溶胶—凝胶法制备ＴiO2纳米薄膜的晶粒长大机理研究

通过sol-gel法在普通钠钙玻璃表面制备了均匀透明的锐钛矿型ＴiO2纳米薄膜,用透射电镜（TEM)、Ｘ射线衍射（ＸＲＤ）和紫外可见吸收光谱（ＵＶ－ＶＩＳ）等对薄膜的晶粒大小和透光率进行了表征,结果表明,随着镀膜次数和热处理时间的增加,薄膜中的平均晶粒大小接近线性增加,仅增加ＴiO２薄膜的热处理时间,薄膜中晶粒长大不明显,其吸收阀值未发生明显的红移,因此,薄膜中晶粒长大的机理可能是：上一次镀的ＴiO2晶粒成了下一次镀ＴiO2溶胶的晶核,并在此基础上逐渐长大。     

SiO2／TiO2复合薄膜光催化性能的研究

采用溶胶-凝胶法和浸渍提拉法在玻璃表面镀制了SiO2/TiO2复合薄膜,以SEM,XPS,UV-Vis等手段对其进行了表征;通过对亚甲基蓝的降解反应,研究了SiO2/TiO2复合薄膜在紫外光下的光催化性能。结果表明:在玻璃片上预镀SiO2层使TiO2薄膜中的Na 和Mg2 含量明显降低,同时,有利于TiO2薄膜中晶粒的长大,提高了光催化性能。     

退火温度对TiO2薄膜结构和表面形貌的影响

研究了退火温度对中频交流反应磁控溅射技术制备的TiO2 薄膜结构和表面形貌的影响。利用X射线衍射仪和原子力显微镜 ,检测了TiO2 薄膜的晶体结构和表面形貌。实验结果显示 :沉积态TiO2 薄膜为非晶态 ;低温 (70 0℃以下 )退火后 ,TiO2 薄膜出现锐钛矿相 ,晶粒长大不明显 ;高温退火 (90 0℃以上 )后 ,薄膜转变为金红石相 ,晶粒由柱状转变为棱状 ,并迅速长大至微米量级     

微器件用Ni-W合金薄膜热稳定性的研究

研究了低应力柠檬酸胺-1-羟基乙烷二膦酸(HEDP)镀液体系中电流密度、pH值、脉冲参数和热处理条件等对Ni-W合金薄膜硬度的影响.结果表明,电镀工艺条件对硬度提高有限,热处理对Ni-W合金薄膜的硬度有明显提高.同时研究对比了沉积态及550℃热处理后Ni和Ni-W硬度、干摩擦条件下耐磨性以及微观结构的变化.实验发现:多晶的Ni薄膜经过热处理后,晶粒尺寸显著长大,硬度、耐磨性约下降2/3;而Ni-W合金薄膜经过热处理后,微观结构由非晶转变成纳米晶,薄膜仍保持良好的耐磨性,硬度提高了1倍.Ni-W合金薄膜优异的热稳定性,有望在特殊环境下取代Ni薄膜在MEMS器件上获得应用.     

热处理温度对溶胶-凝胶法制备的氧化镍薄膜的影响

以醋酸镍为原料 ,用溶胶 -凝胶法在石英衬底上制备了氧化镍薄膜 ,并利用X射线衍射、紫外 -可见吸收谱对样品进行了表征。结果表明 ,当热处理温度低于 80 0℃时 ,随着温度升高 ,石英衬底上生长的氧化镍薄膜的晶粒逐渐长大 ,其 (2 0 0 )面对应的衍射峰的强度增加 ,取向度提高。当热处理温度超过 80 0℃后 ,晶粒尺寸不但不再增加 ,反而略有下降 ,同时 ,取向度也略有下降。因此就晶粒大小及取向度而言 ,最佳热处理温度为 80 0℃ ,此时薄膜的晶粒尺寸最大 ,(2 0 0 )取向度最高。紫外 -可见吸收谱分析表明 ,氧化镍薄膜的禁带宽度也随着处理温度的变化而变化 ,其变化趋势与晶粒尺寸的变化正好相反 ,即禁带宽度在热处理温度为 80 0℃时有极小值。纳米尺寸粒子中存在的量子约束效应可以说明这一变化趋势。     

