不同基底对TiO2和SiO2薄膜的光学性能的影响

采用溶胶-凝胶法分别在K9玻璃、单晶硅和石英玻璃基底上制备了纳米TiO₂和SiO₂薄膜。利用SEM、UV-Vis及反射式椭圆偏振光谱仪对薄膜的微观结构及光学特性进行了表征和分析。结果表明:3种基底中, 单晶硅基底上TiO₂和SiO₂薄膜折射率最大;在非晶态K9玻璃和石英玻璃基底上TiO₂薄膜折射率和透光率差异较大;SiO₂薄膜在非晶态基底上折射率、透光率相近;3种基底上薄膜的折射率和消光系数都有随波长增大而减小的趋势, 同时Cauchy模型能较好的描述单晶硅基底上两种薄膜在400~800 nm波段的光学性能。     

不同基底对TiO2和SiO2薄膜的光学性能的影响

采用溶胶-凝胶法分别在K9玻璃、单晶硅和石英玻璃基底上制备了纳米TiO₂和SiO₂薄膜。利用SEM、UV-Vis及反射式椭圆偏振光谱仪对薄膜的微观结构及光学特性进行了表征和分析。结果表明：3种基底中, 单晶硅基底上TiO₂和SiO₂薄膜折射率最大;在非晶态K9玻璃和石英玻璃基底上TiO₂薄膜折射率和透光率差异较大;SiO₂薄膜在非晶态基底上折射率、透光率相近;3种基底上薄膜的折射率和消光系数都有随波长增大而减小的趋势, 同时Cauchy模型能较好的描述单晶硅基底上两种薄膜在400~800 nm波段的光学性能。     

氧化钼-二氧化钛复合膜的可见光致变色性能研究

采用溶胶凝胶法制备了一系列氧化钼-二氧化钛纳米复合物, 用柠檬酸作分散剂, 将得到的纳米复合物粉末分散成溶胶, 涂膜制备了具有可见光变色性能的均匀透明的光致变色(λ≥420 nm)复合膜. 通过红外、XPS、ESR测定表明, 在氧化钼、二氧化钛复合界面上生成了Mo—O—Ti键, 此键的存在是该复合膜具有可见光致变色响应的内在原因. 在可见光的照射下, 电子从二氧化钛的价带经由Mo—O—Ti键, 被激发到氧化钼的导带上. 研究了光致变色过程的动力学, 发现光致变色反应的速率取决于膜中复合物的摩尔比([MoO₃]/[TiO₂])以及电荷转移能量(CTE).     

Preparation and Characterization of Nanocrystalline Fe-Doped TiO2 Film on Different Substrates and Its Application in Degrading Dyeing Water

TiO₂ and Fe-doped TiO₂ thin films were prepared on the substrates (glass plates and glass microballs) after dipped in colloid and calcined at 500°C. The films have been characterized by UV-absorption, x-ray diffraction and atomic force microscopy (AFM). The investigated Fe-doped TiO₂ (A nominal 10 wt% Fe₂O₃ was impregnated) thin films were obtained by sol-gel method. The characterization results suggest that the calcined thin films primarily consist of TiO₂ anatase. And the light absorption curve of the TiO₂ films modified with Fe showed that red shift had happened by the dope of Fe. TiO₂/beads as photocatalyst were used to degrade the simulated dyeing water which contains reactive deep-blue dye (K-R). Through the degradation experiment, we found that the dope of Fe promoted the photocatalytic activities. The results showed that the dyeing water can be decomposed more effectively by the photocatalytic oxidation of Fe/TiO₂ film on glass micro-balls than glass plates.     

