水热处理对ZnO薄膜微结构及光学性能的影响

基于溶液工艺和水热处理制备了ZnO薄膜。采用椭圆偏振光谱分析仪,原子力显微镜,X射线衍射仪研究和分析了水热处理温度对薄膜的微观形貌,光学特性,晶体结构的影响。实验结果表明,水热处理温度由110℃升高到130℃,薄膜光学带隙由3.19eV增大到3.31eV,而薄膜表面粗糙度从19.3nm降到12.9nm。然而,当处理温度超过140℃后,与130℃下处理的膜相比质量显著劣化。此外,130℃下水热处理的膜与500℃下高温退火的膜对比表明水热法有相似的光学特性,同时,XRD分析表明水热处理能改善晶体特性。证明了利用水热处理能够极大地降低溶液法制备ZnO薄膜所需的退火温度。     

X射线反射法和椭圆偏振法结合测量热处理溶胶-凝胶ZrO2薄膜的结构和光学参数

采用溶胶-凝胶法在硅片基底上制备ZrO2薄膜,在150℃～750℃范围内不同温度下进行热处理,研究了热处理对膜层结构和光学性能的影响。X射线反射用于膜层厚度和界面粗糙度分析,结果表明热处理温度由150℃升至750℃,膜层厚度由常温状态下的112.3nm减小到34.0nm,表面和界面粗糙度均小于2nm。以X射线反射法测得的膜层厚度为初始值,对椭圆偏振仪的测量结果进行拟合,得到不同温度的膜层折射率,结果表明热处理温度为550℃时膜层折射率达到最大值。X射线反射作为直接的膜层厚度测试手段,所得结果为准确分析椭偏光谱提供了参考。     

偏压对电弧离子沉积锆膜性能的影响

为研究偏压对通过电弧离子沉积法沉积的锆膜性能的影响,并探究锆膜在不同存储条件下的氧化程度,通过调整沉积过程偏压的大小以及占空比制备多组试样,利用扫描电子显微镜、X射线测厚仪、X射线衍射仪以及纳米划痕仪对薄膜的表面形貌、沉积速率、薄膜结构、膜基结合力进行了研究。并利用X射线光电子能谱测试了锆膜在不同存储状态下的氧化程度。结果表明,偏压的增大会提升膜层表面光洁度。但因高能粒子反溅射作用的增强,会降低薄膜的沉积速率。同时,膜基结合力随着偏压的增大有升高的趋势,且膜层的(100)晶面择优趋势会逐渐减小。另外,偏压占空比的增加也会导致沉积速率下降。锆膜表面的氧化层厚度随着时长会逐渐增大,且膜层在大气中暴露一天的氧化程度比真空存储(10^-5 Pa)半年严重。     

不同周期数GDC/YSZ多层电解质薄膜的电学性能与结构稳定性

利用反应磁控溅射方法在蓝宝石单晶衬底上制备了调制周期相同、周期数不同的GDC/YSZ纳米多层薄膜,采用X射线衍射、原子力显微镜对薄膜结构、粗糙度、生长形貌进行了表征,利用交流阻抗谱仪测试了多层薄膜不同温度下的电学性能。结果表明衬底上首层薄膜是整个多层膜的生长模板,首先沉积GDC时多层膜呈无规则生长而首先沉积YSZ时多层膜为（111）织构;GDC/YSZ多层膜的生长是一个逐渐粗糙化的过程,随着薄膜厚度的增大（周期数的增多）,多层膜粗糙度与晶粒尺寸增大;随着周期数的增多,多层膜电导率逐渐增大,但电导活化能基本保持不变（约1.3eV）;在500～800℃下退火,多层膜结构稳定,但由于薄膜晶粒长大,导致其电导率小幅降低（降低百分比〈5%）。     

离子束溅射制备CdS多晶薄膜及性能研究

采用离子束溅射的方法在玻璃衬底上制备CdS多晶薄膜,研究了沉积过程中基底温度(100～400℃)与薄膜厚度(35～200nm)对其微结构与光电性能的影响。结果表明,不同基底温度下制备的CdS薄膜均属于六方相多晶结构且具有(002)择优取向生长特征;随着基底温度的升高,(002)特征衍射峰强度增加,半高宽变小相应薄膜结晶度增大,有利于颗粒的生长;分析CdS薄膜的光谱图线可知,薄膜在可见光区平均透射率高于75%,光学带隙值随着基底温度升高而增大(2.33～2.42eV)且薄膜电阻高达109Ω;在基底温度为400℃条件下制备不同厚度的CdS薄膜,发现(50～100nm)较薄的CdS薄膜具有较为明显的六方相CdS多晶薄膜结构、较优光学性能和高电阻值,满足CIS基太阳电池中缓冲层材料的基本要求。     