快速热处理对(Ba,Sr)TiO3薄膜晶化行为的影响

采用射频溅射法在Si(111)基片上制备了(Ba,Sr)TiO3(BST)薄膜,并对制备的薄膜进行了快速退火热处理.采用X射线衍射和原子力显微镜分析了退火温度、退火时间和加热速度对BST薄膜晶化行为的影响.研究结果表明,BST薄膜的晶化行为强烈依赖于退火温度、退火时间和加热速度.BST薄膜的结晶度随退火温度的升高而提高.适当的热处理可降低BST薄膜的表面粗糙度,BST薄膜的表面粗糙度随退火温度的升高经历了一个先降低后增大的过程,但退火后BST薄膜的表面粗糙度都小于制备态薄膜的表面粗糙度.BST薄膜的晶粒尺寸随退火温度的升高经历了一个先增大后减小的过程.随退火时间的延长,BST薄膜的特征衍射峰越来越强,薄膜的晶化程度越来越高.随退火时问的延长,BST薄膜的晶粒尺寸和表面粗糙度也经历了一个先增大后减小的过程.BST薄膜的晶粒大小主要由退火温度决定.高的升温速率可获得较小的晶粒.     

电子束蒸发法制备TiO2薄膜的折射率研究

用电子束蒸发法制备TiO2薄膜,并对其进行300℃、400℃、850℃热处理和掺杂.详细研究了工艺参数、热处理和掺杂对TiO2薄膜折射率的影响.实验结果表明:镀制高折射率的氧化钛薄膜最佳工艺参数为基片温度200℃、真空度2×10-2 Pa、沉积速率0.2 nm/s;随着热处理温度的升高,薄膜折射率也逐渐增大;适量掺杂CeO2(CeO2:Ti0质量比1.7:12)会提高薄膜的折射率,过量掺杂CeO2反而会降低折射率.     

TiO2/SiO2复合薄膜的晶化特征和结构转变研究

对TiO2／SiO2复合薄膜的晶化特征进行了分析，研究表明，随着TiO2含量的增加，其晶化温度降低，而由锐钛矿相完全转变为金红石相的速度减慢．SiO2的析晶温度也随着TiO2含量的增加而降低，即TiO2具有诱导SiO2析晶的作用．锐钛矿晶粒尺寸的增加幅度随着TiO2含量的降低和热处理温度的升高而增大．其晶粒尺寸的大小与热处理时间的平方根成正比．认为由于TiO2含量的不同，造成薄膜中由锐钛矿相完全转变成金红石相的速度差异主要来自于薄膜中应力的作用．     

金属网格对制备TiO2薄膜及其光学特征的影响

使用直流磁控溅射装置,通过在溅射过程中加入不同的金属网格,300 ℃条件下在玻璃衬底上制备了不同晶粒尺寸的TiO2薄膜.利用X射线衍射谱(XRD)、场发射扫描电子显微镜(SEM)对薄膜的结构和表面形貌进行了分析,并使用紫外一可见分光光度计研究了TiO2薄膜的透射和吸收光谱.研究结果表明:金属网格在磁控溅射过程中能有效减小TiO2薄膜的晶粒尺寸,金属网格的网孔尺寸越小,晶粒尺寸越小,吸收边蓝移越明显.     

沉积时间对磁控反应溅射制备TiO2薄膜性能的影响

应用直流磁控反应溅射法,在玻璃基体上制备了具有光催化活性的TiO2薄膜.TiO2薄膜的厚度随沉积时间的增加而均匀增长.基体温度则在溅射的最初1h很快上升到110℃,溅射7h基体温度不超过130℃.溅射2h得到的是非晶态TiO2薄膜,而溅射3～7h制备的薄膜为锐钛矿型结构.非晶态和小晶粒TiO2薄膜的紫外一可见透射光谱谱带边沿与结晶较好的TiO2薄膜相比有明显的蓝移,薄膜的透射率随沉积时间的增加而下降.钛以四价钛的形式存在于TiO2薄膜中.TiO2薄膜的光催化活性随沉积时间争薄膜厚度的增加而有较大提高.     

