Sol-Gel Deposited Sb-Doped Tin Oxide Films

The structural, electrical and optical properties of single sol-gel derived antimony-doped tin oxide (ATO) films sintered at 550°C have been measured. The reproducibility of both the preparation and the characterization procedures have been tested by a round-robin test involving eight laboratories within a Concerted European Action (CEA) project. The resistivity measured as a function of Sb content has been obtained by electric and reflectance and transmission measurements. Their differences are discussed in terms of structural and grain boundary effects. An increase of Sb content results in a decrease of the crystallite size (7.0 to 5.4 nm) and a greater influence of the grain boundary.     

Structural and Electrochromic Properties of Co-Oxide and Co/Al/Si-Oxide Films Prepared by the Sol-Gel Dip Coating Technique

The sol-gel dip-coating technique was used for depositing cubic spinel Co₃O₄ and amorphous Co/Al/Si-oxide thin films. Both types of films exhibit similar electrochrochemical properties which are accompanied by the hydration of the structure. The electrochromic properties of Co/Al/Si-oxide surpass those already known for Co-oxide based electrochromic materials. The change in transmittance for spinel Co₃O₄ is 25%, while for Co/Al/Si-oxide films exceeds 50%. The electrochromic efficiency () for Co₃O₄ and Co/Al/Si-oxide films was 22 cm² C^-1, which is comparable to other electrochromic oxides. Good electrochromic properties of the Co/Al/Si-oxide films make them promising materials for active counter electrode in electrochromic devices.     

Optical and Electrical Properties of the PLT Films with Various Compositions Deposited by Sol-Gel Process

In order to study optical and electrical properties of (Pb_1-xLa_x)TiO₃ (PLT) films with varying La concentration, the PLT films were deposited by sol-gel process. X-ray diffraction revealed that a pseudocubic phase of the PLT film became dominant with increasing La concentration due to decrease of lattice constant of c-axis. Three-dimensional atomic force microscopy images showed that the grain size and root mean square surface roughness decreased by addition of La. The optical band gap of the PLT films became wider when Pb was substituted with La. The addition of La increased the transparency of the PbTiO₃ film and shifted the threshold for initiation of absorption to shorter wavelength. Hysteresis loops of the PLT films showed that remanent polarization and coercive field decreased with increasing La concentration. In addition, we modified the surface of the PLT film with La concentration of 5% using a keV oxygen ion beam at different doses. The optical band gap of the PLT film was changed by the oxygen ion beam irradiation although the XRD patterns and the transmittance values were not significantly changed. In measuring AFM images of the surface of modified PLT film, significant changes of the grain shape and size were not found. Moreover, polarization and dielectric constant were not changed after oxygen ion irradiation. These results suggested that addition of La could affect the optical and electrical properties of the PbTiO₃ and PLT films and that surface modification by oxygen ion beam modification with 1 keV energy can change the surface property but not bulk property.     

Photoelectrochemical Properties of Sol-Gel Nb2O5 Films

Structural, optical, electro and photoelectrochemical properties of amorphous and crystalline sol-gel Nb₂O₅ coatings have been determined. The coatings are n-type semiconductor with indirect allowed transition and present an overall low quantum efficiency ( < 4%) for UV light to electric conversion. The photoconducting behavior of the coatings is discussed within the framework of the Gärtner and Södergren models. Improvement can be foreseen if Nb₂O₅ coatings can be made of 10–20 nm size nanoparticles.     

Optical and Structural Properties of Doped ZnS Nanoparticles Produced by the Sol-Gel Method

Optical and structural properties of Mn2+-doped ZnS nanoparticles in an organic matrix are experimentally and theoretically studied. The nanoparticles, which were produced by the sol-gel method, are nearly monodisperse with a diameter of approximately 3 nm and show the characteristic orange-red luminescence of Mn2+ centers in a crystalline ZnS matrix. The absorption spectrum of the embedded ZnS nanoparticles is slightly blue shifted and broadened compared to the reference system containing ZnS microparticles. This blue shift is caused by quantum size effects, whereas the broadening is due to defects such as lattice distortions, and vacancies, which are probably located close to the surface in the case of small particles. With increasing temperature the absorption spectra shift to the red and are broadened due to thermal activated diffusion of ions close to the surface. In contrast, the spectral feature of the emission spectra via the Mn2+ center is nearly unchanged compared to the ZnS microparticles. Furthermore, the quantum efficiency is increased and the decay time of the electron-hole pairs is shortened to the nanosecond regime because of the enhanced probability of the electron-hole pairs to see the Mn2+ center. Therefore, the only effect of doping of ZnS nanoparticles with Mn2+ center is the suppression of the relaxation of electron-hole pairs via surface defects generating a highly efficient and fast relaxation of the electron-hole pairs via the Mn2+ center.     

