Comparison of TiO2 and ZrO2 Films Deposited by Electron-Beam Evaporation and by Sol-Gel Process

TiO2 and ZrO2 films are deposited by electron-beam （EB） evaporation and by sol-gel process. The film properties are characterized by visible and Fourier-transform infrared spectrometry, x-ray diffraction analysis, surface roughness measure, absorption and laser-induced damage threshold （LIDT） test. It is found that the sol-gel films have lower refractive index, packing density and roughness than EB deposited films due to their amorphous structure and high OH group concentration in the film. The high LIDT of sol-gel films is mainly due to their amorphous and porous structure, and low absorption. LIDT of EB deposited film is considerably affected by defects in the film, and LIDT of sol-gel deposited film is mainly effected by residual organic impurities and solvent trapped in the film.     

Structural study of sol-gel Au/TiO2 films from nanopowders

TiO₂ represents one of the most important sol-gel materials, due to its photocatalytic properties, in the case of both powders and coatings. Nanostructured titania has been reported to be used in many applications in different fields ranging from optics to gas sensor via solar energy. Recent researches point out the existence of new procedures used in order to enhance the efficiency of the photocatalytic process. The metal ion doping is such an example. Two types of 2 wt.% Au containing TiO₂ powders have been embedded in sol-gel vitreous TiO₂ matrices. Au-doped TiO₂ films have been prepared from these sols, by dipping procedure using quartz microscopic slides, as substrates. The relationship between the synthesis conditions and the properties of titania nanosized materials, such as thermal stability, phase composition, crystallinity, and the influence of dopant was investigated. The hydrophilic properties of the films were correlated with their structure, composition and surface morphology.     

溶胶-凝胶法制备发光薄膜现状

发光薄膜在对比度、分辨率、热传导、均匀性、与基底的附着性、释气速率等方面都显示出较强的优越性,在平板显示领域具有很好的应用背景。本文结合我们的工作综述了通过溶胶－凝胶工艺制备发光薄膜的基本过程、薄膜的表征方法、发光薄膜的当前发展及应用情况。依据组成特点,溶胶－凝胶法制备的发光薄膜可分为无机发光薄膜和有机／无机杂化发光薄膜,它们的光致发光、阴极射线发光、场发射发光和电致发光等性质都已被广泛研究。我们除了采用硅酸酯为主要原料制备了一些硅酸盐基发光薄膜外,还以无机盐为主要原料通过Pechini溶胶－凝胶法制备了稀土离子掺杂的钒酸盐发生薄膜,并结合毛细管微模板技术实现了发光薄膜的图案化。最后,我们对未来溶胶－凝胶法制备发光薄膜的发展及应用情况进行了展望。     

Fiber-optic pH sensor based on sol-gel film immobilized with neutral red

In this study, we developed a fiber-optic pH sensor based on a sol-gel film immobilized with neutral red (NR). A solgel film was prepared by mixing tetramethylorthosilicate (TMOS), trimethoxymethylsilane (MTMS), ethanol (EtOH), distilled water (H₂O), and NR powder. Accordingly, the thin pH sol-gel film was fabricated through a sol-gel process with a dip-coating method. The thickness and diameter of the fabricated pH sol-gel film are 0.11 and 0.6 mm, respectively. We measured the optical absorbance and the light intensity with the spectra of reflected light, which change with the color variation of the pH sol-gel film in the fiber-optic sensing probe. From the experimental results, we demonstrated that the proposed fiber-optic pH sensor has good reversibility, reproducibility, and a fast response time, in which the optical properties of the NR-based pH sol-gel film change with the pH value.     

Fabrication and characterization of superhydrophobic thin films based on TEOS/RF hybrid

Preparation of superhydrophobic silica-based thin film by adjusting different concentration of reverse (W/O) emulsion of resorcinol formaldehyde resin (re-RF) which was hybridised with silica sol has been developed. The hybrid films were coated by the mixing solution which included precursor solution (sol-gel process) and re-RF (sol-gel process). Rough surfaces were obtained by removing the organic polymer at high temperature and then the hydrophobic groups bonded onto the films were obtained by the reaction with trimethylchlorosilane (TMCS). Characteristic properties of the as-prepared cross-section and surface of the films were analyzed by scanning electron microscopy (SEM) and atom force microscopy (AFM). The experimental parameters are mainly varied the weight ratio of re-RF to silica sol from 0.2 to 4.0. The result showed that the contact angle of the modified silica film was greater than 160° when the weight ratio of re-RF to silica sol was 2.0.     