Si片上PbTiO3薄膜的XPS研究

用溶胶 凝胶方法在Si上成功地制备了钙钛矿型的PbTiO3薄膜。X射线衍射结果显示 ,在热处理温度为 750～ 90 0℃范围内 ,随温度升高 ,薄膜由多晶结构转变为定向结晶。X射线光电子能谱分析发现 ,薄膜表面存在SiO2 薄层 ,其厚度大约为 0 6nm ,该薄层是在制膜过程中衬底Si通过PbTiO3薄膜扩散到表面与大气中的O2 反应而形成的。在 750℃热处理的薄膜 ,膜层中不含SiO2 ,但温度升高 ,膜层中存在SiO2 成分 ,这可能是Si在向表面扩散过程中与膜中的O反应生成的。表面SiO2 可通过Ar离子的轻微溅射而消除 ,而膜内SiO2 成分只能通过调节工艺参数来消除     

PECVD下基底温度对SiC薄膜形态、成分及生长速度的影响

在单晶Si和多晶Cu基底表面上使用等离子体增强化学气相沉积(PECVD)方法沉积了SiC薄膜. 通过高分辨透射电子显微镜(HRTEM)、X射线光电子能谱仪(XPS)及扫描电子显微镜(SEM)研究基底温度对SiC薄膜成分、结构及生长速度的影响规律。结果表明: 在60~500℃基底温度下制备的SiC薄膜均为非晶态薄膜, 薄膜的生长速度随基底温度的升高而线性降低, 并且在相同沉积条件下, 薄膜在Si基底上的生长速度要高于Cu基底。此外, 薄膜中的硅碳原子比随基底温度的升高而降低, 当基底温度控制在350℃左右时, 可以获得硅碳比为1:1较理想的SiC薄膜。     

溅射Si/Ge多层膜及其发光誊性研究

采用离子束溅射技术,在玻璃衬底上制备了不同周期数的Si/Ge多层膜样品.利用X射线小角衍射、Raman散射光谱和室温光致发光(PL)对样品进行表征.结果表明,2.0～2.3eV之间的发光带是由薄膜中的各种缺陷形成的;1.77～1.84eV之间的发光带来自薄膜中的非晶结构和晶粒间的缺陷;1.53eV发光峰则可能源于纳米Ge晶粒发光.     

真空热处理制备β-FeSi2光电薄膜的研究

磁控溅射法沉积的Fe／Si多层膜和Fe单层膜经真空热处理后制备了β-FeSi2薄膜。[Fe1nm／Si3.2nm]60多层膜在〈880℃温度下真空热处理2h后，样品均呈现β（220）／（202）择优取向，而Fe单层膜制备的样品则易形成β-FeSi2与ε-FeSi相的混合物，且取向杂乱。在920℃真空热处理后，两种样品都形成了α-FeSi2薄膜。原子力显微镜分析表明，样品表面粗糙度随热处理温度升高而变大，最大表面均方根粗糙度约为16nm。卢瑟福背散射分析发现，Fe／Si多层膜样品热处理过程中元素再分布很小。根据光吸收谱测量，Fe／Si多层膜制备的β-Fesi2薄膜的禁带宽度为0．88eV。     

基于原子层沉积技术制备氧化钽薄膜及其特性研究

本工作以单晶硅为衬底,乙醇钽和水分别为钽源和氧源,研究原子层沉积技术制备氧化钽薄膜的工艺,考察了乙醇钽温度、衬底温度、脉冲时间等工艺条件对氧化钽薄膜的生长速率、粗糙度和表面形貌等特性的影响.通过椭偏仪、原子力显微镜、扫描电子显微镜以及高分辨X射线光电子能谱测试分析表明,制备获得的氧化钽薄膜表面光滑,粗糙度小于1 nm,薄膜生长速率受工艺参数的影响较大,其中在乙醇钽源瓶温度170℃、脉冲时间0.1 s以及衬底温度200℃时,氧化钽的生长速率为0.253?/cycle.本工作基于原子层沉积高性能氧化钽薄膜的工艺研究,将对氧化钽薄膜在介质材料、存储介质以及光学涂层等领域的应用奠定基础.     

Thickness dependent properties of nickel oxide thin films deposited by dc reactive magnetron sputtering

Nickel oxide thin films of various thicknesses were grown on glass substrates by dc reactive magnetron sputtering technique in a pure oxygen atmosphere with sputtering power of 150 W and substrate temperature of 523 K. Crystalline properties of NiO films as a function of film thickness were investigated using X-ray diffraction. XRD analysis revealed that (200) is the preferred orientation and the orientation of the films changed from (200) to (220) at film thickness of 350 nm. The maximum optical transmittance of 60% and band gap of 3.82 eV was observed at the film thickness of 350 nm. The lowest electrical resistivity of 5.1 Ω cm was observed at a film thickness of 350 nm, thereafter resistivity increases with film thickness.     