Optical and Conductivity Properties of PbS Nanocrystals in Amorphous Zirconia Sol-Gel Films

Lead sulfide (PbS) nanocrystals (NCs), embedded in amorphous zirconia sol-gel film with different PbS mole concentration (5–30%), were grown at temperature, ranging from 200°C to 350°C. The size of PbS NCs was determined by TEM and by blue shift of the absorption edge. The size increased with an increase of the synthesis temperature and PbS mole concentration. The optical and electrical properties of various sizes of PbS NCs in zirconia film are investigated utilizing absorption, photoluminescence (PL) and current-voltage measurement. The PL spectra were Stokes shifted from the corresponding absorption edge by about 0.5 eV. The latter can be associated with recombination process from surface state. The electrical properties were investigated by the deposition of the PbS NCs-zirconia films on ITO/glass substrate, followed by their coverage with gold contact. The current-voltage characteristics depend on the PbS NCs size and exhibits nonlinear nearly symmetric curve, associated with the space-charge limited current or the tunneling of carriers through the nanocrystalline film.     

Sol-Gel Derived Hydrated Nickel Oxide Electrochromic Films: Optical, Spectroelectrochemical and Structural Properties

Electrochromic hydrated Ni-oxide films were prepared using a dip-coating technique from a nickel sulphate heptahydrate precursor in combination with glycerol, formamide and polyvinyalcohol. In-situ monochromatic (λ=400 nm) spectroelectrochemical measurements using a potential of −0.4 V to 0.8 V in 0.1M LiOH electrolyte revealed that the electrochromic efficiency was 23.5 cm²/C. The observed colouring/bleaching transmittance of a 100 nm thick film changed during potential cycling (20 cycles) by 45%. Ex-situ FT-IR absorption/reflection measurements performed at near-grazing incidence angle conditions (80°) confirmed transformation of as-deposited α-Ni(OH)₂ phase to β-Ni(OH)₂ at cathodic (bleached state) and β-NiOOH at anodic (coloured state) potentials during extended cycling (200 cycles). Clear evidence of the OH⁻ ions insertion and release of SO ₄ ²⁻ ions from the as-deposited films when soaked (0.5 hour) in 0.1M LiOH are given. These processes are accompanied by the transformation of the residual COO⁻ groups originating from the peptisation with glacial acetic acid into CO ₃ ²⁻ species residing in the films during extensive potential cycling.     

Effect of High-Temperature Treatment on Optical Properties of Silica Films Doped with Al2O3, P2O5 and Rare-Earth Elements

The paper reports effects of high-temperature treatment of silica layers doped with Al₂O₃, P₂O₅, Yb and Er ions, which are coated inside silica substrate tubes and transformed through viscous flow into the core of a preform, on properties of these cores. The gel layers are applied inside the silica substrate tubes from sols based on tetraethoxysilane and corresponding chlorides in isopropanol by controlled lowering the column of the sol. The layers are thermally treated at 500°C and subject to high-temperature treatment from 1000 to 1300°C. The tube with the layers is collapsed into a preform from which fibers are drawn at about 1950°C. The results of concentration measurements show that during the high-temperature treatment the content of silica in the layer increases at least five times in comparison with that of the sol composition. This effect depends on the sol composition and the number of the coated gel layers. Measurements show that in the prepared fibers there is some remaining unsaturated absorption of erbium ions at 1535 nm, which is related to quenching of the erbium ions.     

Optical Properties of Sol-Gel Derived Vanadium Oxide Films

Vanadium oxide gels can be made from vanadate aqueous solutions or from vanadium alkoxides. The condensation of vanadic acid gives long ribbon-like oxide particles which macroscopically orient in the same direction in aqueous sols when their concentration is larger than 0.12 mol·l⁻¹. These anisotropic sols and gels should be considered as lyotropic nematic liquid crystals. Thick films in which ribbons align along the same direction can be deposited. These oriented coatings exhibit improved electrochemical properties as reversible cathodes for lithium batteries. Amorphous oxo-polymers are formed via the controlled hydrolysis of vanadium alkoxides. They allow the deposition of optically transparent thin films that exhibit interesting electrochromic properties and turn reversibly from yellow to green upon electrochemical reduction. Moreover these alkoxide derived films can be easily reduced into vanadium dioxide. These VO₂ thin films exhibit thermochromic properties and could be used as optical switches in the infrared. The transition temperature of these VO₂ films can be modified by doping the vanadium oxide with other cations.     