Preparation of TiO2 Thin Film Photocatalysts by Dip Coating Using a Highly Viscous Solvent

TiO₂ thin film photocatalysts coated onto soda lime glass were prepared by a dip coating process using a highly viscous solvent. The source of the TiO₂ was tetraisopropyl orthotitanate, and -terpineol was used as the solvent. Two types of thin film preparation procedures based on dip coating (a sol-gel system and thermal decomposition system) were used to prepare the samples. TiO₂ thin films were obtained after calcination at 450°C for 1 hour. The film thickness obtained with a single dipping was proportional to the viscosity of the dip coating solutions. The obtained thin films were transparent with a thickness of 1 m. The crystal form of the obtained photocatalyst films was anatase alone. The thin films were formed with aggregated nano-sized TiO₂ single crystals (7–15 nm). The photocatalytic activity of the TiO₂ thin films, as evaluated by the photooxidation of NO (1 ppm) in dry air, was as high as our previous TiO₂ thin films prepared by the sol-gel method.     

Processing of β-BaB2O4 Thin Films Through Metal Organics

β-BaB₂O₄ (β-BBO) thin films were successfully synthesized by the sol-gel method using metallo-organic compounds. A stable BBO precursor solution was prepared from barium metal and boron triethoxide or 2,4,6-triethoxycyclotriboroxane in a mixture solvent of ethanol and 2-ethoxyethanol. As-precipitated powder formed by hydrolysis of the precursor solutions crystallized to ψ phase, which was transformed to β phase at higher temperatures. The transformation temperatures of powders from ψ to β phase of the ethoxide system and the boroxane system were 600 and 680°C, respectively. The calcination of precursor films in a mixture gas of water and oxygen was found to decrease the crystallization temperature of β-BBO films on Pt sheet substrates. The precursor films prepared from the ethoxide system and the boroxane system crystallized to β-BBO on Pt (111)/glass substrates at 500 and 550°C, respectively. The BBO films on Pt(111)/glass substrates showed the strong (006) preferred orientation. The β-BBO films on Pt(111)/glass substrates showed the second harmonic generation (SHG) of the 532 nm light on irradiation with 1064 nm light. The SH power from the BBO films was correlated with the fundamental power through the square-law proportionality based on the theory. The SHG efficiency of the BBO films was dependent upon the film thickness.     

Effect of Glass Substrates on the Formation of Gold-Silver Colloids in Nanocomposite Thin Films

A sol-gel route to synthesize nanocomposite thin films containing phase separated metal colloids of gold (Au) and silver (Ag) was developed. Ag—Au colloids were prepared in silica films using dip coating technique. The annealing of the samples in air results in the formation of phase separated Ag and Au colloids in SiO₂ thin films, showing the surface plasmon peaks at 410 nm and 528 nm. For the synthesis of phase separated Ag and Au colloids on float glass substrates, formation of the silver colloids was found strongly dependent on the surface of the float glass. On the tin rich surface formation of both gold and silver colloids took place, whereas, on the tin poor surface the formation of only gold colloids was observed. The surface dependence of the formation of silver colloids was attributed to the presence of tin as Sn²⁺ state on the glass surface, which oxidizes into Sn⁴⁺ during heat treatment, reducing Ag⁺ into silver colloids.     

White light emission from nano-fibrous ZnO thin films/porous silicon nanocomposite

Nanocomposites composed of nano-fibrous ZnO thin films and porous silicon (PS) were prepared and examined by atomic force microscopy (AFM), X-ray diffraction (XRD), Raman spectroscopy, and photoluminescence (PL) to investigate their structural and optical properties. PS, consisting of irregular and random nanosized-pores, was prepared by electrochemical anodization. The nano-fibrous ZnO thin films were grown on PS by the sol-gel spin-coating method. The texture coefficient (TC _(hkl)) of the nano-fibrous ZnO thin films was calculated to determine the preferred orientation. The nano-fibrous ZnO thin films were grown with a c-axis preferred orientation. The residual stress in the films was reduced in the case of PS. The observed broad PL emission peak from 460 to 598 nm was attributed to coupled emission from ZnO to PS. The results show that white light luminescence with blue, green, and red emission peaks having highly uniform intensities can be obtained from the nanocomposite via a relatively simple and low-cost sol-gel spin-coating method.     

