOVÁ

    2012-12-01

    Full Text Available The objective of the submitted work was to prepare and to characterize two types of silicate coatings prepared by the sol-gel method using the dip-coating technique on a titanium substrate. Efforts have been made to use mechanical properties of bio-inert titanium and bioactive properties of a silicate layer enriched with an admixture of compounds identified below. The first group consisted of silicate coatings containing silver, brushite and monetite. The other group of silicate coatings contained calcium nitrate and triethyl phosphate. Mechanically and chemically treated titanium substrates were dipped into sols and dried and fired. Silicate coatings from the first group were also chemically treated in 10 mol.l-1 solution of sodium hydroxide. All coatings were measured to determine their adhesive and bioactive properties and furthermore the antibacterial properties were tested in the case of first group. Surfaces of the coated substrates were investigated after the firing and after the individual tests with optical and electron microscopy and X-ray microdiffraction. A tape test demonstrated excellent adhesive property of all coatings to the substrate, classified with degree 5. A static in vitro test demonstrated bioactivity of nearly all the coatings. The basic silicate coating from the first group and one type of coating from the second group were identified as inert. Antibacterial properties of silicate coatings containing silver showed to be different when tested against Escherichia coli bacteria. A complete inhibition of the growth of bacteria under our experimental conditions was observed for the coating containing silver and monetite and a partial inhibition of the growth of bacteria for coatings containing silver and silver in combination with brushite.

  7. Hybrid silica-PVA nanofibers via sol-gel electrospinning.

    Science.gov (United States)

    Pirzada, Tahira; Arvidson, Sara A; Saquing, Carl D; Shah, S Sakhawat; Khan, Saad A

    2012-04-03

    We report on the synthesis of poly(vinyl alcohol) (PVA)-silica hybrid nanofibers via sol-gel electrospinning. Silica is synthesized through acid catalysis of a silica precursor (tetraethyl orthosilicate (TEOS) in ethanol-water), and fibers are obtained by electrospinning a mixture of the silica precursor solution and aqueous PVA. A systematic investigation on how the amount of TEOS, the silica-PVA ratio, the aging time of the silica precursor mixture, and the solution rheology influence the fiber morphology is undertaken and reveals a composition window in which defect-free hybrid nanofibers with diameters as small as 150 nm are obtained. When soaked overnight in water, the hybrid fibers remain intact, essentially maintaining their morphology, even though PVA is soluble in water. We believe that mixing of the silica precursor and PVA in solution initiates the participation of the silica precursor in cross-linking of PVA so that its -OH group becomes unavailable for hydrogen bonding with water. FTIR analysis of the hybrids confirms the disappearance of the -OH peak typically shown by PVA, while formation of a bond between PVA and silica is indicated by the Si-O-C peak in the spectra of all the hybrids. The ability to form cross-linked nanofibers of PVA using thermally stable and relatively inert silica could broaden the scope of use of these materials in various technologies.

  8. Mesoporous nanocomposite coatings for photonic devices: sol-gel approach

    Science.gov (United States)

    Islam, Shumaila; Bidin, Noriah; Riaz, Saira; Suan, Lau Pik; Naseem, Shahzad; Sanagi, Mohd. Marsin

    2016-10-01

    Thermally stable, optically active inorganic nanocomposites, i.e., aluminum-silicate (AS) and silica-titania (ST), are synthesized via acid-catalyzed low-temperature sol-gel method in order to get stable, crack-free coating material for photonic devices. The samples are characterized by atomic force microscope, field emission scanning electron microscope (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett--Teller (BET) surface area, Barrett-Joyner-Halenda (BJH) pore size distribution surface analysis and UV-Vis spectroscopy. Microscopic results show good incorporation of ST and AS particles as composites with grain size within range of 12-17 and 62-109 nm, respectively. EDX analysis substantiated the stoichiometric formation of homogeneous nanocomposites. XRD of the films reveals primary polycrystalline anatase titania phase and mullite phase of ST and AS nanocomposites. FTIR confirms the heterogeneous bond linkage between titania, silica and alumina species. Furthermore, the fabricated samples have mesoporous nature with high surface area, large pore volume and diameter. The tunable refractive index of 1.33-1.35 with high transparency is obtained for synthesized nanocomposites. The experimental findings show that these physically modified and thermally stable alumina- and titania-doped silica-based composite coatings are promising for photonic devices modification.

  9. 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.

    Science.gov (United States)

    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.

  10. Investigation on a Sol-gel Coating Containing Inhibitors on 2024-T3 Aluminum Alloy

    Institute of Scientific and Technical Information of China (English)

    SHI Hong-wei; LIU Fu-chun; HAN En-hou; SUN Ming-cheng

    2006-01-01

    For a long time, chromate incorporated conversion coatings have been drawn special attention in corrosion protection of aircraft-used aluminum alloys. However,ever-increasing environmental pressures requires that non-chromate conversion coatings be developed because of the detrimental carcinogenic effects of the chromate compounds. In recent years, the sol-gel coatings doped with inhibitors were developed to replace chromate conversion coatings, and showed real promise. A sol-gel coating was prepared and its anti-corrosion behavior was investigated using the potentiodynamic scanning (PDS) and the electrochemical impedance spectroscopy (EIS). It is found that the sol-gel coating obtained by the hydrolysis and condensation of 3-glycidoxypropyltrimethoxysilane (GPTMS) and tetramethoxysilane (TMOS) is prone to form defects if cured at the room temperature, whereas if cured at a higher temperature (100 ℃), these flaws can be avoided. Furthermore, it can be seen that addition of anti-foam agents and surfactants will reduce the faults if cured at the room temperature. Effects of the corrosion inhibitors, CeCl3 and mercaptobenzothiazole (MBT), in the sol-gel coatings on 2024-T3 aluminum alloy were also investigated. Results show that the corrosion resistance of the sol-gel coatings containing CeCl3 proves to be better than that of the pure and MBT added sol-gel coatings by the electrochemical methods.

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

    Science.gov (United States)

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

    2016-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-07-25

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

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

    Science.gov (United States)

    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.

  14. Influence of precursor ratios on the properties of cotton coated with a sol-gel flame retardant

    CSIR Research Space (South Africa)

    Chapple, Stephen A

    2006-11-01

    Full Text Available and strength), coatings were applied to cotton fabrics using different ratios of sol-gel precursors. The results showed that the ratio of sol-gel precursors influenced fabric stiffness and strength but not flammability. The distribution of the sol-gel flame...

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

    Institute of Scientific and Technical Information of China (English)

    XIE Jiyuan; GUO Wenfeng; WANG Jianzhong

    2011-01-01

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

  16. Entrapment of subtilisin in ceramic sol-gel coating for antifouling applications.

    Science.gov (United States)

    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.

  17. Sol-gel coatings: An alternative route for producing planar optical waveguides

    Energy Technology Data Exchange (ETDEWEB)

    Rey-Garcia, F.; Gomez-Reino, C. [Unidad Asociada de Optica and Microoptica GRIN (CSIC-ICMA), Departamento de Fisica Aplicada, Escola Universitaria de Optica e Optometria, Universidade de Santiago de Compostela, Campus Sur s/n, E-15782 Santiago de Compostela (Spain); Flores-Arias, M.T., E-mail: maite.flores@usc.es [Unidad Asociada de Optica and Microoptica GRIN (CSIC-ICMA), Departamento de Fisica Aplicada, Escola Universitaria de Optica e Optometria, Universidade de Santiago de Compostela, Campus Sur s/n, E-15782 Santiago de Compostela (Spain); De La Fuente, G.F., E-mail: xerman@unizar.es [Instituto de Ciencia de Materiales de Aragon (CSIC-Universidad de Zaragoza), Maria de Luna 3, E-50018 Zaragoza (Spain); Duran, A. [Instituto de Ceramica y Vidrio (CSIC), Kelsen 5, E-28049, Madrid (Spain); Castro, Y., E-mail: castro@icv.csic.es [Instituto de Ceramica y Vidrio (CSIC), Kelsen 5, E-28049, Madrid (Spain)

    2011-09-01

    Inorganic and hybrid planar waveguides with different compositions (silica-titania, methacrylate-silica-cerium oxide, zirconia-cerium oxide and silica-zirconia) have been obtained by sol-gel synthesis followed by dip-coating. Soda-lime glass slides and conventional commercial window glass were used as substrates. The thickness and refractive index of the coatings were determined by profilometry and Spectroscopic Ellipsometry. Waveguide efficiency was measured at ca. 70.8% with a He-Ne laser beam, coupled with an optical microscope objective into and out of the waveguiding layer via a double prism configuration. Thicknesses between 150 and 2000 nm, along with refractive index values ranging between 1.45 and {approx} 1.99 ({lambda} = 633 nm) were obtained depending on the sol composition and the dip-coating conditions. This wide range of values allows designing multilayered guides that can be used in a variety of applications.

  18. Sol-gel fabrication and optical absorption properties of C-NiO nanocomposite coatings

    CSIR Research Space (South Africa)

    Tile, N

    2010-12-01

    Full Text Available of the sunlight as possible, then prevent thermal emittance The manufacturing process for most commercial thermal products is complicated C-NiO/Al has been fabricated using a simple and cheap sol-gel procedure combined with spin coating technique C... SOLUTION) Structure directing templateFinal C-NiO gel By suitable choice of precursor, we can engineer novel composite materials Sol-gel technique can be adapted to different coating methods coating substrate Spray coating Spin coating The material...

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

    NARCIS (Netherlands)

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

    1997-01-01

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

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

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2010-09-10

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

  1. Modification of Ti6Al4V implant surfaces by biocompatible TiO2/PCL hybrid layers prepared via sol-gel dip coating: Structural characterization, mechanical and corrosion behavior.

    Science.gov (United States)

    Catauro, Michelina; Bollino, Flavia; Giovanardi, Roberto; Veronesi, Paolo

    2017-05-01

    Surface modification of metallic implants is a promising strategy to improve tissue tolerance, osseointegration and corrosion resistance of them. In the present work, bioactive and biocompatible organic-inorganic hybrid coatings were prepared using a sol-gel dip coating route. They consist of an inorganic TiO2 matrix in which different percentages of poly(ε-caprolactone) (PCL), a biodegradable and biocompatible polymer, were incorporated. The coatings were used to modify the surface of Ti6Al4V substrates in order to improve their wear and corrosion resistance. The chemical structure of the coatings was analyzed by attenuated total reflectance (ATR) Fourier transform infrared (FTIR) spectroscopy. Coating microstructure, mechanical properties and ability to inhibit the corrosion of the substrates were evaluated as a function of the PCL amount. Scanning electron microscopy (SEM) showed that the polymer allows to obtain crack-free coatings, but when high percentages were added uncoated areas appear. Nano-indentation tests revealed that, as expected, surface hardness and elastic modulus decrease as the percentage of polymeric matrix increases, but scratch testing demonstrated that the coatings are effective in preventing scratching of the underlying metallic substrate, at least for PCL contents up to 20wt%. The electrochemical tests (polarization curves acquired in order to evaluate the corrosion resistance) allowed to asses that the coatings have a significant effect in term of corrosion potential (Ecorr) but they do not significantly affect the passivation process that titanium undergoes in contact with the test solution used (modified Dulbecco's phosphate-buffered saline or DPBS). Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Carbon nanotube-coated solid-phase microextraction metal fiber based on sol-gel technique.

    Science.gov (United States)

    Jiang, Ruifen; Zhu, Fang; Luan, Tiangang; Tong, Yexiang; Liu, Hong; Ouyang, Gangfeng; Pawliszyn, Janusz

    2009-05-29

    A novel carbon nanotube (CNT)-coated solid-phase microextraction fiber was prepared based on sol-gel technique. Commonly used fragile fused silica fiber was replaced with stainless steel wire, which made the fiber unbreakable. An approach was also proposed for batch producing, and good reproducibilities for fiber to fiber and between fibers were achieved. Experiments showed that the sol-gel-CNT fiber exhibited high thermal stability to resist 350 degrees C and excellent solvent durability in methanol and acetonitrile. Compared to commercial polydimethylsiloxane (PDMS) fiber, the sol-gel-CNT fiber represented significantly improved extraction efficiencies for both polar (phenols) and non-polar (benzene, toluene, ethylbenzene, and o-xylene) compounds. Meanwhile, no replacement effect, low carry-over and wide linear range demonstrated that the newly prepared sol-gel-CNT coating has liquid properties, which allow a relatively easy quantification procedure. Moreover, the characterization of the sol-gel-CNT coating was also evaluated with McReynold probe solutes. The results showed that the coating has better affinity for all the five types of solutes compared to commercial 7microm PDMS fiber, which suggested that the coating has the potential to be developed as GC stationary phase.

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

    Science.gov (United States)

    Jordens, Kurt

    1999-12-01

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

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

    Science.gov (United States)

    Yang, Jianhua; Guo, Linghong; Li, Hui

    2006-10-01

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

  5. Zinc oxide films prepared by sol-gel spin coating technique

    Energy Technology Data Exchange (ETDEWEB)

    Kamaruddin, Sharul Ashikin; Chan, Kah-Yoong; Yow, Ho-Kwang [Multimedia University, Faculty of Engineering, Cyberjaya, Selangor (Malaysia); Zainizan Sahdan, Mohd; Saim, Hashim [Universiti Tun Hussein Onn Malaysia, Faculty of Electrical and Electronics Engineering, Batu Pahat, Johor (Malaysia); Knipp, Dietmar [Jacobs University Bremen, School of Engineering and Science, Bremen (Germany)

    2011-07-15

    Zinc oxide (ZnO) thin films and micro- and nanostructures are very promising candidates for novel applications in emerging thin-film transistors, solar cells, sensors and optoelectronic devices. In this paper, a low-cost sol-gel spin coating technique was used to fabricate ZnO films on glass substrates. The sol-gel fabrication process of the ZnO films is described. The influence of precursor concentration on the material properties of the ZnO films was investigated. Atomic force microscopy and X-ray diffractometry were employed to examine the structural properties of the ZnO films. The optical properties of the ZnO films were characterized with ultraviolet-visible spectroscopy. The experimental results reveal that the precursor concentration in the sol-gel spin coating process exerts a strong influence on the properties of the ZnO films. The effects of the precursor concentration are discussed. (orig.)

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

    Science.gov (United States)

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

    2013-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-02-01

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

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

    NARCIS (Netherlands)

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

    2013-01-01

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

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

    Science.gov (United States)

    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.

  10. A New Approach of Improving Rain Erosion Resistance of Nanocomposite Sol-Gel Coatings by Optimization Process Factors

    Science.gov (United States)

    Hojjati Najafabadi, Akbar; Shoja Razavi, Reza; Mozaffarinia, Reza; Rahimi, Hamed

    2014-05-01

    Erosion protection nanocomposite sol-gel coatings based on tetraethylorthosilicate (TEOS) and 3-glycidoxypropyltrimethoxisilane (GPTMS) are prepared and characterized to protect marine structures susceptible to damage caused by liquid impact, e.g., the submarine body. This study focuses on the optimization of compositional and process parameters of transparent hybrid nanocomposite sol-gel coatings resistant to rain erosion by using statistical design of experimental methodology (DoE) based on Taguchi orthogonal design. The impact of compositional and process parameters of the coatings on the erosion protection performance is investigated by five-factor-four-level design methodology. Hybrid coatings were deposited on AA5083 by a dip coating technique. Optimization coatings are analyzed regarding their adhesion (pull-off), flexibility (impact and mandrel bending), hardness (pencil), wear (Taber wear index), and rain erosion resistance (stationary sample erosion test). The surface morphology and roughness were studied by field-emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM). The optimization coatings showed excellent flexibility and adhesion to the substrate with smooth nanostructure surface; the RMS surface roughness was 1.85 nm. The evaluation of the result obtained from abrasion shows cohesive and interfacial wear with abrasive and adhesive mechanisms, respectively. Liquid impact results show cohesive failure of the coatings without any sign of delamination.

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

    Science.gov (United States)

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

    2004-08-01

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

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

    OpenAIRE

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

    2008-01-01

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

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

    Science.gov (United States)

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

    2016-09-07

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

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

    Science.gov (United States)

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

    2016-12-01

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

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

    NARCIS (Netherlands)

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

    2013-01-01

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

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

    NARCIS (Netherlands)

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

    2007-01-01

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

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

    Science.gov (United States)

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

    2010-05-15

    For the first time, a germania-based sol-gel coating was used in capillary microextraction (CME) in combination with high-performance liquid chromatography (HPLC). A hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide), was covalently bonded into a sol-gel germania matrix in the course of its creation from an alkoxide precursor via hydrolytic polycondensation reactions. A thin layer of this in situ-created sol-gel hybrid material was covalently anchored to the inner walls of a 0.25 mm i.d. fused silica capillary to produce a sol-gel germania triblock polymeric sorbent in the form of a highly stable surface coating. Such a coating served as an effective extracting phase for the preconcentration of a wide range of polar and nonpolar analytes (e.g., alcohols, amines, ketones, phenols, and polycyclic aromatic hydrocarbons) with nanomolar and picomolar detection limits. Most significantly, the sol-gel germania triblock polymer coating demonstrated impressive resistance to extreme pH conditions, surviving 5 days of continuous exposure to 1.0 M HCl (pH approximately 0.0) or 1.0 M NaOH (pH approximately 14.0), practically without any changes in performance. This shows the suitability of sol-gel germania hybrid organic-inorganic hybrid materials for use as sorbents or stationary phases under extreme pH conditions, often needed in a variety of separation and sample preparation techniques and applications, including ion chromatography, hydrophobic interaction chromatography, proteomics, HPLC with electrochemical detection, isoelectric focusing, and extraction of acidic and basic analytes.

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

    Science.gov (United States)

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

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, M., E-mail: michelina.catauro@unina2.it [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Papale, F. [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29 (Italy); Sapio, L.; Naviglio, S. [Department of Biochemistry, Biophysics and General Pathology, Second University of Naples, Via L. De Crecchio 7, 80138 Naples (Italy)

    2016-08-01

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

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

    Science.gov (United States)

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

    2016-08-01

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

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

    OpenAIRE

    Hou, Lisong; Schmidt, Helmut K.

    1996-01-01

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

  2. Structural properties and antibacterial effects of hydrophobic and oleophobic sol-gel coatings for cotton fabrics.

    Science.gov (United States)

    Vilcnik, Aljaz; Jerman, Ivan; Surca Vuk, Angela; Kozelj, Matjaz; Orel, Boris; Tomsic, Brigita; Simoncic, Barbara; Kovac, Janez

    2009-05-19

    In a continuation of previous studies, the wetting properties of the hydrophobic diureapropyltriethoxysilane [bis(aminopropyl)-terminated polydimethylsiloxane (1000)] (PDMSU) sol-gel hybrid, which forms washing-resistant water-repellent finishes on cotton fabrics, were further investigated. The addition of 1H,1H,2H,2H-perfluorooctyltriethoxysilane (PFOTES) to PDMSU resulted in a highly apolar low-energy surface on aluminum with gammaStotal equal to 14.5 mJ/m2 and a DetlaGiwi value of -82 mJ/m2. Mixed PFOTES-PDMSU finishes applied on cotton fabrics increased the water contact angles (thetaw) from approximately 130 degrees (PDMSU) to 147 degrees, also imparting oleophobicity (thetadiiodomethane=130 degrees, thetan-hexadecane=120 degrees) to the finished cotton fabrics. Washing caused breakage of the coating's integrity as established from SEM, which was attributed to the partial removal of PFOTES from the composite films, also shown by subtractive IR attenuated total reflectance (ATR) and XPS spectral measurements made on washed and unwashed fabrics. The antibacterial properties of the PFOTES-PDMSU-finished fabrics were assessed with the transfer method (EN ISO 20743:2007), revealing that the reduction of Escherichia coli bacteria on unwashed cotton fabrics was nearly 100%. Moreover, for washed (10 times) cotton fabrics a much higher bacterial reduction was noted for the PFOTES-PDMSU finishes (60.6+/-10.8%), surpassing PDMSU (30.4+/-6.1%) and commercial fluoroalkoxysilane (FAS) (21.9+/-5.7%) finishes. The structure of PFOTES-PDMSU gels, xerogels, and the corresponding coatings was investigated by analyzing the 29Si NMR and IR ATR spectra and comparing them with the spectra of PFOTES and octameric (T8) PFOTES based polyhedra. The results revealed the tendency of PFOTES to condense in octameric silsesquioxane polyhedra (T8), coexisting in the PDMSU sol-gel network with cyclic tetramers (T4(OH)4) and open cube-like species (T7(OH)3). The presence of -OH

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

    Directory of Open Access Journals (Sweden)

    Awais Khatri

    2013-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-03-15

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

  5. Coating of LaCoO3 thin film with sol-gel dip coating method.

    Science.gov (United States)

    Okuyucu, Hasan; Dahl, Paul Inge; Einarsrud, Mari Ann

    2008-02-01

    LaCoO3 thin film was coated on Al2O3 single crystal by sol-gel route. Appropriate composition of precursors, chelating agents and the solvent put together into a flask and magnetically stirred on a magnetic stirrer. After having the red transparent solution, it was stirred for 12 hours before coating. Ultrasonically cleaned substrate is dipped into the solution and taken immediately into vertical furnace which is preheated at 550 degrees C. A dense amorphous film is coated on the substrate. Fired amorphous films are annealed at temperature between 900 degrees C and 1000 degrees C for 20 minutes in the air. Then coated film was characterized by means of XRD, AFM, and SEM. Conductivity of the film was measured to be -0.1819 for 881 degrees C for the log sigma value by assuming the thickness as

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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 (psol-gel deposition times also revealed significant differences in bond strength among the Dry groups (pcoating of zirconia by sol-gel process resulted in weaker resin bonding than by sandblasting.

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Faure Joel

    2013-11-01

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

  11. 3D Printed PEG-Based Hybrid Nanocomposites Obtained by Sol-Gel Technique.

    Science.gov (United States)

    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.

  12. Sol gel TiO2 antireflection coatings for silicon solar cells

    Directory of Open Access Journals (Sweden)

    L.A. Dobrzański

    2012-05-01

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

  13. Characterization of protective sol-gel coatings on magnesium based on phenyl-triethoxysilane precursor

    Energy Technology Data Exchange (ETDEWEB)

    Yekehtaz, M., E-mail: yekehtaz@ca.tu-darmstadt.d [Technische Universitaet Darmstadt, Department of Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany); Sittner, F.; Ugas-Carrion, R.; Flege, S.; Broetz, J.; Ensinger, W. [Technische Universitaet Darmstadt, Department of Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany)

    2010-07-01

    Sol-gel coatings were deposited from a Phenyl-triethoxysilane precursor for corrosion protection on magnesium samples. Film porosity was measured with potentiodynamic scans and the coating's structure was characterized with secondary ion mass spectrometry and X-ray diffraction analysis. At the interface between substrate and coating a magnesium silicate layer was found which was formed by interdiffusion during the deposition process. The coated samples showed a good corrosion resistance and low porosity after heating at comparatively low temperature.

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

    CERN Document Server

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

    2016-01-01

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

  15. Surface modification of stainless steel orthopedic implants by sol-gel ZrTiO4 and ZrTiO4-PMMA coatings.

    Science.gov (United States)

    Salahinejad, E; Hadianfard, M J; Macdonald, D D; Sharifi Asl, S; Mozafari, M; Walker, K J; Rad, A Tahmasbi; Madihally, S V; Vashaee, D; Tayebi, L

    2013-08-01

    In this paper, the biocompatibility of a medical-grade stainless steel coated with sol-gel derived, nanostructured inorganic ZrTiO4 and hybrid ZrTiO4-PMMA thin films is correlated with surface characteristics. The surfaces of the samples are characterized by atomic force microscopy, the sessile drop technique, and electrochemical corrosion experiments. The viability of adult human mesenchymal stem cells on the surfaces after one day of culture is also assessed quantitatively and morphologically. According to the results, both of the coatings improve the hydrophilicity, corrosion resistance, and thereby cytocompatibility of the substrate. Despite the higher corrosion protection by the hybrid coating, the sample coated with the inorganic thin film exhibits a better cell response, suggesting the domination of wettability. In summary, the ZrTiO4-based sol-gel films can be considered to improve the biocompatibility of metallic implants.

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

    Science.gov (United States)

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

    2010-04-26

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

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

    Science.gov (United States)

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

    2011-04-15

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

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

    OpenAIRE

    2011-01-01

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

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

    Science.gov (United States)

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

    2008-04-01

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

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

    Directory of Open Access Journals (Sweden)

    VLADIMIR V. PANIC

    2007-12-01

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

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

    Science.gov (United States)

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

    2015-04-01

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

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

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-04-16

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

  4. Nanostructured Silica/Gold-Cellulose-Bonded Amino-POSS Hybrid Composite via Sol-Gel Process and Its Properties

    Science.gov (United States)

    Ramesh, Sivalingam; Kim, Heung Soo; Lee, Young-June; Hong, Gwang-Wook; Kim, Joo-Hyung

    2017-06-01

    It is demonstrated in this paper that silica nanoparticles coated with core/shell gold provide efficient thermal, optical, and morphological properties with respect to the cellulose-polyhedral oligomeric silsesquioxanes (POSS) hybrid system. The one-step synthesis of a silica/gold nanocomposite is achieved with a simultaneous hydrolysis and reduction of gold chloride in the presence of formic acid, and the trimethoxysilane group acts as a silica precursor. The focus here comprises the synthesis of cellulose-POSS and silica/gold hybrid nanocomposites using the following two methods: (1) an in situ sol-gel process and (2) a polyvinyl alcohol/tetrakis (hydroxymethyl)phosphonium chloride process. Accordingly, the silica/gold core/shell nanoparticles are synthesized. The growth and attachment of the gold nanoparticles onto the functionalized surface of the silica at the nanometer scale is achieved via both the sol-gel and the tetrakis (hydroxymethyl) phosphonium chloride processes. The cellulose-POSS-silica/gold nanocomposites are characterized according to Fourier transformed infrared spectroscopy, Raman, X-ray diffraction, UV, photoluminescence, SEM, energy-dispersive X-ray spectroscopy, TEM, thermogravimetric, and Brunauer-Emmett-Teller analyses.

  5. External polyacrylate-coating as alternative material for preparation of photopolymerized sol-gel monolithic column.

    Science.gov (United States)

    Vaz, Fernando Antonio Simas; de Castro, Patrícia Mendonça; Molina, Celso; Ribeiro, Sidney José Lima; Polachini, Ferminio César; Messaddeq, Younes; Nunes, Adriana Palombo; de Oliveira, Marcone Augusto Leal

    2008-06-30

    Photopolymerized sol-gel monolithic columns for use in capillary electrochromatography were prepared in 125 microm i.d. polyacrylate-coated fused-silica capillaries. The polyacrylate-coating, unlike the polyimide one, is transparent to the radiation used (approximately 370 nm), and thus, no coating removal is necessary. This is a very important particularity since intrinsic capillary column characteristics, such as flexibility and mechanical resistance, are unchanged. A mixture containing metacryloxypropyltrimethoxysilane (MPTMS) as the polymeric precursor, hydrochloric acid as the catalyst, toluene as the porogen and bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide (Irgacure 819) as the photoinitiator was irradiated at 370 nm for 20 min inside the capillaries to prepare the columns through sol-gel approach. The versatility and viability of the use of polyacrilate as a new capillary external coating were shown through preparation of two columns under different conditions, which were tested in electrochromatography for separation of standard mixture containing thiourea (marker compound), propylbenzene, phenanthrene and pyrene.

  6. Fabrication of inverted zinc oxide photonic crystal using sol-gel solution by spin coating method.

    Science.gov (United States)

    Huang, Kuo-Min; Ho, Chong-Lung; Chang, Heng-Jui; Wu, Meng-Chyi

    2013-01-01

    Inverted zinc oxide photonic crystal structures were fabricated from polystyrene sphere (PSS) template using the sol-gel solution of ZnO by spin-coating method. It is easily able to control and fabricate the photonic crystal structures using the self-organized PSS with a size of 193 nm. The inverted ZnO photonic crystal structures observed show the (111) tendency of the hexagonal compact arrangement formation. The resulting structures possess the photonic band gaps in the near-ultraviolet range and exhibit an enhanced photoluminescence spectrum. The technology can effectively increase the light output intensity or efficiency for the applications of optoelectronic devices.

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

    Directory of Open Access Journals (Sweden)

    Macan, J

    2008-07-01

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

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

    Science.gov (United States)

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

    1999-10-01

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2008-07-18

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

  11. Evolution of microstructure in mixed niobia-hybrid silica thin films from sol-gel precursors.

    Science.gov (United States)

    Besselink, Rogier; Stawski, Tomasz M; Castricum, Hessel L; ten Elshof, Johan E

    2013-08-15

    The evolution of structure in sol-gel derived mixed bridged silsesquioxane-niobium alkoxide sols and drying thin films was monitored in situ by small-angle X-ray scattering. Since sol-gel condensation of metal alkoxides proceeds much faster than that of silicon alkoxides, the incorporation of d-block metal dopants into silica typically leads to formation of densely packed nano-sized metal oxide clusters that we refer as metal oxide building blocks in a silica-based matrix. SAXS was used to study the process of niobia building block formation while drying the sol as a thin film at 40-80°C. The SAXS curves of mixed niobia-hybrid silica sols were dominated by the electron density contrast between sol particles and surrounding solvent. As the solvent evaporated and the sol particles approached each other, a correlation peak emerged. Since TEM microscopy revealed the absence of mesopores, the correlation peak was caused by a heterogeneous system of electron-rich regions and electron poor regions. The regions were assigned to small clusters that are rich in niobium and which are dispersed in a matrix that mainly consisted of hybrid silica. The correlation peak was associated with the typical distances between the electron dense clusters and corresponded with distances in real space of 1-3 nm. A relationship between the prehydrolysis time of the silica precursor and the size of the niobia building blocks was observed. When 1,2-bis(triethoxysilyl)ethane was first hydrolyzed for 30 min before adding niobium penta-ethoxide, the niobia building blocks reached a radius of 0.4 nm. Simultaneous hydrolysis of the two precursors resulted in somewhat larger average building block radii of 0.5-0.6 nm. This study shows that acid-catalyzed sol-gel polymerization of mixed hybrid silica niobium alkoxides can be rationalized and optimized by monitoring the structural evolution using time-resolved SAXS.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    2014-07-01

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

  15. Ultraviolet Stimulated Emission from Sol-Gel Spin Coated ZnO Thin Films

    Directory of Open Access Journals (Sweden)

    Ahmed S. Razeen

    2017-01-01

    Full Text Available Low cost ultraviolet stimulated emission has been generated using optical excitation of ZnO thin films deposited by sol-gel spin coating on n+ As-doped 100 Si-substrate. The number of deposited layers and the heat treatment have been investigated to obtain a film that can generate stimulated emission under optical excitation. The optimum condition for preparation of the film has been presented. X-ray diffraction and scanning electron microscope have been used for structural and morphological investigations. Input-output intensity dependence and spectral width, peak emission wavelength, and the quantum efficiency versus the pump intensity have been presented. A quantum efficiency of about 24.2% has been reported, a power exponent higher than 8 has been obtained in input-output intensity dependence, and a threshold of about 23 Mw/cm2 has been evaluated for the samples. The mechanism by which stimulated emission occurs has been discussed. The results show that sol-gel spin coating is a promising method for generating ultraviolet stimulated emission from ZnO thin films.

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

    Directory of Open Access Journals (Sweden)

    María Aymerich

    2016-08-01

    Full Text Available 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.

  17. The enhancement of benzotriazole on epoxy functionalized silica sol-gel coating for copper protection

    Science.gov (United States)

    Peng, Shusen; Zhao, Wenjie; Li, He; Zeng, Zhixiang; Xue, Qunji; Wu, Xuedong

    2013-07-01

    The influence of the amount of benzotriazole (BTA) on the wetting and anticorrosion ability of the epoxy functionalized silica sol-gel (ESol) coating was studied by various complementary methods. IR results demonstrate that BTA reacted with ESol through a 1:1 addition reaction of Nsbnd H to epoxy group. The water contact angle of the ESol coating increases with an increase in the amount of BTA. SEM and adhesion tests reveal that BTA could improve the adhesion of ESol to copper surface. Moreover, the best protection was achieved when the amount of BTA equals to the molar number of epoxy group in the ESol coating according to the results of electrochemical measurements and salt spray test.

  18. Ultraviolet laser-induced damage on fused silica substrate and its sol-gel coating.

    Science.gov (United States)

    Li, Xiaoguang; Gross, Mark; Green, Katie; Oreb, Bob; Shen, Jun

    2012-06-15

    A comparative study of the laser-induced damage thresholds (LIDTs) of fused silica substrates and their sol-gel silica coatings was carried out with 355 nm laser irradiation. Chemical etching and superpolishing were employed in different ways to improve the substrate. The laser damage tests showed that the coated substrate was no more susceptible to laser damage than the bare substrate, showing that the substrate quality was the dominant factor limiting the LIDT for UV irradiation. In addition, it was found that high value of substrate microroughness was more harmful to the LIDT of the coated than the bare substrate, and that a proper combination of etching and superpolishing can optimize the LIDT.

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

    Energy Technology Data Exchange (ETDEWEB)

    Malik, Abdul; Shearrow, Anne M.

    2017-01-31

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

  20. Evaluation of bulk and surfaces absorption edge energy of sol-gel-dip-coating SnO2 thin films

    Directory of Open Access Journals (Sweden)

    Emerson Aparecido Floriano

    2010-12-01

    Full Text Available The absorption edge and the bandgap transition of sol-gel-dip-coating SnO2 thin films, deposited on quartz substrates, are evaluated from optical absorption data and temperature dependent photoconductivity spectra. Structural properties of these films help the interpretation of bandgap transition nature, since the obtained nanosized dimensions of crystallites are determinant on dominant growth direction and, thus, absorption energy. Electronic properties of the bulk and (110 and (101 surfaces are also presented, calculated by means of density functional theory applied to periodic calculations at B3LYP hybrid functional level. Experimentally obtained absorption edge is compared to the calculated energy band diagrams of bulk and (110 and (101 surfaces. The overall calculated electronic properties in conjunction with structural and electro-optical experimental data suggest that the nature of the bandgap transition is related to a combined effect of bulk and (101 surface, which presents direct bandgap transition.

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

    Directory of Open Access Journals (Sweden)

    ELENA BORSHCHEVA

    2011-12-01

    Full Text Available The aim of the experiment was the obtaining of thin silica coatings on titanium by sol-gel method, using mechanical (SiC - paper No.180 and chemical (leaching in HF pretreatments of the titanium substrates. The solutions were based on TEOS. For the sol-gel dipping process 4 different solutions were prepared: silica, silica with AgNO3 and silica + AgNO3 with brushite (CaHPO4·2H2O or monetite (CaHPO4 powders. The solutions were aged for 7 and 14 days at laboratory temperature. After sol-gel dip-coating process the samples were dried and fired. The adhesion of fired coatings was measured by tape test according to ASTM procedure and the bioactivity of the coatings was tested using in vitro test. The surfaces of the samples after firing, tape test and in vitro test were observed with the optical and electron microscopes. The firing results showed that silica-silver coatings did not change, brushite sol-gel coatings have cracked and the monetite sol-gel coatings have cracked also, but less than brushite ones. In spite of coating´s crackings, the square’s frames made on the surfaces were without any breakdowns after tape tests and the adhesion of all coatings was very good, classified by the highest grade 5. The results of in vitro tests showed that all coatings interacted with simulated body fluid (SBF. After exposition in SBF the new layer formed on substrates. In case of 7 days aged coatings containing brushite the new layer was uniform and compact. In case of 7 days aged coatings containing monetite the new layer was formed by crystals aggregated tightly together. The monetite and brushite coatings prepared from 14 days aged sol were the same as previous ones, but they were thicker. X-ray analyses after in vitro test confirmed dellaite, titanate and hydroxyapatite phases.

  2. Effect of forming technique BixSiyOz coatings obtained by sol- gel and supported on 316L stainless steel

    Science.gov (United States)

    Bautista Ruiz, J.; Olaya Flórez, J.; Aperador, W.

    2016-02-01

    BixSiyOz type coatings via sol-gel synthesized from bismuth nitrate pentahydrate, and tetraethyl orthosilicate as precursors; glacial acetic acid and 2-ethoxyethanol as solvents, and ethanolamine as complexing. The coatings were supported on AISI 316L stainless steel substrate through dip-coating and spin-coating techniques. The study showed that the spin-coating technique is efficient than dip-coating because it allows more dense and homogeneous films.

  3. Sol-Gel-Coated Calix[4]arene Fiber for Solid-Phase Microextraction

    Institute of Scientific and Technical Information of China (English)

    LiXiu-juan; XiaoRui-min; LiHai-bing; ZengZhao-rui

    2003-01-01

    5, 11, 17, 23-tetra-tert-butyl-25, 27-diethoxy-26, 28-dihydroxycalix [4] arene/hydroxy-terminated silicone oil coated fiber was first prepared and applied for solid-phase microextraction with sol-gel technology. The properties of the new coating were investigated by analysis of benzene derivatives, polycyclic aromatic hydrocarbons and aromatic amines.The fiber is characterized by good sensitivity and selectivity to these aromatics. The fiber has stable performance at a high temperature of 380℃ and after a long solvent immersing,thus its lifetime is very long. It shows good fiber-to-fiber and batch-to-batch reproducibility. Furthermore, broad linear ranges and low detection limits are also its characteristics.

  4. Sol-Gel-Coated Calix[4]arene Fiber for Solid-Phase Microextraction

    Institute of Scientific and Technical Information of China (English)

    Li Xiu-juan; Xiao Rui-min; Li Hai-bing; Zeng Zhao-rui

    2003-01-01

    5,11,17,23-tetra-tert-butyl-25, 27-diethoxy-26, 28-dihydroxycalix [4] arene /hydroxy-terminated silicone oil coated fiber was first prepared and applied for solid-phase microextraction with sol-gel technology. The properties of the new coating were investigated by analysis of benzene derivatives, polycyclic aromatic hydrocarbons and aromatic amines. The fiber is characterized by good sensitivity and selectivity to these aromatics. The fiber has stable performance at a high temperature of 380℃ and after a long solvent immersing, thus its lifetime is very long. It shows good fiber-to-fiber and batch-to-batch reproducibility. Furthermore, broad linear ranges and low detection limits are also its characteristics.

  5. Prevention of Staphylococcus epidermidis biofilm formation using a low-temperature processed silver-doped phenyltriethoxysilane sol-gel coating.

    Science.gov (United States)

    Stobie, Niall; Duffy, Brendan; McCormack, Declan E; Colreavy, John; Hidalgo, Martha; McHale, Patrick; Hinder, Steven J

    2008-03-01

    Sol-gel coatings which elute bioactive silver ions are presented as a potential solution to the problem of biofilm formation on indwelling surfaces. There is evidence that high-temperature processing of such materials can lead to diffusion of silver away from the coating surface, reducing the amount of available silver. In this study, we report the biofilm inhibition of a Staphylococcus epidermidis biofilm using a low-temperature processed silver-doped phenyltriethoxysilane sol-gel coating. The incorporation of a silver salt into a sol-gel matrix resulted in an initial high release of silver in de-ionised water and physiological buffered saline (PBS), followed by a lower sustained release for at least 6 days-as determined by graphite furnace-atomic absorption spectroscopy (GF-AAS). The release of silver ions from the sol-gel coating reduced the adhesion and prevented formation of a S. epidermidis biofilm over a 10-day period. The presence of surface silver before and after 24 h immersion in PBS was confirmed by X-ray photoelectron spectroscopy (XPS). These silver-doped coatings also exhibited significant antibacterial activity against planktonic S. epidermidis. A simple test to visualise the antibacterial effect of silver release coatings on neighbouring bacterial cultures is also reported.

  6. Antimicrobial effects and human gingival biocompatibility of hydroxyapatite sol-gel coatings.

    Science.gov (United States)

    Chung, Ren-Jei; Hsieh, Ming-Fa; Huang, Chine-Wen; Perng, Li-Hsiang; Wen, Hsiao-Wei; Chin, Tsung-Shune

    2006-01-01

    The sol-gel method was employed to synthesize hydroxyapatite (HAp) coatings modified with Ag or Zn ions onto Ti-6Al-4V substrate. A bacterial strain Streptococcus mutans (S. mutans) and a human gingival fibroblast (HGF-1) cell line were used to investigate the antimicrobial effect and biocompatibility, respectively. HAp coatings containing 100 ppm Ag(+) ions suppressed the growth of S. mutans. An apparent inhibition zone around the HAp coating was further observed at Ag(+) concentration up to 10,000 ppm. However, for coatings containing Zn(2+) ions, a clear inhibition zone was observed at Zn(2+) concentration of 10,000 ppm. Nevertheless, the results of HGF-1 cultivation demonstrated that the Zn(2+)-modified HAp coatings exhibited better attachment and spread of HGF-1 than did the Ag(+)-modified coatings. Zn(2+) modified HAp coatings also increased the plating efficiency of HGF-1 cells. The cytotoxicity associated with the addition of Ag and the cell-conductive capacity associated with the addition of Zn are proportional to the added concentration, from 100 to 10,000 ppm. The dosages of both Ag(+) and Zn(2+) ions that should be added to HAp coatings were considered to prevent infection and improve biocompatibility. The results of this study ensure that HAp coatings modified with a moderate amount of Ag/Zn efficiently resist microorganisms and improve biocompatibility.

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

    Science.gov (United States)

    Deetz, Joshua David

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-04-21

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

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

    Directory of Open Access Journals (Sweden)

    B. Vlad-Oros

    2007-12-01

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

  10. Mesoporous sol-gel silica cladding for hybrid TiO2/electro-optic polymer waveguide modulators.

    Science.gov (United States)

    Enami, Yasufumi; Kayaba, Yasuhisa; Luo, Jingdong; Jen, Alex K-Y

    2014-06-30

    We report the efficient poling of an electro-optic (EO) polymer in a hybrid TiO(2)/electro-optic polymer multilayer waveguide modulator on mesoporous sol-gel silica cladding. The mesoporous sol-gel silica has nanometer-sized pores and a low refractive index of 1.24, which improves mode confinement in the 400-nm-thick EO polymer film in the modulators and prevents optical absorption from the lower Au electrode, thereby resulting in a lower half-wave voltage of the modulators. The half-wave voltage (Vπ) of the hybrid modulator fabricated on the mesoporous sol-gel silica cladding is 6.0 V for an electrode length (Le) of 5 mm at a wavelength of 1550 nm (VπLe product of 3.0 V·cm) using a low-index guest-host EO polymer (in-device EO coefficient of 75 pm/V).

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

    DEFF Research Database (Denmark)

    Tshabalala, M.A.; Kingshott, P.; VanLandingham, M.R.

    2003-01-01

    with a long hydrocarbon chain to form a polysiloxane network that is hydrophobic. The ultimate effect of the sol-gel deposit can therefore be regarded as not only to decrease the surface concentration of hydrogen-bonding sites, but also to stereochemically hinder the formation of hydrogen bonds between......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 means of ATR-FTIR, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, SEM, and atomic force microscopy indicated that the sol-gel process results in deposition of polysiloxane networks that are bonded to the wood...

  12. Photochromic mesoporous hybrid coatings

    Science.gov (United States)

    Raboin, L.; Matheron, M.; Gacoin, T.; Boilot, J.-P.

    2008-09-01

    Spirooxazine (SO) photochromic molecules were trapped in sol-gel matrices. In order to increase the colourability and improve mechanical properties of sol-gel photochromic films, we present an original strategy in which SO photochromic molecules were dispersed in mesoporous organized films using the impregnation technique. Well-ordered organosilicate mesoporous coatings with the 3D-hexagonal symmetry were prepared by the sol-gel technique. These robust mesoporous films, which contain high amounts of hydrophobic methyl groups at the pore surface, offer optimized environments for photochromic dyes dispersed by impregnation technique. After impregnation by a spirooxazine solution, the photochromic response is only slightly slower when compared with mesostructured or soft sol-gel matrices, showing that mesoporous organized hybrid matrix are good host for photochromic dyes. Moreover, the molecular loading in films is easily adjustable in a large range using multi-impregnation procedure and increasing the film thickness leading to coatings for optical switching devices.