Hydrogen Gas Sensing of High Electrical Conducting-P2O5-SiO2 Glasses Prepared by Sol-Gel Process

High proton-conducting P₂O₅-SiO₂ glass was applied to the electrolyte of the hydrogen concentration cell for hydrogen gas sensing. 5P₂O₅·95SiO₂ glass was prepared using the sol-gel method and its electrical conductivity and electromotive force were measured at 50°C as a function of both the ambient humidity and hydrogen gas concentration. The electrical conductivities increased with increasing humidity and reached 10^–2 S/cm at 90% relative humidity. The electromotive force of the hydrogen concentration cell, where the glass was used as a membrane, showed good Nernstian response to hydrogen pressure in the high relative humidity region.     

Preparation and Optical Characterization of Sol-Gel Deposited Pb(Zr0.45Ti0.55)O3 Films

Homogeneous crack-free lead zirconate titanate (Pb(Zr_0.45Ti_0.55)O₃: PZT 45/55) films were prepared by a chemically modified sol-gel process using lead acetate trihydrate, zirconium n-propoxide, and titanium isopropoxide precursors. The coating solutions were modified by the addition of diethanolamine. Single and multilayer films were deposited with a 2000 rpm spin rate on fused silica and MgO(100) substrates. Multiple spin coating with an intermediate heat treatment in air at 400°C for 3 min between coatings was performed to obtain films up to 2 m in thickness. The formation of the tetragonal perovskite structure was found to depend on the intermediate firing temperature, final annealing temperature, and annealing time. A 650°C rapid thermal annealing treatment in oxygen was required to crystallize the PZT film into the perovskite structure. The films were characterized using optical spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and thermo-gravimetry and differential scanning calorimetry (TG-DSC). The optical constants of the PZT films were evaluated from spectral transmittance and reflectance measurements. Optical constants are presented over the visible and near infrared region.     

Role of Water on Fast Proton Conduction in Sol-Gel Glasses

Fast proton-conducting P2O5-ZrO2-SiO2 glasses were prepared by sol-gel processing of metal alkoxides. Glasses heated to 150 to 400°C exhibited room temperature conductivities of 10–4 S/cm, larger by 2 order of magnitude than that of as-prepared gel, 3 × 10–7 S/cm at 30°C. The conductivity increased quadratically with the increasing product of proton and molecular water concentration. These high conductivities were regarded as fast proton transfer accelerated by molecular water bonded with the hydroxyl groups.     

NiO-SiO2 Sol-Gel Nanocomposite Films for Optical Gas Sensor

Recently nanocomposites with sensoring function are becoming a new area of interest in the field of optical gas sensor. In fact, the optical transmittance of nano-particles or thin films has been reported to be changed by atmosphere gases. In particular it was found that NiO, Co₃O₄ and Mn₃O₄ thin films showed reversible decrease in the Vis-NIR absorption due to CO.Aim of this work is the synthesis and the characterization of SiO₂ sol-gel glass films doped with NiO nanocrystals.Films of composition (100 – X)SiO₂-XNiO with X = 10, 20, 40, were obtained by mixing a matrix solution of Si(OC₂H₅)₄ (TEOS) and CH₃Si(OC₂H₅)₃ (MTES) as SiO₂ precursors, with a doping solution containing NiCl₂ as precursor for NiO particles.3-Aminopropyltriethoxysilane (3-APTES), bearing either an ammine group capable of coordinating the Ni ions and hydrolysable siloxane groups for anchoring the metal complex moiety to the silicate matrix, was used as bifunctional ligand.Transmission electron microscopy micrographs showed a uniform distribution of round shaped nanoparticles in film heated at 500°C with a mean diameter of 2.5 nm.The film composition evaluated from Rutherford backscattering spectrometry was in good agreement with the nominal one. As expected the density of the films heated at 1000°C is much higher than the density of the film heated at 500°C due to a residual porosity. Fourier transform infrared spectra also confirmed the presence of residual porosity in the films heated at 500°C.     

