液氮冷却法全无机智能窗器件的制备及其性能研究

为降低溅射过程中摹片温度的上升,进而成功制备非晶多孔、纳米微晶态电致变色薄膜和非晶态离子导电薄膜,介绍了一种配置于磁控溅射设备的液氮冷却装置.利用该装置制备了由WO3、NiOx和LiNbO3 薄膜组成的单基片全无机电致变色智能窗器件.采用分光光度计对该器件的电致变色性能进行了测试,并计算了它的漂白和着色态在400 nm到800 nm波长范围内的平均透射率.实验结果表明,经过50次循环后,该器件的漂白和着色态的平均透射率分别为61.5%和5.5%.X射线衍射和扫描电镜(SEM)图像显示,组成该器件的WO2、NiOx和LiNbO3薄膜分别为非晶多孔、纳米微晶和非晶态结构.     

非晶态WO3薄膜电致变色特性的研究

采用射频溅射三氧化钨粉末靶的技术，在不同的氧分压条件下沉积得到非晶态WO3电致变色薄膜，分析得知氧分压为1∶10的样品变色性能更好些.采用x射线衍射(XRD)，原子力显微镜(AFM)，伏安特性曲线和分光光度计分析所制备薄膜的特性.将薄膜在15mol/L的LiClO4的丙稀碳酸脂（PC）溶液进行电化学反应.发现氧分压在1∶10的情况下沉积得到的薄膜呈非晶态，薄膜有较多的孔隙，这有利于Li+的抽取，进而显示出很好的变色性能.x射线光电子能谱(XPS)成分分析表明WO3薄膜在原态中只有W和O两种原子电色反应后 关键词： 三氧化钨薄膜 非晶 射频溅射 电致变色     

磁控溅射法制备钛掺杂WO3薄膜结构和性能的研究

采用中频孪生非平衡磁控溅射技术制备钛掺杂WO_3薄膜。运用X射线衍射(XRD),拉曼光谱、紫外分光光度计、计时安培分析仪和原子力显微镜(AFM)等测试手段分析了钛掺杂WO_3薄膜的结构和光学性能。实验结果表明,掺杂后的薄膜在相同的热处理条件下晶化程度降低,晶粒细化,离子抽出和注入的通道大大增多,钛掺杂原子数分数0．051的着色响应速度提高,循环寿命提高了4倍以上,但着色后透射率下降。     

聚合物前驱体法制备WO_3薄膜的电致变色性能

以偏钨酸铵为钨源,Pluronic F127为配位聚合物,在FTO导电玻璃上制备了WO3薄膜,研究了配位聚合物含量对WO3薄膜电致变色性能的影响。实验结果表明,制备的WO3薄膜属于立方晶相;随着Pluronic F127含量的增大,WO3薄膜表面粗糙度增大,电荷容量先增大后减小;当Pluronic F127的含量为26%时,WO3薄膜的电荷容量最大,电致变色性能最好,可见光区域的透光率光学调制范围达到62.68%,光学密度差达到0.864,且着色态的太阳能总透射率低于褪色态的,制备的薄膜具有较好的节能效果。     

新型AgInSbTe相变薄膜的光学及记录性能

利用直流磁控溅射法制备了一种新型AgInSbTe相变薄膜。示差扫描量热(DSC)实验测定的结晶峰温度为193．92℃。X射线衍射(XRD)表明未经热处理的沉积态薄膜是非晶态,而经过200℃热处理,X射线衍射图出现衍射峰,薄膜从非晶态转变到晶态。同时,研究了晶态和非晶态相变薄膜的吸收率、透射率和反射率随波长的变化。测定了650nm激光作用下的相变薄膜的记录性能,分析了记录功率、记录脉宽对薄膜反射率衬比度的影响,在同一记录脉宽条件下,记录功率越大,反射率衬比度也越大;在同一记录功率条件下,随记录脉宽的增加,反射率衬比度也增大。结果表明,新型AgInSbTe相变薄膜在激光作用下具有较高的反射率衬比度,可获得良好的记录性能。     

三氧化钨晶体拓扑结构生长行为及其电致变色性能

本研究利用种子层辅助的水热反应法,在导电玻璃上沉积生长三氧化钨(WO3)晶体结构薄膜.通过调控水热反应溶液中盐酸、草酸的浓度以及后处理温度,分别得到花朵状、海胆状和多孔花瓣状的WO3晶体结构薄膜.采用扫描电子显微镜、X射线衍射、透射电子显微镜和电化学表征等手段研究了不同拓扑结构形成的机理及其对WO3电致变色性能的影响....     