  13. Sol-gel broadband antireflective coatings for advanced laser-glass amplifiers

    Science.gov (United States)

    Floch, Herve G.; Belleville, Philippe F.; Pegon, Philippe M.

    1994-10-01

    The cost of a large laser system is a strong function of the overall electrical to final photon efficiency. To improve the stored energy and therefore the pumping efficiency of sophisticated and costly laser-glass amplifiers, we have developed a novel two-layer broadband antireflective coating for the blast-shield component. The blast-shield is an optic placed between the flashlamps and the laser disk amplifiers to prevent damage of laser disks by possible explosion of a flashlamp. The sol-gel antireflective coating was dip-coated at room temperature onto 8-cm diameter glass samples. The coating basically consisted of a halfwave- thick high-index material such as ZrO2-PVP (PolyVinyl Pyrrolidone) and a quarterwave- thick low-index material such as SiO2-siloxane. To improve the abrasion resistance of the coated part, a lubricating and water-repellent material was applied as a very thin overcoat. In addition to a 6.5 to 7.2% transmission gain over the spectrum of interest, the coating was moderately abrasion resistant and chemically durable. Flashlamp-induced damage to the antireflective coating for 1000 glow discharges at 10 to 12 J/cm2 were minimal and similar to uncoated parts.

  14. Preparation of PDMS-coated microspheres by sol-gel method for sorptive extraction of PAHs

    Institute of Scientific and Technical Information of China (English)

    Chang Guang Yang; Xiang Juan Ji; Xiao Zheng Lan

    2008-01-01

    In this paper, a novel SPME mode, PDMS-coated solid glass microspheres (SGMs), were prepared by sol-gel method. Using homemade thermal desorption unit coupled with CGC-FID, six PAHs as model analytes, the performance of the new mode was characterized. The new extractive phase exhibited high thermal stability and satisfactory extraction capability. The detection limits were 0.01-0.045 ng/mL, and the linearity was from 0.5 ng/mL to 96 ng/mL. The R.S.D.s of repeatability for retention time and peak area were all within 0.074% and 6.7%, respectively. The recoveries of the PAHs were 78-127% from the sarnples taken from river water.

  15. Structural and electrical properties of sol-gel spin coated indium doped cadmium oxide thin films

    Energy Technology Data Exchange (ETDEWEB)

    Rajammal, R. [Department of Physics, M.V.M Govt. Arts College for Women, Dindigul-624001 (India); Savarimuthu, E., E-mail: savari56@gmail.com; Arumugam, S., E-mail: savari56@gmail.com [Department of Physcis, Gandhigram Rural Institute, Gandhigram-624302 (India)

    2014-04-24

    The indium doped CdO thin films have been prepared by the sol-gel spin coating technique and the influence of indium doping concentration on the structural and electrical properties of the deposited films has been investigated. The indium doping concentration in the solution has been varied from 0-10 wt% insteps of 2wt%. A indium doping concentration of 6wt% has been found to be optimum for preparing the films and at this stage a minimum resistivity of 5.92×10{sup −4}Ω cm and a maximum carrier concentration of 1.20×10{sup 20}cm{sup −3} have been realized.

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

    Directory of Open Access Journals (Sweden)

    Yotova L.

    2007-12-01

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

  17. Capillary Column Coated With Heptakis(2,3,6-tri-O-octyl)-β-cyclodextrin Using Sol-gel Technology

    Institute of Scientific and Technical Information of China (English)

    Xiao Xia GE; Ruo Nong FU; Rong Ji DAI; Li Wen LIU; Mei Ling QI

    2004-01-01

    Heptakis(2,3,6-tri-O-octyl)-β-cyclodextrin was coated onto the fused silica capillary by sol-gel technology.Column efficiency and column selectivity were studied. The results indicated that high ability of separation was acquired. Positional isomers of aromatic compounds were well separated.

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

    Science.gov (United States)

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

    2010-08-01

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

  19. Sol-gel based oxidation catalyst and coating system using same

    Science.gov (United States)

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

    2010-01-01

    An oxidation catalyst system is formed by particles of an oxidation catalyst dispersed in a porous sol-gel binder. The oxidation catalyst system can be applied by brush or spray painting while the sol-gel binder is in its sol state.

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

    Science.gov (United States)

    Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan

    2014-12-01

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

  1. Effect of Catalyst on the Formation of Silica Coating on Nickel Substrate by Sol -Gel Processing

    Institute of Scientific and Technical Information of China (English)

    Ali Ghasemi; F.Ashrafizadeh; M.A.Golozar; Ali Ashrafi

    2004-01-01

    In this research work silica coating was produced on nickel substrates by a sol-gel process. In order to increase the rate of hydrolysis and to reduce the rate of polymerization several acid catalysts including nitric acid-hydrochloric acid,acetic acid, hydrochloric acid and nitric acid were add to silica sol. Conversely, in order to control the rate of hydrolysis and to increase the rate of polymerization, basic catalyst of ammonia and ammonia hydroxyl were introduced in to the solution.Nickel specimens of known surface roughness were chemically cleaned and prepared by dipping in the sols. In order to produce a suitable silica coating the drying and firing cycles were optimized on these substrates. The structure and uniformity of the coatings produced were examined by scanning electron microscopy. Coatings composition was determined using glow discharge optical spectroscopy and EDAX microanalysis. Experimental result showed that hydrochloric acid, acetic acid, ammonia and acetic acid - ammonia are suitable catalytic agents for silica coating formation on nickel type substrate.

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

    Science.gov (United States)

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

    2016-04-01

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

  3. Surface-Engineered Fire Protective Coatings for Fabrics through Sol-Gel and Layer-by-Layer Methods: An Overview

    Directory of Open Access Journals (Sweden)

    Giulio Malucelli

    2016-07-01

    Full Text Available Fabric flammability is a surface-confined phenomenon: in fact, the fabric surface represents the most critical region, through which the mass and heat transfers, responsible for fueling the flame, are controlled and exchanged with the surroundings. More specifically, the heat the fabric surface is exposed to is transferred to the bulk, from which volatile products of thermal degradation diffuse toward the surface and the gas phase, hence feeding the flame. As a consequence, the chemical and physical characteristics of the fabric surface considerably affect the ignition and combustion processes, as the surface influences the flux of combustible volatile products toward the gas phase. In this context, it is possible to significantly modify (and improve the fire performance of textile materials by “simply” tailoring their surface: currently, one of the most effective approaches exploits the deposition of tailored coatings able to slow down the heat and mass transfer phenomena occurring during the fire stages. This paper reviews the current state of the art related to the design of inorganic, hybrid, or organic flame-retardant coatings suitable for the fire protection of different fabric substrates (particularly referring to cotton, polyester, and their blends. More specifically, the use of sol-gel and layer-by-layer (LbL methods is thoroughly discussed; then, some recent examples of flame retardant coatings are presented, showing their potential advances and their current limitations.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-08-15

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

  5. High temperature oxidation of chromium with nanometric ceria sol-gel coating

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Isothermal oxidation behavior of chromium with and without nanometric sol-gel CeO2 coating is studied at 1000℃ in air. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) are used to examine the surface morphology and microstructure of their oxide films. It is found that ceria coating greatly improves the anti-oxidation property of chromium. Laser Raman spectrometer and X-ray diffraction spectrometer (XRD) are also used to study the stress level in oxide films formed on ceria-coated and ceria-free Cr. The difference in oxidation behavior is mainly attributed to the fact that ceria greatly reduces the growth speed and grain size of Cr2O3 film, and this fine grain-sized Cr2O3 film probably has better high temperature plasticity, i.e. oxide film can relieve parts of compressive stress by means of creeping. XRD and Raman testing results both show the stress declination due to nano-CeO2 application, and their deviation is analyzed concerning to the rare earth effect.

  6. Synergic combination of the sol-gel method with dip coating for plasmonic devices.

    Science.gov (United States)

    Figus, Cristiana; Patrini, Maddalena; Floris, Francesco; Fornasari, Lucia; Pellacani, Paola; Marchesini, Gerardo; Valsesia, Andrea; Artizzu, Flavia; Marongiu, Daniela; Saba, Michele; Marabelli, Franco; Mura, Andrea; Bongiovanni, Giovanni; Quochi, Francesco

    2015-01-01

    Biosensing technologies based on plasmonic nanostructures have recently attracted significant attention due to their small dimensions, low-cost and high sensitivity but are often limited in terms of affinity, selectivity and stability. Consequently, several methods have been employed to functionalize plasmonic surfaces used for detection in order to increase their stability. Herein, a plasmonic surface was modified through a controlled, silica platform, which enables the improvement of the plasmonic-based sensor functionality. The key processing parameters that allow for the fine-tuning of the silica layer thickness on the plasmonic structure were studied. Control of the silica coating thickness was achieved through a combined approach involving sol-gel and dip-coating techniques. The silica films were characterized using spectroscopic ellipsometry, contact angle measurements, atomic force microscopy and dispersive spectroscopy. The effect of the use of silica layers on the optical properties of the plasmonic structures was evaluated. The obtained results show that the silica coating enables surface protection of the plasmonic structures, preserving their stability for an extended time and inducing a suitable reduction of the regeneration time of the chip.

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

    Institute of Scientific and Technical Information of China (English)

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

    2005-01-01

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

  8. Constructing a superhydrophobic surface on polydimethylsiloxane via spin coating and vapor-liquid sol-gel process.

    Science.gov (United States)

    Peng, Yu-Ting; Lo, Kuo-Feng; Juang, Yi-Je

    2010-04-06

    In this study, a superhydrophobic surface on polydimethylsiloxane (PDMS) substrate was constructed via the proposed vapor-liquid sol-gel process in conjunction with spin coating of dodecyltrichlorosilane (DTS). Unlike the conventional sol-gel process where the reaction takes place in the liquid phase, layers of silica (SiO(2)) particles were formed through the reaction between the reactant spin-coated on the PDMS surface and vapor of the acid solution. This led to the SiO(2) particles inlaid on the PDMS surface. Followed by subsequent spin coating of DTS solution, the wrinkle-like structure was formed, and the static contact angle of the water droplet on the surface could reach 162 degrees with 2 degrees sliding angle and less than 5 degrees contact angle hysteresis. The effect of layers of SiO(2) particles, concentrations of DTS solution and surface topography on superhydrophobicity of the surface is discussed.

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

    Science.gov (United States)

    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.

  10. Zinc oxide films prepared by sol-gel spin-coating

    Energy Technology Data Exchange (ETDEWEB)

    Natsume, Y.; Sakata, H. [Tokai Univ., Hiratsuka, Kanagawa (Japan). Dept. of Appl. Chem.

    2000-08-22

    The d.c. electrical conductivity and optical properties of undoped zinc oxide films prepared by the sol-gel process using a spin-coating technique were investigated. The ZnO films were obtained by 10 cycle spin-coated and dried zinc acetate films followed by annealing in air at 500-575 C. The films deposited on the Pyrex glass substrate were polycrystalline and c-axis oriented. A minimum film resistivity gave 28.2 {omega} cm at an annealing temperature of 525 C. The temperature dependence of the conductivity indicated electron transport in the conduction band due to thermal excitation of donor electrons for temperatures from 250 to 300 K. The grain boundary scattering effect due to thermionic emission was confirmed. For temperatures below 250 K nearest-neighbor hopping conduction was dominant in the films. The films were transparent in the visible range above 400 nm and had sharp ultraviolet absorption edges at 380 nm. The absorption edge analysis revealed that the optical band gap energy for the films was 3.20-3.21 eV and the electronic transition was of the direct transition type. From the Urbach tail analysis the width of the localized state E{sub e}=0.07-0.08 eV. (orig.)

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

    Science.gov (United States)

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

    1992-12-01

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

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

    Science.gov (United States)

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

    2012-06-01

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

  13. Sol-gel immobilized cyano-polydimethylsiloxane coating for capillary microextraction of aqueous trace analytes ranging from polycyclic aromatic hydrocarbons to free fatty acids.

    Science.gov (United States)

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

    2006-08-18

    Sol-gel coating containing highly polar cyanopropyl and nonpolar poly(dimethylsiloxane) components (sol-gel CN-PDMS coating) was developed for capillary microextraction (CME). The sol-gel chemistry provided an efficient means to immobilize the CN-PDMS coating by establishing chemical anchorage between the coating and the fused silica capillary inner surface. This chemical bond provided excellent thermal and solvent stability to the created sol-gel coating. For the extraction of polar and nonpolar analytes, the upper allowable conditioning temperatures were 330 degrees C and 350 degrees C, respectively. To our knowledge, this is the first time when a CN-PDMS thick coating survived such a high operation temperature. The prepared sol-gel CN-PDMS coating provided effective extraction of polar and nonpolar analytes simultaneously from aqueous samples. The cyanopropyl moiety in sol-gel CN-PDMS coatings provided effective extraction of highly polar analytes such as free fatty acids, alcohols, and phenols without requiring derivatization, pH adjustment or salting out procedures. The PDMS moiety, on the other hand, provided efficient extraction of nonpolar analytes. The extraction properties of the sol-gel CN-PDMS coatings can be fine tuned via manipulation of relative proportions of 3-cyanopropyltriethoxysilane and hydroxy-terminated PDMS in the sol solution used to create the coatings. Detection limits of nanogram/liter (ng/L) were achieved for both highly polar and nonpolar analytes directly extracted from aqueous media using sol-gel CN-PDMS coated microextraction capillaries followed by GC analysis.

  14. LONG-TERM OBSERVATION FOR OSSEOINTEGRATION OF CALCIUM PHOSPHATE SOL-GEL COATING ON Ti-6Al-4V IMPLANTS

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Objective To observe the long-term impact of calcium phosphate (CaP) sol-gel coating on bone growth around porous-surfaced implant.Methods The porous-surfaced Ti-6Al-4V implants were prepared with the addition of a thin film of CaP sol-gel coating, and implanted into the tibiae of 8 rabbits, each with two implants. Implanted sites were allowed to heal for 2,8, 12, and 24 weeks, after which specimens were obtained for scanning electron microscope analysis using the freezefracture technique.Results The sol-gel coated implants recovered by freeze-fracture technique showed extensive bone growth from the endosteum along the implant surface. The bone was in direct contact with the CaP layer. The cement line-like layer was clearly demonstrated to be an intervening electron dense afibrillar layer between the CaP coat and the overlying newly deposited bone. The stability and osseointegration of the porous-surfaced implants seemed not to be affected by the osteoclastic resorption of CaP layer occurred during 24 weeks of healing.Conclusion Based on the findings in the long-term observation, the addition of a thin layer of CaP promotes an extensive osseointegrated interface between the porous-surfaced Ti-6Al-4V implants and the newly deposited bone.

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

    Directory of Open Access Journals (Sweden)

    Najmeh Asadi

    2014-06-01

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

  16. Water repellent porous silica films by sol-gel dip coating method.

    Science.gov (United States)

    Rao, A Venkateswara; Gurav, Annaso B; Latthe, Sanjay S; Vhatkar, Rajiv S; Imai, Hiroaki; Kappenstein, Charles; Wagh, P B; Gupta, Satish C

    2010-12-01

    The wetting of solid surfaces by water droplets is ubiquitous in our daily lives as well as in industrial processes. In the present research work, water repellent porous silica films are prepared on glass substrate at room temperature by sol-gel process. The coating sol was prepared by keeping the molar ratio of methyltriethoxysilane (MTES), methanol (MeOH), water (H(2)O) constant at 1:12.90:4.74, respectively, with 2M NH(4)OH throughout the experiments and the molar ratio (M) of MTES/Ph-TMS was varied from 0 to 0.22. A simple dip coating technique is adopted to coat silica films on the glass substrates. The static water contact angle as high as 164° and water sliding angle as low as 4° was obtained for silica film prepared from M=0.22. The surface morphological studies of the prepared silica film showed the porous structure with pore sizes typically ranging from 200nm to 1.3μm. The superhydrophobic silica films prepared from M=0.22 retained their superhydrophobicity up to a temperature of 285°C and above this temperature the films became superhydrophilic. The porous and water repellent silica films are prepared by proper alteration of the Ph-TMS in the coating solution. The prepared silica films were characterized by surface profilometer, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier Transform Infrared (FT-IR) spectroscopy, humidity tests, chemical aging tests, static and dynamic water contact angle measurements.

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

    Science.gov (United States)

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

    2004-09-01

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

  18. Characterizations of multilayer ZnO thin films deposited by sol-gel spin coating technique

    Science.gov (United States)

    Khan, M. I.; Bhatti, K. A.; Qindeel, Rabia; Alonizan, Norah; Althobaiti, Hayat Saeed

    In this work, zinc oxide (ZnO) multilayer thin films are deposited on glass substrate using sol-gel spin coating technique and the effect of these multilayer films on optical, electrical and structural properties are investigated. It is observed that these multilayer films have great impact on the properties of ZnO. X-ray Diffraction (XRD) confirms that ZnO has hexagonal wurtzite structure. Scanning Electron Microscopy (SEM) showed the crack-free films which have uniformly distributed grains structures. Both micro and nano particles of ZnO are present on thin films. Four point probe measured the electrical properties showed the decreasing trend between the average resistivity and the number of layers. The optical absorption spectra measured using UV-Vis. showed the average transmittance in the visible region of all films is 80% which is good for solar spectra. The performance of the multilayer as transparent conducting material is better than the single layer of ZnO. This work provides a low cost, environment friendly and well abandoned material for solar cells applications.

  19. Ceramic membrane by tape casting and sol-gel coating for microfiltration and ultrafiltration application

    Science.gov (United States)

    Das, Nandini; Maiti, H. S.

    2009-11-01

    Alumina membrane filters in the form of thin (0.3-0.8 mm) discs of 25-30 mm diameter suitable for microfiltration application have been fabricated by tape-casting technique. Further using this microfiltration membrane as substrate, boehmite sol coating was applied on it and ultrafiltration membrane with very small thickness was formed. The pore size of the microfiltration membrane could be varied in the range of 0.1-0.7 μm through optimisation of experimental parameter. In addition, each membrane shows a very narrow pore size distribution. The most important factor, which determines the pore size of the membrane, is the initial particle size and its distribution of the ceramic powder. The top thin ultrafiltration, boehmite layer was prepared by sol-gel method, with a thickness of 0.5 μm. Particle size of the sol was approximately 30-40 nm. The structure and formation of the layer was analysed through TEM. At 550 °C formation of the top layer was completed. The pore size of the ultrafiltration membrane measured from TEM micrograph was almost 10 nm. Results of microbial (Escherichia coli—smallest-sized water-borne bacteria) test confirm the possibility of separation through this membrane

  20. Photochromic glass thin film formed by the sol-gel coating method

    Science.gov (United States)

    Nakazumi, Hiroyuki; Nagashiro, Rie; Matsumoto, Shinya; Isagawa, Kakuzoh

    1994-10-01

    The photochromic gel thin films using 1'-butyl-3',3'-dimethyl-6-nitro-spiro[2H-1- benzopyran-2,2'-indoline] (1) and 1'-butyl-spiro[2H-indole-2,3'- [3H]naphtho[2,1-b][1,4]oxazine] (2) dispersed in sol in the sol-gel processing were prepared and photochromic behaviors of these films were investigated. A good transparent coating layer on glass surface was formed in the range of ca. 6 - 10 wt% of 1 or 2 to alkoxysilane, and was colored by UV irradiation. The absorption band formed by UV-irradiation disappeared by thermal decay and also by Vis irradiation for 1. The thermal fading of the colored form to the spiro form 1 or 2 is dependent on a matrix of the gels, the colored forms in the film starting from methyltriethoxysilane (MTES), which is expected to include larger pores than in the film starting from tetraethoxysilane (TEOS) or silane oligomer, show faster thermal fading which roughly follows the first order kinetics. The colored form in the gel is stabilized, compared with that in solution or bulk gel, and it is suggested that there are some kinds of colored species in thin gel films containing spiropyran 1, which may be some aggregates, whereas only a colored species from spironaphthooxazine 2 is suggested. Photochromic behavior of 2 in sol was also examined.

  1. Zinc-oxide nanowires electrochemically grown onto sol-gel spin-coated seed layers

    Energy Technology Data Exchange (ETDEWEB)

    Bojorge, Claudia D.; Canepa, Horacio R. [CINSO, CONICET-CITEDEF, Juan B. de La Salle 4397, CP 1603 Villa Martelli, Buenos Aires (Argentina); Kent, Vladimir R.; Teliz, Erika; Marotti, Ricardo E.; Dalchiele, Enrique A. [Facultad de Ingenieria, Instituto de Fisica, Universidad de la Republica, J. H. Reissig 565, CC 30, CP 11000, Montevideo (Uruguay); Henriquez, Rodrigo; Gomez, Humberto [Facultad de Ciencias, Instituto de Quimica, Pontificia Universidad Catolica de Valparaiso, Casilla 4059, Valparaiso (Chile)

    2011-07-15

    The electrochemical deposition of ZnO nanowires (NW) was optimized by growing onto a previously deposited seed layer. The ZnO seed layer was prepared by a sol-gel process from different precursor solutions and deposited onto FTO/glass by spin coating. Afterwards, NW were electrochemically grown onto those seed layers. The electrolyte was an aqueous solution of the Zn{sup +2} precursor (1 mM zinc acetate) and a supporting electrolyte (0.1 M sodium acetate), saturated with bubbling oxygen. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and optical transmittance. The XRD measurements show typical diffraction pattern of ZnO wurtzite structure. The SEM micrographs show the presence of smooth NW with hexagonal sections with diameters ranging from 40 to 250 nm. The optical transmittance reveals the presence of ZnO with bandgap energy between 3.23 and 3.29 eV. These spectra show a monotonically increasing transmittance from the UV into the red part of the spectrum. This feature may be originated in the dispersion of light at the NW and can be used to enhance below-gap absorption. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  2. Detection of hydrofluoric acid by a SiO2 sol-gel coating fiber-optic probe based on reflection-based localized surface plasmon resonance

    National Research Council Canada - National Science Library

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

    2011-01-01

    ...) 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 SiO(2) sol-gel coating...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-15

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

  4. Mixed Pyridine-phenol Boron Complex Encapsulated in Polymer/Silica Hybrid Sol-gel Matrix

    Institute of Scientific and Technical Information of China (English)

    DONG Wei; TANG Jun; WANG Yue

    2008-01-01

    A novel pyridine-phenol boron complex[(dppy)BF]was encapsulated into polymer/silica composite matrix by sol-gel process.UV-Vis absorption spectra show that this process can control the aggregation structure of complex(dppy)BF.The results of photoluminescence of(dppy)BF in sol-gel composite film indicate that both fluorescence intensity and photostability are markedly increased using this method compared with other methods,which increases the practical significance of such composite film.

  5. Evaluation of tetraethoxysilane (TEOS) sol-gel coatings, modified with green synthesized zinc oxide nanoparticles for combating microfouling.

    Science.gov (United States)

    Krupa, A Nithya Deva; Vimala, R

    2016-04-01

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

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

    OpenAIRE

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

    2012-01-01

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

  7. Vibrational spectroscopic studies of triethoxy(4-(trifluoromethyl)-phenyl) silane and its sol-gel coating.

    Science.gov (United States)

    Li, Ying-Sing

    2012-10-01

    We have prepared a silica sol-gel using triethoxy (4-(trifluoromethyl)-phenyl) silane (TETFMPS) as a precursor in ethanol solution under acidic condition. The prepared sol-gel was applied to the surface treatment of aluminum for corrosion prevention. Infrared and Raman spectra of the silane coupling agent, sol-gel and sol-gel films on metal have been collected. Infrared spectroscopy has been used to study the thermal effect on the chemical composition of xerogel. Results suggested that TETFMPS molecule has a C(s) point group symmetry with the plane of reflection orthogonal to the phenyl ring and the organic part of the sol-gel film remains essentially unchanged at or below 450 °C but decomposes at or above 550 °C. After the decomposition of the organic branch, the remaining film is composed of silica. Vibrational assignments were suggested by using the collected spectroscopic data in different states along with the group vibrational frequencies and other related references.

  8. Blade-coated sol-gel indium-gallium-zinc-oxide for inverted polymer solar cell

    Directory of Open Access Journals (Sweden)

    Yan-Huei Lee

    2016-11-01

    Full Text Available The inverted organic solar cell was fabricated by using sol-gel indium-gallium-zinc-oxide (IGZO as the electron-transport layer. The IGZO precursor solution was deposited by blade coating with simultaneous substrate heating at 120 °C from the bottom and hot wind from above. Uniform IGZO film of around 30 nm was formed after annealing at 400 °C. Using the blend of low band-gap polymer poly[(4,8-bis-(2-ethylhexyloxy-benzo(1,2-b:4,5-b’dithiophene-2,6-diyl-alt- (4-(2-ethylhexanoyl-thieno [3,4-b]thiophene--2-6-diyl] (PBDTTT-C-T and [6,6]-Phenyl C71 butyric acid methyl ester ([70]PCBM as the active layer for the inverted organic solar cell, an efficiency of 6.2% was achieved with a blade speed of 180 mm/s for the IGZO. The efficiency of the inverted organic solar cells was found to depend on the coating speed of the IGZO films, which was attributed to the change in the concentration of surface OH groups. Compared to organic solar cells of conventional structure using PBDTTT-C-T: [70]PCBM as active layer, the inverted organic solar cells showed significant improvement in thermal stability. In addition, the chemical composition, as well as the work function of the IGZO film at the surface and inside can be tuned by the blade speed, which may find applications in other areas like thin-film transistors.

  9. Blade-coated sol-gel indium-gallium-zinc-oxide for inverted polymer solar cell

    Science.gov (United States)

    Lee, Yan-Huei; Tsai, Pei-Ting; Chang, Chia-Ju; Meng, Hsin-Fei; Horng, Sheng-Fu; Zan, Hsiao-Wen; Lin, Hung-Cheng; Liu, Hung-Chuan; Tseng, Mei-Rurng; Yeh, Han-Cheng

    2016-11-01

    The inverted organic solar cell was fabricated by using sol-gel indium-gallium-zinc-oxide (IGZO) as the electron-transport layer. The IGZO precursor solution was deposited by blade coating with simultaneous substrate heating at 120 °C from the bottom and hot wind from above. Uniform IGZO film of around 30 nm was formed after annealing at 400 °C. Using the blend of low band-gap polymer poly[(4,8-bis-(2-ethylhexyloxy)-benzo(1,2-b:4,5-b')dithiophene)-2,6-diyl-alt- (4-(2-ethylhexanoyl)-thieno [3,4-b]thiophene-)-2-6-diyl)] (PBDTTT-C-T) and [6,6]-Phenyl C71 butyric acid methyl ester ([70]PCBM) as the active layer for the inverted organic solar cell, an efficiency of 6.2% was achieved with a blade speed of 180 mm/s for the IGZO. The efficiency of the inverted organic solar cells was found to depend on the coating speed of the IGZO films, which was attributed to the change in the concentration of surface OH groups. Compared to organic solar cells of conventional structure using PBDTTT-C-T: [70]PCBM as active layer, the inverted organic solar cells showed significant improvement in thermal stability. In addition, the chemical composition, as well as the work function of the IGZO film at the surface and inside can be tuned by the blade speed, which may find applications in other areas like thin-film transistors.

  10. Characterization of nanocrystalline ZnO:Al films by sol-gel spin coating method

    Energy Technology Data Exchange (ETDEWEB)

    Gareso, P. L., E-mail: pgareso@gmail.com; Rauf, N., E-mail: pgareso@gmail.com; Juarlin, E., E-mail: pgareso@gmail.com [Department of Physics, Faculty of Mathematics and Natural Sciences, Hasanuddin University, Makassar 90245 (Indonesia); Sugianto,; Maddu, A. [Department of Physics, Faculty of Mathematics and Natural Sciences, Bogor Institute of Culture, IPB Bogor (Indonesia)

    2014-09-25

    Nanocrystalline ZnO films doped with aluminium by sol-gel spin coating method have been investigated using optical transmittance UV-Vis and X-ray diffraction (X-RD) measurements. ZnO films were prepared using zinc acetate dehydrate (Zn(CH{sub 3}COO){sub 2}@@‡2H{sub 2}O), ethanol, and diethanolamine (DEA) as a starting material, solvent, and stabilizer, respectively. For doped films, AlCl{sub 3} was added to the mixture. The ZnO:Al films were deposited on a transparent conductive oxide (TCO) substrate using spin coating technique at room temperature with a rate of 3000 rpm in 30 sec. The deposited films were annealed at various temperatures from 400°C to 600°C during 60 minutes. The transmittance UV-Vis measurement results showed that after annealing at 400°C, the energy band gap profile of nanocrystalline ZnO:Al film was a blue shift. This indicated that the band gap of ZnO:Al increased after annealing due to the increase of crystalline size. As the annealing temperature increased the bandgap energy was a constant. In addition to this, there was a small oscillation occurring after annealing compared to the as–grown samples. In the case of X-RD measurements, the crystalinity of the films were amorphous before annealing, and after annealing the crystalinity became enhance. Also, X-RD results showed that structure of nanocrystalline ZnO:Al films were hexagonal polycrystalline with lattice parameters are a = 3.290 Å and c = 5.2531 Å.

  11. LaCoO3 nanosystems by a hybrid CVD/sol-gel approach.

    Science.gov (United States)

    Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Gasparotto, Alberto; Maragno, Cinzia; Tondello, Eugenio; Sada, Cinzia

    2005-05-01

    LaCoO3 nanosystems are receiving increasing attention for the development of innovative fuel cells and heterogeneous catalysts. In this report, we describe the synthesis of nanophasic LaCoO3 thin films by a hybrid chemical vapor deposition (CVD)/sol-gel (SG) approach. The adopted strategy consists in the CVD of La-O-based systems on SG cobalt oxide xerogels CoOx(OH)y at temperatures as low as 200 degrees C and in the subsequent thermal treatment in air (400-800 degrees C, 2-8 h). In this context, particular attention is devoted to achieving an intimate La/Co intermixing already in the as-prepared systems, in order to favor reactions yielding a single La-Co-O phase with uniform composition. The obtained results point out to the formation of pure and structurally homogeneous LaCoO3 nanosystems after annealing at 700 degrees C, 2 h, with a typical grain-like morphology. More severe thermal treatment resulted in the thermal decomposition of LaCoO3 nanocrystallites.

  12. Electrochemical codeposition of sol-gel films on stainless steel: controlling the chemical and physical coating properties of biomedical implants.

    Science.gov (United States)

    Okner, Regina; Favaro, Gregory; Radko, Anna; Domb, Abraham Jacob; Mandler, Daniel

    2010-12-14

    The electrochemically assisted codeposition of sol-gel thin films on stainless steel is described. Specifically, electrodeposition of films based on aminopropyltriethoxysilane (APTS), and its codeposition with propyltrimethoxysilane (PrTMOS) and phenyltrimethoxysilane (PhTMOS) has been accomplished by applying negative potentials. The latter increases the concentration of hydroxyl ions on the stainless steel surface and thus catalyzes the condensation and deposition of the sol-gel films. The films were characterized by profilometry, electrochemical impedance spectroscopy (EIS), alternating current voltammetry (ACV), goniometry, atomic force microscopy (AFM) and scanning electron microscopy (SEM). AFM and SEM analysis of codeposited APTS:PrTMOS films disclosed the structural changes induced by altering the deposition solution composition and the applied potential. Codeposited APTS:PhTMOS did not show any structural differences from their electrodeposited homopolymers, while Nano Scratch Test clearly revealed the changes in the elastic and adhesion properties, suggesting the formation of an APTS:PhTMOS composite. EIS of the films showed good resistance towards penetration of hydrophilic species, such as hexacyanoferrate. ACV measurements of the homo and codeposits showed the decrease of the interfacial capacity as a result of the electrochemical deposition. In essence, controllable sol-gel films with tunable chemical and physical properties based on controlling the combination of the precursors, pH and electrochemical properties can be electrodeposited on conducting surfaces. The application of this approach has been demonstrated by coating a stainless steel coronary stent.

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

    Science.gov (United States)

    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.

  14. A moisture-resistant antireflective coating by sol-gel process for neodymium-doped phosphate laser glass

    Institute of Scientific and Technical Information of China (English)

    Ruijun Liu; Ruoyu Zhan; Yongxing Tang; Jianqiang Zhu

    2006-01-01

    @@ Using methyl triethoxysilicane as precursor, a moisture-resistant coating for neodymium-doped laser glass was developed by the sol-gel process. Colloidal silica was added in coating solution as modifier. The refractive index of this coating varied from 1.31 to 1.42. A porous antireflective (AR) silica coating with the index of 1.27 was coated on the moisture-resistant coating surface. The two-layer coating possessed transmission up to 99.1% at wavelength of 966 nm, surface root-mean-square (RMS) roughness of 1.245nm, and roughness of average (RA) of 0.961 nm. In the case of laser of 1053-nm laser wavelength and 1-ns pulse duration, the damage threshold of the two-layer coatings was more than 15 J/cm2.

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

    Science.gov (United States)

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

    2010-10-01

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

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

    Science.gov (United States)

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

    2014-09-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Kokkoris, M. E-mail: kokkoris@mail.demokritos.gr; Trapalis, C.C. E-mail: trapalis@ims.demokritos.gr; Kossionides, S.; Vlastou, R.; Nsouli, B.; Groetzschel, R.; Spartalis, S.; Kordas, G.; Paradellis, Th

    2002-04-01

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

  18. Synthesis and characterization of transparent conductive zinc oxide thin films by sol-gel spin coating method

    Science.gov (United States)

    Winarski, David

    Zinc oxide has been given much attention recently as it is promising for various semiconductor device applications. ZnO has a direct band gap of 3.3 eV, high exciton binding energy of 60 meV and can exist in various bulk powder and thin film forms for different applications. ZnO is naturally n-type with various structural defects, which sparks further investigation into the material properties. Although there are many potential applications for this ZnO, an overall lack of understand and control of intrinsic defects has proven difficult to obtain consistent, repeatable results. This work studies both synthesis and characterization of zinc oxide in an effort to produce high quality transparent conductive oxides. The sol-gel spin coating method was used to obtain highly transparent ZnO thin films with high UV absorbance. This research develops a new more consistent method for synthesis of these thin films, providing insight for maintaining quality control for each step in the procedure. A sol-gel spin coating technique is optimized, yielding highly transparent polycrystalline ZnO thin films with tunable electrical properties. Annealing treatment in hydrogen and zinc atmospheres is researched in an effort to increase electrical conductivity and better understand intrinsic properties of the material. These treatment have shown significant effects on the properties of ZnO. Characterization of doped and undoped ZnO synthesized by the sol-gel spin coating method was carried out using scanning electron microscopy, UV-Visible range absorbance, X-ray diffraction, and the Hall Effect. Treatment in hydrogen shows an overall decrease in the number of crystal phases and visible absorbance while zinc seems to have the opposite effect. The Hall Effect has shown that both annealing environments increase the n-type conductivity, yielding a ZnO thin film with a carrier concentration as high as 3.001 x 1021 cm-3.

  19. Role of precursors and coating polymers in sol-gel chemistry toward enhanced selectivity and efficiency in solid phase microextraction.

    Science.gov (United States)

    Bagheri, Habib; Piri-Moghadam, Hamed; Ahdi, Tayebeh

    2012-09-12

    To evaluate the selectivity and efficiency of solid phase microextraction (SPME) fiber coatings, synthesized by sol-gel technology, roles of precursors and coating polymers were extensively investigated. An on-line combination of capillary microextraction (CME) technique and high performance liquid chromatography (HPLC) was set up to perform the investigation. Ten different fiber coatings were synthesized in which five of them contained only the precursor and the rests were prepared using both the precursor and coating polymer. All the coatings were chemically bonded to the inner surface of copper tubes, intended to be used as the CME device and already functionalized by self-assembly monolayers of 3-(mercaptopropyl)trimethoxysilane (3MPTMOS). The selected precursors included tetramethoxysilane (TMOS), 3-(trimethoxysilyl)propylmethacrylate (TMSPMA), 3-(triethoxysilyl)-propylamine (TMSPA), 3MPTMOS, [3-(2,3-epoxypropoxy)-propyl]-trimethoxysilane (EPPTMOS) while poly(ethyleneglycol) (PEG) was chosen as the coating polymer. The effects of different precursors on the extraction efficiency and selectivity, was studied by selecting a list of compounds ranging from non-polar to polar ones, i.e. polycyclic aromatic hydrocarbon, herbicides, estrogens and triazines. The results from CME-HPLC analysis revealed that there is no significant difference between precursors, except TMOS, in which has the lowest extraction efficiency. Most of the selected precursors have rather similar interactions toward the selected analytes which include Van der Walls, dipole-dipole and hydrogen bond while TMOS has only dipole-dipole interaction and therefore the least efficiency. TMOS is silica but the other sorbents are organically modified silica (ORMOSIL). Our investigation revealed that it is rather impossible to prepare a selective coating using conventional sol-gel methodologies. The comparison study performed among the fiber coatings contained only a precursor and those synthesized by a

  20. Polycrystalline BiFeO3 thin film synthesized via sol-gel assisted spin coating technique for photosensitive application

    Science.gov (United States)

    Bogle, K. A.; Narwade, R. D.; Phatangare, A. B.; Dahiwale, S. S.; Mahabole, M. P.; Khairnar, R. S.

    2016-05-01

    We are reporting photosensitivity property of BiFeO3 thin film under optical illumination. The thin film used for photosensitivity work was fabricated via sol-gel assisted spin coating technique. I-V measurements on the Cu/BiFeO3/Al structure under dark condition show a good rectifying property and show dramatic blue shit in threshold voltage under optical illumination. The microstructure, morphology and elemental analysis of the films were characterized by using XRD, UV-Vis, FTIR, SEM and EDS.

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

    OpenAIRE

    Schmidt, Helmut K.; Kasemann, Reiner

    1994-01-01

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

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

    OpenAIRE

    Schmidt, Helmut K.; Kasemann, Reiner

    1993-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

    JI Guo-Jun; SHI Zhi-Ming

    2010-01-01

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

  4. Electrochemical Properties of Poly(ethylene oxide)(PEO) Doped TiO2-PEO Films Prepared by Sol-gel Dip Coating Technique

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    PEO modified TiO2-PEO organic-inorganic hybrid thin films were prepared via sol-gel dipping process on glass substrate pre-coated with ITO. The preparation parameters were studied. Electrochemical and optical properties of the films were characterized by cyclic voltammetric response and visible transmittance. X-ray diffraction (XRD) was used to determined the crystalline structure of the gel. The results show the sols added with PEO have acceptable stable periods for practical use. The PEO modified optical transitivity of the hybrid films has heavy effects on the crystallization of TiO2 during structural evolution because of the interaction between PEO and TiO2. PEO- TiO2 films have better electrochemical activity than the TiO2 equivalent behaved as higher Li+ insertion/extraction current density and cyclic reversibility.

  5. Thermal Annealing Effect on Optical Properties of Binary TiO2-SiO2 Sol-Gel Coatings

    Directory of Open Access Journals (Sweden)

    Xiaodong Wang

    2012-12-01

    Full Text Available TiO2-SiO2 binary coatings were deposited by a sol-gel dip-coating method using tetrabutyl titanate and tetraethyl orthosilicate as precursors. The structure and chemical composition of the coatings annealed at different temperatures were analyzed by Raman spectroscopy and Fourier Transform Infrared (FTIR spectroscopy. The refractive indices of the coatings were calculated from the measured transmittance and reflectance spectra. An increase in refractive index with the high temperature thermal annealing process was observed. The Raman and FTIR results indicate that the refractive index variation is due to changes in the removal of the organic component, phase separation and the crystal structure of the binary coatings.

  6. Influence of New Sol-gel Refractory Coating on the Casting Properties of Cold Box and Furan Cores for Grey Cast iron

    DEFF Research Database (Denmark)

    Nwaogu, Ugochukwu Chibuzoh; Poulsen, T.; Bischoff, C

    2010-01-01

    New Sol-Gel coated sand cores made from coldbox and furan binder systems were investigated. The idea of the coating was to improve the surface quality of castings. Grey iron was cast on the cores in a sand casting process. The effect of the high temperature of the melt on the cores was assessed...... transport zone (VTZ) when in contact with the melt is larger than it is in a coldbox which means the furan cores have higher moisture content. The new sol-gel coating has the potential for improving the surface quality of castings without negative effects on the graphite distribution. The surface...... of castings made using the new sol-gel coated furan cores show better surface quality than those made using the coldbox....

  7. Silica/polyacrylonitrile hybrid nanofiber membrane separators via sol-gel and electrospinning techniques for lithium-ion batteries

    Science.gov (United States)

    Yanilmaz, Meltem; Lu, Yao; Zhu, Jiadeng; Zhang, Xiangwu

    2016-05-01

    Silica/polyacrylonitrile (SiO2/PAN) hybrid nanofiber membranes were fabricated by using sol-gel and electrospinning techniques and their electrochemical performance was evaluated for use as separators in lithium-ion batteries. The aim of this study was to design high-performance separator membranes with enhanced electrochemical performance and good thermal stability compared to microporous polyolefin membranes. In this study, SiO2 nanoparticle content up to 27 wt% was achieved in the membranes by using sol-gel technique. It was found that SiO2/PAN hybrid nanofiber membranes had superior electrochemical performance with good thermal stability due to their high SiO2 content and large porosity. Compared with commercial microporous polyolefin membranes, SiO2/PAN hybrid nanofiber membranes had larger liquid electrolyte uptake, higher electrochemical oxidation limit, and lower interfacial resistance with lithium. SiO2/PAN hybrid nanofiber membranes with different SiO2 contents (0, 16, 19 and 27 wt%) were also assembled into lithium/lithium iron phosphate cells, and high cell capacities and good cycling performance were demonstrated at room temperature. In addition, cells using SiO2/PAN hybrid nanofiber membranes with high SiO2 contents showed superior C-rate performance compared to those with low SiO2 contents and commercial microporous polyolefin membrane.

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

    Directory of Open Access Journals (Sweden)

    YASSUKO IAMAMOTO

    2000-03-01

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

  9. Sensitive detection of influenza viruses with Europium nanoparticles on an epoxy silica sol-gel functionalized polycarbonate-polydimethylsiloxane hybrid microchip.

    Science.gov (United States)

    Liu, Jikun; Zhao, Jiangqin; Petrochenko, Peter; Zheng, Jiwen; Hewlett, Indira

    2016-12-15

    In an effort to develop new tools for diagnosing influenza in resource-limited settings, we fabricated a polycarbonate (PC)-polydimethylsiloxane (PDMS) hybrid microchip using a simple epoxy silica sol-gel coating/bonding method and employed it in sensitive detection of influenza virus with Europium nanoparticles (EuNPs). The incorporation of sol-gel material in device fabrication provided functionalized channel surfaces ready for covalent immobilization of primary antibodies and a strong bonding between PDMS substrates and PC supports without increasing background fluorescence. In microchip EuNP immunoassay (µENIA) of inactivated influenza viruses, replacing native PDMS microchips with hybrid microchips allowed the achievement of a 6-fold increase in signal-to-background ratio, a 12-fold and a 6-fold decreases in limit-of-detection (LOD) in influenza A and B tests respectively. Using influenza A samples with known titers, the LOD of influenza µENIA on hybrid microchips was determined to be ~10(4) TCID50 titer/mL and 10(3)-10(4) EID50 titer/mL. A comparison test indicated that the sensitivity of influenza µENIA enhanced using the hybrid microchips even surpassed that of a commercial laboratory influenza ELISA test. In addition to the sensitivity improvement, assay variation was clearly reduced when hybrid microchips instead of native PDMS microchips were used in the µENIA tests. Finally, infectious reference viruses and nasopharyngeal swab patient specimens were successfully tested using μENIA on hybrid microchip platforms, demonstrating the potential of this unique microchip nanoparticle assay in clinical diagnosis of influenza. Meanwhile, the tests showed the necessity of using nucleic acid confirmatory tests to clarify ambiguous test results obtained from prototype or developed point-of-care testing devices for influenza diagnosis.