Preparation, structural and photoluminescent properties of CeO2:Eu films derived by Pechini sol-gel process

In this study, CeO₂ and CeO₂:Eu films were prepared by a simple Pechini sol-gel process and dip-coating method. CeO₂ were successfully synthesized by hydrolysis of cerium nitrate. Thermogravimetric analysis was used to study the thermal chemical properties of sol-gel powder. Structural properties of CeO₂ films annealed at different temperature ranging from 400 to 900 °C were investigated by X-ray diffraction, field emission scanning electron microscopy, and Fourier transform infrared spectroscopy. Luminescent properties of CeO₂:Eu³⁺ films were investigated by excitation and emission spectra. Our results show that CeO₂ is a good host material for rare earth ions doping and Pechini sol-gel process is a useful method to derive high quality, macrocrack free, pure and doped CeO₂ films.     

Structural and optical properties of ZnO thin films prepared by sol-gel method with different thickness

In this work, ZnO thin films with different thickness were prepared by sol-gel method on glass substrates and the structural and optical properties of these films were studied by X-ray diffractometer, atomic force microscope, UV-visible spectrophotometer, ellipsometer and fluorophotometer, respectively. The structural analyses show that all the samples have a wurtzite structure and are preferentially oriented along the c-axis perpendicular to the substrate surface. The growth process of highly c-axis oriented ZnO thin films derived from sol-gel method is a self-template process. With the increase of film thickness, the structural disorder decreases and the crystalline quality of the films is gradually improved. A transition of crystal growth mode from vertical growth to lateral growth is observed and the transition point is found between 270 and 360 nm thickness. The optical analyses show that with the increase of film thickness, both the refractive index and ultraviolet emission intensity are improved. However, the transmittance in the visible range is hardly influenced by the film thickness, and the averages are all above 80%.     

长周期光纤光栅气敏薄膜传感器结构优化

基于三包层长周期光纤光栅模型,研究了包层表面涂覆一层溶胶凝胶气敏薄膜的长周期光纤光栅化学传感器的灵敏度Sn与薄膜光学参量(折射率n3和厚度h3)和光纤光栅结构参量(光栅周期、折变量和光栅长度)之间的关系。采用最优化数值方法,找到了获得高灵敏度所需的最佳膜层光学参量和光栅结构参量。理论计算表明,该类型传感器对膜层折射率的测量分辨率高达10-8。实验上制作了对乙醇气体敏感的传感器,并证实了传感器结构优化的必要性。     

间苯二酚-甲醛凝胶自发成膜技术研究

 以间苯二酚和甲醛为原料，对水相溶胶-凝胶聚合自发成膜技术获得间苯二酚-甲醛(RF)凝胶薄膜进行了研究。主要研究了溶胶-凝胶过程中冰醋酸（HAC）含量和反应温度对凝胶过程的影响，分析了RF有机凝胶自发成膜的形成机理。IR和SEM分析表明，所得到的凝胶膜具有典型的RF有机气凝胶结构，薄膜厚度大约为50 μm，膜由直径10 μm左右的粒子组成，没有观察到明显的孔洞结构。分析认为，在间苯二酚和甲醛占总溶液的质量分数为67％左右及控制pH值在一定的酸性范围，RF凝胶自发成膜过程和机理可以用RF凝胶的收缩机理加以解释，RF自发膜的表面形貌及形成机理与均匀泡沫的连续相分离机理类似。     

Influence of annealing process on conductive properties of Nb-doped TiO2 polycrystalline films prepared by sol-gel method

Nb-doped TiO₂ (TNO) thin films were prepared by sol-gel dip-coating method with Nb content in a wide range of 0-20 at.%. The prepared films were preheated at 400 °C and then undertaken by two different post-annealing processes: (a) three times vacuum annealing and (b) multi-round annealing. The designed multi-round annealing was shown to be an effective way to improve the conductive properties of the films, compared to the traditional vacuum annealing process. The minimum resistivity reached approximately 0.5 Ω cm with Nb doping concentration around 12 at.%, and the carrier density increased with Nb-doping concentration until the critical point of 12 at.%, which might be the optimal doping content for our TNO films prepared by sol-gel method.     