WO3/Ag复合薄膜的制备及其电致变色性能

通过水热法在导电玻璃上合成WO_3纳米块,利用电沉积技术在WO_3纳米块上负载不同含量(20 s、50 s、80 s)的Ag纳米粒子,成功制备出WO_3/Ag复合薄膜.通过X射线衍射分析、扫描电子显微镜与能谱对WO_3/Ag复合薄膜进行表征,利用电化学测试与光谱测试,得到电致变色可逆性、响应时间、着色效率和光谱透过率等参数,并对其电致变色性能进行分析.结果表明,对比单一WO_3纳米块薄膜的电致变色性能,WO_3/Ag复合薄膜的电致变色性能显著增强.同时研究了不同Ag纳米粒子含量对WO_3/Ag复合薄膜电致变色性能的影响,研究表明沉积50 s的WO_3/Ag复合薄膜具有最优异的电致变色性能.     

氧化法结合快速热处理制备VOx薄膜及其性质研究

采用磁控溅射法在单晶Si〈100〉基底上沉积金属钒(V)薄膜,在高纯氧环境下快速热处理制备具有相变特性的氧化钒(VOx)薄膜.利用X射线衍射仪、X射线光电子能谱和扫描电子显微镜对薄膜结晶结构、薄膜中V的价态与组分及表面微观形貌进行分析,应用四探针测试方法和太赫兹时域频谱技术对样品的电学和光学特性进行测试.结果表明:在一定范围的快速热处理保温温度和保温时间下,都可以制备出具有热致相变特性的氧化钒薄膜,相变前后薄膜的方块电阻变化超过两个数量级,薄膜成分主要由V2O5和VO2混合组成,薄膜中V整体价态不因热处理条件改变而不同.在快速热处理条件范围内,500℃ 25 s左右条件下(中温区)制备出的氧化钒薄膜相变特性最佳,并且对THz波有一定的调制作用.     

旋涂法制备WO3薄膜电致变色性能

"智能窗"大规模推广顺应可持续发展潮流,三氧化钨(WO_3)是生产"智能窗"的一种重要电致变色材料,但调控WO_3薄膜电致变色性能机制仍待进一步研究。采用旋涂法制备WO_3薄膜,重点研究了溶液浓度和旋涂次数对调控WO_3薄膜电致变色性能的影响。通过表面轮廓仪测量薄膜厚度,X射线衍射(XRD)测量薄膜结晶情况,原子力显微镜(AFM)和扫描电子显微镜(SEM)分析薄膜表面形貌,光谱仪测量薄膜初始态、着色态和褪色态的透射率。实验结果表明,随着溶液浓度增加(0. 2～1. 0 mol/L),薄膜厚度从9. 7 nm增加到33. 3 nm,透射率调制能力从0%提升到37. 0%;多次旋涂薄膜厚度线性增长,线性拟合优度(R~2)达0. 98,5次旋涂后透射率调制能力达51. 3%。改变溶液浓度和旋涂次数都是调控薄膜透射率调制能力的有效手段,精准调控薄膜透射率调制能力对设计不同应用场景的电致变色器件具有重大意义。     

全固态塑料电致变色器件

电致变色器件是一种典型的光学薄膜和电子学薄膜相结合的光电子薄膜器件,能够在外加低压驱动的作用下实现可逆的色彩变化。将电致变色材料制备在塑料衬底上,将极大地推动电致变色器件的应用。讨论了全固态塑料电致变色器件的制备工艺和电致变色特性,通过采用低压反应离子镀工艺分别在ITO塑料衬底上制备了WO3和NiO电致变色薄膜。采用高分子聚合物MPEO-LiClO4作电解质,制备plastic/ITO/WO3/MPEO-LiClO4/NiO/ITO/plastic透射型全固态塑料电致变色器件。在二电极电池石英盒中采用恒电位方式测试全固态塑料电致变色器件的电致变色特性,驱动电压为±3V。采用分光光度计直接测试透射光谱的变化,测试范围为300～900nm,经过十几次循环后达到稳定的变色,变色调制范围达到30%左右,器件样品显示出均匀深蓝色的电致变色效果。实验结果证明了所提出的全固态塑料电致变色器件的制备工艺的可行性。     

温度条件对反应电子束蒸发制备TiO2薄膜结构和性能的影响

研究基片温度(120～300 ℃)和热处理温度(400℃)对电子束蒸发TiO₂薄膜的结构和光学性能的影响.XRD分析表明,在120 ℃, 200 ℃和300 ℃的普通玻璃基片上采用电子枪加热蒸发制备的TiO₂薄膜具有非晶态结构,沉积态薄膜经过400 ℃保温1 h的热处理后得到的相为具有(004)取向的锐钛矿相,晶粒大小在3.6～8.1 nm之间.透射谱分析表明,薄膜的折射率随着基片温度的升高而增加;热处理后,薄膜的折射率也相应提高,其原因来自于薄膜的晶化.     