  10. Synthesis of biocompatible hydrophobic silica-gelatin nano-hybrid by sol-gel process.

    Science.gov (United States)

    Smitha, S; Shajesh, P; Mukundan, P; Nair, T D R; Warrier, K G K

    2007-03-15

    Silica-biopolymer hybrid has been synthesised using colloidal silica as the precursor for silica and gelatin as the biopolymer counterpart. The surface modification of the hybrid material has been done with methyltrimethoxysilane leading to the formation of biocompatible hydrophobic silica-gelatin hybrid. Here we are reporting hydrophobic silica-gelatin hybrid and coating precursor for the first time. The hybrid gel has been evaluated for chemical modification, thermal degradation, hydrophobicity, particle size, transparency under the UV-visible region and morphology. FTIR spectroscopy has been used to verify the presence of CH(3) groups which introduce hydrophobicity to the SiO2-MTMS-gelatin hybrids. The hydrophobic property has also been tailored by varying the concentration of methyltrimethoxysilane. Contact angle by Wilhelmy plate method of transparent hydrophobic silica-gelatin coatings has been found to be as high as approximately 95 degrees . Oxidation of the organic group which induces the hydrophobic character occurs at 530 degrees C which indicates that the surface hydrophobicity is retained up to that temperature. Optical transmittance of SiO2-MTMS-gelatin hybrid coatings on glass substrates has been found to be close to 100% which will enable the hybrid for possible optical applications and also for preparation of transparent biocompatible hydrophobic coatings on biological substrates such as leather.

  11. Structure and Properties of BaFe12O19 Coated Fly Ash Cenospheres by Sol-Gel Process

    Institute of Scientific and Technical Information of China (English)

    ZENG Aixiang; XIONG Weihao; WANG Caifang; ZHOU Qionghua

    2006-01-01

    Thin films of barium hexaferrite were prepared on fly ash cenosphere particles by the sol-gel method using Fe(NO3)3·9H2O,Ba(NO3)2 and citric acid as raw materials. The prepared films were characterized by differential thermal and thermogravimetric analysis (DTA-TG), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and vibrating sample magnetometry. The magnetic and structural properties of barium hexaferrite coated cenosphere particles were also studied. The experimental results show that even and continual barium hexaferrite coatings were prepared on fly ash cenospheres, and the magnetic conductivity was imparted to these non-conducting oxide ceramic particles. The low density barium hexaferrite coated cenosphere particles may be utilized for manufacturing microwave absorbing materials.

  12. Characterizing Sintered Nano-Hydroxyapatite Sol-Gel Coating Deposited on a Biomedical Ti-Zr-Nb Alloy

    Science.gov (United States)

    Jafari, Hassan; Hessam, Hamid; Shahri, Seyed Morteza Ghaffari; Assadian, Mahtab; Shairazifard, Shahin Hamtaie Pour; Idris, Mohd Hasbullah

    2016-03-01

    In this study, sol-gel dip-coating method was used to coat nano-hydroxyapatite on specimens of Ti-14Zr-13Nb alloy for orthopedic applications. The coated specimens were sintered at three different temperatures and time spans to evaluate the impact of sintering process on microstructure, mechanical, bio-corrosion, and bioactivity properties of the coating. Field-emission scanning electron microscopy and x-ray diffraction were used to analyze the coating microstructure. Coating adhesion and mechanical performance were also investigated by scratch testing. Besides, electrochemical corrosion and immersion tests were performed in simulated body fluid to examine the sintering effect on corrosion performance and bioactivity of the coatings, respectively. The evaluations of coated specimens displayed that sintering at elevated temperatures leads to higher surface integrity and improves crystallinity of the nano-hydroxyapatite to approximately 89% which brings about distinctively enhanced mechanical properties. Similarly, it improved the corrosion rate for about 17 times through sintering at 700 °C. Immersion test proved that the coating increased the bioactivity resulted from the dissolution of calcium phosphates into the corresponding environment. It is noticeable that sintering the dip-coated specimens in the nano-hydroxyapatite improves corrosion performance and maintains bioactive behaviors as well.

  13. Mechanical properties of chemically bonded sand core materials dipped in sol-gel coating impregnated with filter

    DEFF Research Database (Denmark)

    Nwaogu, Ugochukwu Chibuzoh; Tiedje, Niels Skat

    2012-01-01

    -displacement curve from which the mechanical properties of the materials are deduced. The fracture surfaces were examined using a stereomicroscope and a scanning electron microscope. From the results, the strengths of the core materials were slightly reduced by the coating in tensile and flexural modes, while...... the strengths were increased under compression. The mode of fracture of the chemically bonded sand core materials was observed to be intergranular through the binder. The stiffness of the chemically bonded sand core materials was determined. For better understanding of the mechanical properties......A novel sol-gel coating impregnated with filter dust was applied on chemically bonded sand core materials by dipping. After curing, the strengths of the core materials were measured under uniaxial loading using a new strength testing machine (STM). The STM presents the loading history as a force...

  14. Preparation of Poly (ethylene oxide) (PEO) Modified Tungsten Oxide Hybrid Films via Sol-Gel Processing

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Poly (ethylene axide) (PEO) modified WO3 thin films were prepared on glass substrates with special temperature.The sol-gel transition proess was investigated by using DTA-TG,SEM and XRD.The electrochemical characteristic of the films was studied by cyclic voltmmetry measurement.The results show that PEO has heavy effects on the crystallization of WO3 during structure evolution because of the interaction between PEO and WO3.It increases the crystallization temperature of the gels and thus improves the electrochemical properties and cyclic life of WO3 film as electrochromic materials.

  15. Microstructure and Property of TiN-TiB2 Hardened Coating Prepared by Hybrid Method Combined Sol-Gel with Laser Hardening%激光复合溶胶-凝胶法制备TiN-TiB2强化涂层的组织与性能

    Institute of Scientific and Technical Information of China (English)

    张群莉; 曾启; 姚建华; 潘颐

    2012-01-01

    The compound powder consisted of TiO2、BN and graphitic was prepared by sol-gel method at first, and was preplaced on the surface of 45 steel substrate, and then was irradiated by high density laser to get the enhanced coating with TiN and TiB2 in this paper. The microstructures, elements composition and phases were investigated by scanning electron microscope, spectrum analyzer and x-ray diffraction respectively. The microhardness of the coating was tested as well. The results show that the coating has a good combination with the matrix and no cracks, holes and other defects. The granular TiN and whisker TiB2 which were in situ generated are uniformly distributed in the hardened layer. The hardness of the coating is up to 956 HV0.1, which shows that the hybrid strengthening technique significantly improves the hardness of the matrix.%采用溶胶-凝胶法制备得到含有Ti02、BN和C的复合粉末,将其预置在45钢基体表面,然后通过激光强化原位制备出含有TiN和TiB2颗粒的强化涂层.利用扫描电镜、能谱仪和X射线衍射仪对涂层组织、成分和物相进行了分析,并测试了涂层显微硬度.结果表明,强化涂层与基体结合良好,涂层中无裂纹、气孔等缺陷,原位生成的颗粒状TiN和须状TiB2均匀分布在强化层中.涂层最高硬度达到956 HV0.1,显著地提高了45钢的硬度.

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

    Energy Technology Data Exchange (ETDEWEB)

    Krueger, Hannes

    2009-09-24

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

  17. High Refractive Organic–Inorganic Hybrid Films Prepared by Low Water Sol-Gel and UV-Irradiation Processes

    Directory of Open Access Journals (Sweden)

    Hsiao-Yuan Ma

    2016-03-01

    Full Text Available Organic-inorganic hybrid sols (Ti–O–Si precursor were first synthesized by the sol-gel method at low addition of water, and were then employed to prepare a highly refractive hybrid optical film. This film was obtained by blending the Ti–O–Si precursor with 2-phenylphenoxyethyl acrylate (OPPEA to perform photo-polymerization by ultraviolet (UV irradiation. Results show that the film transparency of poly(Ti–O–Si precursor-co-OPPEA film is higher than that of a pure poly(Ti–O–Si precursor film, and that this poly(Ti–O–Si precursor-co-OPPEA hybrid film exhibits a high transparency of ~93.7% coupled with a high refractive index (n of 1.83 corresponding to a thickness of 2.59 μm.

  18. SYNTHESIS AND OPTICAL PROPERTIES OF A NOVEL ORGANIC/INORGANIC HYBRID NONLINEAR OPTICAL POLYMER VIA SOL-GEL PROCESS

    Institute of Scientific and Technical Information of China (English)

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

    2001-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-07-20

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

  20. Electrochemical and Oxidation Behavior of Yttria Stabilized Zirconia Coating on Zircaloy-4 Synthesized via Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    S. Rezaee

    2013-01-01

    Full Text Available Sol-gel 8 wt.% Yttria Stabilized Zirconia (YSZ thin films were prepared on zirconium (zircaloy-4 alloy by dip-coating technique followed by heat treating at various temperatures (200°C, 400°C, and 700°C in order to improve both electrochemical corrosion and high temperature oxidation properties of the substrate. Differential thermal analysis and thermogravimetric analysis (DTA-TG revealed the coating formation process. X-ray diffraction (XRD was used to determine the crystalline phase structure transformation. The morphological characterization of the coatings was carried out using scanning electron microscopy (SEM. The electrochemical behavior of the coated and uncoated samples was investigated by means of open circuit potential, Tafel, and electrochemical impedance spectroscopy (EIS in a 3.5 wt.% NaCl solution. The homogeneity and surface appearance of coatings produced was affected by the heat treatment temperature. According to the corrosion parameters, the YSZ coatings showed a considerable increase in the corrosion resistance, especially at higher heat treatment temperatures. The coating with the best quality, from the surface and corrosion point of view, was subjected to oxidation test in air at 800°C. The coated sample presented a 25% reduction in oxidation rate in comparison with bare substrate.

  1. Spectral pH dependence of erythrosin B in sol-gel silica coatings and buffered solutions

    Directory of Open Access Journals (Sweden)

    Montero, E.

    2008-02-01

    Full Text Available Thin coatings optically sensitive against pH are obtained by entrapping erythrosin B molecules in a sol-gel silica matrix. Comparisons between optical spectra of erythrosin B in solutions and those once entrapped in silica coatings are performed for pH ranging from 0.5 to 12.0. Significant differences between both kinds of spectra (solutions and coatings of erythrosin B are observed. Main changes are displayed in the absorption spectra for neutral to basic pH. Furthermore, the erythrosin B doped coatings show memory effect or hysteresis in their spectral response against pH. This means that absorption spectra depend on the direction of the pH change. Likewise, the photoluminescent spectra of erythrosin B in buffered solutions exhibit pH dependence and a maximized response in the basic pH range. On contrast, no significant photoluminescence from the erythrosin B entrapped in the silica coatings is observed. Results are mainly discussed on the basis of different optical response of polyprotic forms of erythrosin B and possible interactions between the molecule and oxygen as well as the porous walls of the sol-gel silica matrix. In addition, the presence of diffusional barriers, which hamper the flowing of protons and other associated ions, is taken into account. Good agreement with previous observations about low absorption of polyprotic cationic and neutral forms of erythrosin B is found.

    Se han obtenido recubrimientos delgados ópticamente sensibles al pH mediante atrapamiento de moléculas de eritrosina B en matrices de sílice obtenidas por sol-gel. Se compara la respuesta espectral de la eritrosina B en solución y atrapada en los recubrimientos de sílice para un intervalo de pH comprendido entre 0,5 y 12. Se observan apreciables diferencias entre ambos tipos de espectros (en solución y en recubrimiento de la eritrosina B. Los principales cambios aparecen en los espectros de absorción para el intervalo neutro y básico de pH. Adem

  2. Silver Doped TiO2 Nanostructure Composite Photocatalyst Film Synthesized by Sol-Gel Spin and Dip Coating Technique on Glass

    OpenAIRE

    Mojtaba Nasr-Esfahani; Mohammad Hossein Habibi

    2008-01-01

    New composite films (P25SGF-MC-Ag, MPC500SGF-MC-Ag, and ANPSGF-MC-Ag) have been synthesized by a modified sol-gel method using different particle sizes of TiO2 powder and silver addition. Nanostructure TiO2/Ag composite thin films were prepared by a sol-gel spin and dip coating technique. while, by introducing methyl cellulose (MC) porous, TiO2/Ag films were obtained after calcining at a temperature of 500°C. The as-prepared TiO2 and TiO2/Ag films were characterized by X-ray diffractometry, a...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Amir A. El Hadad

    2017-01-01

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

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

    Science.gov (United States)

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

    2014-07-15

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

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

    Institute of Scientific and Technical Information of China (English)

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

    2011-01-01

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

  7. Enhanced Photophysical Properties of Nanopatterned Titania Nanodots/Nanowires upon Hybridization with Silica via Block Copolymer Templated Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Dinakaran Kannaiyan

    2010-10-01

    Full Text Available We fabricated titanium dioxide (TiO2-silica (SiO2 nanocomposite structures with controlled morphology by a simple synthetic approach using cooperative sol-gel chemistry and block copolymer (BCP self-assembly. Mixed TiO2-SiO2 sol-gel precursors were blended with amphiphilic poly(styrene-block-ethylene oxide (PS-b-PEO BCPs where the precursors were selectively incorporated into the hydrophilic PEO domains. Changing the volumetric ratio of TiO2-SiO2 sol-gel precursor from 5% to 20%, a stepwise structural inversion occurred from nanodot arrays to discrete nanowires. Template free hybrid inorganic nanostructures were produced after the removal of PS-b-PEO by irradiation of UV light. The morphological evolution and photophysical properties were investigated by microscopic studies, UV-visible absorption and photocatalytic properties.

  8. Effect of Catalyst on the Formation of Silica Coating on Nickel Substrate by Sol-Gel Processing

    Institute of Scientific and Technical Information of China (English)

    AliGhasemi; F.Ashrafizadeh; M.A.Golozar; AliAshrafi

    2004-01-01

    In this research work silica coating was produced on nickel substrates by a sol-gel process. In order to increase the rate of hydrolysis and to reduce the rate of polymerization several acid catalysts including nitric acid-hydrochloric acid, acetic acid, hydrochloric acid and nitric acid were add to silica sol. Conversely, in order to control the rate of hydrolysis and to increase the rate of polymerization, basic catalyst of ammonia and ammonia hydroxyl were introduced in to the solution. Nickel specimens of known surface roughness were chemically cleaned and prepared by dipping in the sols. In order to produce a suitable silica coating the drying and firing cycles were optimized on these substrates. The structure and uniformity of the coatings produced were examined by scanning electron microscopy. Coatings composition was determined using glow discharge optical spectroscopy and EDAX microanalysis. Experimental result showed that hydrochloric acid, acetic acid, ammonia and acetic acid-ammonia are suitable catalytic agents for silica coating formation on nickel type substrate.

  9. Effect of Doping with Zn-Al-[V10O28]6-Layered Double Hydroxide on the Properties of Hybrid Sol-Gel Coatings on the LY12 Aluminum Surface%Zn-Al-[V10O28]6-双层氢氧化物掺杂对LY12铝合金表面溶胶-凝胶涂层性能的影响

    Institute of Scientific and Technical Information of China (English)

    李松梅; 尹晓琳; 刘建华; 张优; 薛冰

    2014-01-01

    Zn-Al-[V10O28]6-layered double hydroxide (LDH-V) as a type of corrosion inhibitor was prepared with the co-precipitation method using one solution containing zinc and aluminum nitrates precursors and a second solution containing Na3VO4, where the decavanadate anion is speciated at pH 4.5. The hybrid sol-gel solution was prepared from 3-glycydoxypropyltrimethoxysilane (GPTMS) as the organic precursor sol and zirconium n-propoxide (TPOZ) as the inorganic precursor sol. The doped coatings were obtained by dip coating the way that the samples were immersed into solutions with different LDH-V concentrations (0.0, 0.25×10-3, 0.75×10-3, 1.5×10-3, 3.0×10-3 mol∙L-1). The morphology and corrosion resistance of the sol-gel coating doped with different LDH-V concentrations were studied. The sol-gel coatings were investigated by scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy. The salt spray test was used to evaluate the corrosion resistance of the different coatings. The corrosion behavior of the coatings was evaluated by electrochemical impedance spectroscopy (EIS) during immersion in 0.05 mol∙L-1 NaCl solution. The results showed that LDH-V not only improves the corrosion resistance of the coating, but also provides a function for self-healing of broken coatings. However, when the LDH-V doping concentration was high, it destroyed the integrity of the coatings and decreased the corrosion resistance of the coatings. The best LDH-V doping concentration was 1.5×10-3 mol∙L-1.%采用共沉淀法制备Zn-Al-[V10O28]6-双层氢氧化物(以下简称LDH-V),研究不同添加浓度(0.0、0.25×10-3、0.75×10-3、1.5×10-3、3.0×10-3 mol∙L-1)的LDH-V对LY12铝合金溶胶-凝胶涂层形貌、耐蚀性的影响.采用扫描电子显微镜(SEM)和傅里叶变换红外(FTIR)光谱研究LDH-V对涂层形貌和结构的影响.运用中性盐雾实验对涂层进行耐蚀性评估.利用电化学方法对涂层在0.05 mol∙L-1的NaCl

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

    Science.gov (United States)

    Ji, Guo-Jun; Shi, Zhi-Ming

    2010-09-01

    Ce3+ -doped and undoped TiO2 nanofilms are prepared on glass surface using a sol-gel method. Crystal structure, surface morphology, chemical composition and element distribution of both glass substrates and TiO2 films were characterized by x-ray diffractometer (XRD), atomic force microscopy (AFM) and x-ray photoelectron spectroscopy (XPS). The XRD results indicate that the Ce3+-doped TiO2 films are solely composed of the anatase phase whereas in the undoped films a small amount of the rutile phase of TiO2 is present. AFM observations show that there exist many micro-cracks and micro-holes on glass substrate surface. In contrast, the surface of pure titania films is crack-free and the average crystallite size of the films is less than 50 nm. For the films doped with Ce3+, not only does it appear to be more uniform and compact, but also the corresponding crystal size is decreased. XPS results indicate that element interdiffusion occurs between the titania nanofilm and the glass substrate during the sintering process. The film is firmly adhered onto the glass surface through the chemical combination of Ti-O-Si bonds, and the combination is more enhanced by Ce3+-doping.

  11. Silica-Copper Oxide Composite Thin Films as Solar Selective Coatings Prepared by Dipping Sol Gel

    Directory of Open Access Journals (Sweden)

    E. Barrera-Calva

    2008-01-01

    Full Text Available Silica-copper oxide (silica-CuO composite thin films were prepared by a dipping sol-gel route using ethanolic solutions comprised TEOS and a copper-propionate complex. Sols with different TEOS/Cu-propionate (Si/Cu molar ratios were prepared and applied on stainless steel substrates using dipping process. During the annealing process, copper-propionate complexes developed into particulate polycrystalline CuO dispersed in a partially crystallized silica matrix, as indicated by the X-ray diffraction (XRD and X-ray photoelectron spectroscopy (XPS analyses. The gel thermal analysis revealed that the prepared material might be stable up to 400°C. The silica-CuO/stainless steel system was characterized as a selective absorber surface and its solar selectivity parameters, absorptance (α, and emittance (ε were evaluated from UV-NIR reflectance data. The solar parameters of such a system were mostly affected by the thickness and phase composition of the SiO2-CuO film. Interestingly, the best solar parameters (α = 0.92 and ε = 0.2 were associated to the thinnest films, which comprised a CuO-Cu2O mixture immersed in the silica matrix, as indicated by XPS.

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

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

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

  13. [Study on the preparation and properties of novel silica microporous antireflective coating by sol-gel process].

    Science.gov (United States)

    Shang, Meng-Ying; Cao, Lin-Hong; Liu, Miao; Luo, Xuan; Ren, Hong-Bo; Ye, Xin; Tang, Yong-Jian; Jiang, Xiao-Dong

    2013-04-01

    Silica sol was prepared by acid catalyzed sol-gel process using tetraethylorthosilicate (TEOS) as precursor and dimethyldietoxysilane (DDS) as pore-forming agent. A novel kind of monolayer microporous silica anti-reflective (AR) coating was obtained on K9 glass substrate by dip-coating technique and then heat treated at 500 degrees C. The effects of different DDS/TEOS molar ratios on refractive index, transmittance and hardness were investigated. A positive correlation was found between the transmittance and the DDS/TEOS molar ratio due to the increasing porosity. The maximum transmittance can reach 99.7% with the molar ratio of DDS/TEOS rising to 1 : 1. Meanwhile, the refractive index was found quite close to the ideal value 1.22. Nevertheless, higher molar ratio will lead to a bad film-forming property. On the other hand, the hardness of the coatings decreased with the DDS increasing but still remained more than 2 h when the transmittance reached highest. Besides, these coatings exhibit a well abrasion-resistance and excellent adhesivity. The maximum transmittance was only dropped by 0.071% and 0.112% after abrasion for 500 and 1 000 times respectively. Accelerated corrosion tests indicated that the transmittance of traditional coatings rapidly fell down to the substrate level (-92%) after immersion for 5 min, while the transmittance of our novel coating almost linearly decreased and was kept 93.2% after 56 min. In other words, the environment-resistance of our novel silica AR coating is ten times higher than that of traditional ones. The promotions of the coating performances benefit from its micropore structure (-0. 4 nm) with which water molecule can be effectively prevented. With its high transmittance, good mechanical properties and high environment-resistance, this kind of novel coating has a potential application in the field of solar glass modification to improve its anti-reflective properties.

  14. Effect of Different TiO2-SiO2 Multilayer Coatings Applied by Sol-Gel Method on Antireflective Property

    Science.gov (United States)

    lari, Najme; Ahangarani, Shahrokh; Shanaghi, Ali

    2015-07-01

    Multilayer thin films prepared using the sol-gel process have been used in many antireflection applications. In this paper, antireflective nanoscale multilayer TiO2-SiO2 coatings were formed on both sides of the glass substrates by combining sol-gel method and dip coating techniques. The coatings were carried out using tetraethyl orthosilicate as precursor for SiO2 and tetrabutyl orthotitanate as precursor for TiO2. The coatings prepared in this work were characterized using scanning electron microscope, Fourier-transformed infrared spectrophotometer and UV-Visible spectrophotometer. The SiO2 top layer coatings showed excellent antireflection in the wavelength range of 400-800 nm where the transmittance of glass substrate is significantly lower. By increasing the number of double TiO2-SiO2 layers, the transmission of the coated glasses increased due to applied multilayer coating properties. Six-layer sol-gel TiO2-SiO2 coatings showed the highest visible transmittance about 99.25% at the band of 550-650 nm.

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

    Science.gov (United States)

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

    2011-02-01

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

  16. The shape dependence of core-shell and hollow titania nanoparticles on coating thickness during layer-by-layer and sol-gel synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Nelson, Kimberly; Deng Yulin [School of Chemical and Biomolecular Engineering, Georgia Institute of Technology, 500 10th Street, N.W., Atlanta, GA 30332-0620 (United States)

    2006-07-14

    Titania core-shell and hollow nanoparticles with different aspect ratios were synthesized using layer-by-layer assembly and sol-gel nanocoating methods with cellulose nanowhiskers as the template. During growth of the coating layer, the shape of the nanoparticles did not maintain the shape of the high aspect ratio template, as previously assumed. The shape of the coated particles is a function of the coating thickness. It is suggested that the overall particle shape and aspect ratio of the nanoparticles are tunable by choosing an appropriate template and coating thickness in layer-by-layer or sol-gel templating synthesis. The nanorods and hollow titania particles synthesized by these methods were characterized by transmission electron microscopy, scanning electron microscopy and x-ray diffraction.

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

    Institute of Scientific and Technical Information of China (English)

    XU W; HU W Y; LI M H; MA Q Q; P. D. HODGSON; WEN C E

    2006-01-01

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

  18. Fabrication of ceramic oxide-coated SWNT composites by sol-gel process with a polymer glue

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Cheng; Gao Lei; Chen Yongming, E-mail: ymchen@iccas.ac.cn [Institute of Chemistry, Chinese Academy of Sciences, Laboratory of Polymer Physics and Chemistry (China)

    2011-09-15

    The functional copolymer bearing alkoxysilyl and pyrene groups, poly[3-(triethoxysilyl)propyl methacrylate]-co-[(1-pyrene-methyl) methacrylate] (TEPM{sub 13}-co-PyMMA{sub 3}), was synthesized via atom transfer radical polymerization. Attributing the {pi}-{pi} interaction of pyrene units with the walls of single-walled carbon nanotubes (SWNTs), this polymer could disperse and exfoliate SWNTs in different solvents through physical interaction as demonstrated by TEM, UV/Vis absorption, and FT-IR analysis. The alkoxysilyl groups functionalized SWNTs were reacted with different inorganic precursors via sol-gel reaction, and, as a results, silica, titania, and alumina were coated onto the surface of SWNTs, respectively via copolymers as a molecular glue. The nanocomposites of ceramic oxides/SWNTs were characterized by SEM analysis. Dependent upon the feed, the thickness of inorganic coating can be tuned easily. This study supplies a facile and general way to coat SWNTs with ceramic oxides without deteriorating the properties of pristine SWNTs.

  19. Plasma Sprayed Dense MgO-Y2O3 Nanocomposite Coatings Using Sol-Gel Combustion Synthesized Powder

    Science.gov (United States)

    Wang, Jiwen; Jordan, Eric H.; Gell, Maurice

    2010-09-01

    MgO-Y2O3 nanostructured composite powder (volume ratio of 50:50) was synthesized by a sol-gel combustion process which generated crystal sizes in the 10-20 nm range. The MgO-Y2O3 nanopowder was plasma sprayed using a conventional, DC arc plasma spray system. X-ray diffraction analysis shows that the as-sprayed MgO-Y2O3 coating is composed of cubic MgO and Y2O3 phases and has ~95% density. Microstructure characterization by SEM reveals that the as-sprayed coating has fine grain sizes of 100-300 nm as a result of rapid solidification. The hardness of the coating, 7.5 ± 0.6 GPa, is higher than that of coarse-grained, dense MgO, and Y2O3 ceramics. This approach demonstrates the potential of plasma spray processes for making thick, dense MgO-Y2O3 nanocomposite performs for applications as durable, infrared windows.

  20. Effect of Chelating Agents on the Stability of Nano-TiO2 Sol Particles for Sol-Gel Coating.

    Science.gov (United States)

    Maeng, Wan Young; Yoo, Mi

    2015-11-01

    Agglomeration of sol particles in a titanium alkoxide (tetrabutyl orthotitanate (TBOT), > 97%) solution during the hydrolysis and condensation steps makes the sol solution difficult to use for synthesizing homogeneous sol-gel coating. Here, we have investigated the effect of stabilizing agents (acetic acid and ethyl acetoacetate (EAcAc)) on the agglomeration of Ti alkoxide particles during hydrolysis and condensation in order to determine the optimized conditions for controlling the precipitation of TiO2 particles. The study was conducted at R(AC) ([acetic acid]/[TBOT]) = 0.1-5 and R(EAcAc)([EAcAc]/[TBOT]) = 0.05-0.65. We also studied the effects of a basic catalyst ethanolamine (ETA), water, and HCl on sol stability. The chelating ligands in the precursor sol were analyzed with FT-IR. The coating properties were examined by focused ion beam. The stabilizing agents (acetic acid and EAcAc) significantly influenced the agglomeration and precipitation of TBOT precursor particles during hydrolysis. As R(AC) and R(EAcAc) increased, the agglomeration remarkably decreased. The stability of the sol with acetic acid and EAcAc arises from the coordination of the chelating ligand to TBOT that hinders hydrolysis and condensation. A uniform fine coating (thickness: 30 nm) on stainless steel was obtained by using an optimized sol with R(AC) = 0.5 and R(EAcAc) = 0.65.

  1. An abrasion-resistant and broadband antireflective silica coating by block copolymer assisted sol-gel method.

    Science.gov (United States)

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

    2014-09-02

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

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

    Science.gov (United States)

    Rojaee, Ramin; Fathi, Mohammadhossein; Raeissi, Keyvan

    2013-10-01

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

  3. Optical response of Ce(III and Eu(II doped hybrid materials synthesised by Sol-Gel processing

    Directory of Open Access Journals (Sweden)

    Cordoncillo, E.

    2000-02-01

    Full Text Available This study deals with the preparation of two hybrid organic-inorganic matrices via sol–gel, starting from alkylalkoxisilanes Si(CH3(OCH2CH33 (MTEOS–SiH(CH3(OCH2CH32 (MDES, A system, and SiH(CH3(OCH2CH32 (MDES SiH(OCH2CH33 (TREOS, B system, together with zirconium n-propoxide. Another type-A is carried out by adding acetylacetone, A-acac system. The matrices are characterised by infrared spectroscopy, nuclear magnetic resonance (NMR-MAS, and chemical analysis. Optical characteristics of the matrices have been studied. A-acac and B matrices are doped with an Eu(III salt, and A and B matrices are doped with a Ce(IV salt. Absorption and emission studies show the presence of Eu(II and Ce(III. The transition metal alkoxide that catalysed cleavage of the Si–H bonds was used to reduce in situ at room temperature, the rare earth cations. Depending on chemical strategy, the resulting hybrid materials can be processed as transparent bulks or coatings which exhibit a good transparency in the UV–visible domain. Both the undoped and the rare earth doped matrices exhibit a strong blue emission.

    En este trabajo se aborda la preparación de dos matrices híbridas orgánico-inorgánicas por vía sol-gel, a partir de mezclas de alquilalcoxisilanos Si(CH3(OCH2CH33 (MTEOS–SiH(CH3(OCH2CH32 (MDES, sistema A, y SiH(CH3(OCH2CH32 (MDES–SiH(OCH2CH33 (TREOS, sistema B, en presencia de n-propóxido de circonio. Se efectúa una variación del sistema A por adición de acetilacetona, sistema A-acac. Las matrices se caracterizan por espectroscopia infrarroja, resonancia magnética nuclear (RMN-MAS y análisis químico. Se estudian las características ópticas de los materiales obtenidos. Las matrices A-acac y B se dopan con una sal de Eu(III y las matrices A y B con una sal de Ce(IV. Los estudios de absorción y emisión indican la presencia de Eu(II y Ce(III, es decir estos estados de oxidación se han generado in situ a temperatura ambiente en los

  4. Efficient reverse saturable absorption of sol-gel hybrid plasmonic glasses

    Science.gov (United States)

    Lundén, H.; Lopes, C.; Lindgren, M.; Liotta, A.; Chateau, D.; Lerouge, F.; Chaput, F.; Désert, A.; Parola, S.

    2017-07-01

    Monolithic silica sol-gel glasses doped with platinum(II) acetylide complexes possessing respectively four or six phenylacetylene units (PE2-CH2OH and PE3-CH2OH) in combination with various concentrations of spherical and bipyramidal gold nanoparticles (AuNPs) known to enhance non-linear optical absorption, were prepared and polished to high optical quality. The non-linear absorption of the glasses was measured and compared to glasses doped solely with AuNPs, a platinum(II) acetylide with shorter delocalized structure, or combinations of both. At 532 nm excitation wavelength the chromophore inhibited the non-linear scattering previously found for glasses only doped with AuNPs. The measured non-linear absorption was attributed to reverse saturable absorption from the chromophore, as previously reported for PE2-CH2OH/AuNP glasses. At 600 nm strong nonlinear absorption was observed for the PE3-CH2OH/AuNPs glasses, also attributed to reverse saturable absorption. But contrary to previous findings for PE2-CH2OH/AuNPs, no distinct enhancement of the non-linear absorption for PE3-CH2OH/AuNPs was observed. A numerical population model for PE3-CH2OH was used to give a qualitative explanation of this difference. A stronger linear absorption in PE3-CH2OH would cause the highly absorbing triplet state to populate quicker during the leading edge of the laser pulse and this would in turn reduce the influence from two-photon absorption enhancement from AuNPs.

  5. Silica/quercetin sol-gel hybrids as antioxidant dental implant materials

    Science.gov (United States)

    Catauro, Michelina; Papale, Ferdinando; Bollino, Flavia; Piccolella, Simona; Marciano, Sabina; Nocera, Paola; Pacifico, Severina

    2015-06-01

    The development of biomaterials with intrinsic antioxidant properties could represent a valuable strategy for preventing the onset of peri-implant diseases. In this context, quercetin, a naturally occurring flavonoid, has been entrapped at different weight percentages in a silica-based inorganic material by a sol-gel route. The establishment of hydrogen bond interactions between the flavonol and the solid matrix was ascertained by Fourier transform infrared spectroscopy. This technique also evidenced changes in the stretching frequencies of the quercetin dienonic moiety, suggesting that the formation of a secondary product occurs. Scanning electron microscopy was applied to detect the morphology of the synthesized materials. Their bioactivity was shown by the formation of a hydroxyapatite layer on sample surface soaked in a fluid that simulates the composition of human blood plasma. When the potential release of flavonol was determined by liquid chromatography coupled with ultraviolet and electrospray ionization tandem mass spectrometry techniques, the eluates displayed a retention time that was 0.5 min less than quercetin. Collision-activated dissociation mass spectrometry and untraviolet-visible spectroscopy were in accordance with the release of a quercetin derivative. The antiradical properties of the investigated systems were evaluated by DPPH and ABTS methods, whereas the 2,7-dichlorofluorescein diacetate assay highlighted their ability to inhibit the H2O2-induced intracellular production of reactive oxygen species in NIH-3T3 mouse fibroblast cells. Data obtained, along with data gathered from the MTT cytotoxicity test, revealed that the materials that entrapped the highest amount of quercetin showed notable antioxidant effectiveness.

  6. Bonding mechanism and performance of ceramic coatings by sol-gel process

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Thin alumina coatings were prepared on carbide tools to enhance their wear-resistant ability by dip coating from an aluminum alkoxide solution. The coating eventually obtained was perfectly integrated, without any macroscopic defect, and showed good performance in turning medium carbon steel, which presented a novel and promising coating method for cutting tools. The coating morphology before and after heat treatment was examined with the aid of a scanning electron microscope (SEM). The composition of coating and interface layer as well as the crystal structure of coating was characterized by X-ray diffraction (XRD). The elemental distribution near the interlayer was analyzed by electron probe microanalysis (EPMA).

  7. Plunger-in-needle solid-phase microextraction with graphene-based sol-gel coating as sorbent for determination of polybrominated diphenyl ethers.

    Science.gov (United States)

    Zhang, Hong; Lee, Hian Kee

    2011-07-15

    A solid-phase microextraction (SPME) device, assembled with a commercially available plunger-in-needle microsyringe, with the plunger coated with graphene via a sol-gel approach, was developed for the gas chromatographic-mass spectrometric determination of polybrominated diphenyl ethers (PBDEs) in environmental samples. This is the first application of graphene-based sol-gel coating as SPME sorbent. Parameters affecting the extraction efficiency were investigated in detail. The new coating exhibited enrichment factors for PBDEs between 1378 and 2859. The unique planar structure of graphene enhanced the π-π interaction with the aromatic PBDEs; additionally, the sol-gel coating technique created a porous three-dimensional network structure which offered larger surface area for extraction. The stainless steel plunger provided firm support for the coating and enhanced the durability of the assembly. The plunger-in-needle microsyringe represents a ready-made tool for SPME implementation. Under the optimized conditions, the method detection limits for five PBDEs were in the range of 0.2 and 5.3 ng/L (at a signal/noise ratio of 3) and the precision (% relative standard deviation, n=5) was 3.2-5.0% at a concentration level of 100 ng/L. The linearities were 5-1000 or 10-1000 ng/L for different PBDEs. Finally, the proposed method was successfully applied to the extraction and determination by gas chromatography-mass spectrometry of PBDEs in canal water samples.

  8. Inexpensive sol-gel synthesis of multiwalled carbon nanotube-TiO2 hybrids for high performance antibacterial materials.

    Science.gov (United States)

    Abbas, Nadir; Shao, Godlisten N; Haider, M Salman; Imran, Syed Muhammad; Park, Sung Soo; Jeon, Sun-Jeong; Kim, Hee Taik

    2016-11-01

    This study reports an inexpensive sol-gel method to synthesize TiO2-CNT hybrid materials. Synthesized TiO2-CNT materials show strong antibacterial activity in the absence of light. Cheap TiO2 source TiOCl2 is used during synthesis in the absence of high temperatures, high pressures and organic solvents. TiO2-CNT materials with 0, 2, 5, 10, 15 and 20wt% of CNT were synthesized and compared for antibacterial activity, surface area, porosity, crystalline structure, chemical state, and HaCaT cell proliferation. The antibacterial strength of hybrid materials increased significantly with the increase in CNT loading amount, and the TiO2-CNT samples with a CNT loading of 10wt% or more nearly removed all of the E.coli bacteria. HaCaT cell proliferation studies of synthesized hybrid materials illustrated that prepared TiO2-CNT systems exhibit minimum cytotoxicity. The characteristics of prepared materials were analyzed by means of XRD, FTIR, Raman spectroscopy, XPS, TEM, and nitrogen gas physisorption studies, compared and discussed. Copyright © 2016. Published by Elsevier B.V.

  9. Synthesis of Bioactive Chlorogenic Acid-Silica Hybrid Materials via the Sol-Gel Route and Evaluation of Their Biocompatibility.

    Science.gov (United States)

    Catauro, Michelina; Pacifico, Severina

    2017-07-21

    Natural phenol compounds are gaining a great deal of attention because of their potential use as prophylactic and therapeutic agents in many diseases, as well as in applied science for their preventing role in oxidation deterioration. With the aim to synthetize new phenol-based materials, the sol-gel method was used to embed different content of the phenolic antioxidant chlorogenic acid (CGA) within silica matrices to obtain organic-inorganic hybrid materials. Fourier transform infrared (FTIR) measurements were used to characterize the prepared materials. The new materials were screened for their bioactivity and antioxidant potential. To this latter purpose, direct DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azinobis-(3-ethylbenzothiazolin-6-sulfonic acid) methods were applied: radical scavenging capability appeared strongly dependent on the phenol amount in investigated hybrids, and became pronounced, mainly toward the ABTS radical cation, when materials with CGA content equal to 15 wt% and 20 wt% were analyzed. The in vitro biocompatibility of the synthetized materials was estimated by using the MTT assay towards fibroblast NIH 3T3 cells, human keratinocyte HaCaT cells, and the neuroblastoma SH-SY5Y cell line. As cell viability and morphology of tested cell lines seemed to be unaffected by new materials, the attenuated total reflectance (ATR)-FTIR method was applied to deeply measure the effects of the hybrids in the three different cell lines.

  10. Sol-gel synthesis and characterization of SiO2/PEG hybrid materials containing quercetin as implants with antioxidant properties

    Science.gov (United States)

    Catauro, Michelina; Bollino, Flavia; Gloria, Antonio

    2016-05-01

    In the present work, Silica/Polyethylene glycol (PEG) hybrid nanocomposites containing an antioxidant agent, the quercetin, were synthesized via sol-gel to be used as implants with antioxidant properties. Fourier transform infrared (FT-IR) analysis proved that a modification of both polymer and quercetin occurs due to synthesis process. Scanning electron microscope (SEM) showed that the proposed materials were hybrid nanocomposites. The bioactivity was ascertained by soaking the samples in a simulated body fluid (SBF).

  11. Sol-gel synthesis and characterization of SiO{sub 2}/PEG hybrid materials containing quercetin as implants with antioxidant properties

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, Michelina; Bollino, Flavia [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 21, 81031 Aversa (Italy); Gloria, Antonio [Institute of Polymers, Composites and Biomaterials - National Research Council of Italy, V.le J. F. Kennedy 54 - Mostra d’Oltremare Pad. 20, 80125 Naples (Italy)

    2016-05-18

    In the present work, Silica/Polyethylene glycol (PEG) hybrid nanocomposites containing an antioxidant agent, the quercetin, were synthesized via sol-gel to be used as implants with antioxidant properties. Fourier transform infrared (FT-IR) analysis proved that a modification of both polymer and quercetin occurs due to synthesis process. Scanning electron microscope (SEM) showed that the proposed materials were hybrid nanocomposites. The bioactivity was ascertained by soaking the samples in a simulated body fluid (SBF).

  12. Influence of Different Sol-gel Spin Coating Speed on Memristive Behaviour of Pt/TiO2/ZnO/ITO Device

    Science.gov (United States)

    Kasim, S. M. M.; Shaari, N. A. A.; Bakar, R. A.; Aznilinda, Z.; Mohamad, Zulfakri; Herman, S. H.

    2015-11-01

    Composite titanium dioxide (TiO2) and zinc oxide (ZnO) thin films were deposited on indium tin oxide (ITO) substrates using sol-gel spin coating technique. The electrical and physical characterizations of three different sol-gel spin coating speed were investigated using two-probe current-voltage (I-V) measurement, field emission scanning electron microscopy (FESEM) and surface profiler (SP) respectively. The I-V measurement results showed the pinched hysteresis loop for every single of devices thus indicate that all the devices are memristive. ROFF/RON ratio which was defined from the hysteresis loop of device with higher spin speed was slightly higher compared to others.

  13. Optical enhancement of Au doped ZrO2 thin films by sol-gel dip coating method

    Science.gov (United States)

    John Berlin, I.; Joy, K.

    2015-01-01

    Homogeneous and transparent Au doped ZrO2 thin films were prepared by sol-gel dip coating method. The films have mixed phase of tetragonal, monoclinic and face centered cubic with crack free surface. Due to the increase in Au doping concentration many-body interaction occurs between free carriers and ionized impurities causing decrease in optical band gap from 5.72 to 5.40 eV. Localized surface plasmon resonance peak of the Au doped films appeared at 610 nm. Conversion of photons to surface plasmons allows the sub-wavelength manipulation of electromagnetic radiation. Hence the prepared Au doped ZrO2 thin films can be applied in nanoscale photonic devices such as lenses, switches, waveguides etc. Moreover the photoluminescence (PL) intensity of Au doped ZrO2 thin films decrease due to decrease in the radiative recombination, life time of the excitons and suppression of grain growth of ZrO2 with increasing Au dopant.

  14. High-κ TiO2 thin film prepared by sol-gel spin-coating method

    Science.gov (United States)

    Kumar, Arvind; Mondal, Sandip; Rao, K. S. R. Koteswara

    2015-06-01

    High-k TiO2 thin film on p-type silicon substrate was fabricated by a combined sol-gel and spin coating method. Thus deposited titania film had anatase phase with a small grain size of 16 nm and surface roughness of ≅ 0.6 nm. The oxide capacitance (Cox), flat band capacitance (CFB), flat band voltage (VFB), oxide trapped charge (Qot), calculated from the high frequency (1 MHz) C-V curve were 0.47 nF, 0.16 nF, - 0.91 V, 4.7x10-12 C, respectively. As compared to the previous reports, a high dielectric constant of 94 at 1 MHz frequency was observed in the devices investigated here and an equivalent oxide thickness (EOT) was 4.1 nm. Dispersion in accumulation capacitance shows a linear relationship with AC frequencies. Leakage current density was found in acceptable limits (2.1e-5 A/cm2 for -1 V and 5.7e-7 A/cm2 for +1 V) for CMOS applications.

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

    Science.gov (United States)

    Kadhim, Imad H.; Abu Hassan, H.

    2016-12-01

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

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

    Science.gov (United States)

    Kadhim, Imad H.; Abu Hassan, H.