基底温度对直流溅射Nb掺杂TiO2薄膜性能的影响

采用陶瓷靶直流磁控溅射,以玻璃为基底制备2.5wt%Nb掺杂TiO2薄膜,控制薄膜厚度在300~350 nm,研究了不同基底温度下所制得薄膜的结构、形貌和光学特性.XRD分析表明,基底温度为150℃、250℃和350℃时,薄膜分别为非晶态、锐钛矿(101)和金红石相(110)结构.基底温度250℃时,锐钛矿相薄膜的晶粒尺寸最大,约为32 nm.薄膜表面形貌的SEM分析显示,薄膜粗糙度和致密度随基底温度升高得到改善.薄膜的平均可见光透过率在基底温度为250℃以内约为70%,随基底温度升高至350℃,平均透过率下降为59%,金红石相的存在不利于可见光透过.Nb掺杂TiO2薄膜的光学带宽在3.68~3.78 eV之间变化.基底温度为250℃时,锐钛矿相薄膜的禁带宽度最大,为3.78 eV.     

纳米TiO2薄膜的脉冲激光沉积及其光学特性

采用脉冲激光沉积技术(PLD)在硅基片上生长了二氧化钛纳米晶氧化物薄膜, 系统讨论了基片温度、氧分压等因素对薄膜结构特性的影响.X射线衍射结果表明在氧气氛下, 生长的薄膜为锐钛矿结构, 其结晶性随着基片温度的升高而增强, 在750℃、5Pa氧压的情况下为完全c轴取向的锐钛矿相TiO₂薄膜, 在750℃、5Pa氩气氛下则为(110)取向的金红石相薄膜. 场发射扫描电子显微镜结果表明薄膜表面致密, 呈纳米晶结构, 其晶粒尺寸在35nm左右.用傅立叶红外光谱和拉曼光谱对不同条件下制备的TiO₂薄膜进行了表征.紫外-可见透射光谱的测试结果表明, 薄膜在可见光区具有良好的透过率, 计算得到制备的锐钛矿和金红石相TiO₂薄膜在550nm处的折射率分别为2.3和2.5, 其光学带隙分别为3.2和3.0eV.因此通过沉积条件的改变可得到结晶性能和光学性能都不同的TiO₂薄膜.     

ZnO thin films prepared by pulsed laser deposition

Zinc oxide (ZnO) thin films were deposited on soda lime glass substrates by pulsed laser deposition (PLD) in an oxygen-reactive atmosphere. The structural, optical, and electrical properties of the as-prepared thin films were studied in dependence of substrate temperature and oxygen pressure. High quality polycrystalline ZnO films with hexagonal wurtzite structure were deposited at substrate temperatures of 100 and 300 °C. The RMS roughness of the deposited oxide films was found to be in the range 2-9 nm and was only slightly dependent on substrate temperature and oxygen pressure. Electrical measurements indicated a decrease of film resistivity with the increase of substrate temperature and the decrease of oxygen pressure. The ZnO films exhibited high transmittance of 90% and their energy band gap and thickness were in the range 3.26-3.30 eV and 256-627 nm, respectively.     

Effect of Al Doping on Structural, Electrical, Optical and Photoluminescence Properties of Nano-Structural ZnO Thin Films

The nano-structural Al-doped ZnO thin films of different morphologies deposited on glass substrate were successfully fabricated at substrate temperature of 350 C by an inexpensive spray pyrolysis method. The structural, electrical, optical and photoluminescence properties were investigated. X-ray diffraction study revealed the crystalline wurtzite (hexagonal) structure of the films with nano-grains. Scanning electron mi- croscopy (SEM) micrographs indicated the formation of a large variety of nano-structures during film growth. The spectral absorption of the films occurred at the absorption edge of ～410 nm. In the present study, the optical band gap energy 3.28 eV of ZnO decreased gradually to 3.05 eV for 4 mol% of Al doping. The deep level activation energy decreased and carrier concentrations increased substantially with increasing doping. Exciting with the energy 3.543 eV (λ=350 nm), a narrow and a broad characteristic photoluminescence peaks that correspond to the near band edge (NBE) and deep level emissions (DLE), respectively emerged.     