Optical properties of high transmittance aluminum oxynitride thin films for spectral range from near ultraviolet to visible

In this study, high transmittance aluminum oxynitride films were deposited by ion beam sputtering at room temperature. The nitrogen working gas was fed into the ion source and the oxygen gas fed near the sputtered target. The properties of the aluminum oxynitride films were examined by a Varian Cary-5E spectrometer, atomic force microscopy, X-ray diffraction and Fourier transform infrared spectroscope. The films show high transmittance at near UV and visible light regions. The optical constants of the films, refractive index and extinction coefficient, can be controlled by varying the oxygen partial pressure.     

The effect of temperature on the preparation of electrochromic nickel oxide by an electroless method

The advantages of nickel oxide as an electrochromic material are due to its good contrast of transmittance and its suitable use as a secondary electrochrome. Compared to other methods of depositing eletrochromic nickel oxide, coating nickel oxide by electroless is simple and easy to scale-up for industrial application. This study presents the preparation of nickel oxide film on an ITO substrate by an electroless method and oxidizing it with heat treatment. The influence of oxidizing temperature in heat treatment procedures is notable. The morphology of the film was analyzed by a scanning electron microscope (SEM) and X-ray diffraction (XRD). Heat temperature at 380 °C obtained optimal of electrochromic properties. The transmittance difference (ΔT) of the film at 630 nm was maintained at 69%, and the amount of transferred charge during cyclic voltammetry was approximately 0.8 mC/cm² after 1000 cycles of redox, which was operated between −1.5 and +1.5 V potential step. The degradation of the film was decreased by increasing the oxidizing temperature. The evidences showed electrochromic abilities of nickel oxide were affected by heat-treatment procedures. All these analyses provided a novel method for preparing the electrochromic nickel oxide in a low-cost way.     

生长条件对脉冲激光沉积制备ZnO：Al薄膜光电性能的影响

本文研究了脉冲激光沉积(PLD)生长过程中, 铝掺量、氧压及衬底温度等实验参数对ZnO:Al(AZO)薄膜生长的影响, 并利用扫描电子显微镜、原子力显微镜、X射线衍射、霍尔效应、光透射光谱等实验手段对其透明导电性能进行了探讨. 变温霍尔效应和光透射测量表明, 当靶材中铝掺量大于0.5 wt%时, 所制备AZO薄膜中铝施主在80 K时已完全电离, 因Bernstein-Moss (BM) 效应其带隙变大, 均为重掺杂简并半导体. 进一步系统研究了氧压和衬底温度对AZO薄膜透明导电性能的影响, 实验发现当氧压为1 Pa, 衬底温度为200 ℃时, AZO 导电性能最好, 其霍尔迁移率为28.8 cm²/V·s, 薄膜电阻率最小可达2.7×10^-4 Ω·cm, 且在可见光范围内光透过率超过了85%. 氧压和温度的增加, 都会导致薄膜电阻率变大. 关键词： 脉冲激光沉积法 ZnO：Al薄膜 透光性 导电性     

在不同衬底上制备的ZnO薄膜透射率的研究

采用反应磁控溅射在不同结构衬底上生长ZnO薄膜,通过X-ray衍射(XRD)及透射光谱来分析薄膜的成膜情况,并得出在Al₂O₃/AlN复合基上溅射沉积的ZnO薄膜比单独在AlN薄膜衬底的结晶质量好且透过率也较高。而经不同的快速热退火温度验证,发现在400 ℃时,ZnO薄膜的结晶化及在(002)方向上的择优取向达到最好,并在可见光范围内的平均透过率达到88%以上。当退火温度超过450 ℃时,温度过高改变了ZnO薄膜的内部结构,使其氧原子和锌原子发生了较大距离的位移,导致薄膜内部缺陷的增多,从而存在过多的晶界,增加了其薄膜的散射机制,使光的透过性变差,退火温度为500 ℃时,薄膜的平均透过率为80%。     

Electrochromic and photoluminescence properties of cobalt oxide thin films prepared by spray pyrolysis

Cobalt oxide thin films were prepared by a facile spray pyrolysis technique, using a perfume atomizer with an aqueous solution of hydrated cobalt chloride salt with a molar concentration of 0.025?M as a source of cobalt. The films were deposited onto glass substrates at temperature of 350?°C. The structural, morphological, and electrochromic properties of the obtained films were studied. It was found from X-ray diffraction analysis that the films were polycrystalline in nature with spinel-type cubic structure and preferred orientation along [111] direction. The Scanning Electron Microscopy images revealed a porous structure with the average grain size around 200?nm. The cyclic voltammetry measurements revealed that Cobalt oxide thin film is an anodically coloring electrochromic material with a transmittance variation in the visible range of 31%, and a fast response time (about 2?seconds) and a good cycling stability. These electrochromic performances make cobalt oxide thin film an attractive material for using as an anodic electrochromic material in smart windows devices. The photoluminescence spectra exhibited a strong emission in the visible region confirming the good crystallinity properties of Co₃O₄ thin films.     