Loss of phosphorous in silica-phosphate sol-gel films

Phosphosilicate films with 90%SiO₂-10%P₂O₅ molar composition, derived from tetraethoxysilane as SiO₂ precursor and triethylphosphate, triethylphosphite or phosphoric acid as P₂O₅ precursors were prepared using the sol-gel method. The films were deposited on glass and ITO coated glass supports. The influence of the type of P₂O₅ precursor, type of substrate and of the thermal treatment (200, 300 and 500°C) on their structure and properties was studied. By spectroellipsometric and XPS measurements the high vaporization of the phosphorous during the densification of the films by thermal treatment was noticed when alkoxide were used, underlying that the mentioned precursors are not recommended for thin phosphosilicate films preparation. The phosphoric acid that forms chemical bond with silica network during the sol-gel process lead to better incorporation of P in the silica network as compared to the P-alkoxides.     

Fluorescence spectroscopic study of dip coated sol-gel thin film internal environment using fluorescent probes Hoechst33258 and Pyranine

The characterization of physicochemical properties of the internal environment of sol-gel thin films is required for understanding and designing applications in optical biosensors. We have investigated the dip coated tetraethyl-orthosilicate (TEOS) derived sol-gel thin films deposited on microscopic glass cover slips using molar ratio (water or ethanol / TEOS) R=32 using fluorescence spectroscopic measurements (emission, lifetime and anisotropy) on entrapped fluorescent probes. The effect of water and/or ethanol was studied as a function of storage (60 days) using fluorescent probes Hoechst 33258 (H258) and Pyranine (PY). Distribution of fluorescent probes in thin film was studied using confocal microscope. Emission maxima of H258 entrapped thin films from sol prepared using water as solvent showed emission maximum at 503 nm indicating the presence of water like environment which did not change during storage. On the contrary, PY entrapped thin films depicted emission bands at 434 nm and 513 nm, characteristics of ethanol and water respectively, up to the first few weeks and then the band at 434 nm prevailed (60 days), suggesting heterogeneous internal environment. Thin films from sol prepared using ethanol as solvent showed presence of ethanol through out storage. Fluorescence lifetime data of these probes in both sol-gel and thin films also suggested presence of heterogeneous internal environment. Thin films prepared from sol-gel using water as solvent suggested release of ethanol in the pores during hydrolysis and condensation reaction, which were clearly indicated by PY. The effect of sodium phosphate buffer was also studied in sol-gel and thin films. The results of these measurements showed that both the probes H258 and PY could be used effectively in monitoring the physicochemical properties of internal environment of thin films and sol-gel as a function of storage.     

Nitrogen Doping and Carbon Coating Affects Substrate Selectivity of TiO2 Photocatalytic Organic Pollutant Degradation

A series of carbon-coated, nitrogen-doped titanium dioxide photocatalysts was produced and characterized. N-doped TiO₂ powder samples were prepared using a sol-gel method and subsequently used for making doped-TiO₂ thin films on glass substrates. Carbon layers were coated on the films by a thermal decomposition method using catechol. Diffuse reflectance spectra and Mott-Schottky analyses of the samples proved that nitrogen doping and carbon coating can slightly lower the band gap of TiO₂, broaden its absorption to visible light and enhance its n-type character. According to photocatalytic tests against model contaminants, carbon-coated nitrogen-doped TiO₂ films have better performance than simple TiO₂ on the degradation of Rhodamine B dye molecules, but are poorly effective for degrading 4-chlorophenol molecules. Several possible explanations are proposed for this result, supported by scavenging experiments. This reveals the importance of a broad substrate scope when assessing new photocatalytic materials for water treatment, something which is often overlooked in many literature studies.     