Chemical and structural analysis of low-temperature excimer-laser annealing in indium-tin oxide sol-gel films

We investigated the influence of excimer-laser annealing (ELA) on the electrical, chemical, and structural properties of indium–tin oxide (ITO) films prepared by a solution process. The ITO film was prepared by the sol-gel method and annealed by excimer-laser pulses with an energy density up to 240?mJ/cm². Hall measurements showed that the ELA substantially enhanced the electrical properties of the ITO films, including their resistivity, carrier density, and mobility, as increasing the laser energy density. In-depth x-ray photoelectron spectroscopy analysis of the chemical states in the film surface showed that the ELA reduced carbon species and promoted both an oxidation and crystallization. These changes were consistent with results of x-ray diffraction and transmission electron microscopy measurements, where expansions in the microcrystal growth were observed for higher laser energy density. We comprehensively understand that the chemical rearrangement and concomitant crystallization are the main factors for achieving the electrical properties during the ELA. These results suggest the potential of the ELA-treated sol-gel films for providing high-quality ITO films at low temperatures toward the flexible device applications.     

退火对ZnO:Al薄膜光致发光性能的影响

 采用溶胶-凝胶工艺在石英衬底上制备ZnO:Al（AZO）薄膜，通过不同温度的退火处理，研究了退火对AZO薄膜结构和光致发光特性的影响。XRD图谱表明：所制备的薄膜具有c轴高度择优取向，随着退火温度的升高，(002)峰的强度逐渐增强，同时(002)峰的半高宽逐渐减小,表明晶粒在不断增大。未退火样品的光致发光（PL）谱由361 nm附近的紫外带边发射峰和500 nm附近的深能级发射峰组成。样品经退火后，以500 nm为中心的绿带发射逐渐减弱，而带边发射强度有所增强,并且逐渐红移到366 nm附近，与吸收边移动的测试结果相吻合。对经过不同时间退火的样品分析表明，AZO薄膜的发光特性与退火时间也有很大关系，时间过短可见波段的发射较强，但时间过长会使晶粒发生团聚，导致紫外发射峰强度减弱。     

溶胶-凝胶-蒸镀法制备高性能FTO薄膜

以SnCl_4·5H_2O为锡源,SnF_2为氟源,采用溶胶-凝胶-蒸镀法制备F掺杂的SnO_2透明导电氧化物薄膜(FTO薄膜).通过正交实验研究确定最佳反应温度、反应时间和蒸镀温度等制备条件.主要研究元素F的掺杂和膜的结构对FTO薄膜性能的影响,并采用傅里叶变换红外光谱仪、热重-差热分析、X射线衍射、高分辨透射电子显微镜和扫描电子显微镜等进行样品的性能表征.研究结果表明,当反应温度50?C、反应时间5 h、烧结(蒸镀)温度600?C、镀膜次数1次、而F/Sn=14 mol%时,FTO薄膜性能指数ΦTC最大,综合光电性能最优,表面电阻为14.7?·cm-1,平均透光率为74.4%.FTO薄膜内颗粒的平均粒径为20 nm,呈四方金红石型结构,F的掺入替代了部分的O,形成了SnO_(2-x)F_x晶体结构.F的掺杂量是影响FTO薄膜的主要因素,F过多或过少均不利于SnO_(2-x)F_x晶体的生长;FTO薄膜的结构、颗粒形状、大小等三维信息也是影响薄膜性能的因素,主要表现为分形维数越小,薄膜表面越平整,势垒越低,导电性能越好.     

溶胶-凝胶法制备ZnO薄膜及其光致发光性质

利用溶胶-凝胶法在石英衬底上制备了ZnO薄膜,通过测量样品的透射谱、X射线衍射谱、扫描电子显微镜(SEM)图像和光致发光谱研究了其结构特征和发光性质.结果表明:在衍射角2θ=34.32°处出现了对应(002)晶面的强衍射峰,ZnO膜呈多晶状态,具有六角纤矿晶体结构和良好的C轴择优取向,薄膜中颗粒的平均粒径为56nm;光致发光呈多发光峰状,有中心波长为378nm的紫带,520nm绿带,446nm附近的蓝带以及发现未见报道过的绿带以后中心波长为586nm和570nm两个弱发射峰.实验结果表明,制备的ZnO薄膜具有发光特性,但内部与深能级发射相关的结构缺陷浓度还是较高,样品中两个低能量光致发光应来源于晶粒间界的缺陷能级,多缺陷能级导致了多发射峰的光致发光谱.     