Nanoporous nickel oxide thin films and its improved electrochromic performance: Effect of thickness

Electrochromic properties of chemically bath deposited nanoporous NiO thin films were investigated as a function of film thickness using Ni sulphate precursor, aqueous ammonia and potassium persulphate as complexing and oxidizing agents respectively. The films were characterized for their structural, morphological, optical and electrochromic properties using X-ray diffraction, scanning electron microscopy, FT-IR spectroscopy, cyclic voltammetry, chronoamperometry and optical transmittance studies. X-ray diffraction patterns show that the films are polycrystalline, consisting of NiO cubic phase. Infrared spectroscopy results show the presence of free hydroxyl ion and water in NiO thin films. SEM micrographs revealed nanoporous nature composed of interconnected nanoporous network, forming well defined 3D nano envelopes. The optical band gap energy was found to be decreased from 3.22 to 2.80 eV with increasing film thickness. The electrochromic properties of all the films were investigated in aqueous (KOH) and non aqueous (LiClO₄-PC) electrolyte by means of cyclic voltammetry (CV), chronocoulometry (CC) and optical studies. The transmittance modulations or optical density differences during the coloring/bleaching process were found to be increased with the film thickness. This increment in optical differences led to an increase in coloration efficiency (CE) to about 95 cm²/C, which is two times more than that observed in KOH and response time of 2.9 s for bleaching (reduction) and 3.5 s for coloration (oxidation) observed for the film deposited at 60 min with excellent electrochemical stability up to 3000 c/b cycles in LiClO₄-PC electrolyte.     

Influence of post-deposition annealing on the structural,optical and electrical properties of Li and Mg co-doped ZnO thin films deposited by sol–gel technique

Lithium (Li) and magnesium (Mg) co-doped zinc oxide (ZnO) thin films were deposited by sol–gel method using spin coating technique. The films were deposited on glass substrates and annealed at different temperatures. The effects of annealing temperature on the structural, optical and electrical properties of the deposited films were investigated using X-ray diffraction (XRD), Ultraviolet–Visible absorption spectra (UV–VIS), photoluminescence spectra (PL), X-ray photo electron spectroscopy (XPS) and Hall measurements. XRD patterns indicated that the deposited films had a polycrystalline hexagonal wurtzite structure with preferred (0 0 0 2) orientation. All films were found to exhibit a good transparency in the visible range. Analysis of the absorption edge revealed that the optical band gap energies of the films annealed at different temperatures varies between 3.49 eV and 3.69 eV. Room temperature PL spectra of the deposited films annealed at various temperatures consist of a near band edge emission and visible emission due to the electronic defects, which are related to deep level emissions, such as oxide antisite (O_Zn), interstitial zinc (Zn_i), interstitial oxygen (O_i) and zinc vacancy (V_Zn) which are generated during annealing process. The influence of annealing temperature on the chemical state of the dopants in the film was analysed by XPS spectra. Ion beam analysis (Rutherford back scattering) experiments were performed to evaluate the content of Li and Mg in the films. Hall measurements confirmed the p-type nature of the deposited films.     

热处理对制备辉光放电聚合物薄膜结构及光学性能的影响

利用低压等离子体聚合技术制备了约5 μm的辉光放电聚合物薄膜, 将所制备的样品放入热处理炉中通入氩气保护, 分别在280 ℃, 300 ℃, 320 ℃, 340 ℃进行热处理. 对热处理后的样品采用傅里叶变换红外吸收光谱(FT-IR)分析了不同热处理温度对薄膜结构的影响. 对CH振动区进行了分峰高斯拟合, 定量的分析了个官能团的变化. 利用紫外可见光谱仪分析了热处理前后薄膜在紫外–可见光区域内光学透过率及光学带隙的变化. 结果表明: 随着热处理温度的升高,薄膜中H含量减少, 薄膜中甲基相对含量减少, 而双键、芳香环结构相对含量增加, 在600 nm以后的可见光区, 薄膜的透过率减小. 薄膜光透过率的截止波长红移, 光学带隙减小. 关键词： 热处理 薄膜结构 等离子体聚合 光学性能