Influence of thermal treatment on the ion-storage capacity of Ce oxide and Ce-V mixed oxide films

Thin films and the corresponding xerogels of CeO₂ and Ce-V mixed oxides with a molar ratio equal to 2 (Ce/V=2) were prepared from CeCl₃·7H₂O and NH₄VO₃ precursors using the sol-gel route and the dip-coating technique. The thermal decomposition of both forms of samples (thin films and xerogels) were studied by dynamic TG and DSC in two different atmospheres (air and argon). For the thermal studies the thin films were deposited on aluminium foil to reduce the unfavourable substrate to film mass ratio S/F, which is a consequence of using a glass substrate. The mode of heat treatment in a tube furnace of films deposited on conductive glass was defined from the TG curves of the films. The influence of annealing conditions (temperature, atmosphere and time) on the charge capacity of the films during application of the cycling process is reported.     

TiO2光致亲水性及其在免处理版材中的应用研究

用溶胶-凝胶法制备了SiO₂和TiO₂薄膜,并涂覆于玻璃基片上,研究了TiO₂薄膜在紫外光照射下其超亲水性能的变化与光照时间的关系,分析了SiO₂薄膜对覆于其上的TiO₂薄膜的耐摩擦性能的影响.结果表明:TiO₂薄膜经紫外光照射后,疏水性急剧降低,显示亲水性能,与水的接触角可达到5°以下;当其覆膜于载玻片上后,具有良好的耐摩擦性和耐候性;TiO₂薄膜的超亲水性使其有望成为一种新型的环保可重复利用的印刷版材.     

Anatase TiO2 porous thin films prepared by sol-gel method using CTAB surfactant

Anatase TiO₂ porous thin films were prepared on glass substrates by sol-gel method with Cetyltrimethylammonium Bromide (CTAB) as a pore-forming agent, Tetrabutylorthotitanate as Ti precursor, ethanol as solvent and diethanolamine as chelating agent respectively. IR, TG-DSC, XRD and SEM analyzed the chemical and physical changes during sol-gel process and characteristics of the films. Effects of the amount of CTAB, alkane and water on morphology of the films were discussed and the principle of forming porous structure was proposed. It was shown that the diameter of pores was changed in the range of 30–400 nm.     

A Highly Sensitive and Selective Non-enzymatic Hydrogen Peroxide Sensor Based on Nanostructured Co3O4 Thin Films Using the Sol-gel Method

In this work we report an easy and efficient way to fabricate nanostructured cobalt oxide (Co₃O₄) thin films as a non-enzymatic sensor for H₂O₂ detection. Co₃O₄ thin films were grown on ITO glass substrates via the sol-gel method and characterized with several techniques including X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and optical absorbance. The Co₃O₄ thin films’ performance regarding hydrogen peroxide detection was studied in a 0.1 M NaOH solution using two techniques, cyclic voltammetry (CV) and amperometry. The films exhibited a high sensitivity of 1450 μA.mM⁻¹.cm⁻², a wide linear range from 0.05 μM to 1.1 mM, and a very low detection limit of 18 nM. Likewise, the Co₃O₄ thin films produced showed an exceptional stability and a high selectivity.     

Structure and photochromic properties of molybdenumphosphoric acid/TiO<Subscript>2</Subscript> composite films

TiO₂ sol-gel composite films with dropping molybdenumphosphoric acid (PMoA) have been prepared by sol-gel method. The structure and constitute of composite thin films were studied with Fourier transforms infrared spectroscopy (FT-IR) atomic force microscopy (AFM), and X-ray diffraction (XRD) patterns, respectively. The photochromic behavior and mechanism of composite thin films were investigated with ultraviolet-visible spectra (UV-vis) and electron spin resonance (ESR). FT-IR results showed that the Keggin geometry of PMoA was still preserved inside PMoA/TiO₂ composite thin films, and a charge transfer bridge was built at the interface of PMoA and TiO₂ through the Mo-O-Ti bond. Surface topography of the composite film showed obvious changes before/after adding PMoA, and the surface topography of composite films showed obvious changes before/after irradiating as well. Composite thin film had reversible photochromic properties. Irradiated with UV light, transparent films changed from colorless to blue and they can bleach completely with ambient air in the dark. ESR results showed that TiO₂ were excitated by UV light to produce electrons, which deoxidized PMoA to produce heteropolyblues. The photochromic process of PMoA/TiO₂ system was carried through electron transfer mechanism.     