    2017-03-01

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

  17. Structural, Optical Constants and Photoluminescence of ZnO Thin Films Grown by Sol-Gel Spin Coating

    Directory of Open Access Journals (Sweden)

    Abdel-Sattar Gadallah

    2013-01-01

    Full Text Available We report manufacturing and characterization of low cost ZnO thin films grown on glass substrates by sol-gel spin coating method. For structural properties, X-ray diffraction measurements have been utilized for evaluating the dominant orientation of the thin films. For optical properties, reflectance and transmittance spectrophotometric measurements have been done in the spectral range from 350 nm to 2000 nm. The transmittance of the prepared thin films is 92.4% and 88.4%. Determination of the optical constants such as refractive index, absorption coefficient, and dielectric constant in this wavelength range has been evaluated. Further, normal dispersion of the refractive index has been analyzed in terms of single oscillator model of free carrier absorption to estimate the dispersion and oscillation energy. The lattice dielectric constant and the ratio of free carrier concentration to free carrier effective mass have been determined. Moreover, photoluminescence measurements of the thin films in the spectral range from 350 nm to 900 nm have been presented. Electrical measurements for resistivity evaluation of the films have been done. An analysis in terms of order-disorder of the material has been presented to provide more consistency in the results.

  18. Preparation of CuAlO2 Thin Films by Sol-Gel Method Using Nitrate Solution Dip-Coating

    Directory of Open Access Journals (Sweden)

    Ehara Takashi

    2016-01-01

    Full Text Available CuAlO2 thin films are prepared by sol-gel dip-coating followed by annealing in nitrogen atmosphere using copper nitrate and aluminum nitrate as metal source materials. X-ray diffraction (XRD patterns show (003, (006 and (009 oriented peaks of CuAlO2 at annealing temperature of 800 – 1000°C. This result indicates that the CuAlO2 films prepared in the present work are c-axis oriented. XRD peak intensity increase with annealing temperature and becomes maximum at 850°C. The CuAlO2 XRD peak decreased at annealing temperature of 900°C with appearance of a peak of CuO, and then increased again with annealing temperature until 1000 °C. The films have bandgap of 3.4 eV at annealing temperature of 850°C in which the transparency becomes the highest. At the annealing temperature of 850°C, scanning electron microscope (SEM observation reveals that the films are consist of amorphous fraction and microcrystalline CuAlO2 fraction.

  19. Sol-gel layers for ceramic microsystems application

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2016-07-01

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

  1. Using sol-gel component as additive to foundry coatings to improve casting quality

    DEFF Research Database (Denmark)

    Nwaogu, Ugochukwu Chibuzoh; Poulsen, T.; Gravesen, B.

    2012-01-01

    parameter design. The effects of the sol‐gel component on viscosity, density, °Baumé, core coverage and permeability are shown. Numerical simulations were used to predict defect areas. The thermal profiles of the core materials during casting were determined, and the surface quality of the castings......The improvement of foundry coatings to enhance performance is important. This paper investigates the effect of using sol‐gel component as an additive to foundry coatings applied on chemically bonded sand cores. Three parameters at three levels each were investigated using Taguchi experimental...... was evaluated. The results show that the surface quality of castings obtained by adding the sol‐gel component to the coatings for cold box cores has no significant difference from castings produced with coatings without sol‐gel component. On the other hand, the addition of the sol‐gel component in coatings...

  2. Detection of hydrofluoric acid by a SiO2 sol-gel coating fiber-optic probe based on reflection-based localized surface plasmon resonance.

    Science.gov (United States)

    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 SiO(2) sol-gel coating. This fiber-sensor was utilized to assess the relationship between HF concentration and SiO(2) 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.

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

    Directory of Open Access Journals (Sweden)

    S. J. O’Shea

    2003-10-01

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

  4. Sol-gel synthesis of tantalum oxide and phosphonic acid-modified carbon nanotubes composite coatings on titanium surfaces.

    Science.gov (United States)

    Maho, Anthony; Detriche, Simon; Delhalle, Joseph; Mekhalif, Zineb

    2013-07-01

    Carbon nanotubes used as fillers in composite materials are more and more appreciated for the outstanding range of accessible properties and functionalities they generate in numerous domains of nanotechnologies. In the framework of biological and medical sciences, and particularly for orthopedic applications and devices (prostheses, implants, surgical instruments, …), titanium substrates covered by tantalum oxide/carbon nanotube composite coatings have proved to constitute interesting and successful platforms for the conception of solid and biocompatible biomaterials inducing the osseous regeneration processes (hydroxyapatite growth, osteoblasts attachment). This paper describes an original strategy for the conception of resistant and homogeneous tantalum oxide/carbon nanotubes layers on titanium through the introduction of carbon nanotubes functionalized by phosphonic acid moieties (-P(=O)(OH)2). Strong covalent C-P bonds are specifically inserted on their external sidewalls with a ratio of two phosphonic groups per anchoring point. Experimental results highlight the stronger "tantalum capture agent" effect of phosphonic-modified nanotubes during the sol-gel formation process of the deposits compared to nanotubes bearing oxidized functions (-OH, -C=O, -C(=O)OH). Particular attention is also paid to the relative impact of the rate of functionalization and the dispersion degree of the carbon nanotubes in the coatings, as well as their wrapping level by the tantalum oxide matrix material. The resulting effect on the in vitro growth of hydroxyapatite is also evaluated to confirm the primary osseous bioactivity of those materials. Chemical, structural and morphological features of the different composite deposits described herein are assessed by X-ray photoelectron spectroscopy (XPS), scanning (SEM) and transmission (TEM) electronic microscopies, energy dispersive X-rays analysis (EDX) and peeling tests.

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

    Science.gov (United States)

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

    2014-11-11

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

  6. Sol-gel/nanoclay composite as a solid-phase microextraction fiber coating for the determination of organophosphorus pesticides in water samples.

    Science.gov (United States)

    Saraji, Mohammad; Jafari, Mohammad Taghi; Sherafatmand, Hossein

    2015-02-01

    A novel solid-phase microextraction (SPME) fiber coated with a sol-gel/nanoclay composite was prepared by the sol-gel technique involving the hydrolysis reaction of alkoxysilanes and the subsequent condensation reaction with hydroxyl groups of the nanoclay on a stainless steel wire. A method based on direct immersion SPME and gas chromatography-corona discharge ion mobility spectrometry was developed for the determination of four organophosphorus pesticides in aqueous samples. The effect of different experimental parameters on the extraction efficiency of the method was investigated. The sol-gel/nanoclay fiber showed higher extraction performance for the organophosphorus pesticides compared with Ppy/nanoclay, sol-gel coating, and three commercial fibers (polydimethylsiloxane (PDMS), PDMS/divinylbenzene (DVB), and polyacrylate (PA)). Limits of detection (LOD) and quantitation (LOQ) of the method were in the range of 0.003-0.012 and 0.01-0.02 μg L(-1), respectively. The calibration curves were linear in a concentration range from 0.01 to 2.0 μg L(-1) (r (2)  > 0.995). The relative standard deviations for intra- and inter-day precision were 3.3-5.6 and 6.4-8.4 %, respectively. Fiber-to-fiber reproducibility for three prepared fibers was 7.4-10.2 %. Finally, the method was successfully applied for the extraction of the studied compounds from water samples. The relative recovery obtained for the spiked real-water samples were 86-104 %.

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

    Directory of Open Access Journals (Sweden)

    Seyed Morteza Naghib

    2012-03-01

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

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

    Directory of Open Access Journals (Sweden)

    E. P. Avés

    2008-12-01

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

  9. Fabrication of the flexible nanogenerator from BTO nanopowders on graphene coated PMMA substrates by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Sankar Ganesh, R. [Department of Physics and Nanotechnology, SRM University, Kattankullathur, Chennai, 603203, Tamil Nadu (India); Research Institute of Electronics, Shizuoka University, 3-5-1 Johoku, Naka-ku, Hamamatsu, Shizuoka, 432-8011 (Japan); Sharma, Sanjeev K., E-mail: sksharma@dongguk.edu [Department of Semiconductor Science, Dongguk University-Seoul, Jung-gu, Seoul, 04620 (Korea, Republic of); Abinnas, N. [Department of Physics and Nanotechnology, SRM University, Kattankullathur, Chennai, 603203, Tamil Nadu (India); Durgadevi, E. [Research Institute of Electronics, Shizuoka University, 3-5-1 Johoku, Naka-ku, Hamamatsu, Shizuoka, 432-8011 (Japan); Raji, P. [Department of Physics, Mepco Schlenk Engineering College, Sivakasi, 626 005, Tamil Nadu (India); Ponnusamy, S., E-mail: suruponnus@gmail.com [Department of Physics and Nanotechnology, SRM University, Kattankullathur, Chennai, 603203, Tamil Nadu (India); Muthamizhchelvan, C. [Department of Physics and Nanotechnology, SRM University, Kattankullathur, Chennai, 603203, Tamil Nadu (India); Hayakawa, Y. [Research Institute of Electronics, Shizuoka University, 3-5-1 Johoku, Naka-ku, Hamamatsu, Shizuoka, 432-8011 (Japan); Kim, Deuk Young [Department of Semiconductor Science, Dongguk University-Seoul, Jung-gu, Seoul, 04620 (Korea, Republic of)

    2017-05-01

    Nanostructured bismuth titanate (Bi{sub 4}Ti{sub 3}O{sub 12}) or BTO powders were synthesized by the combustion method. The crystalline phase of BTO nanopowders was evaluated from X-ray diffraction (XRD) and further confirmed by selected area electron diffraction (SAED) pattern. The SEM and TEM micrographic images clearly showed the nanosheets like morphology of BTO nanopowder. The EDS spectrum of BTO nanopowder showed the elemental peaks of O, Bi and Ti at 0.53 keV, 2.41 keV and 4.49 keV, respectively. FTIR band peaks were observed at 815 and 595 cm{sup -1} corresponding to the stretching vibrations of Bi-O and Ti-O. The red shift in optical absorption of BTO was observed and the bandgap decreased from 3.18 to 3.08 eV as the calcined temperature increased from 600 to 800 °C. The sandwich structure, called the nanogenerator, Graphene/BTO-PDMS/Graphene (G/BTO/G), was fabricated on graphene coated polymethyl methacrylate (PMMA) substrates, which produced a peak voltage (10 mV) by applying the pressure from human's finger. The switching mechanism of BTO nanosheets was observed to be dependent on the polarity and intrinsic dipole formation. - Highlights: • Bi{sub 4}Ti{sub 3}O{sub 12} (BTO) nanosheets synthesized from a simple combustion method. • SEM & TEM images confirmed the nanosheets structure with a hexagonal shape. • XRD and SAED pattern of BTO nanosheets confirmed the orthorhombic crystal structure. • Flexible G/BTO/G nanogenerator fabricated by sol-gel method. • Peak voltage was observed to be 10 mV by applying pressure from human's finger.

  10. Microstructure of TiC-Based Coatings on Cemented Carbide Derived by Sol-Gel Routes

    Science.gov (United States)

    Yang, Mei; Guo, Zhixing; Qi, Kaifeng; Huang, Kun; Deng, Jianxiong; Liu, Jia

    2016-12-01

    TiC-based coating is prepared by depositing TiO2 sol on cemented carbide compact and liquid phase sintering. TiC forms due to carbothermal reduction reaction of TiO2 and then reacts with WC and transforms to TiC-based solid solution. Ti content changes the WC growth mechanism and results in the multi-stepped morphology. When sintered cemented carbide is used as substrate, WC keeps the equilibrium truncated triangle prism morphology due to the relatively weak diffusion among Ti, WC, and Co.

  11. Microstructure of TiC-Based Coatings on Cemented Carbide Derived by Sol-Gel Routes

    Science.gov (United States)

    Yang, Mei; Guo, Zhixing; Qi, Kaifeng; Huang, Kun; Deng, Jianxiong; Liu, Jia

    2017-02-01

    TiC-based coating is prepared by depositing TiO2 sol on cemented carbide compact and liquid phase sintering. TiC forms due to carbothermal reduction reaction of TiO2 and then reacts with WC and transforms to TiC-based solid solution. Ti content changes the WC growth mechanism and results in the multi-stepped morphology. When sintered cemented carbide is used as substrate, WC keeps the equilibrium truncated triangle prism morphology due to the relatively weak diffusion among Ti, WC, and Co.

  12. Electrogenerated chemiluminescence biosensor with alcohol dehydrogenase and tris(2,2'-bipyridyl)ruthenium (II) immobilized in sol-gel hybrid material.

    Science.gov (United States)

    Xu, Zhiai; Guo, Zhihui; Dong, Shaojun

    2005-09-15

    An ethanol biosensor based on electrogenerated chemiluminescence detection was developed. Electrogenerated chemiluminescence reagent tris(2,2'-bipyridyl)ruthenium (II) and alcohol dehydrogenase were immobilized in the same sol-gel hybrid film. The copolymer poly(vinyl alcohol) with 4-vinylpyridine and cation exchanger Nafion were incorporated into sol-gel film to provide the microenvironment for retaining the activity of enzyme and immobilize tris(2,2'-bipyridyl)ruthenium (II). The design was simpler than the previous two-layer format. The experimental conditions, such as scan rate, pH and concentration of the cofactor were investigated. The intensity of electrogenerated chemiluminescence increased linearly with ethanol concentration from 2.5x10(-5) to 5.0x10(-2) M and detection limit was 1.0x10(-5) M. The prepared biosensor exhibited high sensitivity, wide linear range and good stability.

  13. Epitaxial growth of ZnO on quartz substrate by sol-gel spin-coating method

    Science.gov (United States)

    Chebil, W.; Boukadhaba, M. A.; Fouzri, A.

    2016-07-01

    ZnO thin films grown on Quartz substrates using sol-gel method were synthesized and annealing at different temperature (700 °C, 900 °C and 1000 °C). The structural, optical and morphological comparison of ZnO layers elaborated with that obtained by the sophisticated and expensive technique MOCVD demonstrates the success of the ZnO epitaxial growth on quartz substrate by sol-gel process. Sol-gel ZnO film deposited on quartz substrate annealed at 1000 °C exhibit only (00l) XRD peak which is similar to the diffraction patterns of epitaxial ZnO grown on sapphire by MOCVD. The Surface morphology was examined by SEM which revealed that the grain size becomes larger and faceted as increasing annealing temperature. Pl emission peak of sol-gel ZnO annealed at 1000 °C revealed a close similarity with that obtained by MOCVD ZnO but with a weaker intensity.

  14. Fabrication and properties of zinc oxide thin film prepared by sol-gel dip coating method

    Directory of Open Access Journals (Sweden)

    Kayani Zohra Nazir

    2015-09-01

    Full Text Available ZnO thin films were deposited on a glass substrate by dip coating technique using a solution of zinc acetate, ethanol and distilled water. Optical constants, such as refractive index n and extinction coefficient k. were determined from transmittance spectrum in the ultraviolet-visible-near infrared (UV-Vis-NIR regions using envelope methods. The films were found to exhibit high transmittance, low absorbance and low reflectance in the visible regions. Absorption coefficient α and the thickness of the film t were calculated from interference of transmittance spectra. The direct optical band gap of the films was in the range of 3.98 to 3.54 eV and the thickness of the films was evaluated in the range of 173 to 323 nm, while the refractive index slightly varied in the range of 1.515 to 1.622 with an increase in withdrawal speed from 100 to 250 mm/s. The crystallographic structure of the films was analyzed with X-ray diffractometer. The films were amorphous in nature.

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

    Institute of Scientific and Technical Information of China (English)

    Yoshiki; Chujo

    2007-01-01

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

  16. Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

    Science.gov (United States)

    Catauro, M; Papale, F; Bollino, F

    2016-01-01

    The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0sol-gel route starting from tetraethyl orthosilicate and calcium nitrate tetrahydrate. Those materials, still in the sol phase, have been used to coat titanium substrates by means of the dip-coating technique. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) allowed the materials to be characterized and a microstructural analysis of the coatings obtained was performed using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated titanium was immersed in simulated body fluid (SBF) for 21 days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. To investigate cell-material interactions, mouse embryonic fibroblast cells (3T3) were seeded onto the specimens and the cell viability was evaluated by a WST-8 assay.

  17. Fabrication of TiO{sub 2} {mu}-donuts by sol-gel spin coating using a polymer mask

    Energy Technology Data Exchange (ETDEWEB)

    Saleema, N. [Atmospheric Icing Engineering of Power Networks (CIGELE) and Atmospheric Icing of Power Network Equipment (INGIVRE), Universite du Quebec a Chicoutimi, 555 Blvd. University, Quebec, G7H 2B1 (Canada)], E-mail: snoormoh@uqac.ca; Farzaneh, M. [Atmospheric Icing Engineering of Power Networks (CIGELE) and Atmospheric Icing of Power Network Equipment (INGIVRE), Universite du Quebec a Chicoutimi, 555 Blvd. University, Quebec, G7H 2B1 (Canada); Paynter, R.W. [INRS, Centre Energie Materiaux Telecommunications, 1650 Boulevard Lionel-Boulet, Varennes, Quebec, J3X 1S2 (Canada)

    2009-03-15

    TiO{sub 2} {mu}-donuts have been fabricated on glass and silicon substrates using polymer masks in combination with a sol-gel technique. Cylindrical poly(methyl methacrylate) (PMMA) nanopillars have been created using a composite polymer of polystyrene (PS) and PMMA followed by careful removal of the PS. Atomic force microscopy (AFM) analyses show that the height and diameter of the PMMA cylinders used as the mask are 440 {+-} 5 nm and 2.1 {+-} 0.2 {mu}m, respectively. The cylindrical PMMA nanopillars have been coated with the sol of the TiO{sub 2} precursor by a spin coating technique and annealed in air at elevated temperature to remove the PMMA mask. Removal of the PMMA mask has resulted in the formation of well ordered {mu}-donuts of TiO{sub 2} on silicon surfaces. The interior and exterior heights of the TiO{sub 2} {mu}-donuts are found to be 373 {+-} 152 nm and 457 {+-} 136 nm, respectively; and the interior and exterior diameters of the TiO{sub 2} {mu}-donuts are found to be 1.33 {+-} 0.63 {mu}m and 2.82 {+-} 0.50 {mu}m, respectively. X-ray photoelectron spectroscopy (XPS) spectra of the TiO{sub 2} {mu}-donuts as well as the smooth TiO{sub 2} thin film showed signals from Ti and O confirming the presence of TiO{sub 2} with Ti 2p{sub 3/2} and O 1s peaks at 458.8 eV and 530.4 eV, respectively. The O 1s peak of the TiO{sub 2} {mu}-donuts shows another peak at binding energy 532.0 eV due to SiO{sub 2}, as during annealing, the PMMA evaporates and the Si substrate is exposed. The X-ray diffractometer (XRD) pattern of the smooth TiO{sub 2} thin film indicates that the anatase phase is present, with the characteristic peaks observed at 2{theta} values of 25.4{sup o}, 37.4{sup o}, and 48{sup o} corresponding to (1 0 1), (0 0 4), and (2 0 0) planes, respectively. UV-vis absorption spectra of TiO{sub 2} {mu}-donuts on glass showed an unusual absorption of light in the visible region at {approx}524 nm in addition to the usual UV absorption at {approx}337 nm.

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

    Science.gov (United States)

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

    2009-03-15

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

  19. Preparation and characterization of BaMgAl10O17:Eu phosphor coated with MgF2 by sol-gel process

    Institute of Scientific and Technical Information of China (English)

    LI Feng; WANG Yu-hua

    2005-01-01

    In order to prevent BaMgAl10 O17 : Eu (BAM) phosphor from thermal degradation, MgF2-coatings on the surface of BAM were prepared by a sol-gel process. The coatings were characterized by X-ray photoelectron spectroscopy and scanning electron microscopy. The results indicate that BAM is successfully coated with homogenous, close MgF2 coatings. The photoluminescence and anti-thermal degradation properties of coated BAM were investigated under 254 and 147 nm excitations. The optimum anti-thermal degradation properties are obtained at the mass ratio of MgF2 to BAM 0. 2% under 254 nm excitation and 0. 5% under 147 nm excitation, respectively. It is considered that trace MgO formed after baked would cause different optimum coating thicknesses under 254 and 147 nm excitations.

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

    Science.gov (United States)

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

    2004-01-30

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

  1. PEMBUATAN SENSOR GAS HIDROGEN BERBASIS FILM TIPIS GaN DENGAN TEKNIK SOL GEL SPIN COATING UNTUK KOMPONEN PADA SISTEM PENDETEKSI KEBOCORAN GAS

    OpenAIRE

    Rusdiana, D.

    2013-01-01

    Penelitian ini bertujuan untuk membuat sensor gas dengan sensitivitas baik, dipergunakan sebagai komponen dalam sistem pendeteksi kebocoran gas hidrogen. Bahan dasar sensor berbahan  film tipis semikonduktor Gallium Nitrida (GaN) yang ditumbuhkan di atas substrat sapphire (Al2O3) menggunakan teknik sol gel spin coating. Parameter penumbuhan film tipis temperatur penumbuhan 8500 C, laju spinner 1000 rpm, molaritas Ga2O3 1,33 M dan laju aliran gas nitrogen 100 sccm.  Hasil pengujian sifat lis...

  2. Effect of Heat Treatment on the Structural Properties of TiO2 Films Produced by Sol-Gel Spin Coating Technique

    Science.gov (United States)

    Nebi, M.; Peker, D.

    2016-10-01

    Due to have superior properties as fotocatalyst and have wide band gap, TiO2 thin films often investigated by researchers and used by technological applications widely. In this study TiO2 films were deposited on glass substrate by Sol-Gel Spin Coating Technic. TiO2 films were deposited at different number of layer and then annealed at 400o C, 500o C, and 600o C in air. Effect of anneal temperature to structural properties were investigated by XRD analysis. It was observed by the light of XRD results that the structural properties of films had changed by anneal temperature.

  3. Gd doping effect on structural, electrical and magnetic properties of ZnO thin films synthesized by sol-gel spin coating technique

    Science.gov (United States)

    Kumar, Sanjeev; Thangavel, Rajalingam

    2017-03-01

    Nanocrystalline Gd-doped ZnO thin films were deposited on sapphire (0001) substrates using sol-gel spin coating technique. The structural and optical properties of deposited thin films were characterized by X-ray diffraction (XRD) and micro Raman spectroscopy. Structural and optical studies show that the doped Gd ions occupy Zn sites retaining the wurtzite symmetry. Photoluminescence (PL) studies reveal the presence of oxygen vacancies in Gd doped ZnO thin films. The resistivity of Gd doped ZnO thin film decreases with increase in Gd doping upto 4%. Gd-doped ZnO films demonstrate weak magnetic ordering at room temperature.

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

    OpenAIRE

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

    1997-01-01

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

  5. Characterizations of Tb:Zn2SiO4 films on silicon wafer prepared by sol-gel dip-coating and solid-phase reaction

    Institute of Scientific and Technical Information of China (English)

    Ji Zhen-Guo; Zhao Shi-Chao; Xiang Yin; Song Yong-Liang; Ye Zhi-Zhen

    2004-01-01

    Terbium-doped Zn2SiO4 films were successfully prepared on Si wafers by a simple sol-gel dip-coating and solidphase reaction method of ZnO and SiO2. X-ray diffraction (XRD) and UV-Vis absorption results revealed that films processed below 850℃ were ZnO in wurzite structure, and films processed above 850℃ were Zn2SiO4 in wellimite structure. Photoluminescence measurements of the Tb-doped Zn2SiO4 films showed two strong emission bands at 490and 545nm. The photoluminescence lifetime was 4.6ms.

  6. Research on Technics of TiC Hardened Coating Prepared by Hybrid Process of Laser and Sol-Gel%激光复合溶胶一凝胶法制备TiC强化涂层的工艺研究

    Institute of Scientific and Technical Information of China (English)

    曾启; 张群莉; 徐柠; 姚建华

    2012-01-01

    采用Nd∶YAG激光对预置有溶胶一凝胶法制备的TiO2/C混合粉末的45#钢表面进行激光强化实验,制备TiC增强强化涂层.研究了激光工艺参数以及TiO2/C的成分配比对强化层生成物相的影响,探寻生成TiC的最佳工艺组合和粉末材料的成分配比.采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、能谱仪(EDS)测试方法对激光强化样品进行物相、显微组织以及元素分析.结果表明,能生成TiC的最佳工艺组合为激光电流250 A,脉冲频率18 Hz,脉冲宽度2.5 ms,扫描速度为50 mm/min,TiO2与C的物质的量比为1∶5.在上述工艺条件下,可在45#钢表面原位合成TiC增强相,并获得TiC颗粒均匀分布的强化涂层.%Laser hardening experiments are performed by Nd: YAG laser on the surface of 45 steel with TiO2 /C compound powder prepared by sol-gel to get TiC enhanced coating. The influence of laser parameters and ratio of the powder materials on phases of hardened coating are investigated to explore the optimum technics. The phases, microstructures and elemental analysis are tested by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectrometer (EDS), respectively. The results show that the optimum processing parameters should be laser current of 250 A, pulse frequency of 18 Hz, pulse width of 2.5 ms, laser velocity of 50 mm/min, and the mole ratio of TiQ. and C should be 1 :5. Under the above condition, TiC reinforcing phase can be in-situ synthesized on the surface of 45# steel and the hardened coating with TiC particles uniformly distributed can be obtained.

  7. WO3-Doped TiO2 Coating on Charcoal Activated with Increase Photocatalytic and Antibacterial Properties Synthesized by Microwave-Assisted Sol-Gel Method

    Directory of Open Access Journals (Sweden)

    Weerachai Sangchay

    2017-01-01

    Full Text Available WO3-doped TiO2 coating on charcoal activated (CA was prepared by microwave-assisted sol-gel method. The samples calcined at the temperature of 500°C for 2 h with a heating rate of 10°C/min were characterized by XRD, EDS, and SEM. The photocatalytic and antibacterial activities of WO3-doped TiO2 coating on CA were investigated by means of degradation of a methylene blue (MB solution and against the bacteria E. coli, respectively. The effects of WO3 concentration were discussed. The 1% WO3-doped TiO2 coated CA seems to exhibit the higher photocatalytic and antibacterial activity than other samples. The WO3-doped TiO2 coated on CA are expected to be applied as a photocatalyst for water purification.

  8. Inorganic-organic hybrid membranes with anhydrous proton conduction prepared from 3-aminopropyltriethoxysilane and sulfuric acid by the sol-gel method.

    Science.gov (United States)

    Tezuka, Teruaki; Tadanaga, Kiyoharu; Hayashi, Akitoshi; Tatsumisago, Masahiro

    2006-12-27

    Inorganic-organic hybrid membranes with anhydrous proton conduction were prepared from 3-aminopropyltriethoxysilane and H2SO4 by the sol-gel method. The membrane has a unique structure: a hexagonal phase formed by the stacking of rodlike polysiloxanes with ion complexes of ammonium groups and HSO4- extruded outside. The membranes showed high conductivity of 2 x 10-3 S cm-1 at 200 degrees C under dry atmosphere. In the membrane, protons probably migrate through the outside of the rodlike polysiloxanes along hydrogen-bond chains formed among HSO4- anions.

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

    Science.gov (United States)

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

    2010-01-01

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

  10. Sol-gel synthesis and characterization of SiO2/PCL hybrid materials containing quercetin as new materials for antioxidant implants.

    Science.gov (United States)

    Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando; Piccolella, Simona; Pacifico, Severina

    2016-01-01

    The development of biomaterials with intrinsic antioxidant properties could represent a valuable strategy for preventing peri-implant disease onset. In this context quercetin, a naturally occurring flavonoid, has been entrapped, at different weight percentages in a silica/poly(ε-caprolactone)-based hybrid material by a sol-gel route. FT-IR and UV spectroscopic techniques were employed in order to characterize the hybrids. FT-IR analysis indicated changes in stretching frequencies of the quercetin dienonic moiety, suggesting that a flavonol oxidized derivative was formed during the sol-gel process. The establishment of hydrogen-bonded interactions between quercetin and silica and polymer matrices,was strongly affected by the amount of polymer. Poly(ε-caprolactone) did not interact with quercetin when it was loaded at high doses (50 wt.%). The morphology of the synthesized materials was observed by using SEM. The obtained images proved that the materials are hybrid nanocomposites. Their bioactivity was shown by the formation of a hydroxyapatite layer on samples' surface soaked in a fluid simulating the composition of the human plasma. The antiradical properties of the investigated systems were evaluated by DPPH and ABTS methods and their cytotoxicity by the MTT assay. Data obtained revealed that the synthesized materials are biocompatible and that the hybrid system,with 6 wt.% of PCL and 15 wt.% of quercetin, produced the strongest antiradical efficacy.

  11. Photocatalytic Graphene-TiO2 Thin Films Fabricated by Low-Temperature Ultrasonic Vibration-Assisted Spin and Spray Coating in a Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Fatemeh Zabihi

    2017-05-01

    Full Text Available In this work, we communicate a facile and low temperature synthesis process for the fabrication of graphene-TiO2 photocatalytic composite thin films. A sol-gel chemical route is used to synthesize TiO2 from the precursor solutions and spin and spray coating are used to deposit the films. Excitation of the wet films during the casting process by ultrasonic vibration favorably influences both the sol-gel route and the deposition process, through the following mechanisms. The ultrasound energy imparted to the wet film breaks down the physical bonds of the gel phase. As a result, only a low-temperature post annealing process is required to eliminate the residues to complete the conversion of precursors to TiO2. In addition, ultrasonic vibration creates a nanoscale agitating motion or microstreaming in the liquid film that facilitates mixing of TiO2 and graphene nanosheets. The films made based on the above-mentioned ultrasonic vibration-assisted method and annealed at 150 °C contain both rutile and anatase phases of TiO2, which is the most favorable configuration for photocatalytic applications. The photoinduced and photocatalytic experiments demonstrate effective photocurrent generation and elimination of pollutants by graphene-TiO2 composite thin films fabricated via scalable spray coating and mild temperature processing, the results of which are comparable with those made using lab-scale and energy-intensive processes.

  12. Optical and structural properties of nanocrystalline anatase (TiO{sub 2}) thin films prepared by non-aqueous sol-gel dip-coating

    Energy Technology Data Exchange (ETDEWEB)

    Haimi, E., E-mail: eero.haimi@tkk.fi [Department of Materials Science and Engineering, Aalto University, P.O. Box 16200, FI-00076 Aalto (Finland); Lipsonen, H.; Larismaa, J. [Department of Materials Science and Engineering, Aalto University, P.O. Box 16200, FI-00076 Aalto (Finland); Kapulainen, M. [VTT, Technical Research Centre of Finland, Tietotie 3, Espoo P.O. Box 1000, FI-02044 VTT (Finland); Krzak-Ros, J. [Institute of Materials Science and Applied Mechanics, Wroclaw University of Technology, PL-50371, Wroclaw (Poland); Hannula, S.-P. [Department of Materials Science and Engineering, Aalto University, P.O. Box 16200, FI-00076 Aalto (Finland)

    2011-07-01

    Anatase (TiO{sub 2}) thin films were grown by non-aqueous sol-gel dip-coating using titanium (IV) n-butoxide as precursor and 1-butanol as solvent. High withdrawal speed of 4.7 mm/s in dip-coating resulted in defect free films of 100 nm average film thickness after subsequent heat treatments. According to scanning electron microscope and X-ray diffraction measurements, the films consisted of nanocrystalline anatase with 30 nm mean crystallite size. Refractive index n({lambda}) and extinction coefficient k({lambda}) were determined over the wavelength range from 200 to 1650 nm. The optical band gap of the film material was approximately 3.2 eV. The results showed very similar optical characteristics to those that are accomplished with chemically more reactive aqueous sol-gel processes. Furthermore, it was found that in addition to porosity, coordination number of Ti atoms to nearest oxygen neighbors is likely to have a significant role in explaining differences of optical properties between bulk anatase and thin film materials of the present work.

  13. Ultra-high-stability, pH-resistant sol-gel titania poly(tetrahydrofuran) coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    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).

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

    Science.gov (United States)

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

    2016-07-01

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

  15. Fourier transform infrared spectroscopic monitoring of sol-gel process in synthesis of PbS-TiO{sub 2} hybrid nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Khanmohammadi, Mohammadreza, E-mail: mrkhanmohammadi@gmail.co [Chemistry Department, Faculty of Science, IKIU, Qazvin (Iran, Islamic Republic of); Fard, Hassan Ghafoori [Electrical Engineering Department, Amir-Kabir University of Technology, Tehran (Iran, Islamic Republic of); Garmarudi, Amir Bagheri; Khoddami, Nafiseh [Chemistry Department, Faculty of Science, IKIU, Qazvin (Iran, Islamic Republic of)

    2010-09-30

    A typical hybrid nanostructure was prepared consisting of lead sulfide (PbS) nano-crystals, embedded in titanium oxide (TiO{sub 2}) using sol-gel method. The synthesis procedure was monitored by Fourier transform infrared spectroscopy. Spectroscopic investigations indicated that PbS nano-crystals are embedded in the TiO{sub 2} matrix with no strong Ti-O-Pb-S bonding. The size of PbS hybrid nanostructures decreased with diminishing lead and sulfur mole concentrations. The smallest size of NCs has been obtained in 10% of mole concentration (30-45 nm particle size for the hybrid nanostructure). The morphology and microstructure of the nano hybrid was investigated by scanning electron microscope and X-ray diffraction.

  16. Silver Doped TiO2 Nanostructure Composite Photocatalyst Film Synthesized by Sol-Gel Spin and Dip Coating Technique on Glass

    Directory of Open Access Journals (Sweden)

    Mojtaba Nasr-Esfahani

    2008-01-01

    Full Text Available New composite films (P25SGF-MC-Ag, MPC500SGF-MC-Ag, and ANPSGF-MC-Ag have been synthesized by a modified sol-gel method using different particle sizes of TiO2 powder and silver addition. Nanostructure TiO2/Ag composite thin films were prepared by a sol-gel spin and dip coating technique. while, by introducing methyl cellulose (MC porous, TiO2/Ag films were obtained after calcining at a temperature of 500°C. The as-prepared TiO2 and TiO2/Ag films were characterized by X-ray diffractometry, and scanning electron microscopy to reveal the structural and morphological differences. In addition, the photocatalytic properties of these films were investigated by degrading methyl orange (MO under UV irradiation. After 500°C calcination, the microstructure of MC-TiO2 film without Ag addition exhibited a microstructure, while significant sintering effect was noticed with Ag additions and the films exhibited a porous microstructure. Nanostructure anatase-phase TiO2 can be observed with respect to the sharpening of XRD diffraction peaks. The photodegradation of porous TiO2 deposited with 5×10−4 mol Ag exhibited the best photocatalytic efficiency, where 69% methyl orange can be decomposed after UV exposure for 1 hour.

  17. Electrospun Polyhydroxybutyrate/Poly(ε-caprolactone)/58S Sol-Gel Bioactive Glass Hybrid Scaffolds with Highly Improved Osteogenic Potential for Bone Tissue Engineering.

    Science.gov (United States)

    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 .

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

    Science.gov (United States)

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

    2015-12-01

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

  19. Two highly stable and selective solid phase microextraction fibers coated with crown ether functionalized ionic liquids by different sol-gel reaction approaches.

    Science.gov (United States)

    Shu, Jianjun; Xie, Pengfei; Lin, Danni; Chen, Rongfeng; Wang, Jiang; Zhang, Beibei; Liu, Mingming; Liu, Hanlan; Liu, Fan

    2014-01-02

    In this work, two novel crown ether functionalized ionic liquid (FIL)-based solid phase microextraction (SPME) fibers were prepared by sol-gel technology using the synthesized 1-(trimethoxysily)propyl 3-(6'-oxo-benzo-15-crown-5 hexyl) imidazolium bis(trifluoromethanesulphonyl)imide ([TMSP(Benzo15C5)HIM][N(SO2CF3)2]) and 1-allyl-3-(6'-oxo-benzo-15-crown-5 hexyl) imidazolium bis(trifluoromethanesulphonyl)imide ([A(Benzo15C5)HIM][N(SO2CF3)2]) as selective stationary phases. Owing to the introduction of trimethoxysilypropyl to the imidazole cation, the [TMSP(Benzo15C5)HIM][N(SO2CF3)2] could be chemically bonded to the formed sol-gel silica substrate through the hydrolysis and polycondensation reaction. Similarly, the [A(Benzo15C5)HIM][N(SO2CF3)2] was able to participate in the formation of the organic-inorganic copolymer coatings through the free radical crosslinking reaction. These two fibers were determined to have "bubble-like" surface characteristics analogous to a previously prepared [A(Benzo15C5)HIM][PF6]-based fiber. Their thermal stabilities were much higher than that of the [A(Benzo15C5)HIM][PF6]-based coating. They were capable of withstanding temperatures as high as 400°C without evident loss of the crown ether FILs. They also had strong solvent, acid and alkali resistance, good coating preparation reproducibility and high selectivity for medium polar to polar compounds. The high selectivity of these two fibers could be attributed to the strong ion-dipole, hydrogen bonding and π-π interactions provided by the synergetic effect of ILs and benzo-15-crown-5 functionalities. Moreover, the selectivity of these two fibers was rather different although the structures of these two crown ether FILs were very similar. This is maybe because the relative contents of the crown ether FILs chemically bonded to the organic-inorganic copolymer coatings were quite different when prepared by different sol-gel reaction approaches.

  20. Characterizations of Cuprous Oxide Thin Films Prepared by Sol-Gel Spin Coating Technique with Different Additives for the Photoelectrochemical Solar Cell

    Directory of Open Access Journals (Sweden)

    D. S. C. Halin

    2014-01-01

    Full Text Available Cuprous oxide (Cu2O thin films were deposited onto indium tin oxide (ITO coated glass substrate by sol-gel spin coating technique using different additives, namely, polyethylene glycol and ethylene glycol. It was found that the organic additives added had a significant influence on the formation of Cu2O films and lead to different microstructures and optical properties. The films were characterized by X-ray diffraction (XRD, field emission scanning electron microscopy (FESEM, and ultraviolet-visible spectroscopy (UV-Vis. Based on the FESEM micrographs, the grain size of film prepared using polyethylene glycol additive has smaller grains of about 83 nm with irregular shapes. The highest optical absorbance film was obtained by the addition of polyethylene glycol. The Cu2O thin films were used as a working electrode in the application of photoelectrochemical solar cell (PESC.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1995-06-01

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

  2. Effect of the size of silica nanoparticles on wettability and surface chemistry of sol-gel superhydrophobic and oleophobic nanocomposite coatings

    Science.gov (United States)

    Lakshmi, R. V.; Bera, Parthasarathi; Anandan, C.; Basu, Bharathibai J.

    2014-11-01

    Superhydrophobic sol-gel nanocomposite coatings have been fabricated by incorporating silica nanoparticles with different particle sizes separately in an acid-catalyzed sol of methyltriethoxysilane (MTEOS). Water contact angle (WCA) of the coatings increased with increase in the concentration of silica nanoparticles in both the cases. The coatings became superhydrophobic at an optimum silica concentration. The water repellency was further improved by the addition of fluoroalkylsilane (FAS). The optimum silica concentration was found to depend on the size of silica nanoparticles and FAS content and the coatings exhibited WCA of about 160° and water sliding angle (WSA) of oleophobicity of the coatings. The coatings exhibited oil-repellency with a lubricant oil contact angle of 126° and ethylene glycol contact angle of 153.3°. Surface morphology of the coatings analyzed using field emission scanning electron microscopy (FESEM) showed a rough surface with microscale bumps and nanoscale pores. XPS was used to study the surface composition of the coatings. The superhydrophobic property of the coatings was due to the synergistic effect of surface chemistry and surface microstructure and can be explained using Cassie-Baxter model.

  3. Thickness and structure change of titanium(IV) oxide thin films synthesized by the sol-gel spin coating method

    Science.gov (United States)

    Lewkowicz, Aneta; Synak, Anna; Grobelna, Beata; Bojarski, Piotr; Bogdanowicz, Robert; Karczewski, Jakub; Szczodrowski, Karol; Behrendt, Mirosław

    2014-08-01

    Titanium dioxide is a well-known material in nanotechnology, while it provides new opportunities due to its interesting properties, for example, as a semiconductor with a quite significant forbidden band gap energy of 3.2 eV. In this study, thin films of titanium dioxide (TiO2) were synthesized in amorphous and crystallographic systems using the sol-gel process. Atomic Force Microscopy (AFM), Raman spectroscopy and X-ray diffraction (XRD) techniques were applied to obtain structural characteristics of the prepared films. We estimated that TiO2 thin films crystallize in anatase phase between temperatures 380 °C and 700 °C, and into anatase-rutile phase at 650 °C, while rutile phase exists alone above 800 °C. The changes in porosity of materials in relation to temperature were calculated as well. The refractive index of titanium dioxide thin films from ellipsometric measurements is also provided.

  4. Electrophoretic Deposition, Microstructure, and Corrosion Resistance of Porous Sol-Gel Glass/Polyetheretherketone Coatings on the Ti-13Nb-13Zr Alloy

    Science.gov (United States)

    Moskalewicz, Tomasz; Zych, Anita; Łukaszczyk, Alicja; Cholewa-Kowalska, Katarzyna; Kruk, Adam; Dubiel, Beata; Radziszewska, Agnieszka; Berent, Katarzyna; Gajewska, Marta

    2017-02-01

    In this study, microporous composite sol-gel glass/polyetheretherketone (SGG/PEEK) coatings were produced on the Ti-13Nb-13Zr titanium alloy by electrophoretic deposition. Coatings with different levels of high open porosity were developed by introducing SGG particles of varying diameters into the PEEK matrix. The microstructure of the coatings was characterized by electron microscopy and X-ray diffractometry. The coatings with 40-50 µm thickness were composed of semicrystalline SGG particles consisting of hydroxyapatite, CaSiO3, some Ca2SiO4, and an amorphous phase containing Ca, Si, P, and O, homogeneously embedded in a semicrystalline PEEK matrix. The size of SGG particles present in the coatings strongly influenced the formation of microcracks and their adhesion to the underlying substrate. Microscratch tests showed that the coating containing SGG particles with a diameter smaller than 45 µm and open porosity of 45 pct exhibited good adhesion to the titanium alloy substrate, much better than the coating containing particles with a diameter smaller than 85 µm and total open porosity equal to 48 pct. The corrosion resistance was investigated in Ringer's solution at a temperature of 310 K (37 °C) for a pH equal to 7.4 and in deaerated solutions with the use of open-circuit potential, potentiodynamic polarization, and electrochemical impedance spectroscopy. The SGG/PEEK-coated alloy indicated better electrochemical corrosion resistance compared with the uncoated alloy.

  5. Electrophoretic Deposition, Microstructure, and Corrosion Resistance of Porous Sol-Gel Glass/Polyetheretherketone Coatings on the Ti-13Nb-13Zr Alloy

    Science.gov (United States)

    Moskalewicz, Tomasz; Zych, Anita; Łukaszczyk, Alicja; Cholewa-Kowalska, Katarzyna; Kruk, Adam; Dubiel, Beata; Radziszewska, Agnieszka; Berent, Katarzyna; Gajewska, Marta

    2017-05-01

    In this study, microporous composite sol-gel glass/polyetheretherketone (SGG/PEEK) coatings were produced on the Ti-13Nb-13Zr titanium alloy by electrophoretic deposition. Coatings with different levels of high open porosity were developed by introducing SGG particles of varying diameters into the PEEK matrix. The microstructure of the coatings was characterized by electron microscopy and X-ray diffractometry. The coatings with 40-50 µm thickness were composed of semicrystalline SGG particles consisting of hydroxyapatite, CaSiO3, some Ca2SiO4, and an amorphous phase containing Ca, Si, P, and O, homogeneously embedded in a semicrystalline PEEK matrix. The size of SGG particles present in the coatings strongly influenced the formation of microcracks and their adhesion to the underlying substrate. Microscratch tests showed that the coating containing SGG particles with a diameter smaller than 45 µm and open porosity of 45 pct exhibited good adhesion to the titanium alloy substrate, much better than the coating containing particles with a diameter smaller than 85 µm and total open porosity equal to 48 pct. The corrosion resistance was investigated in Ringer's solution at a temperature of 310 K (37 °C) for a pH equal to 7.4 and in deaerated solutions with the use of open-circuit potential, potentiodynamic polarization, and electrochemical impedance spectroscopy. The SGG/PEEK-coated alloy indicated better electrochemical corrosion resistance compared with the uncoated alloy.