预涂SiO2的二氧化钛薄膜光催化活性与结构关系

载玻片上浸涂一层常温常压合成的SiO2溶胶后再浸涂TiO2溶胶制备预涂SiO2的TiO2薄膜光催化剂,结果发现浸涂一层SiO2会诱导金红石相TiO2生成,并使TiO2光催化活性提高71．75％,但预涂二层SiO2的TiO2薄膜仅有锐钛型且光催化活性较纯TiO2薄膜降低。这说明适量金红石型／锐钛型的混晶型TiO2具有更好的光催化活性。对TiO2微结构分析显示,TiO2薄膜点阵应变越大,薄膜光催化性能越好。X射线光电子能谱研究表明,预涂一层SiO2的Ti02薄膜Ti^3 含量较纯TiO2薄膜高,预涂二层SiO2的TiO2薄膜Ti^3 含量较纯TiO2薄膜低。扫描电镜分析说明,预涂SiO2的TiO2薄膜表面颗粒粒径较纯TiO2薄膜更小,薄膜颗粒粒径与光催化活性不是简单的一一对应关系。     

TiO2与聚合物复合薄膜的离子自组装制备及表征

在常温下,以钛酸丁酯[(C4H9O)4Ti]和聚四苯乙烯磺酸钠(PSS)作为前驱物在普通载玻片上用离子自组装法制备了TiO2纳米粒子/PSS复合薄膜,复合薄膜的透过率随镀膜次数或薄膜厚度的增加而呈现周期性变化。透射电镜(TEM)测试结果表明,TiO2呈板钛矿晶体结构,薄膜连续而均匀,TiO2的平均粒径是3.6nm。光电子能谱仪(XPS)测试结果显示,薄膜中含有Ti、O、C元素,载玻片表面完全被TiO2纳米复合薄膜所覆盖。     

Influence of P doping on transparent conductive property of SnO<Subscript>2</Subscript>:P thin film

P doped SnO₂ (PTO) thin films had been prepared by sol–gel dip coating method. The effect of phosphorus doping content, annealing temperature and coating times on microstructure and phase composition and optoelectrical properties of the PTO thin films were investigated by X-ray diffraction (XRD), Scanning electron microscope (SEM), four-point probe and UV–Vis spectrophotometer. The results showed that the PTO thin films exhibited the tetragonal rutile structure under all the experimental conditions. The square resistance of the PTO thin films decreased firstly and then increased with the increase of phosphorus doping content, annealing temperature and coating times. The surface smoothness and grain compactness were increased when annealing temperature increased. The PTO thin films had an optimal square sheet resistance of 8.9 kΩ/□ and high transparency of 95% in the visible region when P/Sn ratio was 2 mol% and annealing temperature was 450?°C and coating times was 14 layer.     

微波辐射溶胶-凝胶法制备TiO2薄膜及其降解铬黑T的活性

通过微波辐射溶胶一凝胶法（sol-gel）法在导电玻璃（ITO）基体上制备TiO2纳米薄膜光催化剂，考察不同加热方式、微波时间、酸处理、薄膜层数等对TiO2纳米粒子及薄膜的影响。以可见光谱（UV-VIS）、X射线衍射（XRD）对TiO2薄膜进行了表征，并通过薄膜光催化降解铬黑T溶液的性能进行了研究。实验表明，ITO玻璃表面的TiO2纳米薄膜经HNO3和微波处理后，因协同效应使薄膜的光催化活性大大增强。     

Titania powder modified sol-gel process for photocatalytic applications

Thick films of TiO₂ were prepared on glass and stainless steel substrates using an alkoxide sol-gel process modified by addition of Degussa P-25 powder. The prepared films were characterized by SEM, EDS, XRD and other methods. The TiO₂ films obtained from the powder modified sol were compared to films obtained from the alkoxide sol-gel without modification. The films obtained from the modified sol-gel were about ten times thicker for a single dip coating/heat treatment cycle than the films obtained from the sol without powder addition. The prepared thick films were smooth and free of macrocracking, fracture or flaking. The grain size of these films was uniform and in the range 100–150 nm and the films were a mixture of anatase and rutile TiO₂. The films obtained from the powder modified sol on the stainless steel substrate were also much harder compared to the films obtained from sols without modification and displayed excellent adhesion to the substrate.     

