Structural, Optical and Luminescence Properties of ZnO Thin Films Prepared by Sol-Gel Spin-Coating Method： Effect of Precursor Concentration

Transparent zinc oxide（ZnO） thin films are fabricated by a simple sol-gel spin-coating technique on glass substrates with different solution concentrations（0.3-1.2 M） using zinc acetate dehydrate [Zn（CH_3COO）_2·2H_2O] as precursor and isopropanol and monoethanolamine（MEA） as solvent and stabilizer, respectively. The molar ratio of zinc acetate dehydrate to MEA is 1.0. X-ray diffraction, ultraviolet-visible spectroscopy and photoluminescence spectroscopy are employed to investigate the effect of solution concentration on the structural and optical properties of the ZnO thin films. The obtained results of all thin films are discussed in detail and are compared with other experimental data.

Preparation Nano-Diamond Film by Sol-Gelled Coating Method for Field Emission Display

The mixture of Nano-graphite and organic vehicles doped to Nano-diamond paste. The suitable paste proportion was found. Nano-diamond film (NDF) was prepared by sol-gel coating method on ITO glass at 3000/min. The field emission characteristics of luminance-current, luminance-voltage and luminance-power of Nano-diamond film were analyzed and tested. Comparing these tested curves, the luminance was well proportional to current was got. Theoretic, the inner resistance of NDF field emission display (FED) consumes electric energy and real voltage change between the cathode and the anode of NDF-FED was very small after electrons emit. So the characteristic of NDF-FED was preferable to describe by luminance-current linear relationship, which was advantageous to device tested and designed.

Sol-gel derived HA/TiO_2 double coatings on Ti scaffolds for orthopaedic applications

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 dipping-coating method at a speed of 12 cm/min, followed by a heat treatment at 600 ℃ for 20 min. The HA la lyaeyre wr wasa ssu cbosaetqeude bnytl ya 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

Structure distortion, optical and electrical properties of ZnO thin films co-doped with Al and Sb by sol-gel spin coating

ZnO thin films co-doped with A1 and Sb with different concentrations and a fixed molar ratio of AlCl3 to SbCl3 at 1：2, are prepared by a sol-gel spin-coating method on glass annealed at 550 ℃ for 2 h in air. The x-ray diffraction results confirm that the ZnO thin films co-doped with Al distortion, and the biaxial stresses are 1.03× 10^8. 3.26× 10^8 and Sb are of wurtzite hexagonal ZnO with a very small 5.23 × 10^8, and 6.97× 10^8 Pa, corresponding to those of the ZnO thin films co-doped with Al and Sb in concentrations of 1.5, 3.0, 4.5, 6.0 at% respectively. The optical properties reveal that the ZnO thin films co-doped with Al and Sb have obviously enhanced transmittance in the visible region. The electrical properties show that ZnO thin film co-doped with Al and Sb in a concentration of 1.5 at% has a lowest resistivity of 2.5 Ω·cm.

Simple Preparation and Characterization of Nano-Crystalline Zinc Oxide Thin Films by Sol-Gel Method on Glass Substrate

Nanocrystalline ZnO thin films have been fabricated by a multi-step solgel method using spin coating technique. Zinc acetate dihydrate, 2-methoxyethanol and monoethanolamine were used as a starting material, solvent and stabilizer, respectively. X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) were employed to characterize structure and morphologies of the as-deposited samples. The results of XRD and SEM showed that the heat treatment conditions, final rotational (spinning) speed, fume exhaust and precise control of concentration of reactants (precursor and solvent used) strongly affect the crystallographic orientation and morphology of the resultant ZnO films. The XRD pattern showed that the ZnO films formed the preferred orientation along c-axis and the grain size is 16nm for the samples. Only one peak corresponding to the (002) plane at 2θ = 34.34 appears on the diffractograms. The as-deposited films had a transparency of greater than 80% in the visible-near IR region from 400 nm - 800 nm. The optical band gap energy and thickness were calculated to be 3.296 eV and 266 nm respectively.

Anticorrosion of WO₃-Modified TiO₂Thin Film Prepared by Peroxo Sol-Gel Method

The aim of this study was to develop a method to prepare WO3-TiO2 film which has high anticorrosion property when it was coated on type 304 stainless steel. A series of WO3-modified TiO2 sols were synthesized by peroxo-sol gel method using TiCl4 and Na2WO4 as the starting materials. TiCl4 was converted to Ti(OH)4 gel. H2O2 and Na2WO4 were added in Ti(OH)4 solution and heated at 95°C. The WO3-TiO2 sol was transparent, in neutral (pH^7) solution, stable suspension without surfactant, nano-crystallite and no annealing is needed after coating, and very stable for 2 years in stock. WO3-TiO2 sol was formed with anatase crystalline structure. These sols were characterized by XRD, TEM, and XPS. The sol was used to coat on stainless steel 304 by dip-coating. The WO3-TiO2 was anatase in structure as characterized by X-ray diffraction. There were no WO3 XRD peaks in the WO3-TiO2 sols, indicating that WO3 particles were very small, possibly incorporating into TiO2 structure, providing the amount of WO3 was very small. The TiO2 particles were rhombus shape. WO3-TiO2 had smaller size area than pure TiO2. The SEM results showed that the film coated on the glass substrate was very uniform. All films were nonporous and dense films. Its hardness reached 2 H after drying at 100°C, and reached 5 H after annealing at 400°C. The WO3-TiO2 film coated on 304 stainless steel had better anticorrosion capability than the unmodified TiO2 film under UV light illumination. The optimum weight ratio of TiO2: WO3 was 100:4.