退火温度对溶胶-凝胶法制备Na掺杂 ZnO薄膜的结构和光学特性的影响

采用溶胶-凝胶旋涂法在Si(100)衬底上制备Na掺杂ZnO薄膜,退火温度分别为873,973,1 073 K。研究了退火温度对Na掺杂ZnO薄膜形貌、微观结构和光学性能的影响。室温光致发光谱显示,在973 K下退火的样品具有中心位于361 nm处尖锐而强的紫外发光峰,在388,425 nm处各有一个比较弱的紫色和蓝色发光峰,在可见光范围内发光峰的强度很弱。     

Study on the properties of Pb(Zr,Ti)O3 thin films grown alternately by pulsed laser deposition and sol-gel method

In order to prepare good quality Pb(Zr,Ti)O₃ (PZT) thin films, we consider the method of alternately growing PZT thin films on Pt (111)/Ti/SiO₂/Si (100) substrates by pulsed laser deposition (PLD) and sol-gel. In this work, we conducted comparative experiments on different film preparation methods, and 1.0 um thick PZT film was grown on platinized silicon wafers by an alternate PLD and sol-gel method. The microstructure and electrical properties of the films is analyzed. Through the study of X-ray diffraction, SEM, AFM, PFM, and ferroelectric testing, it is found that the alternating growth of a film by the alternate PLD and sol-gel method has good compactness, excellent ferroelectric properties, and smaller leakage current compared to film prepared by the sol-gel method alone.     

采用溶胶凝胶协同自组装方法制备SiO2反蛋白石结构薄膜及其光学性质研究

研究了溶胶凝胶协同自组装制备大面积高质量SiO₂反蛋白石结构薄膜的方法. 向单分散的聚苯乙烯(PS)胶体溶液中添加SiO₂前驱物溶液,用垂直自组装法一步得到微球空隙中均匀填充有凝胶的 复合PS胶体晶体薄膜,在空气中烧结去除PS后得到SiO₂反蛋白石结构薄膜.通过对添加前驱物溶液比例、 自组装温度以及烧结温度等参数的研究,用不同粒径的PS微球制备了不同孔径的高质量SiO₂反蛋白石结构薄膜. 用扫描电子显微镜和X射线能量色散谱仪对制备得到的薄膜样品进行显微形貌和成分表征,并测试了其透射光谱. 结果表明:溶胶凝胶协同自组装法制备的SiO₂反蛋白石结构薄膜大面积高度有序,孔径可以控制且选择范围宽; 薄膜的透射光谱带隙明显,带隙中心波长与理论计算结果相符.     

New insights in the structural and morphological properties of sol-gel deposited ZnO multilayer films

This study shows how the structural and morphological properties of sol-gel deposited ZnO films can be precisely tuned and selectively controlled. For that purpose, ZnO films have been deposited through a multilayer sol-gel route using solutions of zinc acetate dihydrate (ZAD) diluted in 1-butanol. The opto-geometrical, morphological, and structural properties of these films have been thoroughly studied in relation to the ZAD concentration in butanol, number of deposited single-layers, and heat-treatment conditions. On this basis, different physical processes occurring over the multilayer deposition procedure have been discussed to explain how the experimental parameters influence the film properties and enable to tune the grain size, texture coefficient, and surface coverage rate in a wide range of values. This work is a first step toward the optimized growth of ZnO nanowires on sol-gel films and their subsequent integration in 2D or 3D nanowire-based biosensors.     

有机掺杂溶胶-凝胶法制备pH敏感膜及其光谱响应的研究

使用四甲氧基硅烷（TMOS）和二甲基二甲氧基硅烷（DiMe-DMOS)为共先驱体，采用溶胶－凝胶的有机掺杂，制备对pH具有宽程响应的敏感膜。详细考察了包埋溴酚蓝和溴酚绿的敏感膜对pH的响应值、响应时间、泄漏和可逆性等响应性能指标，并进行了溴酚蓝和溴酚绿在水相与膜内吸收光谱的研究。     

(Li,Cu)掺杂ZnO薄膜的发光性质

利用溶胶-凝胶(Sol-gel)法在n型si(100)衬底上制备(Li,Cu)掺杂ZnO薄膜,研究了室温下薄膜的结构、形貌和光致发光性能.研究结果表明,随着Li掺杂浓度的增加,可见光发光强度增加,可见光发射可能是源于单电离氧窄位到价带顶以及单电离氧空位到Li替位Zn(Lizn)受主跃迁的双重作用.与此类似,Cu掺杂Zn...