  6. 溶胶-凝胶法制备光致变色镀膜玻璃%Photochromic Glass Prepared by Sol-Gel Coating

    Institute of Scientific and Technical Information of China (English)

    张麒

    2013-01-01

    Several photochromic glasses were prepared by sol - gel coating method. The WO3 - H2C2O4 -TiO2 film coated photochromic glass in which the ratio of element titanium to tungsten is 5% shows better properties than the others. The transmittance of visible light of this glass decreases about 10% -12% and the shading coefficient decreases about 0. 13 -0. 15 after 3-5 min under sunlight. It indicates excellent heat insulation property of this kind of photochromic glass. The transmittance of this glass increased about 40% after 60 min in dark area and then faded completely after 5 h. The photochromic behavior and fading process can be well repeated. The photochromic glass prepared by this sol - gel coating method is worthy of further study.%利用溶胶-凝胶法制备了多种光致变色镀膜玻璃,特别是Ti与W元素比为5%的WO3-H2C2O4-TiO2镀膜玻璃,在太阳光照射3~5 min内,透过率下降10% ~ 12%,可推算出其遮阳系数下降0.13 ~0.15,表明该光致变色镀膜玻璃有明显的隔热效果.变色后的该镀膜玻璃在无光照60 min后透光率可恢复40%左右,在无光照5h左右,可恢复到光照前的透光率,即完全褪色.用溶胶-凝胶法制备的该光致变色膜系变色-褪色重复性好,有一定的研发价值.

  7. Organic/inorganic hybrid coatings for anticorrosion

    Science.gov (United States)

    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

  8. SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

    Institute of Scientific and Technical Information of China (English)

    Jie-bin Pang; Kun-yuan Qiu; Yen Wei

    2000-01-01

    Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder Xray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m2/g) and pore volumes (e.g. 0.6 cm3/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

  9. PREPARATION OF TITANIA SOL-GEL COATINGS CONTAINING SILVER IN VARIOUS FORMS AND MEASURING OF THEIR BACTERICIDAL EFFECTS AGAINST E. COLI

    Directory of Open Access Journals (Sweden)

    Diana Horkavcova

    2015-09-01

    Full Text Available The work describes titania coatings containing various forms of silver applied on a titanium substrate by a dip-coating sol-gel technique. Silver was added into the basic titania sol in form of colloid particles of Ag, crystals of AgNO3, particles of AgI, particles of Ag3PO4 and Ag3PO4 developed in situ (in the sol by reaction of AgNO3 with added calcium phosphate (brushite or monetite. Mechanically and chemically treated titanium substrates were dipped at a constant rate into individual types of sols. Subsequently, they were slowly fired. The fired coatings contained microcracks. All over the surface there were evenly distributed spherical nanoparticles of silver (Ag, AgNO3 or microcrystals of AgI and Ag3PO4. The prepared coatings were tested under static conditions for their bactericidal effects against gram-negative bacteria Escherichia coli (E. coli. The coated substrates were immersed into a suspension of E. coli in physiological solution for 24 and 4 hours. The basic titania coatings with no silver demonstrated no bactericidal properties. Very good bactericidal effect against E. coli in both types of bactericidal test showed the titania coatings with AgNO3, Ag3PO4 crystals and Ag3PO4 developed in situ.

  10. Polypyrrole/sol-gel composite as a solid-phase microextraction fiber coating for the determination of organophosphorus pesticides in water and vegetable samples.

    Science.gov (United States)

    Saraji, Mohammad; Rezaei, Behzad; Boroujeni, Malihe Khalili; Bidgoli, Ali Akbar Hajialiakbari

    2013-03-01

    A novel solid-phase microextraction (SPME) fiber coated with polypyrrole/sol-gel composite was prepared through electrochemical deposition. The composite polymer coating was prepared using a three-electrode electrochemical system and directly deposited on a stainless steel wire by applying a constant potential (1.2V for 1000 s). The coating has porous surface structure, stable performance in high temperature, and good coating preparation reproducibility. The SPME composite coating was evaluated by analyzing some organophosphorus pesticides (OPPs) in water and vegetable samples followed by gas chromatography and nitrogen phosphorus detection. Different SPME parameters influencing the extraction efficiency such as coating thickness, salt concentration, stirring rate, extraction time and temperature, desorption time and desorption temperature were investigated. Under the optimized conditions, the coating showed better extraction efficiency than polypyrrole and commercial SPME fibers. The detection limits were 1.5-10 ng L(-1). Relative standard deviations for intra- and inter-day precision for a single fiber were in the range of 1.1-2.9% and 2.2-4.2%, respectively. Fiber to fiber reproducibility was in the range of 6.0-10.1% (n=3). The calibration curves were linear in the concentration range from 5 to 2000 ng L(-1) (r(2)>0.9953). Finally, the developed method was applied for the analysis of cucumber, lettuce, tap and well water samples and the relative recovery was found to be in the range of 80-109%, at the optimum conditions.

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

    Science.gov (United States)

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

    2015-05-01

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

  12. Fabrication of ZnO Thin Films by Sol-Gel Spin Coating and Their UV and White-Light Emission Properties

    Science.gov (United States)

    Kumar, Mirgender; Dubey, Sarvesh; Rajendar, Vanga; Park, Si-Hyun

    2017-10-01

    ZnO thin films have been fabricated by the sol-gel spin-coating technique and annealed under different conditions, and their ultraviolet (UV) and white-light emission properties investigated. Different ambient conditions including oxygen, nitrogen, zinc-rich nitrogen, and vacuum were used to tune the main properties of the ZnO thin films. The resistivity varied from the conductive to semi-insulating regime, and the luminescence emission from fairly intense UV to polychromatic. The emission intensity was also found to be a function of the annealing conditions. Possible routes to compensate the loss of emission characteristics are discussed. X-ray photoelectron spectroscopy (XPS) analysis was carried out to detect the chemical states of the zinc/oxygen species. The changes in the electrical and emission properties are explained based on annihilation/formation of inherent donor/acceptor-type defects. Such ZnO thin films could have potential applications in solid-state lighting.

  13. Synthesis and Properties of Nd-doped TiO2 thin films by sol-gel dip-coating method

    Directory of Open Access Journals (Sweden)

    Wang Jun

    2016-01-01

    Full Text Available TiO2 thin films doped with neodymium(Nd in the range from 0 at.% to 10at. % were prepared on glass substrates by sol-gel dip-coating method. Water contact angle on the Nd-doped TiO2 films were measured by contact angle analyzer. The water contact angle measurement result showed that the hydrophily of the films improved when the Nd3+ concentration increased to 5 at.%. The photocatalytic activity of the undoped and Nd-doped TiO2 thin films were investigated by the degradation of methylene blue under high-voltage mercury lamp. The results showed that 5 at.% Nd-doped TiO2 thin film exhibited the highest photocatalytic efficiency.

  14. Densification of In{sub 2}O{sub 3}:Sn multilayered films elaborated by the dip-coating sol-gel route

    Energy Technology Data Exchange (ETDEWEB)

    Daoudi, K.; Canut, B.; Blanchin, M.G.; Sandu, C.S.; Teodorescu, V.S.; Roger, J.A

    2003-11-24

    Indium Tin Oxide (ITO) thin films have been deposited by the Sol-Gel Dip-Coating technique, the starting solutions being prepared from chlorides. These multilayered films were crystallized by means of a classical heat treatment at temperatures ranging from 500 to 600 deg. C. Five stacked layers are necessary to obtain a global electrical resistivity value of 2.9x10{sup -3} {omega} cm, for 500 deg. C annealed film. The paper focuses on the study of the structure of such multilayered deposits, and on the densification process, using transmission electron microscopy, Rutherford Back-scattering Spectrometry and electrical resistivity measurements. This analysis reveals structural inhomogeneities and different crystallite growth processes as a function of annealing temperature and number of deposited layers.

  15. Sol-gel spin coated well adhered MoO3 thin films as an alternative counter electrode for dye sensitized solar cells

    Science.gov (United States)

    Mutta, Geeta R.; Popuri, Srinivasa R.; Wilson, John I. B.; Bennett, Nick S.

    2016-11-01

    In this work, we aim to develop a viable, inexpensive and non-toxic material for counter electrodes in dye sensitized solar cells (DSSCs). We employed an ultra-simple synthesis process to deposit MoO3 thin films at low temperature by sol-gel spin coating technique. These MoO3 films showed good transparency. It is predicted that there will be 150 times reduction of precursors cost by realizing MoO3 thin films as a counter electrode in DSSCs compared to commercial Pt. We achieved a device efficiency of about 20 times higher than that of the previous reported values. In summary we develop a simple low cost preparation of MoO3 films with an easily scaled up process along with good device efficiency. This work encourages the development of novel and relatively new materials and paves the way for massive reduction of industrial costs which is a prime step for commercialization of DSSCs.

  16. Optically enhanced SnO{sub 2}/CdSe core/shell nanostructures grown by sol-gel spin coating method

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Vijay, E-mail: vijaynadda83@gmail.com; Goswami, Y. C. [School of Physical Sciences, ITM University, Turari, Gwalior, MP 474001 (India); Rajaram, P. [School of Studies in Physics, Jiwaji University, Gwalior MP 474011 (India)

    2015-08-28

    Synthesis of SnO{sub 2}/CdSe metal oxide/ chalcogenide nanostructures on glass micro slides using ultrasonic sol-gel process followed by spin coating has been reported. Stannous chloride, cadmium chloride and selenium dioxide compounds were used for Sn, Cd and Se precursors respectively. Ethylene glycol was used as complexing agent. The samples were characterized by XRD, SEM, AFM and UV-spectrophotometer. All the peaks shown in diffractograms are identified for SnO{sub 2}. Peak broadening observed in core shell due to stress behavior of CdSe lattice. Scanning electron microscope and AFM exhibits the conversion of cluster in to nanorods structures forms. Atomic force microscope shows the structures in nanorods form and a roughness reduced 1.5194 nm by the deposition of CdSe. Uv Visible spectra shows a new absorption edge in the visible region make them useful for optoelectronic applications.

  17. Sol-gel deposited aluminum-doped and gallium-doped zinc oxide thin-film transparent conductive electrodes with a protective coating of reduced graphene oxide

    Science.gov (United States)

    Zhu, Zhaozhao; Mankowski, Trent; Balakrishnan, Kaushik; Shikoh, Ali Sehpar; Touati, Farid; Benammar, Mohieddine A.; Mansuripur, Masud; Falco, Charles M.

    2016-04-01

    Using a traditional sol-gel deposition technique, we successfully fabricated aluminum-doped zinc oxide (AZO) and gallium-doped zinc oxide (GZO) thin films on glass substrates. Employing a plasma treatment method as the postannealing process, we produced thin-film transparent conductive electrodes exhibiting excellent optical and electrical properties, with transmittance greater than 90% across the entire visible spectrum and the near-infrared range, as well as good sheet resistance under 200 Ω/sq. More importantly, to improve the resilience of our fabricated thin-film samples at elevated temperatures and in humid environments, we deposited a layer of reduced graphene oxide (rGO) as protective overcoating. The stability of our composite AZO/rGO and GZO/rGO samples improved substantially compared to that of their counterparts with no rGO coating.

  18. Optically enhanced SnO2/CdSe core/shell nanostructures grown by sol-gel spin coating method

    Science.gov (United States)

    Kumar, Vijay; Rajaram, P.; Goswami, Y. C.

    2015-08-01

    Synthesis of SnO2/CdSe metal oxide/ chalcogenide nanostructures on glass micro slides using ultrasonic sol-gel process followed by spin coating has been reported. Stannous chloride, cadmium chloride and selenium dioxide compounds were used for Sn, Cd and Se precursors respectively. Ethylene glycol was used as complexing agent. The samples were characterized by XRD, SEM, AFM and UV-spectrophotometer. All the peaks shown in diffractograms are identified for SnO2. Peak broadening observed in core shell due to stress behavior of CdSe lattice. Scanning electron microscope and AFM exhibits the conversion of cluster in to nanorods structures forms. Atomic force microscope shows the structures in nanorods form and a roughness reduced 1.5194 nm by the deposition of CdSe. Uv Visible spectra shows a new absorption edge in the visible region make them useful for optoelectronic applications.

  19. PEMBUATAN SENSOR GAS HIDROGEN BERBASIS FILM TIPIS GaN DENGAN TEKNIK SOL GEL SPIN COATING UNTUK KOMPONEN PADA SISTEM PENDETEKSI KEBOCORAN GAS

    Directory of Open Access Journals (Sweden)

    D. Rusdiana

    2013-06-01

    Full Text Available Penelitian ini bertujuan untuk membuat sensor gas dengan sensitivitas baik, dipergunakan sebagai komponen dalam sistem pendeteksi kebocoran gas hidrogen. Bahan dasar sensor berbahan  film tipis semikonduktor Gallium Nitrida (GaN yang ditumbuhkan di atas substrat sapphire (Al2O3 menggunakan teknik sol gel spin coating. Parameter penumbuhan film tipis temperatur penumbuhan 8500 C, laju spinner 1000 rpm, molaritas Ga2O3 1,33 M dan laju aliran gas nitrogen 100 sccm.  Hasil pengujian sifat listrik dalam lingkungan gas hidrogen ternyata resistansi listrik sensor gas menurun secara tajam dari 1,5 x 10-2 Ohm.cm menjadi 7 x 10-3 Ohm.cm bila laju aliran gas diperbesar dari 20 sccm hingga 150 sccm. Pengujian sensitivitas sensor gas dilakukan dalam lingkungan gas hidrogen dan gas nitrogen. Hasil pengujian sensor gas dalam lingkungan gas hidrogen memiliki sensitivitas sekitar 60 % sedangkan dalam lingkungan gas nitrogen sekitar 50 % laju aliran gas 100 sccm. Tingkat sensitivitas sensor gas dalam lingkungan gas hidrogen lebih tinggi dibandingkan dalam lingkungan gas nitrogen. This research aims to make the gas sensors using GaN films that grown on sapphire substrate (Al2O3 by sol gel spin coating techniques with growth temparature 8500 C, spinner rate 1000 rpm, molarity of Ga2O3 1.33 M and nitrogen flow rate 100 sccm. Upon exposure to volatile organic compound (VOC, especially to hydrogen gas, the electrical resistance of semiconducting GaN thin film was found to rapidly decrease from 1.5 x 10-2 Ohm.cm to 7 x 10-3 Ohm.cm after increasing the hydrogen gas flow rate from 20 sccm to 150 sccm. The gas sensors exhibited good sensitivity of about 60 % in 100 sccm flowing hydrogen gas and about 50 % in 100 sccm flowing nitrogen gas.

  20. PEMBUATAN SENSOR GAS HIDROGEN BERBASIS FILM TIPIS GaN DENGAN TEKNIK SOL GEL SPIN COATING UNTUK KOMPONEN PADA SISTEM PENDETEKSI KEBOCORAN GAS

    Directory of Open Access Journals (Sweden)

    D. Rusdiana

    2013-01-01

    Full Text Available Penelitian ini bertujuan untuk membuat sensor gas dengan sensitivitas baik, dipergunakan sebagai komponen dalam sistem pendeteksi kebocoran gas hidrogen. Bahan dasar sensor berbahan  film tipis semikonduktor Gallium Nitrida (GaN yang ditumbuhkan di atas substrat sapphire (Al2O3 menggunakan teknik sol gel spin coating. Parameter penumbuhan film tipis temperatur penumbuhan 8500 C, laju spinner 1000 rpm, molaritas Ga2O3 1,33 M dan laju aliran gas nitrogen 100 sccm.  Hasil pengujian sifat listrik dalam lingkungan gas hidrogen ternyata resistansi listrik sensor gas menurun secara tajam dari 1,5 x 10-2 Ohm.cm menjadi 7 x 10-3 Ohm.cm bila laju aliran gas diperbesar dari 20 sccm hingga 150 sccm. Pengujian sensitivitas sensor gas dilakukan dalam lingkungan gas hidrogen dan gas nitrogen. Hasil pengujian sensor gas dalam lingkungan gas hidrogen memiliki sensitivitas sekitar 60 % sedangkan dalam lingkungan gas nitrogen sekitar 50 % laju aliran gas 100 sccm. Tingkat sensitivitas sensor gas dalam lingkungan gas hidrogen lebih tinggi dibandingkan dalam lingkungan gas nitrogen. This research aims to make the gas sensors using GaN films that grown on sapphire substrate (Al2O3 by sol gel spin coating techniques with growth temparature 8500 C, spinner rate 1000 rpm, molarity of Ga2O3 1.33 M and nitrogen flow rate 100 sccm. Upon exposure to volatile organic compound (VOC, especially to hydrogen gas, the electrical resistance of semiconducting GaN thin film was found to rapidly decrease from 1.5 x 10-2 Ohm.cm to 7 x 10-3 Ohm.cm after increasing the hydrogen gas flow rate from 20 sccm to 150 sccm. The gas sensors exhibited good sensitivity of about 60 % in 100 sccm flowing hydrogen gas and about 50 % in 100 sccm flowing nitrogen gas.

  1. Advanced polymer-inorganic hybrid hard coatings utilizing in situ polymerization method.

    Science.gov (United States)

    Takaki, Toshihiko; Nishiura, Katsunori; Mizuta, Yasushi; Itou, Yuichi

    2006-12-01

    Hard coatings are frequently used to give plastics high scratch resistance. Coating hardness and adhesion to the substrate are considered to be key factors influencing scratch resistance, but it is difficult to produce coatings that have both properties. Hybridization of polymers and inorganic materials is a promising approach for solving this problem. We prepared polymer-silica hybrid coatings by using in situ polymerization to carry out radical polymerization of vinyl monomers in a sol-gel solution of alkoxysilanes, and measured the abrasion resistance of the coatings. However, the expected properties were not obtained because the sol-gel reaction did not perfectly proceed on the surface of the coatings under the N2 conditions. We found that curing the hybrid coatings by UV irradiation in air promoted the sol-gel reaction on the surface, resulting in coatings having excellent abrasion resistance.

  2. In Situ Formation of Decavanadate-Intercalated Layered Double Hydroxide Films on AA2024 and their Anti-Corrosive Properties when Combined with Hybrid Sol Gel Films

    Directory of Open Access Journals (Sweden)

    Junsheng Wu

    2017-04-01

    Full Text Available A layered double hydroxide (LDH film was formed in situ on aluminum alloy 2024 through a urea hydrolysis method, and a decavanadate-intercalated LDH (LDH-V film fabricated through the dip coating method. The microstructural and morphological characteristics were investigated by scanning electron microscopy (SEM. The corrosion-resistant performance was analyzed by electrochemical impedance spectroscopy (EIS, scanning electrochemical microscopy (SECM, and a salt-spray test (SST.The SEM results showed that a complete and defect-free surface was formed on the LDH-VS film. The anticorrosion results revealed that the LDH-VS film had better corrosion-resistant properties than the LDH-S film, especially long-term corrosion resistance. The mechanism of corrosion protection was proposed to consist of the self-healing effect of the decavanadate intercalation and the shielding effect of the sol-gel film.

  3. Thin films of calcium phosphate and titanium dioxide by a sol-gel route: a new method for coating medical implants.

    Science.gov (United States)

    Piveteau, L D; Girona, M I; Schlapbach, L; Barboux, P; Boilot, J P; Gasser, B

    1999-03-01

    Titanium is a commonly used biomaterial for dental and orthopaedic applications. To increase its ability to bond with bone, some attempts were made to coat its surface with calcium phosphate (CaP). This paper describes a new type of coating. Instead of a pure CaP layer, a mixing of titanium dioxide (TIO2) and CaP is fabricated and deposited as a coating. These layers are deposited by a sol-gel route on pure titanium substrates using various pre-treatments. The method consists of mixing a solution of tetrabutyl ortho-titanate or a sol of titanium dioxide with a solution of calcium nitrate and phosphorous esters. This composite is deposited on to commercially pure titanium plates, mechanically polished or blasted with pure crystalline aluminum oxide, using the spin-coating technique. These coatings are then fired at 650 or 850 degrees C for various times. The samples are characterized by X-ray diffraction for their crystallinity, X-ray photoelectron spectroscopy for their surface chemical composition and scanning electron microscopy for their topography. Samples treated at 850 degrees C present a well-pronounced crystallinity, and a high chemical purity at the surface. The topography is strongly related to the viscosity of the precursor and the substrate pre-treatment. Possibilities to structure the outermost layer are presented.

  4. Sol-gel coatings in the ZrO{sub 2}-SiO{sub 2} system for protection of historical works of glass

    Energy Technology Data Exchange (ETDEWEB)

    Carmona, N. [Fundacion Centro Nacional del Vidrio, Real Fabrica de Cristales. Po Pocillo, 1. 40100 La Granja de San Ildefonso (Segovia) (Spain)]. E-mail: ncarmona@cenim.csic.es; Villegas, M.A. [Centro Nacional de Investigaciones Metalurgicas, CSIC. Avda, Gregorio del Amo, 8. 28040 Madrid (Spain); Fernandez Navarro, J.M. [Instituto de Optica Daza de Valdes, CSIC. C. Serrano, 121. 28006 Madrid (Spain)

    2006-12-05

    Different kinds of protective treatments based on sol-gel coatings have been designed and prepared. Final application of these coatings would be used for protection and preventive conservation of a wide variety of historical glasses from several times and provenance. Historical glasses show a superficial deterioration depending on the exhibition conditions submitted by the ancient objects since their origin. The coatings effectiveness was confirmed by means of accelerated ageing tests under simulated atmospheric polluted conditions by using SO{sub 2} as a pollutant and different kind of glasses as reference substrates. Coatings with compositions 100SiO{sub 2} and 10ZrO{sub 2}.90SiO{sub 2} (mol%) proved to be highly protective when they were densified up to 250 and 400 deg. C for 1 h. Those coatings densified at lower temperature (for instance, 60 deg. C for 3 days) appeared partially cracked and detached after the ageing tests. For compositions 50ZrO{sub 2}.50SiO{sub 2} and 100ZrO{sub 2} the major problem was concerned to the high surface reflectance provided by the zirconium oxide, which modifies very much the appearance of the substrate glasses.

  5. CuCr2O4 Spinel Ceramic Pigments Synthesized by Sol-Gel Self-Combustion Method for Solar Absorber Coatings

    Science.gov (United States)

    Ma, Pengjun; Geng, Qingfen; Gao, Xianghu; Yang, Shengrong; Liu, Gang

    2016-07-01

    A series of CuCr2O4 spinel ceramic pigments have been successfully synthesized via a facile and cost-effective sol-gel self-combustion method. The reaction mechanism was systematically studied using the corresponding characterization technologies. The results suggested that CuCr2O4 spinel ceramic pigments could be obtained at annealing temperature of 600 °C for 1 h, and the size, morphology, and crystallinity of CuCr2O4 spinel were greatly influenced by the annealing temperature. The as-burnt powder and CuCr2O4 spinel ceramic pigment were then employed to fabricate thickness sensitive spectrally selective (TSSS) paint coatings by a convenient spray-coating technique. The results revealed that spectral selectivity of TSSS paint coatings based on CuCr2O4 spinel ceramic pigments was much better than that of paint coatings based on the as-burnt powders. Furthermore, the effect of surface features of TSSS paint coatings on its optical property and hydrophobicity was investigated in detailed.

  6. Realization of MMI Power Splitter by UV-light Imprinting Technique Using Hybrid Sol-Gel SiO2 Materials

    Institute of Scientific and Technical Information of China (English)

    WANG Yue; WU Yuan-Da; LI Jian-Guang; WANG Hong-Jie; HU Xiong-Wei

    2008-01-01

    An efficient fabrication scheme of buried ridge, waveguide devices is demonstrated by UV-light imprinting technique using organic-inorganic hybrid sol-gel Zr-doped SiO2 materials. The refractive indices of a guiding layer and a cladding layer for the buried ridge waveguide structure are 1.537 and 1.492 measured at 1550nm, respectively. The tested results show more circular mode profiles due to existence of the cladding layer. A buried ridge single-mode waveguide operating at 1550nm has a low propagation loss (O.088 dB/cm) and the 1 × 2 MMI power splitter exhibits uniform outputs, with a very low splitting loss of O.029dB at 1549nm.

  7. In-Situ Sol-Gel Composition of Hybrid Precursors to Synthesize SrTiO3 :Pr3+ Red Ceramic Phosphors

    Institute of Scientific and Technical Information of China (English)

    Yan Bing; Zhou Kun

    2004-01-01

    Praseodymium coordination polymers with ortho hydroxylbenzoic acid was used as the precursors of luminescent species to compose with polyethylene glycol (PEG), and inorganic/organic hybrid polymeric dispersing media were assembled by a modified in-situ sol-gel process of tert-n-butyl titanate (Ti( OC4H9 )4 ) and further thermal decomposed to achieve rare earth oxysalts ceramic phosphor SrTiO3: Pr3 +. Both XRD and SEM indicate that the particle sizes of them were in the range of around 1 μm. The excitation spectra presented a brand spectral band in visible blue-violet region of the maximum excitation peak of 445 nm, and the corresponding emission spectra exhibit wide emission with maximum peak of 619 nm, which was ascribed to be the characteristic transition of Pr3+ (1D2→3 H4). It can be expected to be applied in the visible light conversion materials.

  8. Correlation between microstructure and optical properties of nano-crystalline TiO{sub 2} thin films prepared by sol-gel dip coating

    Energy Technology Data Exchange (ETDEWEB)

    Mechiakh, R., E-mail: raouf_mechiakh@yahoo.fr [Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar, Batna (Algeria); Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Laboratoire de Ceramiques, Universite Mentouri Constantine (Algeria); Sedrine, N. Ben; Chtourou, R. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Bensaha, R. [Laboratoire de Ceramiques, Universite Mentouri Constantine (Algeria)

    2010-11-15

    Titanium dioxide thin films have been prepared from tetrabutyl-orthotitanate solution and methanol as a solvent by sol-gel dip coating technique. TiO{sub 2} thin films prepared using a sol-gel process have been analyzed for different annealing temperatures. Structural properties in terms of crystal structure were investigated by Raman spectroscopy. The surface morphology and composition of the films were investigated by atomic force microscopy (AFM). The optical transmittance and reflectance spectra of TiO{sub 2} thin films deposited on silicon substrate were also determined. Spectroscopic ellipsometry study was used to determine the annealing temperature effect on the optical properties and the optical gap of the TiO{sub 2} thin films. The results show that the TiO{sub 2} thin films crystallize in anatase phase between 400 and 800 deg. C, and into the anatase-rutile phase at 1000 deg. C, and further into the rutile phase at 1200 deg. C. We have found that the films consist of titanium dioxide nano-crystals. The AFM surface morphology results indicate that the particle size increases from 5 to 41 nm by increasing the annealing temperature. The TiO{sub 2} thin films have high transparency in the visible range. For annealing temperatures between 1000 and 1400 deg. C, the transmittance of the films was reduced significantly in the wavelength range of 300-800 nm due to the change of crystallite phase and composition in the films. We have demonstrated as well the decrease of the optical band gap with the increase of the annealing temperature.

  9. Optical Properties of Titania Coatings Prepared by Inkjet Direct Patterning of a Reverse Micelles Sol-Gel Composition

    Directory of Open Access Journals (Sweden)

    Veronika Schmiedova

    2015-08-01

    Full Text Available Thin layers of titanium dioxide were fabricated by direct inkjet patterning of a reverse micelles sol-gel composition onto soda-lime glass plates. Several series of variable thickness samples were produced by repeated overprinting and these were further calcined at different temperatures. The resulting layers were inspected by optical and scanning electronic microscopy and their optical properties were investigated by spectroscopic ellipsometry in the range of 200–1000 nm. Thus the influence of the calcination temperature on material as well as optical properties of the patterned micellar titania was studied. The additive nature of the deposition process was demonstrated by a linear dependence of total thickness on the number of printed layers without being significantly affected by the calcination temperature. The micellar imprints structure of the titania layer resulted into significant deviation of measured optical constants from the values reported for bulk titania. The introduction of a void layer into the ellipsometric model was found necessary for this particular type of titania and enabled correct ellipsometric determination of layer thickness, well matching the thickness values from mechanical profilometry.

  10. Nanocrystal/sol-gel nanocomposites

    Science.gov (United States)

    Petruska, Melissa A.; Klimov, Victor L.

    2007-06-05

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

  11. Scratch resistance of SiO{sub 2} and SiO{sub 2} - ZrO{sub 2} sol-gel coatings on glass-ceramic obtained by sintering; Resistencia al desgaste de recubrimientos sol-gel de SiO{sub 2} y SiO{sub 2} - ZrO{sub 2} sobre materiales vitroceramicos obtenidos por sinterizacion

    Energy Technology Data Exchange (ETDEWEB)

    Soares, V. O.; Soares, P.; Peitl, O.; Zanotto, E. D.; Duran, A.; Castro, Y.

    2013-10-01

    The sol-gel process is widely used to obtain coatings on glass-ceramic substrates in order to improve the scratch and abrasion resistance, also providing a bright and homogeneous appearance of a glaze avoiding expensive final polishing treatments. This paper describes the preparation of silica and silica / zirconia coatings by sol-gel method on Li{sub 2}O-Al{sub 2}O3-SiO{sub 2} (LAS) glassceramic substrates produced by sintering. The coatings were deposited by dip-coating on LAS substrates and characterized by optical microscopy and spectral ellipsometry. On the other hand, hardness and elastic modulus, coefficient of friction and abrasion and scratch resistance of the coatings were determined and compared with the substrate properties. Coatings deposited on LAS glass-ceramic confere the substrate a bright and homogeneous aspect, similar to a glaze, improving the appearance and avoiding the final polishing. However these coatings do not increase the scratch resistance of the substrate only equaling the properties of the glass-ceramic. (Author)

  12. Impact of Overlapping Fe/TiO2 Prepared by Sol-Gel and Dip-Coating Process on CO2 Reduction

    Directory of Open Access Journals (Sweden)

    Akira Nishimura

    2016-01-01

    Full Text Available Fe-doped TiO2 (Fe/TiO2 film photocatalyst was prepared by sol-gel and dip-coating process to extend its photoresponsivity to the visible spectrum. To promote the CO2 reduction performance with the photocatalyst, some types of base materials used for coating Fe/TiO2, which were netlike glass fiber and Cu disc, were investigated. The characterization of prepared Fe/TiO2 film coated on netlike glass fiber and Cu disc was analyzed by SEM and EPMA. In addition, the CO2 reduction performance of Fe/TiO2 film coated on netlike glass disc, Cu disc, and their overlap was tested under a Xe lamp with or without ultraviolet (UV light, respectively. The results show that the concentration of produced CO increases by Fe doping irrespective of base material used under the illumination condition with UV light as well as that without UV light. Since the electron transfer between two overlapped photocatalysts is promoted, the peak concentration of CO for the Fe/TiO2 double overlapping is approximately 1.5 times as large as the Fe/TiO2 single overlapping under the illumination condition with UV light, while the promotion ratio is approximately 1.1 times under that without UV light.

  13. Magneto-optical mode conversion in a hybrid glass waveguide made by sol-gel and ion-exchange techniques

    Science.gov (United States)

    Royer, François; Amata, Hadi; Parsy, François; Jamon, Damien; Ghibaudo, Elise; Broquin, Jean-Emmanuel; Neveu, Sophie

    2012-01-01

    The integration of magneto-optical materials with classical technologies being still a difficult problem, this study explores the possibility to realize a mode converter based on a hybrid structure. A composite magneto-optical layer made of a silica/zirconia matrix doped by magnetic nanoparticles is coated on the top face of ion-exchanged glass waveguides. Optical characterizations that have been carried out demonstrated the efficiency of these hybrid structures in terms of lateral confinement. Furthermore, TE to TM mode conversion has been observed when a longitudinal magnetic field is applied to the device. The amount of this conversion is analysed taking into account the magneto-optical confinement and the modal birefringence of the structure.

  14. Preparation of polypyrrole composite solid-phase microextraction fiber coatings by sol-gel technique for the trace analysis of polar biological volatile organic compounds.

    Science.gov (United States)

    Zhang, Zhuomin; Zhu, Li; Ma, Yunjian; Huang, Yichun; Li, Gongke

    2013-02-21

    Two novel polypyrrole (PPy) composite solid-phase microextraction (SPME) fiber coatings involving polypyrrole β-naphthalenesulfonic acid (PPy/β-NSA) and polypyrrole graphene (PPy/GR) composite SPME fiber coatings were prepared by a simple sol-gel technique for selectively sampling relatively polar biological volatile organic compounds (VOCs). Crucial preparation conditions of the PPy composite SPME fiber coatings were optimized and are discussed in detail. Physical tests suggested that the PPy composite SPME fiber coatings possessed a porous surface morphology, stable chemical and thermal properties. Due to the inducing polar functional groups in the PPy molecule, the PPy composite SPME fiber coatings achieved a higher extraction capacity and special selectivity for the polar biological VOCs with conjugate structures, compared with commercial SPME fiber coatings. Enrichment factors of most of the VOCs by the PPy/β-NSA and PPy/GR SPME fibers were much higher than those achieved by common commercially available SPME fiber coatings. Finally, the PPy/β-NSA and PPy/GR SPME fiber coatings were applied for the trace analysis of typical polar VOCs from ant and coriander samples coupled with gas chromatography/mass spectrometry (GC/MS) detection, respectively. It was satisfactory that the average contents of 4-heptanone, 4-heptanol, 4-nonanone and methyl 5-methylsalicylate from ant samples were actually found to be 28.0, 58.7, 3.0 and 0.6 μg g(-1), and the average contents of nonane, decanal, undecanal and dodecanal from coriander samples were actually found to be 0.79, 0.13, 0.06 and 0.21 μg g(-1). The results suggested that PPy composite SPME coatings will be a potentially excellent sampling technique for the trace analysis of polar biological VOCs.

  15. 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.

    Science.gov (United States)

    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 Pporcelain.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-07-01

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

  17. Preparation and characterization of hybrid materials of epoxy resin type bisphenol a with silicon and titanium oxides by sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Carrillo C, A.; Osuna A, J. G., E-mail: acc.carrillo@gmail.com [Universidad Autonoma de Coahuila, Facultad de Ciencias Quimicas, Blvd. Venustiano Carranza y Jose Cardenas Valdes, 25000 Saltillo, Coahuila (Mexico)

    2011-07-01

    Hybrid materials were synthesized from epoxy resins as a result bisphenol type A-silicon oxide and epoxy resin bisphenol type A-titanium oxide were obtained. The synthesis was done by sol-gel process using tetraethyl orthosilicate (Teos) and titanium isopropoxide (I Ti) as inorganic precursors. The molar ratio of bisphenol A to the inorganic precursors was the studied variable. The materials were characterized by thermal analysis, infrared spectroscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy. The hybrid nature of the materials was demonstrated through thermal analysis and infrared spectroscopy. In both systems, as the amount of alkoxide increased, the bands described above were more defined. This behavior indicates the interactions between the resin and the alkoxides. Hybrids with Teos showed a smoother and homogeneous surface in its entirety, without irregularities. Hybrids with titanium isopropoxide had low roughness. Both Teos and I Ti hybrids showed a decrease on the atomic weight percentage of carbon due to a slight reduction of the organic part on the surface. (Author)

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

    Directory of Open Access Journals (Sweden)

    Agda Aline Rocha de Oliveira

    2009-06-01

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

  19. Nano-structure TiO2 film coating on 316L stainless steel via sol-gel technique for blood compatibility improvement

    Directory of Open Access Journals (Sweden)

    Mohammadreza Foruzanmehr

    2014-04-01

    Full Text Available   Objective(s: Titanium oxides are known to be appropriate hemocompatible materials which are suggested as coatings for blood-contacting devices. Little is known about the influence of nanometric crystal structure, layer thickness, and semiconducting characteristics of TiO2 on blood hemostasis.   Materials and Methods: Having used sol-gel dip coating method in this study, TiO2 thin films were deposited on nano-scale electro-polished stainless steel 316L with 1 to 5 nano-sized layers. Surface morphology and structure of the film were studied with X-ray diffraction and atomic force microscopy. Blood compatibility was also determined by measuring the platelet activation (CD62P expression, platelet adhesion (Scanning Electron Microscopy, and the blood clotting time on these samples. Results: The films were compact and smooth and existed mainly in the form of anatase. By increasing the number of TiO2 thin layer, clotting time greatly extended, and the population of activated platelet and P-selectine expression changed according to the surface characteristics of each layer. Conclusion: The findings revealed that stainless steel 316L coated with nano-structured TiO2 layer improved blood compatibility, in terms of both blood platelet activity and coagulation cascade, which can decrease the thrombogenicity of blood contacting devices which were made from stainless steel.

  20. CO2 Reforming Performance and Visible Light Responsibility of Cr-Doped TiO2 Prepared by Sol-Gel and Dip-Coating Method

    Directory of Open Access Journals (Sweden)

    Akira Nishimura

    2010-01-01

    Full Text Available A Cr-doped TiO2 film was prepared by sol-gel and dip-coating method and used as the photocatalyst for CO2 reforming under the visible light. The ratio of amount of Cr added to amount of Ti in TiO2 sol solution (R varied from 0 to 100 wt%. The total layer number of Cr-doped TiO2 film (N coated was up to 7. The CO2 reforming performance with the Cr-doped TiO2 film was evaluated by illuminating under a Xe lamp with or without ultraviolet (UV light. The concentration of CO which was a product from CO2 reforming was maximized for =70 wt% when N equals to 1. The visible light responsibility was also maximized for =70 wt%. The amount of Cr within TiO2 film coated on copper disc was increased with the increase in R up to 70 wt% and started to decrease when R is over 70 wt%. The CO2 reforming performance of TiO2 film with one layer Cr-doped was found better than that of TiO2 film with multi Cr-doped layers under illuminating of UV light. Under the visible light, the performance was maximized at =70 wt% and =7 with one layer Cr-doped.

  1. Corrosion protection of AA 2024-T3 aluminium alloys using 3, 4-diaminobenzoic acid chelated zirconium-silane hybrid sol-gels

    Energy Technology Data Exchange (ETDEWEB)

    Varma, P.C. Rajath; Colreavy, John [Centre for Research on Engineering Surface Technology (CREST), FOCAS Institute, Dublin Institute of Technology, 13 Camden Row, Dublin 8 (Ireland); Cassidy, John [School of Chemical and Pharmaceutical Sciences, Dublin Institute of Technology, Kevin St., Dublin 8 (Ireland); Oubaha, Mohamed; McDonagh, Colette [National Centre for Sensor Research (NCSR), Dublin City University, Dublin 9 (Ireland); Duffy, Brendan, E-mail: bduffy@dit.i [Centre for Research on Engineering Surface Technology (CREST), FOCAS Institute, Dublin Institute of Technology, 13 Camden Row, Dublin 8 (Ireland)

    2010-08-02

    Organic-inorganic polymers formed by hydrolysis/condensation reactions of alkoxide precursors, such as organically modified silanes (Ormosils) are used for several industrial applications such as electronic, optical and protective anticorrosion coatings. Such materials possess superior chemical stability, physical strength and scratch resistance characteristics when compared to organic polymers. Further performance improvement can be achieved through the incorporation of zirconium and titanium based nanoparticles, also formed through from precursors via the sol-gel process. However due to the inherent reactivity differences of the above precursors, they must be hydrolysed separately before being combined for final condensation. Zirconium precursors are commonly chelated using acetic acid or acetyl acetonate prior to hydrolysis, to lower the hydrolysis rate. In this body of work, 3,4-diaminobenzoic acid (DABA) and acetyl acetonate (acac) were compared as chelating ligands for controlling the hydrolysis reactions of zirconium n-propoxide to form nanoparticles within a silane sol matrix. The sols were applied as coatings on aerospace grade aluminium alloy AA 2024-T3 and characterised by physical, spectroscopical, microscopical, electrochemical and calorimetric techniques. The electrochemical properties of the coatings, as characterised by EIS and PDS, correlated with neutral salt spray evaluations confirming that the use of DABA as a chelating ligand significantly improved the coating performance when compared to the traditional diketone ligand. The data indicates the anticorrosion properties of the nitrogen rich chelate have a key role in protecting the alloy through the formation of smaller zirconium nanoparticles, thus improving the polymer network stability.

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

    Science.gov (United States)

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

    2016-10-28

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

  3. Effects of dip-coating speed and annealing temperature on structural, morphological and optical properties of sol-gel nano-structured TiO2 thin films

    Science.gov (United States)

    Touam, Tahar; Atoui, Mohamed; Hadjoub, Ilhem; Chelouche, Azeddine; Boudine, Boubekeur; Fischer, Alexis; Boudrioua, Azzedine; Doghmane, Abdellaziz

    2014-09-01

    We reported material characterization of the nano-structured TiO2 thin films prepared by the sol-gel dip-coating process on glass substrates. The dependence of the structural, morphological and optical properties of the synthesized films on the fabrication parameters such as withdrawal velocity and annealing temperature were investigated by the techniques of X-ray diffraction (XRD), Raman spectroscopy (RS), scanning electron microscopy (SEM), atomic force microscopy (AFM) and UV-visible spectrophotometry. The results indicate that for the TiO2 films annealed at 500 °C there exhibits (1 0 1) XRD peak corresponding to the anatase phase of TiO2. The latter is consistent with the recorded Raman signal observed at 142 cm-1 (Eg mode) and 391 cm-1 (B1g mode), respectively. From the analyses made on the SEM micrographs and AFM images, it was revealed that the morphology and surface roughness of the thin films would depend on the withdrawal speed and the heat treatment temperature. The UV-visible spectroscopy analyses show that all the films were transparent in the visible region with an average transmittance of more than 70%. With an increase on the dip-coating speed from 1 cm/min to 3 cm/min, we observed a spectral red shift of the absorption edge from 3.76 eV to 3.71 eV, indicating a decrease in the bandgap energy (Eg) of the films.

  4. CO2 Reforming Characteristics under Visible Light Response of Cr- or Ag-Doped TiO2 Prepared by Sol-Gel and Dip-Coating Process

    Directory of Open Access Journals (Sweden)

    Akira Nishimura

    2012-01-01

    Full Text Available A Cr- or Ag-doped TiO2 film was prepared by sol-gel and dip-coating process and used as the photocatalyst for CO2 reforming under the visible light. The ratio of amount of Cr or Ag added to amount of Ti in TiO2 sol solution (R varied from 0 to 100 wt% or 0 to 50 wt%, respectively. The total layer number of Cr- or Ag-doped TiO2 film (N coated was changed. The CO2 reforming performance with the Cr- or Ag-doped TiO2 film was tested under a Xe lamp with or without ultraviolet (UV light. As a result, when N equals to 1, the concentration of CO which was a product from CO2 reforming was maximized in Cr doping case for R = 70 wt% and in Ag doping case for R = 1 wt%, respectively. The best result of concentration of CO = 8306 ppmV, concentration of CH4 = 1367 ppmV, concentration of C2H6 = 1712 ppmV is obtained when top=7 with Cr doping in this study.

  5. Fabrication Process of Sol-Gel Spin Coating for SrBi2Ta2O9 Films Applied to FeRAM

    Institute of Scientific and Technical Information of China (English)

    JIA Ze; REN Tian-Ling; ZHANG Zhi-Gang; LIU Tian-Zhi; WEN Xin-Yi; XIE Dan; LIU Li-Tian

    2006-01-01

    @@ We investigate SrBi2Ta2O9 (SBT) films prepared by the sol-gel spin method with different spin rates or different anneal conditions for the first layer of SBT, as promising ferroelectric layer materials applied to ferroelectric random access memory (FeRAM). All the specimens in this experiment have similar SBT crystal orientations of (115), (020), (220), and (135). The Pt/SBT/Pt capacitor with coating of 3000rpm spin rate has a perfect rectangle shape of hysteresis loops, remanent polarization of 7.57μC/cm2 and coercive voltage of 0.816 V at 5 V voltage amplitude. These characteristics are better than those with coating of 3500rpm spin rate, which is attributed to the influence for thickness and grain size of the film from depressed spin rate. Slow-rate anneal in the furnace for the first layer of SBT can improve the crystallization processes and properties for SBT layers slightly, compared with rapid thermal annealing. The ion damage from etching for the top electrode can influence leakage current characteristics of the Pt/SBT/Pt capacitor at positive voltage bias.