La0.8Sr0.2Ga0.8Mg0.2O3－α陶瓷的质子导电性能研究

采用溶胶-凝胶法合成了La_0.8Sr_0.2Ga_0.8Mg_0.2O_3－a陶瓷样品, 用XRD, DSC-TGA, SEM, 交流阻抗谱, 气体浓差电池及气体电化学透过等方法对样品的结构和性质进行了表征和测试. 首次对该样品的质子导电性能进行了研究. 该陶瓷样品具有良好的微观结构, 相对密度达95.1%; 氢浓差电池电动势的实测值与理论值吻合, 离子迁移数为1; 在干燥的氧气气氛中是一个纯的氧离子导体; 氢的电化学透过速率的实测值与理论值吻合, 证明该样品在氢气气氛中几乎是一个纯的质子导体, 质子电导率在1000 ℃时高达0.14 S•cm^－1.     

Structure and Optical Properties of 0.1BiFeO3-0.9SrBi2Nb2O9 Thin Films Using a Modified Sol-Gel Technique

Fe-doped SrBi₂Nb₂O₉ precursor solution was synthesized using bismuth nitrate Bi(NO₃)₃·5H₂O, strontium nitrate Sr(NO₃)₂, iron nitrate Fe(NO₃)₃·9H₂O, and niobium ethoxide Nb(OC₂H₅)₅ as starting materials, ethylene glycol monomethyl ether (C₃H₈O₂) as the solvent. 0.1BiFeO₃-0.9SrBi₂Nb₂O₉ thin films were prepared on fused quartz substrates using sol-gel processing. The surface morphology and crystal structure and optical properties of the thin films were investigated. The thin film annealing at 400°C were found to be amorphous, and the thin films crystallize to a perovskite structure after a post-deposition annealing at 600°C for 1 h in air. The grain of thin film was evenly distributed. The thin films exhibit the designed optical transmission, while the optical transition is indirect in nature. Their optical band gap is about 2.5 eV.     

TiN基IrO2-Ta2O5涂层析氢电极的催化性能

 采用热分解法制备了以离子镀TiN膜为基体的IrO2-Ta2O5涂层电极,通过循环极化曲线并结合扫描电镜、 X射线能谱和X射线衍射研究了涂层的析氢电催化性能. 结果表明,涂层呈多孔多裂纹的结构,焙烧温度对涂层的表面形貌和电催化活性影响很大. 420 ℃下焙烧的涂层具有最优的电催化活性. 涂层电极的析氢反应电极电位为-0.26 V(vs SCE), 低析氢过电位下的Tafel斜率为-0.04 V, 而在高析氢过电位下,电极表面吸附的大量氢原子改变了氧化物电极的结构,从而抑制了氧的阴极还原反应.     

PEO掺杂氧化镍薄膜的溶胶-凝胶法制备及电致变色性能研究

以无水醋酸镍、乙醇为前驱液, 加入适量正丁醇及PEO2000等为稳定剂, 采用改进的溶胶-凝胶法制备了稳定的PEO2000纳米Ni(OH)₂复合溶胶体系, 采用旋涂法在ITO (In₂O₃∶Sn)导电玻璃上形成均匀的氧化镍薄膜. 研究了溶胶组分对成膜性能的影响, 采用TG-DSC分析、X射线衍射仪和扫描电镜, 研究了热处理过程中的结构变化和表面形貌. 循环伏安和可见光透过率测试表明该氧化镍薄膜具有良好的电致变色性能和阳极着色效应.     

Optical and Electrical Properties of Ferroelectric SBN Thin Films Prepared by Sol-Gel Process

Strontium barium niobate thin films were prepared by sol-gel method on various substrates using an improved process, two-step heating process. The two-step heating process applies an additive heat-treatment before crystallization for enhancement of the densification and the nucleation of films. Also, highly c-axis oriented SBN thin films with various compositions were obtained on MgO(100) and Pt(100)/MgO(100) substrates. Their optical and electrical properties such as optical propagation loss, refractive index, P-E hysteresis, and dielectric constant, were characterized as a function of the film composition.     

Sol-Gel Synthesis and Characterization of SiO2—P2O5—ZrO2

Zirconia phosphosilicates were prepared by the sol-gel method using tetraethylorthosilicate, triethyl phosphate, and zirconium n-propoxide. Monolithic, transparent gels were formed with 10 mole% ZrO₂, and 10, 20 or 30 mole% P₂O₅. The influence of the mole% P₂O₅, treatment temperature and water content, on thermal behavior, water adsorption, and proton conductivity were studied. A heat treatment at 200°C was effective in removal of residual organics, creating a porous material capable of good water retention upon rehydration.