Atomic Force Microscopic Studies of Porous TiO2 Thin Films Prepared by the Sol-Gel Method

Porous titanium dioxide thin films were prepared from alkoxide solutions with and without polyethylene glycol (PEG) by the sol-gel method on soda-lime glass. The effects of PEG addition to the precursor solution on the microstructure and roughness of the resultant thin films were investigated by atomic force microscopy (AFM). It was found that TiO₂ films prepared from the precursor solution without PEG had granular microstructure and flat texture, and was composed of about 100 nm spherical particles. With an increase in the times of coating cycles, the roughness of films decreased and the size of TiO₂ particles increased. On the other hand, the larger the amount and molecular weight of the added PEG in precursor solutions, the larger the diameter and the depth of pores in the resultant films on the decomposition of PEG during heat-treatment. The surface of the films was also rougher, and fewer pores were produced during heat-treatment. The mechanism of porous structure formation in the TiO₂ films was explained using the principle of spinodal phase separation.     

Magnetic and magneto-optical properties of Cu-doped Bi,Ga:DyIG and Bi,Al:DyIG films prepared by sol-gel

Cu doped Bi,Al:DyIG and Bi,Ga:DyIG thin films have been prepared on glass substrates by sol-gel method. As-deposited films were amorphous, and after annealing polycrystalline magnetic thin films could be obtained. X-ray diffraction pattern showed that the films were garnet phase with no preferred crystal orientation. The H _c value of 7 kOe was obtained in Cu doped Bi, Al:DyIG films, and the Faraday rotation angle was about 7°/µm at the wavelength of 500 nm. An extremely high H _c value of 13 kOe at room temperature has been got in Bi, Ga:DyIG films, and the Faraday rotation angle was 8°/µm at the wavelength of 510 nm for the optimum value of Ga content. The perpendicular magnetic anisotropy (Ku) of garnet films on glass substrate resulted from the inverse magnetostriction. The influence of doping and garnet composition on magnetostriction has been studied. The mechanism of increasing coercive force by Cu doping could be attributed to Cu entering lattice sites.     

Properties and Photoelectrocatalytic Behaviour of Sol-Gel Derived TiO2 Thin Films

Titanium dioxide (TiO₂) thin films have been prepared on indium doped tin oxide (ITO) glass by sol-gel dip-coating method. Properties of the films were determined as a function of heat-treatment by X-ray diffraction, scanning electron microscopy and photoelectrochemical tests. The films heat-treated at higher temperatures show better crystallinity and photoresponse. The microscopic structure on the film after heat-treatment is attributed to the incorporation of organic polymer into the precursor solution. The performance of the electrodes treated at different temperature on photoelectrocatalytic degradation of methyl orange was investigated. The effect of applied potential and the ability of the electrode to be repeatedly used in photoelectrocatalytic degradation were also evaluated.     

The Effect of SiO2 Addition on the Grain Size and Photocatalytic Activity of TiO2 Thin Films

The uniform transparent TiO₂/SiO₂ nanometer composite thin films were prepared via sol-gel method on the soda lime glass substrates, and were characterized by X-ray photoelectron spectroscopy (XPS), FTIR spectroscopy, UV-VIS spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and BET surface areas. It was found that the addition of SiO₂ to TiO₂ thin films could suppress the grain growth of TiO₂ crystal and increase the hydroxyl content of the surface of TiO₂ films. The photocatalytic activity of the as-prepared TiO₂/SiO₂ composite thin films increases for SiO₂ content of less than 5 mol%.