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

    Science.gov (United States)

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

    2013-01-01

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

  7. Bifunctional ferromagnetic Eu-Gd-Bi-codoped hybrid organo-silica red emitting phosphors synthesized by a modified Pechini sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Abo-Naf, S.M., E-mail: sm.abo-naf@nrc.sci.eg [Glass Research Department, National Research Centre (NRC), El-Buhouth Str., Dokki, 12622 Cairo (Egypt); Abdel-Hameed, S.A.M.; Marzouk, M.A. [Glass Research Department, National Research Centre (NRC), El-Buhouth Str., Dokki, 12622 Cairo (Egypt); Hamdy, Y.M. [Spectroscopy Department, National Research Centre (NRC), El-Buhouth Str., Dokki, 12622 Cairo (Egypt)

    2017-06-15

    Red phosphor, composed of Eu-Gd-Bi-codoped hybrid organo-silica glass, has been synthesized via a modified Pechini sol-gel process. The synthesized hybrid glass was analyzed with powder X-ray diffraction (XRD), differential thermal analysis coupled with thermogravimetry (DTA-TG) and Fourier transform infrared (FTIR) spectroscopy. XRD and DTA-TG confirmed its amorphous structure up to 1000 °C. Magnetic behavior of the produced phosphor was investigated using vibrating specimen magnetometer (VSM) and the obtained results revealed its unsaturated ferromagnetic behavior. Photoluminescence (PL) properties of the obtained phosphor have been investigated under near-UV excitation at 395 nm. The influence of calcination temperature on the PL intensity and its decay behavior as well as on the ferromagnetic characteristics has been studied to determine the optimal reaction temperature of the phosphor. The PL emission spectra show the characteristic emission bands of Eu{sup 3+} ions in the wavelength range from 580 to 700 nm. These emission spectra have been dominated by the electric dipole {sup 5}D{sub 0}→{sup 7}F{sub 2} transition of the Eu{sup 3+} peaked at 610–620 nm producing the red light emission of the phosphors. It was found that the phosphor performance, expressed by its PL intensity and life time, could be significantly improved by increasing of the heat treatment temperature up to 900 °C. Also, calcination at 900 °C for 6 h greatly increased both of the magnetization and retentivity, while decreased the coercivity value. The organic phenomenon of metal citrate-ethylene glycol chelation and its degradation by calcination were well followed by FTIR spectroscopy. The obtained results are promising and could afford a basis for designing of efficient red phosphors for displays, lighting and bifunctional biosensors for biomedical applications. - Highlights: • Eu-Gd-Bi-codoped hybrid organo-silica phosphor was synthesized by sol-gel method. • Inorganic Eu

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

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

  10. The effect of concentration ratio and type of functional group on synthesis of CNT-ZnO hybrid nanomaterial by an in situ sol-gel process

    Science.gov (United States)

    Hosseini Largani, Sekineh; Akbarzadeh Pasha, Mohammad

    2016-12-01

    In this research, MWCNT-ZnO hybrid nanomaterials were synthesized by a simple sol-gel process using Zn(CH3COO)2·2H2O and functionalized MWCNT with carboxyl(COOH) and hydroxyl(OH) groups. Three different mass ratios of MWCNT:ZnO = 3:1, 1:1 and 1:3 were examined. The prepared nanomaterials were characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FTIR). Successful growth of MWCNT-ZnO hybrids for both COOH and OH functional groups and all the three mass ratios were obtained. The ZnO nanoparticles attached on the surfaces of CNTs have rather spherical shapes and hexagonal crystal structure. By increasing the concentration of ZnO, the number and average size of ZnO nanoparticles decorated the body of CNTs in hybrid structures increase. By increasing the ZnO precursor, the distribution of ZnO nanoparticles that appeared on the surface of CNTs becomes more uniform. The SEM observation beside EDX analysis revealed that at the same concentration ratio the amount of ZnO loading on the surface of MWCNT-COOH is more than MWCNT-OH. Moreover, the average size of ZnO nanoparticles attached on the surface of COOH functionalized CNTs is relatively smaller than that of OH functionalized ones.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-05-01

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

  12. sol-gel

    Directory of Open Access Journals (Sweden)

    Humberto A. Monreal

    2005-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Krzysztof Marycz

    2014-01-01

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

  14. Study on polarization characteristics of BiFeO3 thin films prepared by sol-gel spin-coating technology

    Science.gov (United States)

    Jia, Ze; Wu, Xiao; Zhang, Mingming; Xu, Jianlong; Zhang, Naiwen; Liou, Juin J.

    2015-07-01

    The ferroelectric polarization properties of bismuth ferrite (BFO) thin films deposited on Pt(111)/TiO2/SiO2/Si(100) substrates by sol-gel spin-coating technology affected by the processes and dopants have been studied and analyzed tentatively. The results indicate BFO thin film should be introduced to a rapid thermal annealing (RTA) process at N2 atmosphere. The enhanced ferroelectric polarization properties were observed in Mn and La doped BFO thin films, because ion substitution may improve the inherent volatility of Bi atoms, valence fluctuation of Fe ions and magnetic spin structures, reducing the formation of oxygen vacancies. The increased remnant polarization observed in the BFO thin film with a lead zirconate titanate (PZT) seeding layer has also been analyzed as the probable results of small changes of lattice parameters caused by constraint stress, reduced defects and decreased leakage current density, which are contributed by the PZT seeding layer possibly. Moreover, the remnant polarization approximately 79 μC/cm2 is observed in (Bi0.95La0.05)FeO3 (BLFO) thin film with a PZT seeding layer, which is twice and treble the values of BFO thin films with and without a PZT seeding layer, indicating PZT seeding layer is much more effective for BLFO thin film which has a substitution at A site.

  15. Preparations of TiO2 film coated on foam nickel substrate by sol-gel processes and its photocatalytic activity for degradation of acetaldehyde

    Institute of Scientific and Technical Information of China (English)

    HU Hai; XIAO Wen-jun; YUAN Jian; SHI Jian-wei; CHEN Ming-xia; SHANG GUAN Wen-feng

    2007-01-01

    Anatase TiO2 films were successfully prepared on foam nickel substrates by sol-gel technique using tetrabutyl titanate as precursor. The characteristics of the TiO2 films were investigated by XPS, XRD, FE-SEM, TEM and UV-Vis absorption spectra. The photocatalytic activities of TiO2 films were investigated by photocatalytic degradation reactions of gaseous acetaldehyde, an indoor pollutant, under ultraviolet light irradiation. It was found that Ni2+ doping into TiO2 films due to the foam nickel substrates resulted in the extension of absorption edges of TiO2 films from UV region to visible light region. The pre-heating for foam nickel substrates resulted in the formation of NiO layer, which prevented effectively the injection of photogenerated electrons from TiO2 films to metal nickel. The TiO2 films displayed high photocatalytic activity for the degradation of acetaldehyde, and were enhanced by calcining the substrates and coating TiO2 films repeatedly. The high activity was mainly attributed to the improvement of the characteristics of substrate surface and the increase of active sites on photocatalyst.

  16. Preparations of TiO2 film coated on foam nickel substrate by sol-gel processes and its photocatalytic activity for degradation of acetaldehyde.

    Science.gov (United States)

    Hu, Hai; Xiao, Wen-jun; Yuan, Jian; Shi, Jian-wei; Chen, Ming-xia; Shang Guan, Wen-feng

    2007-01-01

    Anatase TiO2 films were successfully prepared on foam nickel substrates by sol-gel technique using tetrabutyl titanate as precursor. The characteristics of the TiO2 films were investigated by XPS, XRD, FE-SEM, TEM and UV-Vis absorption spectra. The photocatalytic activities of TiO2 films were investigated by photocatalytic degradation reactions of gaseous acetaldehyde, an indoor pollutant, under ultraviolet light irradiation. It was found that Ni2+ doping into Ti02 films due to the foam nickel substrates resulted in the extension of absorption edges of TiO2 films from UV region to visible light region. The pre-heating for foam nickel substrates resulted in the formation of NiO layer, which prevented effectively the injection of photogenerated electrons from TiO2 films to metal nickel. The TiO2 films displayed high photocatalytic activity for the degradation of acetaldehyde, and were enhanced by calcining the substrates and coating TiO2 films repeatedly. The high activity was mainly attributed to the improvement of the characteristics of substrate surface and the increase of active sites on photocatalyst.

  17. Optical properties of double layer thin films zinc oxide doping aluminum (ZnO/Al) were deposited on glass substrates by sol gel method spray coating technique

    Science.gov (United States)

    Permatasari, Anes; Sutanto, Heri; Marito Siagian, Sinta

    2017-01-01

    Thin films of double layer of ZnO/Al has succeeded in deposition on a glass substrate using sol-gel method and spray coating techniques. Variations of doping Al as much as 2%, 4%, 6% and 8%. ZnO precursor synthesized using zinc acetate dehydrate (Zn(COOCH3)2.2H2O), isopropanol ((CH3)2CHOH) and monoethanolamine (MEA) were stirred using a magnetic stirrer for 45 minutes. ZnO precursor get homogeneous and then added of aluminum nitrate nonahydrate predetermined doping concentration and stirred again for 15 minutes. Deposition solution is done by the spray on a glass substrate and then heated at a temperature of 450°C. A layer of ZnO/Al deposited over the ZnO to produce a thin layer of a double layer. Optical properties layer of ZnO/Al characterized using UV-Vis spectrophotometer. Based on data from UV-Vis absorbance was determined the value of the energy band gap. Pure and dopped layers has different energy due the Al dopping. For pure ZnO layer has energy band gap of 3.347 eV and decreased to 3.09 eV for ZnO layer with Al dopant.

  18. Preparation of silane-functionalized silica films via two-step dip coating sol-gel and evaluation of their superhydrophobic properties

    Science.gov (United States)

    Ramezani, Maedeh; Vaezi, Mohammad Reza; Kazemzadeh, Asghar

    2014-10-01

    In this paper, we study the two-step dip coating via a sol-gel process to prepare superhydrophobic silica films on the glass substrate. The water repellency of the silica films was controlled by surface silylation method using isooctyltrimethoxysilane (iso-OTMS) as a surface modifying agent. Silica alcosol was synthesized by keeping the molar ratio of ethyltriethoxysilane (ETES) precursor, ethanol (EtOH) solvent, water (H2O) was kept constant at 1:36:6.6 respectively, with 6 M NH4OH throughout the experiment and the percentages of hydrophobic agent in hexane bath was varied from 0 to 15 vol.%. The static water contact angle values of the silica films increased from 108° to 160° with an increase in the vol.% of iso-OTMS. At 15 vol%. of iso-OTMS, the silica film shows static water contact angle as high as 160°. The superhydrophobic silica films are thermally stable up to 440 °C and above this temperature, the silica films lose superhydrophobicity. By controlling the primer particle size of SiO2 about 26 nm, leading to decrease the final size of silica nanoparticles after modification of nanoparticles by isooctyltrimethoxysilane about 42 nm. The films are transparent and have uniform size on the surface. The silica films have been characterized by atomic force microscopy (AFM), fourier transform infrared spectroscopy (FT-IR), transparency, contact angle measurement (CA), Zeta-potential, Thermal stability by TG-DTA analysis.

  19. Application of poly(dimethylsiloxane) fiber sol-gel coated onto NiTi alloy electrodeposited with zirconium oxide for the determination of organochlorine pesticides in herbal infusions.

    Science.gov (United States)

    Budziak, Dilma; Martendal, Edmar; Carasek, Eduardo

    2008-08-01

    A PDMS fiber sol-gel coated onto an NiTi alloy previously electrodeposited with zirconium oxide (named NiTi-ZrO(2)-PDMS) was applied to the determination of organochlorine pesticides (OCPs) in infusions of peppermint (Mentha piperita L.), lemon grass (Cymbopogon citratus Stapf), chamomile (Matricaria recutita L.), lemon balm (Melissa officinalis L.), and anise seeds (Pimpinella anisum L.). Salting-out effect, extraction time, and extraction temperature were optimized firstly by means of a full-factorial design and then using a Doehlert matrix. No salt addition and 50 min of extraction at 70 degrees C were the optimum conditions. Satisfactory LODs in the range of 2-17 ng/L, as well as good correlation coefficients (at least 0.9981) in the linear range studied, were obtained. Calibration was successfully applied using an infusion of M. recutita L. and recovery tests were performed to ensure the accuracy of the method, with values in the range of 77-120%. Comparison of the NiTi-ZrO(2)-PDMS with commercially available PDMS fibers showed that the proposed fiber has an extraction efficiency comparable to that of PDMS 30 microm for the compounds evaluated, demonstrating its potential applicability.

  20. Studies on visible light photocatalytic and antibacterial activities of nanostructured cobalt doped ZnO thin films prepared by sol-gel spin coating method

    Science.gov (United States)

    Poongodi, G.; Anandan, P.; Kumar, R. Mohan; Jayavel, R.

    2015-09-01

    Nanostructured cobalt doped ZnO thin films were deposited on glass substrate by sol-gel spin coating technique and characterized by X-ray diffraction, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy and UV-Vis spectroscopy. The XRD results showed that the thin films were well crystalline with hexagonal wurtzite structure. The results of EDAX and XPS revealed that Co was doped into ZnO structure. FESEM images revealed that the films possess granular morphology without any crack and confirm that Co doping decreases the grain size. UV-Vis transmission spectra show that the substitution of Co in ZnO leads to band gap narrowing. The Co doped ZnO films were found to exhibit improved photocatalytic activity for the degradation of methylene blue dye under visible light in comparison with the undoped ZnO film. The decrease in grain size and extending light absorption towards the visible region by Co doping in ZnO film contribute equally to the improved photocatalytic activity. The bactericidal efficiency of Co doped ZnO films were investigated against a Gram negative (Escherichia coli) and a Gram positive (Staphylococcus aureus) bacteria. The optical density (OD) measurement showed better bactericidal activity at higher level of Co doping in ZnO.

  1. Carbon coated Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} cathode material prepared by a PVA assisted sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Tao; Pan Wencheng; Wang Jian [College of Materials Science and Engineering, Jilin University, Changchun 130012 (China); Bie Xiaofei; Du Fei [College of Physics and State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); Wei Yingjin, E-mail: yjwei@jlu.edu.c [College of Physics and State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); Wang Chunzhong; Chen Gang [College of Physics and State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China)

    2010-04-30

    Carbon coated Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} cathode material was prepared by a poly(vinyl alcohol) (PVA) assisted sol-gel method. PVA was used both as the gelating agent and the carbon source. XRD analysis showed that the material was well crystallized. The particle size of the material was ranged between 200 and 500 nm. HRTEM revealed that the material was covered by a uniform surface carbon layer with a thickness of 80 A. The existence of surface carbon layer was further confirmed by Raman scattering. The electrochemical properties of the material were investigated by charge-discharge cycling, CV and EIS techniques. The material showed good cycling performance, which had a reversible discharge capacity of 100 mAh g{sup -1} when cycled at 1 C rate. The apparent Li{sup +} diffusion coefficients of the material ranged between 9.5 x 10{sup -10} and 0.9 x 10{sup -10} cm{sup 2} s{sup -1}, which were larger than those of olivine LiFePO{sub 4}. The large lithium diffusion coefficient of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} has been attributed to its special NASICON-type structure.

  2. Studies on visible light photocatalytic and antibacterial activities of nanostructured cobalt doped ZnO thin films prepared by sol-gel spin coating method.

    Science.gov (United States)

    Poongodi, G; Anandan, P; Kumar, R Mohan; Jayavel, R

    2015-09-05

    Nanostructured cobalt doped ZnO thin films were deposited on glass substrate by sol-gel spin coating technique and characterized by X-ray diffraction, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy and UV-Vis spectroscopy. The XRD results showed that the thin films were well crystalline with hexagonal wurtzite structure. The results of EDAX and XPS revealed that Co was doped into ZnO structure. FESEM images revealed that the films possess granular morphology without any crack and confirm that Co doping decreases the grain size. UV-Vis transmission spectra show that the substitution of Co in ZnO leads to band gap narrowing. The Co doped ZnO films were found to exhibit improved photocatalytic activity for the degradation of methylene blue dye under visible light in comparison with the undoped ZnO film. The decrease in grain size and extending light absorption towards the visible region by Co doping in ZnO film contribute equally to the improved photocatalytic activity. The bactericidal efficiency of Co doped ZnO films were investigated against a Gram negative (Escherichia coli) and a Gram positive (Staphylococcus aureus) bacteria. The optical density (OD) measurement showed better bactericidal activity at higher level of Co doping in ZnO.

  3. Influence of pH of colloidal suspension on the electrical conductivity of SnO2 thin films deposited via Sol-Gel-Dip-Coating

    Directory of Open Access Journals (Sweden)

    Leandro Piaggi Ravaro

    2011-03-01

    Full Text Available Tin dioxide (SnO2 thin films are deposited by the dip-coating technique from colloidal suspensions prepared with distinct pH through the sol-gel method. The decrease of the pH contributes to the destruction of an electrical layer adjacent to particles in solution, leading to a high degree of aggregation among these particles due to the generation of cross-linked bonds (Sn-O-Sn between them. The aggregation affects the electrical properties of films, because the pH variation produces particle with distinct sizes in the film. Undoped samples prepared from pH 6 leads to the highest conductivity among the investigated undoped samples, in agreement with X-ray diffractograms, which indicate higher crystallinity for lower pH. Arrhenius plot evaluated from temperature dependent conductivity data leads to activation energies of the deepest level between 67 to 140 meV, for the films prepared from suspensions with pH 6 to 11. The most probable explanation for this variation in the conductivity and activation energy is related to distinct potential barriers between grains, due to distinct packing caused by cross-linked bonds formed during suspension phase. Characterization of samples lightly doped with Er3+ confirms that acid pH leads to higher conductivity, but the highest conduction takes place at even lower pH when compared to undoped thin films.

  4. Effect of Co doping concentration on structural properties and optical parameters of Co-doped ZnO thin films by sol-gel dip-coating method.

    Science.gov (United States)

    Nam, Giwoong; Yoon, Hyunsik; Kim, Byunggu; Lee, Dong-Yul; Kim, Jong Su; Leem, Jae-Young

    2014-11-01

    The structural and optical properties of Co-doped ZnO thin films prepared by a sol-gel dip-coating method were investigated. X-ray diffraction analysis showed that the thin films were grown with a c-axis preferred orientation. The position of the (002) peak was almost the same in all samples, irrespective of the Co concentration. It is thus clear that Co doping had little effect on the position of the (002) peak. To confirm that Co2+ was substituted for Zn2+ in the wurtzite structure, optical measurements were conducted at room temperature by a UV-visible spectrometer. Three absorption peaks are apparent in the Co-doped ZnO thin films that do not appear for the undoped ZnO thin film. As the Co concentration was increased, absorption related to characteristic Co2+ transitions increased because three absorption band intensities and the area underneath the absorption wells between 500 and 700 nm increased with increasing Co concentration. The optical band gap and static dielectric constant decreased and the Urbach energy and extinction coefficient increased with increasing Co concentration.

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

    Science.gov (United States)

    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.

  6. Characterization of ZnO and ZnO:Al thin films deposited by the sol-gel dip-coating technique

    Energy Technology Data Exchange (ETDEWEB)

    Marotti, R.E. [Instituto de Fisica, Facultad de Ingenieria, Universidad de la Republica, J. H. Reissig 565, CC 30, CP 11000, Montevideo (Uruguay)], E-mail: khamul@fing.edu.uy; Bojorge, C.D. [REPSOL-YPF, CITEFA, CINSO, Juan B. de La Salle 4397 - CP 1603 Villa Martelli, Buenos Aires (Argentina); Broitman, E. [Department of Chemical Engineering, Carnegie Mellon University, Pittsburgh PA 15213 (United States); Canepa, H.R. [CINSO, CONICET-CITEFA, Juan B. de La Salle 4397, CP 1603 Villa Martelli, Buenos Aires (Argentina); Badan, J.A.; Dalchiele, E.A. [Instituto de Fisica, Facultad de Ingenieria, Universidad de la Republica, J. H. Reissig 565, CC 30, CP 11000, Montevideo (Uruguay); Gellman, A.J. [Department of Chemical Engineering, Carnegie Mellon University, Pittsburgh PA 15213 (United States)

    2008-12-01

    Nanocrystalline zinc oxide films have been obtained by the sol-gel process. The films were deposited from precursor solutions by dip-coating on quartz substrates, and subsequently transformed into nanocrystalline pure or aluminium-doped ZnO films after a thermal treatment. The film microstructure and composition characterization was studied by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The optical properties were studied by transmittance spectroscopy. The water adsorption energy was measured by temperature programmed desorption (TPD) in the range 90-700 K. The optical transmittance in the UV region gives bandgap energy values of 3.27 eV for undoped samples, and higher than 3.30 eV for the Al-doped ones. The increase in bandgap energy in Al-doped samples may be explained by band-filling effects. The band edge absorption coefficient increases monotonically for the Al-doped samples but has a shoulder for the undoped ones, which may be assigned to room-temperature excitonic absorption.

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

    Science.gov (United States)

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

    2017-03-15

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

  8. Removal of dyes from water using chitosan hydrogel/SiO2 and chitin hydrogel/SiO2 hybrid materials obtained by the sol-gel method.

    Science.gov (United States)

    Copello, Guillermo J; Mebert, Andrea M; Raineri, M; Pesenti, Mariela P; Diaz, Luis E

    2011-02-15

    This work describes the synthesis of chitosan hydrogel/SiO(2) and chitin hydrogel/SiO(2) hybrid mesoporous materials obtained by the sol-gel method for their use as biosorbents. Their adsorption capabilities against four dyes (Remazol Black B, Erythrosine B, Neutral Red and Gentian Violet) were compared in order to evaluate chitin as a plausible replacement for chitosan considering its efficiency and lower cost. Both chitin and chitosan were used in the form of hydrogels. This allowed full compatibility with the ethanol release from tetraethoxysilane. The hybrid materials were characterized by Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR), Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), Nitrogen Adsorption Isotherms and (13)C solid-state Nuclear Magnetic Resonance. Adsorption experimental data were analyzed using Langmuir, Freundlich and Dubinin-Radushkevich isotherm models along with the evaluation of adsorption energy and standard free energy (ΔG(0)). The adsorption was observed to be pH dependent. The main mechanism of dye adsorption was found to be a spontaneous charge associated interaction, except for EB adsorption on chitin/SiO(2) matrix, which showed to involve a lower energy physical adsorption interaction. Aside from highly charged dyes the chitin containing matrix has similar or higher adsorption capacity than the chitosan one.

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

    DEFF Research Database (Denmark)

    Mikkelsen, Morten Bo Lindholm

    2011-01-01

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

  10. Fabrication and Microstructure of SiO2-GeO2 Sol-gel Glass Coatings

    Institute of Scientific and Technical Information of China (English)

    JING Cheng-bin; ZHAO Xiu-jian; TAO Hai-zhen; Wang Xi-na; LIU Ai-yun

    2003-01-01

    SiO2-GeO2 sols and gel glass coatings with different contents of germanium dioxide were fabricated.Stable and transparent sols could only be obtained when the content of GeO2 was under 35%.It is shown by SEM that only one continuous phase is observed in the coating of 65SiO2·35GeO2 and plenty of Ge,O and Si were all found in it.However,the separated phase is found in the coating of 60SiO2·40GeO2 and a large number of Ge and O.It is proved by the Raman scattering investigation that the separated phase in the coating of 60SiO2·40GeO2 is germanium dioxide.The congeries of hydrolystates of Cl3GeCH2CH2COOH play the main role in the formation of the separated phase when the proportion of GeO2 is much higher.Si-O-Ge,Si-O-Si,and Ge-O-Ge bonds form in the coating of 65SiO2·35GeO2 and this coating is homogenous.

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

    CERN Document Server

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

    2002-01-01

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

  12. Separation performance of cucurbit[7]uril in ionic liquid-based sol-gel coating as stationary phase for capillary gas chromatography.

    Science.gov (United States)

    Wang, Xiaogang; Qi, Meiling; Fu, Ruonong

    2014-12-05

    Here we report the separation performance of a new stationary phase of cucurbit[7]uril (CB7) incorporated into an ionic liquid-based sol-gel coating (CB7-SG) for capillary gas chromatography (GC). The CB7-SG stationary phase showed an average polarity of 455, suggesting its polar nature. Abraham system constants revealed that its major interactions with analytes include H-bond basicity (a), dipole-dipole (s) and dispersive (l) interactions. The CB7-SG stationary phase achieved baseline separation for a wide range of analytes with symmetrical peak shapes and showed advantages over the conventional polar stationary phase that failed to resolve some critical analytes. Also, it exhibited different retention behaviors from the conventional stationary phase in terms of retention times and elution order. Most interestingly, in contrast to the conventional polar phase, the CB7-SG stationary phase exhibited longer retentions for analytes of lower polarity but relatively comparable retentions for polar analytes such as alcohols and phenols. The high resolving ability and unique retention behaviors of the CB7-SG stationary phase may stem from the comprehensive interactions of the aforementioned interactions and shape selectivity. Moreover, the CB7-SG column showed good peak shapes for analytes prone to peak tailing, good thermal stability up to 280°C and separation repeatability with RSD values in the range of 0.01-0.11% for intra-day, 0.04-0.41% for inter-day and 2.5-6.0% for column-to-column, respectively. As demonstrated, the proposed coating method can simultaneously address the solubility problem with CBs for the intended purpose and achieve outstanding GC separation performance.

  13. Wood surface modification by in-situ sol-gel deposition of hybrid inorganic-organic thin films

    Science.gov (United States)

    Mandla A. Tshabalala; Li-Piin Sung

    2007-01-01

    Interest in the use of nanoparticles of iron, titanium, aluminum, and zinc oxides in transparent coatings for wood is increasing. Such nano-composite coatings have the potential of not only preserving the natural color of the wood, but also stabilizing the wood surface against the combined degradative effects of sunlight and moisture. The nanoparticles can be used as...

  14. Fabrication of mullite-bonded porous SiC ceramics from multilayer-coated SiC particles through sol-gel and in-situ polymerization techniques

    Science.gov (United States)

    Ebrahimpour, Omid

    In this work, mullite-bonded porous silicon carbide (SiC) ceramics were prepared via a reaction bonding technique with the assistance of a sol-gel technique or in-situ polymerization as well as a combination of these techniques. In a typical procedure, SiC particles were first coated by alumina using calcined powder and alumina sol via a sol-gel technique followed by drying and passing through a screen. Subsequently, they were coated with the desired amount of polyethylene via an in-situ polymerization technique in a slurry phase reactor using a Ziegler-Natta catalyst. Afterward, the coated powders were dried again and passed through a screen before being pressed into a rectangular mold to make a green body. During the heating process, the polyethylene was burnt out to form pores at a temperature of about 500°C. Increasing the temperature above 800°C led to the partial oxidation of SiC particles to silica. At higher temperatures (above 1400°C) derived silica reacted with alumina to form mullite, which bonds SiC particles together. The porous SiC specimens were characterized with various techniques. The first part of the project was devoted to investigating the oxidation of SiC particles using a Thermogravimetric analysis (TGA) apparatus. The effects of particle size (micro and nano) and oxidation temperature (910°C--1010°C) as well as the initial mass of SiC particles in TGA on the oxidation behaviour of SiC powders were evaluated. To illustrate the oxidation rate of SiC in the packed bed state, a new kinetic model, which takes into account all of the diffusion steps (bulk, inter and intra particle diffusion) and surface oxidation rate, was proposed. Furthermore, the oxidation of SiC particles was analyzed by the X-ray Diffraction (XRD) technique. The effect of different alumina sources (calcined Al2O 3, alumina sol or a combination of the two) on the mechanical, physical, and crystalline structure of mullite-bonded porous SiC ceramics was studied in the

  15. Adhesion of E. coli Bacteria Cells to Prosthodontic Alloys Surfaces Modified by TiO2 Sol-Gel Coatings

    Directory of Open Access Journals (Sweden)

    Katarzyna Banaszek

    2013-01-01

    Full Text Available The evaluation of the degree of bacteria E. coli adhesion to modified surfaces of the chosen prosthodontic alloys was presented. The study was carried out on Co-Cr (Wironit, Ni-Cr (Fantocer, and Fe-Cr-Ni (Magnum AN alloys. Bare substrate as a control and titanium dioxide coated samples were used. The samples were placed for 24 hours in bacterial culture medium. After incubation period, a number of bacterial cells were evaluated by scanning electron microscope. The study revealed that modification of the alloy surfaces by titanium dioxide coating significantly decreases the amount of bacteria adhering to the surfaces and that additionally bare metal alloy substrates have a different degree of susceptibility to bacterial adhesion.

  16. Sol-gel derived sorbents

    Science.gov (United States)

    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.

  17. Nanocrystalline sol-gel TiO{sub 2}-SnO{sub 2} coatings: Preparation, characterization and photo-catalytic performance

    Energy Technology Data Exchange (ETDEWEB)

    Kaleji, Behzad Koozegar [Department of Materials Engineering, Faculty of Engineering, Tarbiat Modares University, P.O. Box 14115-143, Tehran (Iran, Islamic Republic of); Sarraf-Mamoory, Rasoul, E-mail: rsarrafm@modares.ac.ir [Department of Materials Engineering, Faculty of Engineering, Tarbiat Modares University, P.O. Box 14115-143, Tehran (Iran, Islamic Republic of)

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer SnO{sub 2} additive enhanced significantly photo-catalytic properties of TiO{sub 2} based thin film for remove of organic compounds. Black-Right-Pointing-Pointer Structural and optical properties are dependent on dopant concentration. Black-Right-Pointing-Pointer TiO{sub 2}-SnO{sub 2} nanocrystalline thin film is promising for photocatalytic properties in visible light. -- Abstract: In this study, preparation of SnO{sub 2} (0-30 mol% SnO{sub 2})-TiO{sub 2} dip-coated thin films on glazed porcelain substrates via sol-gel process has been investigated. The effects of SnO{sub 2} on the structural, optical, and photo-catalytic properties of applied thin films have been studied by X-ray diffraction, Raman spectroscopy, and scanning electron microscopy. Surface topography and surface chemical state of thin films were examined by atomic force microscopy and X-ray photoelectron spectroscopy. XRD patterns showed an increase in peak intensities of the rutile crystalline phase by increasing the SnO{sub 2} content. The prepared Sn doped TiO{sub 2} photo-catalyst films showed optical absorption in the visible light area exhibited excellent photo-catalytic ability for the degradation of methylene blue under visible light irradiation. Best photo-catalytic activity of Sn doped TiO{sub 2} thin films was measured in the TiO{sub 2}-15 mol% SnO{sub 2} sample by the Sn{sup 4+} dopants presented substitution Ti{sup 4+} into the lattice of TiO{sub 2} increasing the surface oxygen vacancies and the surface hydroxyl groups.

  18. DLTS analysis of amphoteric interface defects in high-TiO2 MOS structures prepared by sol-gel spin-coating

    Science.gov (United States)

    Kumar, Arvind; Mondal, Sandip; Rao, K. S. R. Koteswara

    2015-11-01

    High-κ TiO2 thin films have been fabricated from a facile, combined sol - gel spin - coating technique on p and n type silicon substrate. XRD and Raman studies headed the existence of anatase phase of TiO2 with a small grain size of 18 nm. The refractive index `n' quantified from ellipsometry is 2.41. AFM studies suggest a high quality, pore free films with a fairly small surface roughness of 6 Å. The presence of Ti in its tetravalent state is confirmed by XPS analysis. The defect parameters observed at the interface of Si/TiO2 were studied by capacitance - voltage (C - V) and deep level transient spectroscopy (DLTS). The flat - band voltage (VFB) and the density of slow interface states estimated are - 0.9, - 0.44 V and 5.24×1010, 1.03×1011 cm-2; for the NMOS and PMOS capacitors, respectively. The activation energies, interface state densities and capture cross - sections measured by DLTS are EV + 0.30, EC - 0.21 eV; 8.73×1011, 6.41×1011 eV-1 cm-2 and 5.8×10-23, 8.11×10-23 cm2 for the NMOS and PMOS structures, respectively. A low value of interface state density in both P- and N-MOS structures makes it a suitable alternate dielectric layer for CMOS applications. And also very low value of capture cross section for both the carriers due to the amphoteric nature of defect indicates that the traps are not aggressive recombination centers and possibly can not contribute to the device operation to a large extent.

  19. Synthesis and characterization of ZnO:TiO2 nano composites thin films deposited on glass substrate by sol-gel spray coating technique

    Science.gov (United States)

    Sutanto, Heri; Nurhasanah, Iis; Hidayanto, Eko; Wibowo, Singgih; Hadiyanto

    2015-12-01

    In this work, (ZnO)x:(TiO2)1-x nano composites thin films, with x = 1, 0.75, 0.5, 0.25, and 0, have been prepared by sol-gel spray coating technique onto glass substrate. Pure TiO2 and ZnO thin films were synthesized from titanium isopropoxide-based and zinc acetate-based precursor solutions, respectively, whereas the composite films were obtained from the mixture of these solutions at the specific % vol ratios. The properties and performance of nano composite ZnO, TiO2 and ZnO:TiO2 thin films at different composition have been investigated. Ultraviolet - Visible (UV-Vis) Spectrophotometer and Scanning Electron Microscopy (SEM) were employed in order to get morphology and transmittance of thin films. Testing the ability of photocatalytic activity of obtained films was conducted on photodegradation of methylene blue (MB) dye and organic pollutants of wastewater under a 30 watt UV light irradiation, then testing BOD, COD and TPC were conducted. Using the Tauc model, the band-gap energy decreased from 3.12 eV to 3.02 eV for the sample with x = 1 and 0, respectively. This decrease occured along with the replacement of percentage of ZnO by TiO2 on the films. This decrease also reduced the minimum energy that required for electron excitation. Obtained thin films had nanoscale roughness level with range 3.64 to 17.30 nm. The film with x= 0 has the biggest removal percentage on BOD, COD and TPC mesurements with percentage 54.82%, 62.73% and 99.88%, respectively.

  20. Spectroscopic ellipsometry of Zn(1-x)Cu(x)O thin films based on a modified sol-gel dip-coating technique.

    Science.gov (United States)

    Al-Khanbashi, Hibah A; Shirbeeny, W; Al-Ghamdi, A A; Bronstein, Lyudmila M; Mahmoud, Waleed E

    2014-01-24

    Nanocrystalline Zn(1-x)Cu(x)O thin films (x=0, 0.01, 0.02, 0.03, 0.04 and 0.05) were synthesized by sol-gel dip-coating technique on a quartz substrate. These films were annealed at 350°C for 2 h. The X-ray diffraction showed a hexagonal crystal structure with high intensity peak for the (002) reflection plane indicating preferential growth along the c-axis of the crystal lattice. The peak position related to the (002) peak was shifted as a result of the copper ion incorporation, confirming the interstitial substitution of the zinc ions by the copper ions. This interstitial substitution leads to a decrease of an average crystallite size and lattice constants and an increase of the micro-strain up to 2 at.% of the copper amount. The surface morphology was explored by scanning electron microscopy which confirmed the homogenous distribution of nanoparticles in the deposited films along the quartz substrates. The energy dispersion X-ray spectroscopy revealed absence of impurities in the as-deposited films. The high resolution electron microscopy and selected area electron diffraction depicted that the films have polycrystalline nature. The film thickness and optical constants of the Zn(1-x)Cu(x)O thin films were estimated by fitting the spectroscopic ellipsometric data (ψ and Δ) using three different models. The refractive index was fitted using harmonic oscillator model from which the oscillator and the dispersive energies were found. The dielectric constant, dielectric loss, energy loss functions were also determined.

  1. Photoelectrochemical performance of Mn-TiO{sub 2} thin films mounted on FTO prepared by sol-gel spin coating

    Energy Technology Data Exchange (ETDEWEB)

    Chen, J.C.; Song, G.H. [National Central Univ., Taoyuan, Taiwan (China). Dept. of Mechanical Engineering; Lu, C.W. [Jen-Teh Junior College, Hou- Lung, Taiwan (China). Dept. of Information Management; Tseng, C.J. [National Central Univ., Chung-Li, Taoyuan County, Taiwan (China). Dept. of Mechanical Engineering; Cheng, K.W. [Chang Gung Univ., Tao-Yuan, Taiwan (China). Dept. of Chemical and Materials Engineering

    2009-07-01

    Tin oxide (TiO{sub 2}) sol-gels with Mn{sup 2+} molar ratios ranging from 0 to 0.1 per cent were used to form nano-structured Mn(x)Ti(1-x)O(2) thin films. A layer-by-layer spincoating (LLSC) technique was used, in which 10 very thin and uniform coating layers of Mn(x)Ti(1-x)O(2) were deposited on fluorine doped tin oxide (FTO) glass. Properties of the thin films were determined as a function of annealing temperature and molar ratio of the Mn{sup 2+} ions by X-ray diffraction (XRD), scanning electron microscopy (SEM), Atomic Force microscopy (AFM) and photoelectrochemical (PEC) measurements. The PEC measurements were obtained in a dry-type three-electrode cell consisting of sample, platinized and reference Ag/AgCl electrodes. The results revealed that the Mn(x)Ti(1-x)O(2) thin films have better structure and electrochemical characteristics when the annealing temperature is 550 degrees C. The TiO{sub 2} thin films with Mn{sup 2+} ions also had higher photocurrent than undoped TiO{sub 2}. The optimum Mn{sup 2+} loading in this study was found to be 0.1 ml per cent. The maximum photocurrent of Mn(0.1)Ti(0.9)O(2) thin films is about 0.68 mA/cm2 when the bias potential is 0.8 V (vs.Ag/AgCl).

  2. Determination of non-steroidal anti-inflammatory drugs in urine by hollow-fiber liquid membrane-protected solid-phase microextraction based on sol-gel fiber coating.

    Science.gov (United States)

    Sarafraz-Yazdi, Ali; Amiri, Amirhassan; Rounaghi, Gholamhossein; Eshtiagh-Hosseini, Hossein

    2012-11-01

    A new rapid, simple and effective cleanup procedure is demonstrated for the determination of ibuprofen, naproxen and diclofenac in urine samples by using hollow-fiber liquid membrane-protected solid-phase microextraction (HFLM-SPME) based on sol-gel technique and gas chromatography-flame ionization detector (GC-FID). In this technique, a sol-gel coated fiber was protected with a length of porous polypropylene hollow fiber membrane which was filled with water-immiscible organic phase. Subsequently the whole device was immersed into urine sample for extraction. Poly(ethylene glycol) (PEG) grafted onto multi-walled carbon nanotubes (PEG-g-MWCNTs) was used as extraction phase to prepare the sol-gel SPME fiber. Important parameters influencing the extraction efficiency such as desorption temperature and time, organic solvent, extraction temperature and time, pH, stirring speed and salt effect were investigated and optimized. Under the optimal conditions, the method detection limits (S/N=3) were in the range of 0.03-0.07ngmL(-1) and the limits of quantification (S/N=10) between 0.08 and 0.15ngmL(-1). Relative standard deviations for intra-day and inter-day precisions were 4.8-9.0% and 4.9-8.1%, respectively. Subsequently, the method was successfully applied to human urine fractions after administration of ibuprofen, naproxen and diclofenac.

  3. Sol-gel processing of ceramics

    OpenAIRE

    Schmidt, Helmut K.

    1991-01-01

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

  4. Sol-Gel Assembly and Luminescence of SiO2/PEMA Hybrid Material Incorporated with Terbium Complex

    Institute of Scientific and Technical Information of China (English)

    闫冰; 游佳勇

    2002-01-01

    Ethyl methacrylate (EMA) doped with luminescent ternary terbium complex (Tb(acac)3*dam) with acetylacetone (Hacac) and diantipylmethane (dam) was incorporated into the microporous silica gel. With the polymerization of EMA, the hybrid material containing Tb(acac)3*dam was obtained. The hybrid material exhibited good toughness and transparency and higher thermal stability than that of the pure complex and pure polymer matrix. In the range of doping concentration of Tb(acac)3*dam (0.05%, 0.1%, 0.2%, 0.5%, 1.0%, 2.0% and 5.0%), emission intensity increases with the increasing of corresponding doping concentration and concentration quenching effect has not taken place.

  5. Photochromic gratings in sol gel films containing diazo sulfonamide chromophore

    Science.gov (United States)

    Kucharski, Stanisław; Janik, Ryszard

    2005-09-01

    The photochromic sol-gel hybrid materials were prepared by incorporation of an azo chromophore containing sulfonamide fragment into polysiloxane cross-linked network. The materials were used to form transparent films on glass by spin-coating and/or casting. The reversible change of refraction index of the films on illumination with white light was observed by ellipsometry. The experiments with two beam coupling (TBC) and four wave mixing (4 WM) arrangement with green or blue laser beams as writing beams showed formation of a diffraction grating. The diffraction efficiency of the first order was 0.025-0.038 which yielded refraction index modulation in the range of up to 0.0066.

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

    Science.gov (United States)

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

    2015-10-01

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

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

    Science.gov (United States)

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

    2014-08-01

    Orthopedic injuries constitute the majority of wounds sustained by U.S. soldiers in recent conflicts. The risk of infection is considerable with fracture fixation devices. In this pilot study, we examined the use of unique bactericidal micron-thin sol-gel films on fracture fixation devices and their ability to prevent and eradicate infections. External fixation was studied with micron-thin sol-gel coated percutaneous pins releasing triclosan and inserted medially into rabbit tibiae. A total of 11 rabbits received percutaneous pins that were either uncoated or sol-gel/triclosan coated. Internal fracture fixation was also studied using sol-gel coated intramedullary (IM) nails releasing vancomycin in the intramedullary tibiae. Six sheep received IM nails that were coated with a sol-gel film that either contained vancomycin or did not contain vancomycin. All animals were challenged with Staphylococcus aureus around the implant. Animals were euthanized at 1 month postoperative. Rabbits receiving triclosan/sol-gel coated percutaneous pins did not show signs of infection. Uncoated percutaneous pins had a significantly higher infection rate. In the sheep study, there were no radiographic signs of osteomyelitis with vancomycin/sol-gel coated IM nails, in contrast to the observations in the control cohort. Hence, the nanostructured sol-gel controlled release technology offers the promise of a reliable and continuous delivery system of bactericidals from orthopedic devices to prevent and treat infection.

  8. Anticorrosive organic/inorganic hybrid coatings

    Science.gov (United States)

    Gao, Tongzhai

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

  9. Design and characterization of hybrid peptide sol-gel materials for the solid state induction of neuronal differentiation

    Science.gov (United States)

    Jedlicka, Sabrina S.

    2007-12-01

    Cell-based therapeutics are a rapidly growing area of research, with considerable promise in the treatment of neurological diseases. One of the primary limitations to neuronal cell-based devices is the necessity to maintain cells in an immature or undifferentiated state in culture prior to transplantation. In many cases, the undifferentiated cell does not express the desired characteristics for implantation. Biologically functional nanomaterials provide the ability to manipulate the direct extracellular environment surrounding cells; influencing their fate and differentiation path. The ability to engineer the interface between the cells and culture materials provides a repeatable, stable means of directing cells down a specific growth path determined by endogenous signaling pathways. This materials approach to cellular engineering can limit the need for added exogenous growth factors, "feeder" layers, or animal sera, in addition to creating a homogenous cell population for transplantation. In this work, hybrid peptide ormosil materials were developed; designed to mimic the developing mammalian brain during corticogenesis. These materials have been developed to enhance the GABAergic phenotype of P19 embryonic carcinoma cells and immature immortalized neurons. The ability to develop a homogenous, directed cell population has implications in stem cell research, regenerative medicine, cell-based devices and biosensing technology.

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

    Science.gov (United States)

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

    2011-07-01

    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.