用Sol-Gel法在PC上制备有机-无机复合耐磨涂层

用ｓｏｌ－ｇｅｌ法在聚碳酸酯ＰＣ上制备一层耐磨涂层。该涂层为有机－无机复合网络，由γ—缩水甘油醚氧丙基三甲氧基硅烷（γ—ＧＰＴＭＳ）和金属醇盐Ｔｉ（ＯＣ２Ｈ５）４合成。采用浸涂工艺，热固化后可得到几微米厚的透明涂层。用３—氨丙基三乙氧基硅烷（３—ＡＰＳ）对ＰＣ表面进行处理，可使涂层与基体的结合力大大提高。涂层的基本骨架由Ｓｉ－Ｏ－Ｔｉ组成，能显著改善ＰＣ材料的耐磨性能。

sol-gel法制备纳米TiO_2-SiO_2宽带高增透膜

通过模拟计算设计出一种透射比为99%、包含一层TiO2薄膜和一层SiO2薄膜的宽带高增透膜。两层薄膜均由溶胶-凝胶法制得并采用提拉法成形于玻璃基片上。对增透膜样品的透射比、表面形貌、膜厚等进行了表征,考察了提拉速度、退火温度、催化条件等对其透射比、表面均匀性的影响。结果表明:增透膜的使用提高了玻璃基片的透射比;当提拉速度为9cm/min,增透膜厚约为255nm时,基片在400～800nm波段的透射比提高了7%。控制退火温度,可以使增透膜在某些波段的透射比增强。增透膜样品的表面均匀性良好,室温下膜层的均方根表面粗糙度(RMS)为1.682,平均粗糙度(RA)为1.208,在550℃的温度以下,随着退火温度升高,表面粗糙度降低。

sol-gel法制备表面改性纳米氧化锌

采用Zn(NO3)2.6H2O和NH3.H2O及合适的表面改性剂,通过sol-gel前驱体法,制备了高纯度的纳米ZnO粉体。采用激光粒度分析、SEM、XRD等手段,对所制备的粉体进行了表征。并研究了主盐浓度、反应温度、反应体系的pH值、表面改性剂等因素对ZnO晶体形成过程和显微结构的影响。结果表明:在Zn2+浓度为0.1mol/L、反应体系温度为50℃、pH值为6.0,采用聚乙二醇(PEG-2000)作为表面改性剂,将制得的前驱体在400℃分解2h,获得了纯度高、分散性好、结晶完整、粒度分布窄、粒状的纳米ZnO粉体。

无机sol-gel法制备二氧化钒薄膜的研究

采用无机sol-gel法,以分析纯V2O5为原料,在Si衬底、玻璃衬底上空气中加热制备了V2O5薄膜,在不同温度下真空退火,得到了具有择优取向的VO2薄膜。研究了其制备工艺和显微结构。结果表明:在玻璃衬底和硅衬底上薄膜的最佳真空退火工艺均为480℃/2h。所制备的VO2薄膜具有沿<110>晶向生长的择优取向。薄膜表面形貌良好,颗粒尺寸分布均匀。

分散剂在sol-gel法制备PZT粉体中的应用

采用sol-gel法制备了PZT纳米粉体。针对硝酸铅会从干凝胶中析出的问题,分析了硝酸铅的析出原因,采取在溶胶中加入柠檬酸三铵作为分散剂来消除硝酸铅的偏析。实验结果表明:当柠檬酸三铵的加入量为醋酸铅的2.5%(摩尔分数)时,能得到粒度较为均匀,组成与计算配方一致的PZT纳米粉体。

sol-gel法制备纳米晶γ-Al_2O_3∶Eu^(3+)发光粉及发光性能

以异丙醇铝为原料,聚乙二醇(PEG1000)为络合剂,采用sol-gel法制备了纳米晶γ-Al2O3∶Eu3+发光粉,对其结构、形貌、晶粒尺寸及光致发光性能进行了研究。结果表明:采用sol-gel法制备工艺,经过800℃煅烧4h,可以得到发光强度高的纳米晶γ-Al2O3∶Eu3+发光粉,其最佳激发波长为395nm,最佳掺杂量为x(Eu3+)=10%,此时最强的发射峰出现在617nm附近,可以用作红色发光材料。