Influence of annealing temperature on the structural,topographical and optical properties of sol–gel derived ZnO thin films

This investigation deals with the effect of annealing temperature on the structural, topographical and optical properties of Zinc Oxide thin films prepared by sol–gel method. The structural properties were studied using X-ray diffraction and the recorded patterns indicated that all the films had a preferred orientation along (002) plane and the crystallinity along with the grain size were augmented with annealing temperature. The topographical modification of the films due to heat treatment was probed by atomic force microscopy which revealed that annealing roughened the surface of the film. The optical properties were examined by a UV–visible spectrophotometer which exhibited that maximum transmittance reached nearly 90% and it diminished with increasing annealing temperature.     

电泳法制备纳米TiO_2薄膜光催化性能的研究

采用电泳法在导电玻璃上镀纳米TiO2薄膜,制得的TiO2薄膜经高温烧结后进行光降解实验。通过XRD、SEM、DTA、EDS等测试分析,确定了超细微粒TiO2的外观形貌和结构特征。实验结果表明,该法制得的TiO2薄膜具有一定的厚度、均匀平整、粗糙度好。极性溶剂种类、胶体浓度、电泳电压、电泳时间、镀膜次数及掺杂离子等影响电泳成膜质量及膜对甲基橙溶液的光降解效果。     

纳米TiO2薄膜微阵列电极的制备与紫外光电阻特性表征

采用溶胶凝胶法在叉指型微阵列电极表面制备了TiO2纳米薄膜，并对薄膜形貌、厚度以及溶胶粒子尺寸进行了表征，研究了温度、紫外光照对纳米TiO2薄膜微阵列电极的电阻的影响。结果表明，溶胶粒子平均粒径在9nm，单次提拉制备的TiO2纳米薄膜膜厚为120nm，两次提拉薄膜厚度200nm，纳米TiO2薄膜微阵列电极电阻呈现半导体特性，大气环境中，紫外光照下纳米薄膜微电极的低温电阻较无光照时明显减小，表现出紫外光敏感特性。随着温度的升高，紫外光照下的电阻与无光照时电阻差值逐步减小，表明温度对纳米薄膜电阻有更大的影响。     

Low-temperature Preparation of Photocatalytic TiO2 Thin Films on Polymer Substrates by Direct Deposition from Anatase Sol

Anatase TiO2 sol was synthesized under mild conditions （75℃ and ambient pressure） by hydrolysis of titaniumn-butoxide in abundant acidic aqueous solution and subsequent reflux to enhance crystallization. At room temperature and in ambient atmosphere, crystalline TiO2 thin films were deposited on polymethylmethacrylate （PMMA）, SiO2-coated PMMA and SiO2-coated silicone rubber substrates from the as-prepared TiO2 sol by a dip-coating process. SiO2 layers prior to TiO2 thin films on polymer substrates could not only protect the substrates from the photocatalytic decomposition of the TiO2 thin films but also enhance the adhesion of the TiO2 thin films to the substrates. Field-emission type scanning electron microscope （FE-SEM） investigations revealed that the average particle sizes of the nanoparticles composing the TiO2 thin films were about 35-47 nm. The TiO2 thin films exhibited high photocatalytic activities in the degradation of reactive brilliant red dye X-3B in aqueous solution under aerated conditions. The preparation process of photocatalytic TiO2 thin films on the polymer substrates was quite simple and a low temperature route.     

Layer-by-Layer assembly of TiO2 nanoparticles for stable hydrophilic biocompatible coatings

Stable, super-hydrophilic (water contact angle approximately equal to 0 degrees) titanium dioxide nanoparticle thin films have been obtained on substrates with different initial wettability such as glass, poly(methyl methacrylate) and poly(dimethyl siloxane) using layer-by-layer nano-assembly method. Titanium dioxide nanoparticles were alternated with poly(styrene sulfonate) to form films of thickness ranging from 11 nm to 220 nm. The hydrophilicity of these thin films increases with increasing number of deposited PSS/TiO2 bilayers. It was found that 2, 5 and 20 layers were needed to form super-hydrophilic TiO2 coating on glass, PMMA and PDMS respectively. Oxygen plasma treatment of substrate surfaces enhanced the formation of homogeneous TiO2 films and accelerated the formation of hydrophilic layers. Super-hydrophilicity has been shown to be unique to PSS/TiO2 films as compared with other polyelectrolyte/nanoparticle layers, and UV irradiation may restore hydrophilicity even after months of storing of the samples. Biocompatibility of TiO2 nanoparticle films has been demonstrated by the successful cell culture of human dermal fibroblast.