CdS薄膜的SILAR法制备与表征

采用液相薄膜制备工艺-SILAR(连续离子层吸附反应)法,在室温下于玻璃衬底上制备了CdS薄膜.对薄膜的表面形貌,薄膜的生长速率以及热处理与薄膜的成相及其电阻率的关系进行了观察和分析.实验结果表明:薄膜表面较致密,生长速率为2nm/cycle,随循环次数的增加,沉积粒子的尺寸趋于增大.室温下沉积的CdS薄膜为非晶态,经热处理后薄膜的结晶度提高,电阻率显著下降.此外,文章结合实验对薄膜的生长机理进行了初步的讨论.     

Influence of substrate properties on the growth of titanium films: part III

The growth of thin Ti-oxide films (12 nm) on alumina substrate films formed by reactive evaporation of Ti in an oxygen atmosphere was studied by in situ internal stress measurements under ultra high vacuum conditions and transmission electron microscopy. Oxygen pressure and substrate temperatures were the varied parameters of the reactive evaporation. These Ti-oxide-films with different oxygen content (O₂/Ti-films) were then used as substrate films for the deposition of a clean titanium film. The growth stress of the titanium film on the as-deposited O₂/Ti-substrate films is comparable with that previously found for H₂O/Ti-substrates and indicates island growth and the formation of polycrystalline titanium films. Annealing (400°C, 20 min) of the as-deposited – amorphous – O₂/Ti-films gives rise to the formation of crystalline TiO₂. The amount of TiO₂ formed during annealing is strongly dependent on the oxygen content of the O₂/Ti-film. The oxygen content, in return, is dependent on oxygen partial pressure and substrate temperature during O₂/Ti-film deposition. The corresponding changes in the substrate film properties (oxygen content, crystallinity, etc.) are reflected in significant changes in the growth stress of the titanium film. The stress vs. thickness curve of these titanium films appears to indicate a superposition of the growth stress of two different growth modes, i.e. growth of a polycrystalline film with island growth on the as-deposited, amorphous oxide substrate and epitaxial growth of a quasi single crystalline film on the crystalline TiO₂-substrate.     

Ellipsometric studies of microscopic surface roughness of CdS thin films

Analysis of changes in surface roughness of CdS thin films with preparation temperature was carried out using variable angle spectroscopic ellipsometry (VASE). The films studied were prepared by spray pyrolysis technique, in the substrate temperature range 200–360°C. The VASE measurements were carried out in the visible region below the band gap (E _g=2·4eV) of CdS so as to reduce absorption by the film. The thickness of the films was in the range 500–600 nm. Bruggeman’s effective medium theory was used for analysis of the surface roughness of the film. The roughness of the film had a high value (∼ 65 nm) for films prepared at low temperature (200°C) and decreased with increase in substrate temperature. This reached minimum value (∼ 27 nm) in the temperature range 280–300°C. Thereafter roughness increased slowly with temperature. The growth rate of the films was calculated for different temperature ranges. It was found that the deposition rate decreases with the increase in substrate temperature and have an optimum value at 300°C. Above this temperature deposition rate decreased sharply. The scanning electron micrograph (SEM) of the film also showed that the film prepared at 280–300°C had very smooth surface texture.     

A study of thin films of V2O5 containing molybdenum from an evaporation boat

An attempt was made to produce thin films of vanadium oxide by evaporating V₂O₅ in vacuum using molybdenum boats. Following analysis of the films by X-ray photoelectron spectroscopy and Rutherford backscattering spectrometry, it was found that the films contained a large amount of molybdenum (atomic ratio of Mo:V>1). Films were chemically inhomogeneous along the direction of growth such that the value of the atomic ratio decreased from the substrate side of the film to its interface with the air. However, a study of the optical properties of the films revealed that they were optically homogeneous. The films went through a semiconductor-to-metal phase transition at a temperature of approximately 200 °C. When annealed in vacuum at a temperature of 275 °C, it was found that, (a) the films remained amorphous, (b) there was a loss of oxygen leading to an increase in their electrical conductivity, (c) their thickness decreased leading to a larger refractive index of the films, and (d) their band gap energy shifted to a higher photon energy by approximately 0.1 eV.     

TiN/TiC multilayer films deposited by pulse biased arc ion plating

TiN/TiC multilayer films were deposited on high-speed-steel (HSS) substrates using pulse biased arc ion plating. For comparison, TiN and TiC films were also deposited. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Auger electron spectroscopy (AES) were applied to investigate the modulation period thickness, microstructure and content depth distribution of the films, respectively. And microhardness and film/substrate adhesion were also analyzed using knoop tester and scratching method. The results showed that the multilayer films with different modulation period of 40-240 nm exhibit a modulation structure and the interface width is about 20∼30 nm. Microhardness of the multilayer films were not obviously improved compared to that of TiN and TiC film, and the reason was analyzed. In comparison to TiN film, film/substrate adhesion values of the multilayer films were deteriorated with the increasing of modulation period due to the brittle characteristics of TiC film.