  11. Sol-gel precursors and products thereof

    Science.gov (United States)

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

    2017-02-14

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

  12. Sol-gel precursors and products thereof

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-14

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

  13. 溶胶-凝胶法制备含氟聚丙烯酸酯/SiO2杂化材料%Study On Fluoro-Acrylate Polymer/SiO2 Hybrids Prepared by Sol-Gel Process

    Institute of Scientific and Technical Information of China (English)

    钱斯文; 吴文健; 王建方; 刘长利; 张学骜

    2008-01-01

    Silica sols were synthesized by an acid-catalyzed sol-gel process,and fluoro-acrylate polymer/SiO2 hybrid materials were prepared by silica sols in-situ polymerized with acrylate monomers.The structure,morphologies and surface chemical composition of the hybrid system was characterized by FT-IR,FESEM and XPS.It was found that in the hybrid system,SiO2 subsisted in networks,and covalent linked with organic components.The effects of morphology,distribution and interfacial conditions of inorganic disperse phase on the surface,thermal and mechanical properties of hybrids were investigated.The result showed that with the increase of SiO2 content,the water contact angle,thermal stability and hardness of the hybrids were enhanced,but the adhesion of the hybrid coatings increased firstly and then decreased.%用酸催化溶胶-凝胶法制得SiO2溶胶,与丙烯酸酯单体原位聚合,制备了含氟聚丙烯酸酯/SiO2杂化材料.通过红外光谱、场发射扫描电镜、X射线光电子能谱对杂化材料的结构、形态及表面化学组成进行了表征,表明SiO2在杂化体系中以Si-O网络的形式存在,并且与有机相之间有良好键合.并研究了SiO2相的形态、分布和界面状况对杂化材料的表面性能、热学性能和力学性能的影响.测试结果证实,随着SiO2含量的增加,杂化材料的疏水性、热稳定性和硬度都逐渐增强,附着力则是先增大后减小.

  14. Sol-gel derived ceramics

    OpenAIRE

    1990-01-01

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

  15. The Sol-Gel Process

    OpenAIRE

    Khalid Suliman Aboodh

    2015-01-01

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

  16. 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.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Mikosch, Annabel; Kuehne, Alexander J C

    2016-03-22

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

  18. Structural aspects and porosity features of nano-size high surface area alumina-silica mixed oxide catalyst generated through hybrid sol-gel route

    Energy Technology Data Exchange (ETDEWEB)

    Padmaja, P. [Ceramic Technology Division, Regional Research Laboratory (CSIR), Trivandrum 695019, Kerala (India)]. E-mail: padmavasudev@yahoo.com; Warrier, K.G.K. [Ceramic Technology Division, Regional Research Laboratory (CSIR), Trivandrum 695019, Kerala (India)]. E-mail: kgk_warrier@yahoo.com; Padmanabhan, M. [School of Chemical Sciences, Mahatma Gandhi University, Kottayam 686560, Kerala (India); Wunderlich, W. [Graduate School of Engineering, Nagoya Institute of Technology, 466-8555 Nagoya (Japan); Berry, F.J. [Department of Chemistry, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom); Mortimer, M. [Department of Chemistry, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom); Creamer, N.J. [Department of Chemistry, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom)

    2006-01-10

    Alumina-silica mixed oxide nano-catalyst materials with compositions 83.6 wt.% Al{sub 2}O{sub 3}-16.4 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.1SiO{sub 2}), 71.82 wt.% Al{sub 2}O{sub 3}-28.18 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.2SiO{sub 2}), 62.84 wt.% Al{sub 2}O{sub 3}-37.16 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.3SiO{sub 2}) and 56.03 wt.% Al{sub 2}O{sub 3}-43.97 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.4SiO{sub 2}) have been prepared by a hybrid sol-gel technique using boehmite as the precursor for alumina and tetraethoxysilane as that for silica. The bonding characteristics and coordination features around Al and Si in the mixed oxide catalysts have been studied using FTIR and {sup 27}Al MAS NMR after calcination at 400 deg. C which is the temperature region where cross-condensation is seen to take place. A high BET specific surface area of 287 m{sup 2} g{sup -1} is obtained for 3Al{sub 2}O{sub 3}.1SiO{sub 2} mixed oxide composition. The porosity features are further established by BET adsorption isotherms and pore size distribution analysis. The temperature-programmed desorption studies showed more surface active sites for the silica-rich composition, suggesting enhanced catalytic potential. The TEM features of the mixed oxides showed a homogeneous distribution of alumina and silica phases with particle sizes in the nano-range. The low silica-containing mixed oxide showed a needle-like morphology with a high aspect ratio of 1:50 and {approx}10 nm particle size while the silica-rich composition had particle size in a wide range ({approx}20-75 nm)

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

    Science.gov (United States)

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

    2017-02-27

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

  20. Process of forming a sol-gel/metal hydride composite

    Science.gov (United States)

    Congdon, James W.

    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.

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

    Science.gov (United States)

    Liu, Mingming; Zeng, Zhaorui; Fang, Huaifang

    2005-05-27

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

  2. Metal-silica sol-gel materials

    Science.gov (United States)

    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.

  3. Tri-layer antireflection coatings (SiO{sub 2}/SiO{sub 2}-TiO{sub 2}/TiO{sub 2}) for silicon solar cells using a sol-gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Lien, Shui-Yang; Wuu, Dong-Sing [Department of Materials Engineering, National Chung Hsing University, 250 Kuo Kuang Road, Taichung 402, Taiwan (Republic of China); Yeh, Wen-Chang [Department of Electronic Engineering, National Taiwan University of Science & amp; Technoogy, Taipei 106, Taiwan (Republic of China); Liu, Jun-Chin [Industrial Technology Research Institute, Photovoltaic and Optical Materials Research Laboratory, Chutung, Taiwan 310 (Republic of China)

    2006-10-16

    Antireflection coatings (ARCs) have become one of the key issues for mass production of Si solar cells. They are generally performed by vacuum processes such as thermal evaporation, reactive sputtering, and plasma-enhanced chemical vapor deposition. In this work, a sol-gel method has been demonstrated to prepare the ARCs for the non-textured monocrystalline Si solar cells. The spin-coated TiO{sub 2} single-layer, SiO{sub 2}/TiO{sub 2} double-layer and SiO{sub 2}/SiO{sub 2}-TiO{sub 2}/TiO{sub 2} triple-layer ARCs were deposited on the Si solar cells and they showed good uniformity in thickness. The measured average optical reflectance (400-1000nm) was about 9.3, 6.2 and 3.2% for the single-layer, double-layer and triple-layer ARCs, respectively. Good correlation between theoretical and experimental data was obtained. Under a triple-layer ARC condition, a 39% improvement in the efficiency of the monocrystalline Si solar cell was achieved. These indicate that the sol-gel ARC process has high potential for low-cost solar cell fabrication. (author)

  4. Synthesis of Titania Coated Alumina Particles by a Hybrid Sol-gel Method

    Science.gov (United States)

    2003-01-01

    anatase K’ (tetragonal, indexed according to JCPDS file 21- 1272) phase at 400’C. The anatase to rutile S... (tetragonal File 21-1276...transformation initiates at (a) about 600’C (or less) and both these phases coexist .... ...... till 800’C. The ratio of rutile : anatase phases, as a function of...integrated area of (110) rutile peak: (101) anatase peak was taken to be a measure of the rutile : anatase phase content. The dramatic anatase to

  5. Sol-gel electrochromic device

    OpenAIRE

    1994-01-01

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

  6. Polyvinylimidazole/sol-gel composite as a novel solid-phase microextraction coating for the determination of halogenated benzenes from aqueous solutions.

    Science.gov (United States)

    Farjaminezhad, Manoochehr; Saber Tehrani, Mohammad; Aberoomand Azar, Parviz; Hussain, Syed Waqif; Bohlooli, Shahab

    2014-06-01

    A polyvinylimidazole/sol-gel composite is proposed as a novel solid-phase microextraction fiber to extract five halobenzenes from the headspace of aqueous solutions in combination with gas chromatography with mass spectrometry. The prepared fiber was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The obtained results showed that porous polyvinylimidazole/sol-gel composite was chemically deposited on fused silica fiber. The effect of important extraction parameters including extraction temperature, extraction time, and salt content were investigated. The optimum conditions were as follows: extraction temperature 25°C, extraction time 20 min, and salt concentration 30 w/v%. Detection limits and relative standard deviations of the developed method for halogenated benzenes were below 0.1 pg/mL and 15%, respectively. Repeatability of the proposed method, explained by relative standard deviation, varied between 5.48 and 9.15% (n = 5). The limits of detection (S/N = 3) ranged between 0.01 and 0.10 ng/L using gas chromatography with mass spectrometry with selected ion monitoring mode. For real sample analysis, three types of water samples with different matrices (ground, surface, and tap water) were studied. The optimized procedure was applied to extraction and method validation of halogenated benzenes in spiked water samples.

  7. Determination of Aromatic Amines Using Solid-Phase Microextraction Based on an Ionic Liquid-Mediated Sol-Gel Technique.

    Science.gov (United States)

    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%.

  8. Polymer-functionalized single-walled carbon nanotubes as a novel sol-gel solid-phase micro-extraction coated fiber for determination of poly-brominated diphenyl ethers in water samples with gas chromatography-electron capture detection.

    Science.gov (United States)

    Zhang, Weiya; Sun, Yin; Wu, Caiying; Xing, Jun; Li, Jianying

    2009-04-15

    Single-walled carbon nanotubes (SWNTs) were functionalized with a hydroxyl-terminated silicone oil (TSO-OH). It is synthesized by the reactions of carbonyl chloride groups on the surface of SWNTs and hydroxyl groups of silicone oil (TSO-OH). The functionalized product SWNTs-TSO-OH was first used as precursor and selective stationary phase to prepare the sol-gel derived poly(SWNTs-TSO-OH) solid-phase microextraction (SPME) fiber for determination of polybrominated diphenyl ethers (PBDEs) in water samples. The possible major reaction of the sol-gel coating process was discussed and confirmed by IR spectra, Raman spectroscopy, and scanning electron microscopy. Some parameters of SPME fiber for the determination of PBDEs were investigated by headspace SPME/gas chromatography with electron-capture detection (HS-SPME/GC-ECD). Compared with the commercial SPME fiber, the new coated fiber showed higher extraction efficiency to PBDEs, better thermal stability (over 340 degrees C), and longer life span (over 200 times). All of these advantages are mainly due to the incorporation of SWNTs, which enhanced the pi-pi interaction with PBDEs and increased the surface area of extraction in contact with the sample. Moreover, the sol-gel coating technology additionally provided the porous structure of the 3-D silica network and the strong chemical binding provided which also will improve the extraction efficiency. Under optimized conditions, the method detection limits for seven PBDEs were 0.08-0.8 ng/L (S/N = 3) and the precision (RSD, n = 5) was 2.2-7.5% at the 50 ng/L level. The linearity of the developed method is in the range of 5-500 ng/L with coefficients of correlation greater than 0.995. The developed method was successfully applied for the analysis of trace PBDEs in reservoir water and wastewater samples. The recoveries obtained at spiking 50 ng/L were between 74% and 109% (n = 5) for PBDEs in water samples.

  9. Sol-gel zirconia coating capillary microextraction on-line hyphenated with inductively coupled plasma mass spectrometry for the determination of Cr, Cu, Cd and Pb in biological samples.

    Science.gov (United States)

    Wu, Yiwei; Hu, Bin; Jiang, Zucheng; Feng, Yuqi; Lu, Peng; Li, Boyangzi

    2006-01-01

    A sol-gel zirconia coating was developed for the preconcentration/separation of trace Cr, Cu, Cd and Pb by capillary microextraction, and the adsorbed analytes were on-line eluted for detection using inductively coupled plasma mass spectrometry (ICP-MS). By immobilizing sol-gel zirconia on the inner surface of a fused-silica capillary, the sol-gel zirconia coating was simply prepared. Its adsorption properties, stability and the factors affecting the adsorption behaviors of Cr, Cu, Cd and Pb were investigated in detail. In the pH range from 7.8 to 10, the zirconia-coated capillary (35 cm x 0.15 mm) is selective towards Cr, Cu, Cd and Pb, and the analyzed ions could be desorbed quantitatively with 0.2 mL of 0.5 mol/L HNO(3) at a rate of 0.2 mL/min. With a consumption of 1.25 mL sample solution, an enrichment factor of 6.25, and detection limits (3sigma) of 9.9 pg/mL Cr, 17.9 pg/mL Cu, 4.5 pg/mL Cd and 3.7 pg/mL Pb were obtained. The precisions for nine replicate measurements of 1 ng/mL Cr, Cu, Cd and Pb were 4.9% Cr, 2.2% Cu, 2.0% Cd and 3.2% Pb (RSD), respectively. The proposed procedure has been applied to the determination of Cr, Cu, Cd and Pb in human urine, which was subjected to microwave-assisted digestion prior to analysis, and the recoveries for these elements were 89.2-101.8%. In order to validate the developed procedure, a NIES No.10-a Rice Flour-Unpolished certified reference material and a BCR No. 184 Bovine Muscle certified reference material were analyzed, and the results are in good agreement with the certified values. Copyright (c) 2006 John Wiley & Sons, Ltd.

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

    Institute of Scientific and Technical Information of China (English)

    张浩; 王笛

    2013-01-01

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

  11. Annealing temperature effect on the properties of mercury-doped TiO{sub 2} films prepared by sol-gel dip-coating technique

    Energy Technology Data Exchange (ETDEWEB)

    Mechiakh, R., E-mail: raouf_mechiakh@yahoo.fr [Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar Batna, Batna (Algeria); Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia); Ben Sedrine, N. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia); Karyaoui, M. [Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar Batna, Batna (Algeria); Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia); Chtourou, R. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche et des Technologies de l' Energie (CRTEn), BP. 95, Hammam-Lif 2050 (Tunisia)

    2011-04-15

    This work presents the annealing temperature effect on the properties of mercury (Hg)-doped titanium dioxide (TiO{sub 2}). Thin films and polycrystalline powders have been prepared by sol-gel process. The structure, surface morphology and optical properties, as a function of the annealing temperature, have been studied by atomic force microscopy (AFM), Raman, reflectance and ellipsometric spectroscopies. In order to determine the transformation points, we have analyzed the xerogel-obtained powder by differential scanning calorimetry (DSC). Raman spectroscopy shows the crystalline anatase and rutile phases for the films annealed at 400 deg. C and 1000 deg. C respectively. The AFM surface morphology results indicate that the particle size increases from 14 to 57 nm by increasing the annealing temperature. The complex index and the optical band gap (E{sub g}) of the films were determined by the spectroscopic ellipsometry analysis. We have found that the optical band gap decreases by increasing the annealing temperature.

  12. 以sol-gel技术制备太阳能减反射涂层%Solar antireflective coating made with sol-gel technology

    Institute of Scientific and Technical Information of China (English)

    雷振宇

    2009-01-01

    着重介绍了sol-gel(熔胶-凝胶)技术大面积、工业化制备高硬度、耐摩擦太阳能减反射涂层的意义、原理和方法,并从其作为商品工业化的角度,介绍了SiO2单层膜系和TiO2-SiO2双层膜系太阳能减反射涂层生产工艺、设备及环境要求等,给出了部分商业化减反射涂层的性能特征等技术参数.

  13. Neutron detector based on lithiated sol-gel glass

    CERN Document Server

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

    2002-01-01

    A neutron detector technology is demonstrated based on sup 6 Li/ sup 1 sup 0 B doped sol-gel glass. The detector is a sol-gel glass film coated silicon surface barrier detector (SBD). The ionized charged particles from (n, alpha) reactions in the sol-gel film enter the SBD and are counted. Data showing that gamma-ray pulse amplitudes interfere with identifying charged particles that exit the film layer with energies below the gamma-ray energy is presented. Experiments were performed showing the effect of sup 1 sup 3 sup 7 Cs and sup 6 sup 0 Co gamma rays on the SBD detector. The reaction product energies of the triton and alpha particles from sup 6 Li are significantly greater than the energies of the Compton electrons from high-energy gamma rays, allowing the measurement of neutrons in a high gamma background. The sol-gel radiation detection technology may be applicable to the characterization of transuranic waste, spent nuclear fuel and to the monitoring of stored plutonium.

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

    Science.gov (United States)

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

    2016-07-01

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

  15. Effect of Silica Nanoparticles on Performance of Sol-Gel Coatings%SiO2纳米粒子对溶胶凝胶涂层性能的影响

    Institute of Scientific and Technical Information of China (English)

    刘建华; 王强; 于美; 李松梅; 詹中伟; 章骏; 王邈

    2012-01-01

    在高强钢表面制备了防护性溶胶凝胶涂层,并研究了不同浓度二氧化硅纳米粒子的加入对于涂层形貌、耐蚀性和硬度的影响.采用扫描电子显微镜(SEM)和电子能谱(EDS)观察了涂层的微观结构和成分;采用显微硬度计测试了涂层的硬度;采用电化学方法研究了二氧化硅纳米粒子的浓度对于涂层耐蚀性能的影响;采用傅里叶红外光谱研究涂层的化学结构,进而探讨了二氧化硅纳米粒子对于涂层的强化机理.结果显示涂层加入二氧化硅纳米粒子的最佳浓度为500 mg.L-1,此条件下的涂层表面均匀致密,有较高的硬度并且在3.5% NaCl溶液中体现出较好的耐蚀作用.纳米粒子在溶胶中反应形成活性羟基基团并与硅烷发生反应生成空间网状结构,从而强化涂层.%Sol-gel coatings for corrosion protection were fabricated on high strength steel 30CrMnSiA. The effect of silica nanoparticles on performance of sol-gel coatings was studied. The morphology and chemical composition of the coatings were investigated by using scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS), respectively. The hardness of the coatings was tested by using microscopic hardness meters. The corrosion resistance of the coatings was studied by electrochemical impedance spectroscopy (EIS) during immersion in 3.5% NaCl solution. Fourier transform infrared spectroscopy (FTIR) was used to study the chemical structure of the coatings. The results demonstrate that the optimal concentration of silica nanoparticles is 500 mg · L-1, under which the coatings are of the best performance with uniform surface, dense structure, high hardness and excellent corrosion resistance. The doped silica nanoparticles generate active hydroxyl groups in the sol, form covalent bonds with the coating matrix, and thus strengthen the coatings.

  16. Facile Sol-Gel/Spray-Drying Synthesis of Interweaved Si@TiO2&CNTs Hybrid Microsphere as Superior Anode Materials for Li-Ion Batteries

    Science.gov (United States)

    Wang, Jiyun; Hou, Xianhua; Li, Yana; Ru, Qiang; Qin, Haiqing; Hu, Shejun

    2016-11-01

    A unique intertwined structure of silicon-based composite (Si@TiO2&CNTs) has been synthesized by sol-gel and spray drying methods. The Si@TiO2&CNTs is mainly composed of three kinds of materials:the prepared nanosilicon particles, TiO2, and carbon nanotubes (CNTs). A layer of TiO2 particles is found effective for enhancing the electrical conductivity and structure stability of the silicon particles. Additionally, the twisted CNTs are beneficial to build a better conductive network, consequently improving the anode working conditions when the cell is charged or discharged. As a lithium ion battery anode, a specific capacity of approximately 1521 mAh g-1 after 100 cycles is obtained.

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

    Science.gov (United States)

    Huang, Honghua; Yan, Bing

    2006-04-01

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

  18. Novel Thiol-Ene Hybrid Coating for Metal Protection

    Directory of Open Access Journals (Sweden)

    Mona Taghavikish

    2016-04-01

    Full Text Available A novel hybrid anticorrosion coating with dual network of inorganic (Si–O–Si and organic bonds (C–S–C was prepared on metal through an in situ sol-gel and thiol-ene click reaction. This novel interfacial thin film coating incorporates (3-mercaptopropyl trimethoxysilane (MPTS and 1,4-di(vinylimidazolium butane bisbromide based polymerizable ionic liquid (PIL to form a thiol-ene based photo-polymerized film, which on subsequent sol-gel reaction forms a thin hybrid interfacial layer on metal surface. On top of this PIL hybrid film, a self-assembled nanophase particle (SNAP coating was employed to prepare a multilayer thin film coating for better corrosion protection and barrier performance. The novel PIL hybrid film was characterised for structure and properties using Fourier transform infrared spectroscopy (FTIR, differential scanning calorimetry (DSC, and thermogravimetric analysis (TGA. The corrosion protection performance of the multilayer coating was examined using potentiodynamic polarization and electrochemical impedance spectroscopy (EIS. The results reveal that this novel double layer coating on metal offers excellent protection against corrosion and has remarkably improved the barrier effect of the coating.

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

    Science.gov (United States)

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

    2003-11-01

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

  20. The characteristic of carbon-coated LiFePO{sub 4} as cathode material for lithium ion battery synthesized by sol-gel process in one step heating and varied pH

    Energy Technology Data Exchange (ETDEWEB)

    Triwibowo, J., E-mail: joko.triwibowo@lipi.go.id [Research Center for Physics LIPI, Kawasan PUSPIPTEK Serpong (Indonesia); Yuniarti, E.; Suharyadi, E. [Gadjah Mada University, Faculty of Mathematics and Natural Sciences, Sekip Utara Yogyakarta (Indonesia)

    2014-09-25

    This research has been done on the synthesis of carbon coated LiFePO{sub 4} through sol-gel process. Carbon layer serves for improving electronic conductivity, while the variation of pH in the sol-gel process is intended to obtain the morphology of the material that may improve battery performance. LiFePO{sub 4}/C precursors are Li{sub 2}CO{sub 3}, NH{sub 4}H{sub 2}PO{sub 4} and FeC{sub 2}O{sub 4}.H{sub 2}O and citric acid. In the synthesis process, consisting of a colloidal suspension FeC{sub 2}O{sub 4}.H{sub 2}O and distilled water mixed with a colloidal suspension consisting of NH{sub 4}H{sub 2}PO{sub 4}, Li{sub 2}CO{sub 3}, and distilled water. Variations addition of citric acid is used to control the pH of the gel formed by mixing two colloidal suspensions. Sol in this study had a pH of 5, 5.4 and 5.8. The obtained wet gel is further dried in the oven and then sintered at a temperature 700°C for 10 hours. The resulting material is further characterized by XRD to determine the phases formed. The resulting powder morphology is observed through SEM. Specific surface area of the powder was tested by BET, while the electronic conductivity characterized with EIS.

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

    Science.gov (United States)

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

    2011-07-01

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

  2. Fabrication and application of mesoporous TiO2 film coated on Al wire by sol-gel method with EISA

    Science.gov (United States)

    Zhao, Linkang; Lu, Jianjun

    2017-04-01

    Mesoporous TiO2 film on Al wire was fabricated by sol-gel method with evaporation induced self assembly (EISA) process using F127 as templating agent in the mixed solution of ethanol and Tetra-n-butyl Titanate. The Ni/TiO2 film catalyst supported on Al wire was prepared by impregnation and the catalytic performance on methanation was carried out in a titanium alloy micro-reactor tube. It was shown that anatase mesoporous TiO2 film was prepared in this conditions (1 g F127,calcined at 400 °C and aged for 24 h), which has specific surface area of 127 m2 g-1 and narrow pore size distribution of 5.3 nm. Low calcined temperature (300 °C) cannot transfer film to anatase and decompose F127 completely. Ni/TiO2 film on Al wire catalyst was proved to be active in CO methanation reaction. And the CO conversion reaches 99% and CH4 selectivity close is to 80% when the reaction temperature is higher 360 °C.

  3. Nanocrystalline sol-gel Nb{sub 2}O{sub 5} coatings. Preparation, characterisation and application to photovoltaic cell, lithium battery and eletrochromic device

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Yeping

    2002-07-01

    Thick and thin films of Nb{sub 2}O{sub 5} have been prepared by the sol-gel process using cheap niobium pentachloride as precursor and a new synthesis route. The microstructure of the films was tailored by adding poly(ethylene glycol) (PEG) and carbon soot into the sol and varying the sintering temperature. The thesis describes the properties of the sols and their influence on the properties of the resulting nanocrystalline Nb{sub 2}O{sub 5} films as electrodes in dye sensitised solar cells, electrochromic devices and rechargeable lithium batteries. A solar light-to-electric conversion efficiency of Ru(II) sensitised Nb{sub 2}O{sub 5} solar cell as high as 7% under 120 W/m{sup 2} illumination was obtained. An equivalent electric circuit of the dye sensitised electrode/electrolyte interface based on the electrochemical impedance spectroscopy was modelled and found to fit all the results. The values obtained for the electric elements from the simulation of the results were found to relate material parameters to the cell performance and their influence on the cell performance are illustrated. The electrochromism and Li{sup +}-charge and discharge of the Nb{sub 2}O{sub 5} films exhibited also good performance. (orig.)

  4. Fabrication and electrical resistivity of Mo-doped VO2 thin films coated on graphite conductive plates by a sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Choi, W.; Jung, H.M.; Um, S. [Hanyang Univ., Seoul (Korea, Republic of). School of Mechanical Engineering

    2008-07-01

    Vanadium oxides (VO2) can be used in optical devices, thermochromic smart windows and sensors. This paper reported on a study in which vanadium pentoxide (V2O5) powder was prepared and mixed with Molybdenum Oxides (MoO3) to form Mo-doped and -undoped VO2 thin films by a sol-gel method on graphite conductive substrates. The micro-structure and chemical compositions of the Mo-doped and -undoped VO2 thin films was investigated using X-Ray diffraction and scanning electron microscopy. Changes in electrical resistivity were measured as a function of the stoichiometric compositions between vanadium and molybdenum. In this study. Mo-doped and -undoped VO2 thin films showed the typical metal to insulator transition (MIT), where temperature range could be adjusted by modifying the dopant atomic ratio. The through-plane substrate structure of the Mo-doped layer influences the electrical resistivity of the graphite substrate. As the amount of the molybdenum increases, the electrical resistivity of the graphite conductive substrate decreases in the lower temperature range below the freezing point of water. The experimental results showed that if carefully controlled, thermal dissipation of VO2 thin films can be used as a self-heating source to melt frozen water with the electrical current flowing through the graphite substrate. 3 refs., 3 figs.

  5. A solid phase microextraction coating based on ionic liquid sol-gel technique for determination of benzene, toluene, ethylbenzene and o-xylene in water samples using gas chromatography flame ionization detector.

    Science.gov (United States)

    Sarafraz-Yazdi, Ali; Vatani, Hossein

    2013-07-26

    Ionic liquid mediated sol-gel sorbents for head-space solid phase microextraction (HS-SPME) were developed for the extraction of benzene, toluene, ethylbenzene and o-xylene (BTEX) compounds from water samples in ultra-trace levels. The analytes were subsequently analyzed with gas chromatography coupled to flame ionization detector (GC-FID). Three different coating fibers were prepared including: poly(dimethylsiloxane) (PDMS), coating prepared from poly(dimethylsiloxane) in the presence of ionic liquid as co-solvent and conditioned at a higher temperature than decomposition temperature of ionic liquid (PDMS-IL-HT) and coating prepared from poly(dimethylsiloxane) in the presence of ionic liquid as co-solvent and conditioned at a lower temperature than decomposition temperature of ionic liquid (PDMS-IL-LT). Prepared fibers demonstrate many advantages such as high thermal and chemical stabilities due to the chemical bonding of the coatings with the silanol groups on the fused-silica surface fiber. These fibers have shown long life time up to 180 extractions. The scanning electron micrographs of the fibers surfaces revealed that addition of ionic liquid into the sol solution during the sol-gel process increases the fiber coating thickness, affects the form of fiber structure and also leaves high pores in the fiber surface that cause high surface area and therefore increases sample capacity of the fibers. The important parameters that affect the extraction efficiency are desorption temperature and time, sample volume, extraction temperature, extraction time, stirring speed and salt effect. Therefore these factors were investigated and optimized. Under optimal conditions, the dynamic linear range with PDMS-IL-HT, PDMS and PDMS-IL-LT fibers were 0.3-200,000; 50-200,000 and 170-150,000pgmL(-1) and the detection limits (S/N=3) were 0.1-2 and 15-200 and 50-500pgmL(-1), and limit of quantifications (S/N=10) were 0.3-8 and 50-700 and 170-1800, respectively. The relative

  6. Caffeine electrochemical sensor using imprinted film as recognition element based on polypyrrole, sol-gel, and gold nanoparticles hybrid nanocomposite modified pencil graphite electrode.

    Science.gov (United States)

    Rezaei, Behzad; Khalili Boroujeni, Malihe; Ensafi, Ali A

    2014-10-15

    In the present study, a novel sensitive and selective nanocomposite imprinted electrochemical sensor for the indirect determination of caffeine has been prepared. The imprinted sensor was fabricated on the surface of pencil graphite electrode (PGE) via one-step electropolymerization of the imprinted polymer composed of conductive polymer, sol-gel, gold nanoparticles (AuNPs), and caffeine. Due to such combination like the thin film of molecularly imprinted polymer (MIP) with specific binding sites, the sensor responded quickly to caffeine. AuNPs were introduced for the enhancement of electrical response by facilitating charge transfer processes of [Fe(CN)6](3-)/[Fe(CN)6](4-) which was used as an electrochemical active probe. The fabrication process of the sensor was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Several important parameters controlling the performance of the sensor were investigated and optimized. The imprinted sensor has the advantages of high porous surface structure, inexpensive, disposable, excellent stability, good reproducibility and repeatability. The linear ranges of the MIP sensor were in the range from 2.0 to 50.0 and 50.0 to 1000.0 nmol L(-1), with the limit of detection (LOD) of 0.9 nmol L(-1) (S/N=3). Furthermore, the proposed method was successfully intended for the determination of caffeine in real samples (urine, plasma, tablet, green tea, energy and soda drink).

  7. Elaboration et caractérisation d'un vernis antireflet sol-gel innovant pour application dans les systèmes d'écrans embarqués en aéronautique

    OpenAIRE

    Boudot, Mickael

    2014-01-01

    Low refractive index hydrophobic antireflective coatings were synthetized as mesoporous nanometric thin silica films by use of sol gel chemistry coupled with the dip coating process on thermo sensitive polymeric substrates such as poly(methyl methacrylate) (PMMA) and cellulose triacetate (TAC). Thin films of pure and hybrid silica were stiffened by ammonia vapor treatment (AVT) at room temperature. Optical, mechanical and chemical stability of those coatings were optimized and the AVT-induced ...

  8. Magnetization of microorganism cells by sol-gel method

    Institute of Scientific and Technical Information of China (English)

    CHEN Bo; ZHAN TianZhuo; LIAN ZhiYang; ZHANG DeYuan

    2008-01-01

    Microorganism cells could be used as templates during fabrication of magnetic or conductive microstructures in different standard shapes.In this paper,feasibility of magnetizing microorganism cells by sol-gel method,which is to coat cells of Spirulina (a type of natural micro-helical microorganism) with the ferrite (a kind of magnetic material),was discussed and investigated.Then the cell form,compo-nents and the phase structure were observed and analyzed using various tools including optical microscopy,scanning electron microscopy (SEM),energy dis-persive X-ray detector (EDX),transmission electron microscopy (TEM),and X-ray diffraction analysis (XRD).Results showed that spirulina cells could be coated with ferrite after the sol-gel process,with the shape of natural helixes well kept,that the components of different sampling points on the surface layer were consistent and the thickness of layer was uniform,and that the type of the surface ferrite layer formed was cubic Fe304.It was also observed that there were nano-parUcles yielded in the cells and certain deposit on the walls between cells.The kinetics of the cell magnetization technology by sol-gel was also discussed.

  9. Magnetization of microorganism cells by sol-gel method

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Microorganism cells could be used as templates during fabrication of magnetic or conductive microstructures in different standard shapes. In this paper, feasibility of magnetizing microorganism cells by sol-gel method, which is to coat cells of Spirulina (a type of natural micro-helical microorganism) with the ferrite (a kind of magnetic material), was discussed and investigated. Then the cell form, components and the phase structure were observed and analyzed using various tools including optical microscopy, scanning electron microscopy (SEM), energy dispersive X-ray detector (EDX), transmission electron microscopy (TEM), and X-ray diffraction analysis (XRD). Results showed that spirulina cells could be coated with ferrite after the sol-gel process, with the shape of natural helixes well kept, that the components of different sampling points on the surface layer were consistent and the thickness of layer was uniform, and that the type of the surface ferrite layer formed was cubic Fe3O4. It was also observed that there were nano-particles yielded in the cells and certain deposit on the walls between cells. The kinetics of the cell magnetization technology by sol-gel was also discussed.

  10. Preparation and rapid analysis of antibacterial silver, copper and zinc doped sol-gel surfaces.

    Science.gov (United States)

    Jaiswal, Swarna; McHale, Patrick; Duffy, Brendan

    2012-06-01

    The colonisation of clinical and industrial surfaces with microorganisms, including antibiotic-resistant strains, has promoted increased research into the development of effective antibacterial and antifouling coatings. This study describes the preparation of metal nitrate (Ag, Cu, Zn) doped methyltriethoxysilane (MTEOS) coatings and the rapid assessment of their antibacterial activity using polyproylene microtitre plates. Microtitre plate wells were coated with different volumes of liquid sol-gel and cured under various conditions. Curing parameters were analysed by thermogravimetric analysis (TGA) and visual examination. The optimum curing conditions were determined to be 50-70°C using a volume of 200 μl. The coated wells were challenged with Gram-positive and Gram-negative bacterial cultures, including biofilm-forming and antibiotic-resistant strains. The antibacterial activities of the metal doped sol-gel, at equivalent concentrations, were found to have the following order: silver>zinc>copper. The order is due to several factors, including the increased presence of silver nanoparticles at the sol-gel coating surface, as determined by X-ray photoelectron spectroscopy, leading to higher elution rates as measured by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The use of microtitre plates enabled a variety of sol-gel coatings to be screened for their antibacterial activity against a wide range of bacteria in a relatively short time. The broad-spectrum antibacterial activity of the silver doped sol-gel showed its potential for use as a coating for biomaterials.

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

    Science.gov (United States)

    Uchiyama, Hiroaki; Matsui, Tadayuki; Kozuka, Hiromitsu

    2015-11-17

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

  12. Influence of calcinated and non calcinated nanobioglass particles on hardness and bioactivity of sol-gel-derived TiO2-SiO2 nano composite coatings on stainless steel substrates.

    Science.gov (United States)

    Dadash, Mohammad Saleh; Karbasi, Saeed; Esfahani, Mojtaba Nasr; Ebrahimi, Mohammad Reza; Vali, Hojatollah

    2011-04-01

    Thick films of calcinated and non calcinated nanobioglass (NBG)-titania composite coatings were prepared on stainless steel substrates by alkoxide sol-gel process. Dip-coating method was used for the films preparation. The morphology, structure and composition of the nano composite films were evaluated using environmental scanning electron microscope, X-ray diffraction and Fourier transform infrared spectroscope. The SEM investigation results showed that prepared thick NBG-titania films are smooth and free of macrocracking, fracture or flaking. The grain size of these films was uniform and nano scale (50-60 nm) which confirmed with TEM. Also FTIR confirmed the presence of Si-O-Si bands on the calcinated NBG-titania films. The hardness of the prepared films (TiO(2)-calcinated NBG and TiO(2)-Non calcinated NBG) was compared by using micro hardness test method. The results verified that the presence of calcinated NBG particles in NBG-titania composite enhanced gradually the mechanical data of the prepared films. The in vitro bioactivity of these films was discussed based on the analysis of the variations of Ca and P concentrations in the simulated body fluid (SBF) and their surface morphologies against immersion time. Surface morphology and Si-O-Si bands were found to be of great importance with respect to the bioactivity of the studied films. The results showed that calcinated NBG-titania films have better bioactivity than non calcinated NBG-titania films.

  13. Fabrication of sulfonated poly(ether ether ketone)-based hybrid proton-conducting membranes containing carboxyl or amino acid-functionalized titania by in situ sol-gel process

    Science.gov (United States)

    Yin, Yongheng; Xu, Tao; He, Guangwei; Jiang, Zhongyi; Wu, Hong

    2015-02-01

    Functionalized titania are used as fillers to modify the sulfonated poly(ether ether ketone) (SPEEK) membrane for improved proton conductivity and methanol barrier property. The functionalized titania sol which contains proton conductive carboxylic acid groups or amino acid groups are derived from a facile chelation method using different functional additives. Then the novel SPEEK/carboxylic acid-functionalized titania (SPEEK/TC) and SPEEK/amino acid-functionalized titania (SPEEK/TNC) hybrid membranes are fabricated via in situ sol-gel method. The anti-swelling property and thermal stability of hybrid membranes are enhanced owing to the formation of electrostatic force between SPEEK and titania nanoparticles. The hybrid membranes exhibit higher proton conductivity than plain SPEEK membrane because more proton transfer sites are provided by the functionalized titania nanoparticles. Particularly, the proton conductivity of SPEEK/TNC membrane with 15% filler content reaches up to 6.24 × 10-2 S cm-1, which is 3.5 times higher than that of the pure SPEEK membrane. For methanol permeability, the SPEEK/TNC membranes possess the lowest values because the acid-base interaction between sulfonic acid groups in SPEEK and amino groups in functionalized titania leads to a more compact membrane structure.

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

    Science.gov (United States)

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

    2016-01-01

    Sol-gel processing is an attractive method for large-scale surface coating due to its facile and inexpensive preparation, even with the inclusion of precision nanotopographies. These are desirable traits for metal orthopaedic prostheses where ceramic coatings are known to be osteoinductive and the effects may be amplified through nanotexturing. However there are a few concerns associated with the application of sol-gel technology to orthopaedics. Primarily, the annealing stage required to transform the sol-gel into a ceramic may compromise the physical integrity of the underlying metal. Secondly, loose particles on medical implants can be carcinogenic and cause inflammation so the coating needs to be strongly bonded to the implant. These concerns are addressed in this paper. Titanium, the dominant material for orthopaedics at present, is examined before and after sol-gel processing for changes in hardness and flexural modulus. Wear resistance, bending and pull tests are also performed to evaluate the ceramic coating. The findings suggest that sol-gel coatings will be compatible with titanium implants for an optimum temperature of 500 °C.

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

    Directory of Open Access Journals (Sweden)

    Zhong-Min Wang

    2017-02-01

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

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

    Science.gov (United States)

    Allhusen, John S; Conboy, John C

    2013-11-27

    RuO2 conductive thin films were synthesized using the sol-gel method and deposited onto transparent insulating substrates. The optical transmission, film thickness, surface morphology and composition, resistivity, and spectroelectrochemical performance have been characterized. The optical transmission values of these films ranged from 70 to 89% in the visible region and from 56 to 88% in the infrared region. Resistivity values of the RuO2 sol-gel films varied from 1.02 × 10(-3) to 1.13 Ω cm and are highly dependent on the initial solution concentration of RuO2 in the sol-gel. The RuO2 sol-gel films were used as electrodes for the electrochemical oxidation and reduction of ferrocenemethanol. The electrochemical behavior of our novel RuO2 sol-gel films was compared to that of a standard platinum disk electrode and showed no appreciable differences in the half-wave potential (E1/2). The mechanical and chemical stability of the coatings was tested by physical abrasion and exposure to highly acidic, oxidizing Piranha solution. Repeated exposure to these extreme conditions did not result in any appreciable decline in electrochemical performance. Finally, the use of the novel RuO2 sol-gel conductive and transparent films was demonstrated in a spectroelectrochemistry experiment in which the oxidation and reduction of ferrocenemethanol was monitored via UV-vis spectroscopy as the applied potential was cycled.

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

    Science.gov (United States)

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

    2016-03-01

    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.

  18. Removal of dyes from water using chitosan hydrogel/SiO{sub 2} and chitin hydrogel/SiO{sub 2} hybrid materials obtained by the sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Copello, Guillermo J. [Catedra de Quimica Analitica Instrumental, Facultad de Farmacia y Bioquimica, Universidad de Buenos Aires (UBA), Junin 956, C1113AAD Buenos Aires (Argentina); IQUIMEFA (UBA-CONICET), Junin 956, C1113AAD Buenos Aires (Argentina); Mebert, Andrea M.; Raineri, M.; Pesenti, Mariela P. [Catedra de Quimica Analitica Instrumental, Facultad de Farmacia y Bioquimica, Universidad de Buenos Aires (UBA), Junin 956, C1113AAD Buenos Aires (Argentina); Diaz, Luis E., E-mail: ldiaz@ffyb.uba.ar [Catedra de Quimica Analitica Instrumental, Facultad de Farmacia y Bioquimica, Universidad de Buenos Aires (UBA), Junin 956, C1113AAD Buenos Aires (Argentina); IQUIMEFA (UBA-CONICET), Junin 956, C1113AAD Buenos Aires (Argentina)

    2011-02-15

    This work describes the synthesis of chitosan hydrogel/SiO{sub 2} and chitin hydrogel/SiO{sub 2} hybrid mesoporous materials obtained by the sol-gel method for their use as biosorbents. Their adsorption capabilities against four dyes (Remazol Black B, Erythrosine B, Neutral Red and Gentian Violet) were compared in order to evaluate chitin as a plausible replacement for chitosan considering its efficiency and lower cost. Both chitin and chitosan were used in the form of hydrogels. This allowed full compatibility with the ethanol release from tetraethoxysilane. The hybrid materials were characterized by Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR), Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), Nitrogen Adsorption Isotherms and {sup 13}C solid-state Nuclear Magnetic Resonance. Adsorption experimental data were analyzed using Langmuir, Freundlich and Dubinin-Radushkevich isotherm models along with the evaluation of adsorption energy and standard free energy ({Delta}G{sup 0}). The adsorption was observed to be pH dependent. The main mechanism of dye adsorption was found to be a spontaneous charge associated interaction, except for EB adsorption on chitin/SiO{sub 2} matrix, which showed to involve a lower energy physical adsorption interaction. Aside from highly charged dyes the chitin containing matrix has similar or higher adsorption capacity than the chitosan one.

  19. Effect of calcinations temperature on microstructures, photocatalytic activity and self-cleaning property of TiO2 and SnO2/TiO2 thin films prepared by sol-gel dip coating process

    Science.gov (United States)

    Sangchay, Weerachai

    2014-06-01

    The purpose of this research was to study the effect of calcinations temperature on phase transformation, crystallite size, morphology, photocatalytic activity and self-cleaning properties of TiO2 and SnO2/TiO2 thin films. The thin films were preparation by sol-gel dip coating process and calcinations at the temperature of 500 °C, 600 °C and 700 °C for 2 h with the heating rate of 10 °C/mim. The microstructures of the fabricated thin films were characterized by XRD and SEM techniques. The photocatalytic activity of the thin films was also tested via the degradation of methylene blue solution under UV irradiation. Finally, self-cleaning properties of thin films were evaluated by measuring the contact angle of water droplet on the thin films with and without UV irradiation. It was found that SnO2/TiO2 thin films calcinations at the temperature of 500 °C shows the highest of photocatalytic activity and self-cleaning properties.

  20. Effect of annealing treatment on electrical and optical properties of Nb doped TiO2 thin films as a TCO prepared by sol-gel spin coating method

    Science.gov (United States)

    Fallah, Milad; Zamani-Meymian, Mohammad-Reza; Rahimi, Rahmatollah; Rabbani, Mahboubeh

    2014-10-01

    Anatase niobium doped TiO2 thin films (Ti0.94Nb0.06O2) were prepared on quartz substrates by sol-gel spin coating technique and various initial concentrations ([Ti + Nb] in the solution) of 0.1 M and 0.4 M. All the films dried at 100 °C and then the annealing treatment performed by three different procedures. The influence of different annealing processes and total metal concentrations was studied on crystallinity, transparency, conductivity and morphology of thin films by XRD, EDX, FT-IR and UV-vis transmittance spectroscopy, four point probe, AFM and SEM images. It was found that two-step annealing procedure under vacuum is a more proper way to increase the conductivity of TNO thin films compared to one-step annealing process. Two-step method exhibited the minimum resistivity of 4.4 Ω cm and the transparency of about 50% in the visible region with 36 nm thickness.