sol-gel法制备镉掺杂铁酸镧气敏材料

研究了气敏材料的制备条件、相组成、电导和气敏性能。结果表明:固溶体La1–xCdxFeO3(0≤x≤0.15)呈典型的p型半导体。270℃操作温度下,掺杂x(Cd2+)为25%的LaFeO3材料(700℃下热处理4h)对浓度为4.5×10–5mol·dm–3的C2H5OH的灵敏度达81.5。有望开发为一类新型的酒敏传感器。

sol-gel法制备WO_3电致变色薄膜的研究

采用正交实验设计方法,优化了钨粉过氧化聚钨酸sol-gel法制备WO3薄膜的配方,并且通过测定薄膜的物相结构、光透过率和循环伏安特性等研究了薄膜的电致变色性能。结果表明,制备WO3薄膜的最优配方为:钨粉(纯度为99.5%)6g、浓双氧水20mL、无水乙醇22mL、冰醋酸6mL。该配方所制备的薄膜具有非晶态结构,且薄膜在着色态、褪色态下的透过率之差达到50%以上。

sol-gel法制备Sr^2＋掺杂的MnZn铁氧体

以铁、锰、锌和锶的硝酸盐为原料,以酒石酸为凝胶剂,采用sol-gel法制备了Sr2+掺杂的MnZn铁氧体(Mn0.6Zn0.4-xSrxFe2O4)。借助于XRD、SEM和振动样品磁强计(VSM)等表征手段,研究和分析了Sr2+掺杂量对所得MnZn铁氧体样品晶型、晶貌及磁性能的影响。结果表明:当Sr2+的掺杂量为0.10时,所得MnZn铁氧体样品的Ms为2.1646×105A/m。

sol-gel燃烧合成CLST陶瓷

采用sol-gel法合成了CaO-Li2O-Sm2O3-TiO2(CLST)陶瓷粉体。用XRD、TEM等手段对CLST粉体和CLST陶瓷的相结构和形貌进行了表征,同时测试了不同烧结温度的CLST陶瓷的介电性能。结果表明:CLST前驱体在900℃煅烧3h,晶体结构已经完全形成,主晶相为斜方钙钛矿结构,一次粒子粒径约60nm。1150℃烧结3h时,CLST陶瓷表现出优良的介电性能:εr为110,tanδ为0.008,τf为11×10–6/℃。

sol-gel法工艺条件对ZAO薄膜晶面取向性的影响

分析了溶剂、溶胶稳定剂、溶胶浓度和热处理等工艺因素对sol-gel法制备ZAO薄膜结晶及择优取向生长行为的影响。结果发现上述各因素均需优选。采用乙二醇甲醚做溶剂,乙醇胺为稳定剂,溶胶浓度为0.75mol/L,干燥温度为80℃,预热温度为250℃,退火温度为600℃,可获得(002)高度取向的高质量ZAO薄膜,最低电阻率为1.93×10–2?·cm,可见光范围内平均透射率超过90%。

AFM研究Sol-Gel法制备的TiO_2和Al_2O_3-TiO_2-SiO_2涂膜表面形貌

载玻片在金属醇化物的溶胶中浸涂、热处理，获得厚度为５０～９０ｎｍ的ＴｉＯ２和ＸＡｌ２Ｏ３－ＹＴｉＯ２－ＺＳｉＯ２涂膜（Ｘ＝０～３０，Ｙ＝０．２５～０．６０，Ｚ＝０．２０～０．６５，摩尔分数）。使用原子力显微镜（ＡＦＭ）研究涂膜表面纳米范围的形貌。研讨了化学组成，热处理温度与时间，以及热处理前或后的贮存史对表面形貌，ｒｍｓ－均方根粗糙度和锐钛矿结晶的影响。

sol-gel法制备(002)高度定向的Li:ZnO薄膜

用sol-gel法在玻璃载玻片上旋涂3～9层制备氧化锌薄膜.用X射线衍射、扫描电镜等研究了掺Li、旋涂层数、溶胶的浓度以及热处理温度对氧化锌薄膜(002)定向性的影响.结果表明,溶胶中掺入一定量的Li可显著地促进ZnO沿(002)生长;浓度为0.45mol/L旋涂3层或浓度为0.25mol/L旋涂7层的样品,即使有Li的掺入也不能呈现较好的(002)定向性,这是由于薄膜太薄所致;提高热处理温度至610℃,有利于薄膜(002)高度定向.

Sol-Gel法制备莫来石陶瓷涂层的结构及性能

采用溶胶-凝胶法在不锈钢基体上制备了莫来石涂层。研究了助熔剂和灼烧温度对涂层表观形貌的影响。利用XRD、TG-DTA和SEM分析涂层相组成和微观结构,并对涂层的高温抗氧化性和显微硬度进行了评价和测定。结果表明:当B2O3与莫来石溶胶质量比为0.5时,在850℃下灼烧所得涂层结构致密,与基体结合力强,显微硬度高达12 GPa,在800℃下样品具有优异的抗氧化性和良好的高温稳定性。