  1. Fabrication and characterization of a diluted magnetic semiconducting TM co-doped Al:ZnO (TM=Co, Ni) thin films by sol-gel spin coating method.

    Science.gov (United States)

    Siddheswaran, R; Mangalaraja, R V; Tijerina, Eduardo P; Menchaca, J-Luis; Meléndrez, M F; Avila, Ricardo E; Jeyanthi, C Esther; Gomez, M E

    2013-04-01

    Effect of transition metal oxides (TM=Co and Ni) co-doping on the crystallinity, surface morphology, grain growth and magnetic properties of nanostructure Al:ZnO thin films has been studied for diluted magnetic semiconductor applications. Al:ZnO thin films were fabricated by sol-gel spin coating on p-type Si (100) substrates. Fabrication of hexagonal wurtzite TM co-doped Al:ZnO thin films having thickness 2μm was successfully achieved. The Raman spectra of the TM co-doped Al:ZnO thin films showed a broad vibrational mode in the range 520-540cm(-1) due to crystal defects created co-doping elements in the ZnO host lattice. Scanning electron microscopy (SEM) revealed that the films are composed of uniform size, polycrystalline dense ZnO particles with defect free, smooth surfaces. The surface roughness was further verified with atomic force microscopy (AFM). The energy dispersive X-ray spectroscopic analysis (EDX) confirmed the stoichiometric compositions of the TM co-doped Al:ZnO films. The magnetic measurements exhibited that the Co, Al:ZnO and Ni, Al:ZnO thin films were ferromagnetic at room temperature.

  2. Synthesis and characterization of Ca{sub 3}Co{sub 4}O{sub 9} thin films prepared by sol-gel spin-coating technique on Al{sub 2}O{sub 3}(001)

    Energy Technology Data Exchange (ETDEWEB)

    Moubah, R. [Institut de Physique et Chimie des Materiaux de Strasbourg (IPCMS), UMR 7504 UDS-CNRS (UDS-ECPM), 23 rue du Loess, BP 43, F-67034 Strasbourg Cedex 2 (France); Colis, S., E-mail: silviu.colis@ipcms.u-strasbg.f [Institut de Physique et Chimie des Materiaux de Strasbourg (IPCMS), UMR 7504 UDS-CNRS (UDS-ECPM), 23 rue du Loess, BP 43, F-67034 Strasbourg Cedex 2 (France); Leuvrey, C.; Schmerber, G.; Drillon, M.; Dinia, A. [Institut de Physique et Chimie des Materiaux de Strasbourg (IPCMS), UMR 7504 UDS-CNRS (UDS-ECPM), 23 rue du Loess, BP 43, F-67034 Strasbourg Cedex 2 (France)

    2010-06-01

    Ca{sub 3}Co{sub 4}O{sub 9} thin films are deposited on Al{sub 2}O{sub 3}(001) substrates using a sol-gel spin-coating process. X-ray diffraction shows that the film exhibits a single phase of Ca{sub 3}Co{sub 4}O{sub 9} with the (00l) planes parallel to the film surface. The temperature dependence of magnetic susceptibility showed as expected the existence of two magnetic transitions similar to those observed in bulk samples: a ferrimagnetic and a spin-state transition around 19 and 375 K, respectively. At 5 K the magnetization curves along the c-axis of the Al{sub 2}O{sub 3}(001) show that the remanent magnetization and coercive field are close to those obtained for films grown by pulsed laser deposition, which evidences the interest to use such an easy technique to grow complex thin films oxides.

  3. Influences of the iron ion (Fe{sup 3+})-doping on structural and optical properties of nanocrystalline TiO{sub 2} thin films prepared by sol-gel spin coating

    Energy Technology Data Exchange (ETDEWEB)

    Ben Naceur, J. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Mechiakh, R., E-mail: raouf_mechiakh@yahoo.fr [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia); Departement de Medecine, Faculte de Medecine, Universite Hadj Lakhdar, Batna (Algeria); Bousbih, F.; Chtourou, R. [Laboratoire de Photovoltaique de Semi-conducteurs et de Nanostructures, Centre de Recherche des Sciences et Technologies de l' Energie, BP.95, Hammam-Lif 2050 (Tunisia)

    2011-10-01

    Titanium dioxide (TiO{sub 2}) thin films doping of various iron ion (Fe{sup 3+}) concentrations were deposited on silicon (Si) (100) and quartz substrates by sol-gel Spin Coating technique followed by a thermal treatment at 600 deg. C. The structure, surface morphology and optical properties, as a function of the doping, have been studied by X-ray diffractometer (XRD), Raman, ultraviolet-visible (UV-vis) and Spectroscopic Ellipsometry (SE). XRD and Raman analyzes of our thin films show that the crystalline phase of TiO{sub 2} thin films comprised only the anatase TiO{sub 2}, but the crystallinity decreased when the Fe{sup 3+} content increased from 0% to 20%. During the Fe{sup 3+} addition to 20%, the phase of TiO{sub 2} thin film still maintained the amorphous state. The grain size calculated from XRD patterns varies from 29.3 to 22.6 nm. The complex index and the optical band gap (E{sub g}) of the films were determined by the spectroscopic ellipsometry analysis. We have found that the optical band gap decreased with an increasing Fe{sup 3+} content.

  4. Recubrimientos de hidroxiapatita preparados mediante un proceso sol-gel

    Directory of Open Access Journals (Sweden)

    Peón, E.

    2005-12-01

    Full Text Available Hydroxyapatite coatings (HAp have been obtained starting from precursors of sol-gel type. The coatings previously oxidized were deposited on metal surfaces of a based on iron alloy so-called MA956. The alloys were at high temperatures, in order to improve the adhesion with the hydroxyapatite coatings. The sol-gel coating was obtained applying an aqueous route, using triethyl phosphite and aqueous calcium nitrate, as precursors of phosphorous and calcium, respectively. Different sintering thermal treatments were applied on the resulting gels in order to obtain a homogeneous, adherent and crystalline hydroxyapatite coating. The characterization techniques used for this study were optical microscopy, SEM/EDX, XDR and FTIR. Moreover, the adhesion between the hydroxylapatite coating and the substrate was assessed according to the ASTM D 3359-02 standard test method. The results of this study showed that the best thermal treatment is obtained for a sintering temperature of 550 °C during a time of 72 h.

    Se han preparado nuevos recubrimientos de hidroxiapatita (HAp obtenidos a partir de precursores de tipo sol-gel, depositados sobre sustratos metálicos de una aleación de base hierro denominada MA956, previamente oxidados a elevadas temperaturas, para mejorar la adherencia con los recubrimientos de hidroxiapatita. El recubrimiento sol-gel se obtuvo aplicando una ruta acuosa, utilizando como precursores del fósforo y del calcio trietilfosfito y nitrato cálcico tetrahidratado, respectivamente. Sobre los geles resultantes se aplicaron distintos tratamientos térmicos de sinterización, hasta la obtención de recubrimientos de hidroxiapatita homogéneos, adherentes y cristalinos. Las técnicas de caracterización utilizadas para realizar este estudio han sido microscopía óptica, MBE/EDX, DRX y FTIR. Así mismo, se ha determinado la adherencia entre el substrato y el recubrimiento de hidroxiapatita según la norma ASTM D 3359-02. Los resultados

  5. Sol-gel synthesis of lithium aluminate

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-02-01

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

  6. Super magnetic nanoparticles NiFe2O4, coated with aluminum-nickel oxide sol-gel lattices to safe, sensitive and selective purification of his-tagged proteins.

    Science.gov (United States)

    Mirahmadi-Zare, Seyede Zohreh; Allafchian, Alireza; Aboutalebi, Fatemeh; Shojaei, Pendar; Khazaie, Yahya; Dormiani, Kianoush; Lachinani, Liana; Nasr-Esfahani, Mohammad-Hossein

    2016-05-01

    Super magnetic nanoparticle NiFe2O4 with high magnetization, physical and chemical stability was introduced as a core particle which exhibits high thermal stability (>97%) during the harsh coating process. Instead of multi-stage process for coating, the magnetic nanoparticles was mineralized via one step coating by a cheap, safe, stable and recyclable alumina sol-gel lattice (from bohemite source) saturated by nickel ions. The TEM, SEM, VSM and XRD imaging and BET analysis confirmed the structural potential of NiFe2O4@NiAl2O4 core-shell magnetic nanoparticles for selective and sensitive purification of His-tagged protein, in one step. The functionality and validity of the nickel magnetic nanoparticles were attested by purification of three different bioactive His-tagged recombinant fusion proteins including hIGF-1, GM-CSF and bFGF. The bonding capacity of the nickel magnetics nanoparticles was studied by Bradford assay and was equal to 250 ± 84 μg Protein/mg MNP base on protein size. Since the metal ion leakage is the most toxicity source for purification by nickel magnetic nanoparticles, therefor the nickel leakage in purified final protein was determined by atomic absorption spectroscopy and biological activity of final purified protein was confirmed in comparison with reference. Also, in vitro cytotoxicity of nickel magnetic nanoparticles and trace metal ions were investigated by MTS assay analysis. The results confirmed that the synthesized nickel magnetic nanoparticles did not show metal ion toxicity and not affected on protein folding.

  7. Fully compatible magneto-optical sol-gel material with glass waveguides technologies: application to mode converters

    Science.gov (United States)

    Royer, François; Jamon, Damien; Broquin, Jean-Emmanuel; Amata, Hadi; Kekesi, Renata; Neveu, Sophie; Blanc-Mignon, Marie-Françoise; Ghibaudo, Elise

    2011-01-01

    To overcome the difficult problem of the integration of magneto-optical materials with classical technologies, our group has developped a composite magneto-optical material made of a hybrid organic-inorganic silica type matrix doped by magnetic nanoparticles. Thin films of this material are obtained through a soft chemistry sol-gel process which gives a full compatibility with an integration on glass substarte. Due to an interesting magneto optical activity (Faraday rotation of 310°/cm) several magneto-optical functionnalities have been realized. A thin film of such composite material coated on a pyrex™ substrate acts as non-reciprocal TE/TM mode converter. An hybrid stucture made of a composite film coated on an ion-exchanged glass waveguide has been realized with a good propagation of light through a hybrid mode. Finally, the sol gel process has been adapted in order to obtain 3D inverse opals which should behave as magnetophotonic crystals. Transmittance curves reveal the photonic band gap of such opals doped with magnetic nanoparticles.

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

    Science.gov (United States)

    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.

  9. Sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as a new dispersive solid-phase extraction material for acrylamide determination in food with direct gas chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Omar, Mei Musa Ali; Wan Ibrahim, Wan Aini; Elbashir, Abdalla Ahmed

    2014-09-01

    A sol-gel hybrid sorbent, methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was successfully used as new dispersive solid phase extraction (dSPE) sorbent material in the determination of acrylamide in several Sudanese foods and analysis using GC-MS. Several important dSPE parameters were optimised. Under the optimised conditions, excellent linearity (r(2)>0.9998) was achieved using matrix matched standard calibration in the concentration range 50-1000 μg kg(-1). The limits of detection (LOD) and limit of quantification ranged from 9.1 to 12.8 μg/kg and 27.8-38.9 μg/kg, respectively. The precision (RSD%) of the method was ⩽6.6% and recoveries of acrylamide obtained were in the range of 88-103%, (n=3). The LOD obtained is comparable with the LODs of primary secondary amine dSPE. The proposed MTMOS-TEOS dSPE method is direct and safe for acrylamide analysis, showed reliable method validation performances and good cleanup effects. It was successfully applied to the analysis of acrylamide in real food samples.

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

    OpenAIRE

    Avés,E. P.; Galván, J. C.; I.R. Lima; Granjeiro, J.M.; Bastos, I. N.; Soares, G. D.

    2008-01-01

    O recobrimento de ligas metálicas com cerâmicas bioativas visa acelerar a formação óssea ao redor do implante, contribuindo para a sua estabilização. Neste trabalho estudou-se a fase cerâmica de hidroxiapatita depositada pelo processo sol-gel em chapas da liga metálica Ti-6Al-4V. A camada de recobrimento foi caracterizada por microscopia eletrônica de varredura, por difração de raios X e sua adesão ao substrato foi avaliada pelo teste de cisalhamento O teste de citocompatibilidade mostrou que...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1992-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Kueper, T.W.

    1992-05-01

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

  13. 溶胶-凝胶法包覆储氢材料MgH2的性能研究%Study on the Properties of Hydrogen Storage Material MgH2 Coated by Sol-gel Method

    Institute of Scientific and Technical Information of China (English)

    程扬帆; 颜事龙; 马宏昊; 沈兆武

    2015-01-01

    为解决MgH2型水解敏化储氢乳化炸药的发泡过程难以有效控制及后效问题,提高MgH2的贮存稳定性,采用溶胶-凝胶法用石蜡和硬脂酸对 MgH2进行包覆,制备了石蜡和硬脂酸包覆的 MgH2。用扫描电镜对包覆膜的微观结构进行表征,并根据猛度实验结果选择石蜡作为最终包覆材料,对石蜡包覆的 Mg H 2进行防水实验和抗氧化EDS测试。利用水下爆炸实验研究了石蜡包覆的 Mg H 2与乳化基质的相容性和贮存稳定性。结果表明,石蜡膜具有优良的防水性能,但其抗氧化性能不佳,石蜡包覆的 Mg H 2复合敏化乳化炸药的贮存性能符合要求。%In order to solve the controlling and aftereffect problem in foaming process of MgH2 hydrolysis sensitized emulsion explosive,and improve the storage stability of MgH2 ,the hydrogen storage material MgH2 was coated by sol-gel method,and paraffin wax and octadecanoic acid coated MgH2 were produced respectively.The micro structures of the coating films were characterized by scanning electron microscope,and paraffin wax was determined as the final coating material through the brisance experiment.Water resistance and oxidation resistance abilities of the paraffin wax coated MgH2 were tested.The compatability and storagestability of paraffin wax coated MgH2 and emulsion matrix were studied by underwater explosion test.The results show that the paraffin wax film has good water resistance ability,while the oxidation resistance ability is poor.The stability of emulsion explosive sensitized by paraffin wax coated MgH2 meets the requirement.

  14. Synthesis of lithium doped zinc oxide by sol gel

    Science.gov (United States)

    MEZIANE, K.; ELHICHOU, A.; ELHAMIDI, A.; ALMAGGOUSSI, A.; CHHIBA, M.

    2016-10-01

    Li-doped ZnO thin films were prepared by sol-gel method and deposed on glass substrate using spin coating technique. The effects of Li on structural and optical properties were investigated. The X-ray diffraction (XRD) analysis reveals that Li incorporation leads to the great improvement of the crystalline quality of ZnO thin films. Scanning electron microscopy (SEM) images showed that nanowires are aligned nearly perpendicular to the substrate plane and are affected significantly by Li incorporation. The optical transmission of the films was higher than 80% in the visible region. It is found that the optical gap and the refractive index remain practically constant.

  15. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    Science.gov (United States)

    Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna

    1992-01-01

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

  16. Biocompatible Nb2O5 thin films prepared by means of the sol-gel process.

    Science.gov (United States)

    Velten, D; Eisenbarth, E; Schanne, N; Breme, J

    2004-04-01

    Thin biocompatible oxide films with an optimised composition and structure on the surface of titanium and its alloys can improve the implant integration. The preparation of these thin oxide layers with the intended improvement of the surface properties can be realised by means of the sol-gel process. Nb2O5 is a promising coating material for this application because of its extremely high corrosion resistance and thermodynamic stability. In this study, thin Nb2O5 layers ( TiO2 sol-gel coated cp-titanium concerning the spreading of cells, collagen I synthesis and wettability.

  17. Optical sensing of HCl with phenol red doped sol-gels

    Energy Technology Data Exchange (ETDEWEB)

    Wang Enju [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States)]. E-mail: wange@stjohns.edu; Chow, Kwok-Fan [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Wang Wenqun [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Wong, Crystal [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Yee, Cynthia [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Persad, Alvin [Department of Chemistry, St. John' s University, 8000 Utopia Parkway, Jamaica, NY 11439 (United States); Mann, Jonathan [Department of Chemistry, Princeton University, Princeton, NJ 08540 (United States); Bocarsly, Andrew [Department of Chemistry, Princeton University, Princeton, NJ 08540 (United States)

    2005-04-08

    A dye doped sol-gel for the sensing of hydrochloric acid in solution and/or gaseous phase is described. The sol-gel is obtained by acidic hydrolysis of tetraethoxysilane (TEOS) and phenyltriethoxysilane (Ph-TriEOS) in the presence of phenol red (PR) and further spin-coating onto glass slides. The sensitive response is based on an increase of the absorption band at 510 nm of phenol red entrapped in the sol-gel casting when exposed to HCl solution or gas, due to protonation of the dye. The detection limit of the sol-gel response to moisturized gaseous HCl is below 12 ppm, and its response to HCl in solution falls in the range of 0.01-6 M. The sol-gel coating has a response time of less than 40 s in steady-state, and life-time of more than a year. Weak acids such as acetic acid, benzoic acid, salicylate acid, citrate acid, and carbonic acid do not interfere the response. The responses in acid solutions are completely reversible. In the gaseous phase, response of HCl appears to be moisture sensitive.

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

    Science.gov (United States)

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

    1994-09-01

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

  19. Morphological characterization of Al2O3 membrane fabricated by sol-gel dip-coating method%溶胶-凝胶浸渍法制备氧化铝膜的形貌表征

    Institute of Scientific and Technical Information of China (English)

    徐占锋; 张良苗; 陈念贻; 陆文聪; 张振; 吴祖燊

    2006-01-01

    Alumina membranes without pinholes and cracks were prepared by the sol-gel process using ammonium aluminium sulphate as the starting material. The effects of different preparing conditions on morphology characteristics of the membrane were investigated by scanning electron microscopy and 3D rotational microscopy. The preparing conditions include the amounts of drying control chemical additives (DCCA), sintering procedure and sol-gel concentration. The results showed that PVA is a good crack-preventing reagent and the morphology of supported membranes was affected by many factors, including Al2O3 concentration, PVA/Al2O3 ratio, heating rate,membrane thickness and intrinsic defects of the substrate surface.

  20. Optical, photocatalytical and structural properties of TiO2 – SiO2 sol-gel coatings on high content SiO2 enamel surface

    Directory of Open Access Journals (Sweden)

    Kaspars Mālnieks

    2015-03-01

    Full Text Available TiO2 – SiO2 films deposited on enamel surface were investigated for self - cleaning applications. The TiO2 – SiO2 optical films prepared from a sol–gel precursor were deposited on enamel surface using dip - coating techniques. Films were calcined different time from one hour till ten hours to investigate effect of calcination on self-cleaning and structural properties. Effects of film crystal structure, microstructure, photocatalytic activity and optical properties of the films were investigated using XRD, AFM and spectrophotometer and contact angle measurement. The TiO2 – SiO2 dip - coating optical films calcined 1 h resulted in high structured surfaces, which found to increase the photocatalytic activity.DOI: http://dx.doi.org/10.5755/j01.ms.21.1.5188

  1. OPTICAL PROPERTIES OF Al:ZnO THIN FILM DEPOSITED BY DIFFERENT SOL-GEL TECHNIQUES: ULTRASONIC SPRAY PYROLYSIS AND DIP-COATING

    Directory of Open Access Journals (Sweden)

    Ebru Gungor

    2016-08-01

    Full Text Available Undoped and Al-doped ZnO polycrystalline thin films have been fabricated on glass substrates by using a computer-controlled dip coating (DC and ultrasonic spray pyrolysis (USP systems. The film deposition parameters of DC process were optimized for the samples. In this technique, the substrate was exposed to temperature gradient using a tube furnace. In the study, the other solvent-based technique was conventional USP. The zinc salt and Al salt concentrations in the solution were kept constant as 0.1 M and 2% of Zn salt’s molarity, respectively. The optical properties were compared for the films deposited two different techniques. The optical transmission of Al:ZnO/Glass/Al:ZnO sample dip coated and  the optical transmission of Al:ZnO/Glass sample ultrasonically sprayed were determined higher than 80% in the visible and near infrared region. Experimental optical transmittance spectra of the films in the forms of FilmA/Glass/FilmA and FilmA/glass were used to determine the optical constants. It was observed that the optical band gaps of Al doped ZnO films onto glass substrate were increases with increase of Al content and the absorption edge shifted to the shorter wavelength (blue shift compared with the undoped ZnO thin film.

  2. Synthesis and characterization of erbium-doped SiO{sub 2}-TiO{sub 2} thin films prepared by sol-gel and dip-coating techniques onto commercial glass substrates as a route for obtaining active GRadient-INdex materials

    Energy Technology Data Exchange (ETDEWEB)

    Gómez-Varela, Ana I. [Microoptics and GRIN Optics Group, Department of Applied Physics, Faculty of Optics and Optometry and Faculty of Physics, Universidade de Santiago de Compostela, Campus Vida s/n, Santiago de Compostela E-15782 (Spain); Castro, Yolanda, E-mail: castro@icv.csic.es [Instituto de Cerámica y Vidrio (CSIC), Kelsen 5, Campus de Cantoblanco, Madrid 28049 (Spain); Durán, Alicia [Instituto de Cerámica y Vidrio (CSIC), Kelsen 5, Campus de Cantoblanco, Madrid 28049 (Spain); De Beule, Pieter A.A. [Applied Nano-Optics Laboratory, International Iberian Nanotechnology Laboratory, Braga 4715-330 (Portugal); Flores-Arias, María T. [Microoptics and GRIN Optics Group, Department of Applied Physics, Faculty of Optics and Optometry and Faculty of Physics, Universidade de Santiago de Compostela, Campus Vida s/n, Santiago de Compostela E-15782 (Spain); Bao-Varela, Carmen, E-mail: carmen.bao@usc.es [Microoptics and GRIN Optics Group, Department of Applied Physics, Faculty of Optics and Optometry and Faculty of Physics, Universidade de Santiago de Compostela, Campus Vida s/n, Santiago de Compostela E-15782 (Spain)

    2015-05-29

    In this work, SiO{sub 2}-TiO{sub 2} films doped with erbium were prepared by dip-coating sol-gel process onto commercial glass substrates. The surface morphology of the films was characterized using atomic force microscopy, while thickness, refractive index, extinction coefficient and porosity of the films were determined by ellipsometric measurements in a wavelength region of 400-1000 nm. Optical constants and porosity were found to vary with erbium concentration. The proof of principle presented in this paper is applicable to systems of different nature by tailoring the sol-gel precursors in such a way that active GRadient-INdex media described by a complex, parabolic-like refractive index distribution for beam shaping purposes is obtained. - Highlights: • Sol-gel route for preparation of active GRadient-INdex materials is proposed. • SiO{sub 2}-TiO{sub 2} films doped with erbium were prepared by dipping onto commercial glasses. • Morphological and optical characterization of the samples was performed. • Optical constants and porosity were found to vary with erbium concentration. • Refractive index diminishes with dopant content; the contrary occurs for porosity.

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

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    Şadan Özden

    2016-01-01

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

  5. Transparent multi-level resistive switching phenomena observed in ITO/RGO/ITO memory cells by the sol-gel dip-coating method.

    Science.gov (United States)

    Kim, Hee-Dong; Yun, Min Ju; Lee, Jae Hoon; Kim, Kyoeng Heon; Kim, Tae Geun

    2014-04-09

    A reduced graphene oxide (RGO)-based transparent electronic memory cell with multi-level resistive switching (RS) was successfully realized by a dip-coating method. Using ITO/RGO/ITO structures, the memory device exhibited a transmittance above 80% (including the substrate) in the visible region and multi-level RS behavior in the 00, 01, 10, and 11 states by varying the pulse height from 2 V to 7 V. In the reliability test, the device exhibited a good endurance of over 10(5) cycles and a long data retention of over 10(5) s at 85°C in each state. We believe that the RGO-based transparent memory presented in this work could be a milestone for future transparent electronic devices.

  6. Optimisation of a sol-gel synthesis route for the preparation of MgF2 particles for a large scale coating process.

    Science.gov (United States)

    Scheurell, K; Noack, J; König, R; Hegmann, J; Jahn, R; Hofmann, Th; Löbmann, P; Lintner, B; Garcia-Juan, P; Eicher, J; Kemnitz, E

    2015-12-07

    A synthesis route for the preparation of optically transparent magnesium fluoride sols using magnesium acetate tetrahydrate as precursor is described. The obtained magnesium fluoride sols are stable for several months and can be applied for antireflective coatings on glass substrates. Reaction parameters in the course of sol synthesis are described in detail. Thus, properties of the precursor materials play a crucial role in the formation of the desired magnesium fluoride nanoparticles, this is drying the precursor has to be performed under defined mild conditions, re-solvation of the dried precursor has to be avoided and addition of water to the final sol-system has to be controlled strictly. Important properties of the magnesium fluoride sols like viscosity, particle size distribution, and structural information are presented as well.

  7. Sol-Gel Derived Nanocomposites

    OpenAIRE

    2007-01-01

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

  8. TiO{sub 2} Coated Core-Shell Nanoparticles Fabricated through Sol-Gel Reaction of Titanium Precursor on Surface of Silica Core Templates

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Suk Bon [Korea Hydro and Nuclear Power Co. Ltd., Daejeon (Korea, Republic of)

    2015-10-15

    TiO{sub 2} hollow capsules have been mainly investigated through various methods using soft and hard templates such as polymer latex and silica nanoparticles (NPs). However, fabrication of these materials inevitably involves the removal process of polymer latex and silica template used through calcination at high temperature and etching with toxic etchants, respectively. As a result, these processes result in the generation of chemical waste as well as serious environmental concerns. To overcome above mentioned problems, although studies on in situ recrystallization transformation of silica into more useful functional nanostructured silica materials such as microporous zeolites or mesoporous silicas instead of removal of the silica templates were reported in recent, the additional process, including hydrothermal reaction and calcination at high temperature in the removal of the organic templates used is required to fabricate these materials. Resulting TiO{sub 2} coated core-shell NPs showed a smooth surface and uniform TiO{sub 2} shell layer. TiO{sub 2} shell layer after the calcination processes at high temperature under air flowing exhibited the crystal structure corresponding to the anatase phase. The formation of the TiO{sub 2} shell layer on the surface of the silica core templates was investigated through the various analyses. TiO{sub 2} shell layer after the calcination treatment at high temperature exhibited the anatase phase with a crystal size of ca. 5.37 nm. Resulting TiO{sub 2} coated core-shell NPs can be utilized as a photocatalyst.

  9. Photoanodic properties of sol-gel-derived iron oxide thin films with embedded gold nanoparticles: effects of polyvinylpyrrolidone in coating solutions

    Energy Technology Data Exchange (ETDEWEB)

    Hida, Yoshihiro [Department of Materials Science and Engineering, Kansai University, 3-3-35 Yamate-cho, Suita 564-8680 (Japan); Kozuka, Hiromitsu [Department of Materials Science and Engineering, Kansai University, 3-3-35 Yamate-cho, Suita 564-8680 (Japan)]. E-mail: kozuka@ipcku.kansai-u.ac.jp

    2005-04-08

    Fe{sub 2}O{sub 3} thin films containing dispersed Au nanoparticles were prepared on nesa silica glass substrates, using Fe(NO){sub 3}.9H{sub 2}O-HAuCl{sub 4}.4H{sub 2}O-CH{sub 3}COCH{sub 2}COCH{sub 3}-CH{sub 3}OC{sub 2}H{sub 4}OH solutions containing polyvinylpyrrolidone (PVP). The photoanodic properties were studied in a three-electrode cell with the film sample as the working electrode and an aqueous buffer solution of pH=7 as the supporting electrolyte. The Au particles increased photoanodic quantum efficiency at wavelengths <500-600 nm. Quantum efficiency was further increased by modifying the microstructure of the film electrodes through the addition of PVP. The maximum incident photon to current efficiency (IPCE) of about 20% was achieved in an Au-dispersed film prepared from a solution containing PVP. PVP in coating solutions provided the fired films with an increase in size of the grains and voids between them and in donor density, either of which could contribute to the increased IPCE.

  10. Synthesis and characterization of ZnO:TiO{sub 2} nano composites thin films deposited on glass substrate by sol-gel spray coating technique

    Energy Technology Data Exchange (ETDEWEB)

    Sutanto, Heri, E-mail: herisutanto@undip.ac.id; Nurhasanah, Iis; Hidayanto, Eko; Wibowo, Singgih [Department of Physics, Faculty of Natural Sciences and Mathematics, Diponegoro University (Indonesia); Hadiyanto [Department of Chemical Engineering, Faculty of Engineering, Diponegoro University (Indonesia)

    2015-12-29

    In this work, (ZnO){sub x}:(TiO{sub 2}){sub 1-x} nano composites thin films, with x = 1, 0.75, 0.5, 0.25, and 0, have been prepared by sol–gel spray coating technique onto glass substrate. Pure TiO{sub 2} and ZnO thin films were synthesized from titanium isopropoxide-based and zinc acetate-based precursor solutions, respectively, whereas the composite films were obtained from the mixture of these solutions at the specific % vol ratios. The properties and performance of nano composite ZnO, TiO{sub 2} and ZnO:TiO{sub 2} thin films at different composition have been investigated. Ultraviolet – Visible (UV-Vis) Spectrophotometer and Scanning Electron Microscopy (SEM) were employed in order to get morphology and transmittance of thin films. Testing the ability of photocatalytic activity of obtained films was conducted on photodegradation of methylene blue (MB) dye and organic pollutants of wastewater under a 30 watt UV light irradiation, then testing BOD, COD and TPC were conducted. Using the Tauc model, the band-gap energy decreased from 3.12 eV to 3.02 eV for the sample with x = 1 and 0, respectively. This decrease occured along with the replacement of percentage of ZnO by TiO{sub 2} on the films. This decrease also reduced the minimum energy that required for electron excitation. Obtained thin films had nanoscale roughness level with range 3.64 to 17.30 nm. The film with x= 0 has the biggest removal percentage on BOD, COD and TPC mesurements with percentage 54.82%, 62.73% and 99.88%, respectively.

  11. DLTS analysis of amphoteric interface defects in high-TiO2 MOS structures prepared by sol-gel spin-coating

    Directory of Open Access Journals (Sweden)

    Arvind Kumar

    2015-11-01

    Full Text Available High-κ TiO2 thin films have been fabricated from a facile, combined sol – gel spin – coating technique on p and n type silicon substrate. XRD and Raman studies headed the existence of anatase phase of TiO2 with a small grain size of 18 nm. The refractive index ‘n’ quantified from ellipsometry is 2.41. AFM studies suggest a high quality, pore free films with a fairly small surface roughness of 6 Å. The presence of Ti in its tetravalent state is confirmed by XPS analysis. The defect parameters observed at the interface of Si/TiO2 were studied by capacitance – voltage (C – V and deep level transient spectroscopy (DLTS. The flat – band voltage (VFB and the density of slow interface states estimated are – 0.9, – 0.44 V and 5.24×1010, 1.03×1011 cm−2; for the NMOS and PMOS capacitors, respectively. The activation energies, interface state densities and capture cross – sections measured by DLTS are EV + 0.30, EC – 0.21 eV; 8.73×1011, 6.41×1011 eV−1 cm−2 and 5.8×10−23, 8.11×10−23 cm2 for the NMOS and PMOS structures, respectively. A low value of interface state density in both P- and N-MOS structures makes it a suitable alternate dielectric layer for CMOS applications. And also very low value of capture cross section for both the carriers due to the amphoteric nature of defect indicates that the traps are not aggressive recombination centers and possibly can not contribute to the device operation to a large extent.

  12. Ring-Resonator/Sol-Gel Interferometric Immunosensor

    Science.gov (United States)

    Bearman, Gregory; Cohen, David

    2007-01-01

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

  13. Preparation of A New Fiber by Sol-gel Technology in Solid-phase Microextraction (SPME)

    Institute of Scientific and Technical Information of China (English)

    Li Ming WEI; Qing Yu OU; Ju Bai LI

    2004-01-01

    The sol-gel technology is applied for the preparation of solid-phase microextraction (SPME) fiber. The fiber demonstrates high thermal stability, efficient extraction rate and the selectivity for non-polar or low-polar analytes. Efficient SPME-GC-FID analyses of benzene- toluene-ethylbenzene-xylenes (BTEXs) and low-polar halocarbon were achieved by the sol-gel coated DSDA-DDBT-TiO2 fiber. Some parameters of the SPME fiber for the determination of halocarbon in aqueous sample were investigated.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-10-21

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

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

    Science.gov (United States)

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

    2014-10-01

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

  16. Sol-Gel Manufactured Energetic Materials

    Science.gov (United States)

    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.

  17. DLTS analysis of amphoteric interface defects in high-TiO{sub 2} MOS structures prepared by sol-gel spin-coating

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Arvind; Mondal, Sandip; Rao, K. S. R. Koteswara, E-mail: ksrkrao@physics.iisc.ernet.in, E-mail: raoksrk@gmail.com [Department of Physics, Indian Institute of Science, Bangalore, 560012 (India)

    2015-11-15

    High-κ TiO{sub 2} thin films have been fabricated from a facile, combined sol – gel spin – coating technique on p and n type silicon substrate. XRD and Raman studies headed the existence of anatase phase of TiO{sub 2} with a small grain size of 18 nm. The refractive index ‘n’ quantified from ellipsometry is 2.41. AFM studies suggest a high quality, pore free films with a fairly small surface roughness of 6 Å. The presence of Ti in its tetravalent state is confirmed by XPS analysis. The defect parameters observed at the interface of Si/TiO{sub 2} were studied by capacitance – voltage (C – V) and deep level transient spectroscopy (DLTS). The flat – band voltage (V{sub FB}) and the density of slow interface states estimated are – 0.9, – 0.44 V and 5.24×10{sup 10}, 1.03×10{sup 11} cm{sup −2}; for the NMOS and PMOS capacitors, respectively. The activation energies, interface state densities and capture cross – sections measured by DLTS are E{sub V} + 0.30, E{sub C} – 0.21 eV; 8.73×10{sup 11}, 6.41×10{sup 11} eV{sup −1} cm{sup −2} and 5.8×10{sup −23}, 8.11×10{sup −23} cm{sup 2} for the NMOS and PMOS structures, respectively. A low value of interface state density in both P- and N-MOS structures makes it a suitable alternate dielectric layer for CMOS applications. And also very low value of capture cross section for both the carriers due to the amphoteric nature of defect indicates that the traps are not aggressive recombination centers and possibly can not contribute to the device operation to a large extent.

  18. Double component long period waveguide grating filter in sol-gel material.

    Science.gov (United States)

    Moujoud, Abderrafia; Kim, Hyun Jae; Kang, Sung Ho; Oh, Gyong-Jin; Kim, Woo-Soo; Bae, Byeong-Soo; Shin, Sang-Yung

    2007-11-12

    An efficient, tunable Long Period Waveguide Grating (LPWG) filter based on a new hybrid sol-gel material is demonstrated. The LPWG exhibits an attenuation of -22 dB and a high temperature sensitivity of ~3.3 nm/ degrees C. At room temperature the device shows an almost polarization independent wavelength. We took the advantage of the UV-curable sol-gel materials and used soft lithography to demonstrate a simple approach of integrating two LPWG filters on the same structure. The gratings were fabricated on the top and on the bottom of the same ridge waveguide and operate at communication wavelengths of 1550 and 1310 nm, respectively.

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

    Science.gov (United States)

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

    2000-01-01

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

  20. Ionogel Electrolytes through Sol-Gel Processing

    Science.gov (United States)

    Horowitz, Ariel I.

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

  1. Sol-gel applications for ceramic membrane preparation

    Science.gov (United States)

    Erdem, I.

    2017-02-01

    Ceramic membranes possessing superior properties compared to polymeric membranes are more durable under severe working conditions and therefore their service life is longer. The ceramic membranes are composed of some layers. The support is the layer composed of coarser ceramic structure and responsible for mechanical durability under filtration pressure and it is prepared by consolidation of ceramic powders. The top layer is composed of a finer ceramic micro-structure mainly responsible for the separation of components present in the fluid to be filtered and sol-gel method is a versatile tool to prepare such a tailor-made ceramic filtration structure with finer pores. Depending on the type of filtration (e.g. micro-filtration, ultra-filtration, nano-filtration) aiming separation of components with different sizes, sols with different particulate sizes should be prepared and consolidated with varying precursors and preparation conditions. The coating of sol on the support layer and heat treatment application to have a stable ceramic micro-structure are also important steps determining the final properties of the top layer. Sol-gel method with various controllable parameters (e.g. precursor type, sol formation kinetics, heat treatment conditions) is a practical tool for the preparation of top layers of ceramic composite membranes with desired physicochemical properties.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    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 Foerster resonance energy transfer thus opening the way towards very sensitive fluorescent biosensors through biomolecules grafted onto fluorescent nanocrystals. Finally, this controlled dissolution, involving weak concentrated NaOH solution, is a generic process that can be used for the thinning of any kind of sol-gel layer.

  3. SYNTHESIS OF HYBRID MESOPOROUS POLYSTYRENE-SILICA MATERIALS WITH NON-SURFACTANT CITRIC ACID AS TEMPLATE VIA SOL-GEL PROCESS

    Institute of Scientific and Technical Information of China (English)

    Jie Bai; Jin-yu Zheng; Kun-yuan Qiu; Yen Wei

    2002-01-01

    Hybrid mesoporous polystyrene-silica materials were successfully prepared through HCl-catalyzed sol-gelreactions of tetraethyl orthosilicate (TEOS) and triethoxysilyl-functionalized polystyrene obtained via atom transfer radicalpolymerization (ATRP) of styrene, in the presence of citric acid (CA) as non-surfactant template or pore-forming agent andfollowed by ethanol extraction to remove template molecules. The materials were characterized by infrared spectroscopy(IR), N2 adsorption-desorption measurements, powder X-ray diffraction (XRD), thermogravimetric analysis (TGA) andtransmission electron microscopy (TEM). The results indicate that the materials prepared with 50 wt%-60 wt% templatecontents have average pore size s of 2-3 nm and large surface areas (ca. 886 m2/g) as well as high pore volumes (ca.0.53 cm3/g). The mesoporosity arises from interconnected channels and pores with disordered arrangements. The porediameters and pore volumes increase as the template content is increased. The pore diameters show a little change uponheating at 200℃ overnight. However, the materials do not have good hydrothermal stability.

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

    DEFF Research Database (Denmark)

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

    2011-01-01

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

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

    Science.gov (United States)

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

    2002-01-01

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

  6. Elaboration and characterization of a multifunctional silane/ZnO hybrid nanocomposite coating

    Science.gov (United States)

    Nicolay, A.; Lanzutti, A.; Poelman, M.; Ruelle, B.; Fedrizzi, L.; Dubois, Ph.; Olivier, M.-G.

    2015-02-01

    The present study aims at investigating the elaboration of a ZnO/sol-gel nanocomposite coating, which can provide a number of properties such as UV-absorption, mechanical and barrier effects, etc. depending on targeted applications. The sol-gel coating formulation is an inorganic-organic hybrid based on tetraethoxysilane (TEOS) and glycidyloxypropyltrimethoxysilane (GPTMS). In order to ensure good dispersion in the sol-gel matrix, ZnO nanoparticles were surface-modified with a silane coupling agent. The functionalization was confirmed by Fourier transform infrared (FTIR) and thermogravimetric (TGA) analyses. Field emission gun-scanning electron microscopy (FEG-SEM) characterization of the nanocomposite film reveals a homogeneous distribution and dispersion of the ZnO nanoparticles throughout the film. Glow discharge optical emission spectrometry (GDOES) analysis allows evaluating the thickness of coatings and getting a depth composition profile. Some properties such as UV-absorption and barrier effect are highlighted using a UV-visible spectrometer and electrochemical impedance spectroscopy (EIS), respectively. The effect of ZnO concentration is also presented.

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

    Institute of Scientific and Technical Information of China (English)

    李龙芹; 王韶音; 李青

    2013-01-01

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

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

    Science.gov (United States)

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

    2013-02-01

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

  9. Synthesis of Oxide Nanoparticles in Hybrid Nanocomposite Coatings as Nanoreservoirs of Corrosion Inhibitors

    Science.gov (United States)

    Pirhady Tavandashti, Nahid; Sanjabi, Sohrab

    Nanostructured hybrid silica/epoxy films containing boehmite nanoparticles were investigated in the present work as pretreatments for AA2024 alloy. To produce the nanocomposite sol-gel films, boehmite nanoparticles prepared from hydrolysis/condensation of aluminum isopropoxide (AlI) were doped into another hybrid organosiloxane sol. The produced oxide nanoparticles have the capability to act as nanoreservoirs of corrosion inhibitors, releasing them controllably to protect the metallic substrate from corrosion. For this purpose the corrosion inhibitor, cerium nitrate, was introduced into the sol-gel system via loading the nanoparticles. The morphology and the structure of the hybrid sol-gel films were studied by Scanning Electron Microscopy (SEM). The corrosion protection properties of the films were investigated by Potentiodynamic Scanning (PDS) and Electrochemical Impedance Spectroscopy (EIS). The results show that the presence of boehmite nanoparticles highly improved the corrosion protection performance of the silica/epoxy coatings. Moreover, they can act as nanoreservoirs of corrosion inhibitors and provide prolonged release of cerium ions, offering a self-healing property to the film.

  10. Preparation and Properties of Silver-doped Silica Hybrid Membranes by Sol-gel Method%溶胶-凝胶法载银SiO2杂化膜的制备及性能研究

    Institute of Scientific and Technical Information of China (English)

    杨靖; 于春雁; 刘华华

    2011-01-01

    The silver-doped methyl-modified hybrid silica (Ag/M-SiO2) membranes were prepared using the sol-gel method by adding AgNO3 solution to a methyl-modified silica sol. The influence of Ag-doping on the structure and properties of hybrid silica membranes was investigated by using XRD, XPS, UV-visible absorption spectra, N2 adsorption-desorption measurements and gas permeance experiments. The results show that the silver element in the Ag/M-SiO2 membranes exists in the metallic silver with a face centered cubic lattice. The doping of silver nanoparti-cles nearly has no influence on the chemical structure of the methyl-modified silica membranes, but can make the mean pore size and total pore volume slightly increase. Compared with the methyl-modified silica membranes without silver-doping, the H2 permeance and H2/CO2 permselectivities of Ag/M-SiO2 membranes are greater. The introduction of metallic silver facilitates the transport of H2 in silica membranes and improves the steam stability of silica membranes.%采用溶胶-凝胶法,在甲基化改性的SiO2溶胶中掺杂硝酸银,制备Ag/M-SiO2杂化膜.通过XRD、XPS、紫外-可见吸收谱、N2吸附-脱附以及气体渗透性能测试等方法,考察了银掺杂对杂化膜结构和性能的影响.结果表明,Ag/M-SiO2膜中的银元素完全为纳米金属银,具有面心立方结构.金属银的掺杂对Ag/M-SiO2膜的化学结构基本没有影响,但使其孔径和总孔体积略微增大.与未载银的SiO2膜相比,Ag/M-SiO2膜具有更大的H2渗透速率和更好的H2/CO2选择性.金属银的引入增强了H2的表面扩散作用,促进了H2在膜中的传递,提高了SiO2膜的水汽稳定性.

  11. Multilayer crack-free hybrid coatings for functional devices

    Science.gov (United States)

    Islam, Shumaila; Bidin, Noriah; Riaz, Saira; Naseem, Shahzad; Marsin Sanagi, Mohd.; Imran, M.

    2016-04-01

    Porous acid catalyzed TiO2 single, SiO2-TiO2 hybrid, and TiO2/SiO2-TiO2/SiO2 multilayer coatings are synthesized and characterized for optical and electro-optical applications. The reflection value is reasonably reduced from the surface of the glass by integrating sol-gel based spin-coated single and multilayer thin films. Structurally, the films show uniform, crack-free, and porous nanofilms with good surface roughness of below 10 nm, which has potential for optical applications. Wide range tunability of refractive index (2.83 to 1.59) with more than 78% optical transparency is observed. The multilayered reflection profile is obse