感应耦合等离子体增强射频磁控溅射沉积ZrN薄膜及其性能研究

利用感应耦合等离子体(ICP)增强射频磁控溅射技术在Si(111)片和M2钢表面制备了ZrN薄膜,研究了基片的温度和ICP功率对ZrN薄膜的结构以及性能影响.研究发现：在基片温度≤300℃沉积的ZrN薄膜择优取向为(111);基片温度达到450℃时薄膜出现ZrN(200)衍射峰,ZrN(111)晶面的织构系数明显降低.传统磁控溅射沉积薄膜为柱状结构,当ICP为200 W,基片温度为300℃时沉积薄膜中柱状晶体消失;随着基片温度的升高,N/Zr元素比例降低,并且薄膜的电阻率下降;相对于传统溅射,ICP增强射 关键词： 感应耦合等离子体 磁控溅射 ZrN 微结构     

基片温度对磁控溅射HfO2薄膜结构和性能影响分析

在纯氧条件下,采用直流磁控溅射技术在单晶硅基片上沉积氧化铪（HfO2）薄膜,并研究了沉积过程中基片温度对薄膜结构和性能的影响规律。利用X射线衍射仪（XRD）和X射线能谱（XPS）表征了薄膜的晶体结构和组分,利用原子力显微镜（AFM）观察薄膜表面形貌,利用纳米力学测试系统表征了薄膜的纳米硬度和弹性模量。结果表明:磁控溅射制备的HfO2薄膜样品呈(111)择优生长,其晶粒尺寸随着基片温度的升高而增大,但其晶型并不发生转变。随着基片温度的增加,基片中的硅元素向薄膜内扩散,影响了薄膜的化学计量比。沉积薄膜的表面形貌和力学性能亦受到其结构和组分变化的影响。在200 ℃条件下制备的HfO2薄膜纯度高,O、Hf元素化学计量达到了1.99,其表面质量和力学性能均达到了最佳值,随着基片温度升高至300 ℃以上,薄膜纯度下降,表面质量和力学性能均产生劣化。     

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.     

基片温度对SiNx薄膜结晶状态及机械性能的影响

利用微波电子回旋共振增强磁控反应溅射法在不同基片温度下制备无氢SiNx薄膜.通过傅里叶变换红外光谱、透射电子显微镜、台阶仪、纳米硬度仪等表征技术,研究了基片温度对SiNx薄膜结晶状态、晶粒尺寸、晶体取向等结晶性能以及薄膜的生长速率、硬度等机械性能的影响,并探讨了薄膜结晶性能与机械性能之间的关系.研究结果表明,在基片温度低于300℃时制备的SiNx薄膜以非晶状态存在,硬度值仅为18 GPa左右;基片温度在320-620℃范围内,SiNx薄膜中出现纳米晶粒,且晶粒尺寸随沉积温度的增加而增加,在沉积温度为620℃时达到最大,为20±1.5 nm;当沉积温度为700℃时,SiN<,x>薄膜的晶粒尺寸突然减小,但由于此时晶粒密度为最大,因此薄膜硬度达到最大值(36.7 GPa).     

二氧化钛薄膜的制备及退火对其形貌、结构的影响

利用磁控溅射技术,在石英基片上沉积Ti膜,分别在400、600、700、900℃的大气中退火获得TiO2薄膜。采用这种制备方式获得的TiO2薄膜呈现不同的颜色,退火温度为400℃的样品为暗紫红色,600℃时为黑色,而在700℃和900℃时均为黄色。采用X射线衍射、扫描电子显微镜（SEM）以及Raman光谱等手段研究了退火温度对TiO2薄膜的结构和形貌的影响。结果表明：退火温度为400℃时,TiO2薄膜为锐钛矿相,温度升高至600℃时,几乎转变为金红石晶相,但仍存在微量锐钛矿相,温度升高至700℃以上,则完全转变为金红石晶相。由XRD衍射图可知退火温度为700℃和900℃时,薄膜的金红石相沿（101）晶面择优取向。     

离子束溅射沉积Ti-Ni薄膜及其电化学性能的研究

利用离子束溅射沉积的方法在不同基片温度条件下制备了不同成分的Ti-Ni贮氢薄膜，研究了其电化学贮氢性能。结果表明：用离子束溅射沉积制备的Ti-Ni薄膜的结构为非晶状，薄膜对基片的附着力较强，在冲放电循环50次后仍为非晶态；在基片温度为350℃时制备的薄膜的结构为晶态，在多次放电循环后呈现非晶化趋势；Ti-Ni薄膜具有较高的电化学活性，晶化薄膜比晶态薄膜的最大放电容量高，但晶化薄膜的循环稳定性差。     

退火温度对TiO_2纳米薄膜酒精气敏特性影响的研究(英文)

采用直流磁控溅射的方法在Al2O3陶瓷管、硅基片上溅射制备了二氧化钛(TiO2)纳米薄膜材料.将薄膜样品放入管式退火炉中分别在500℃, 700℃和1100℃温度下退火.由于退火温度的不同,薄膜的晶体结构、晶粒尺寸、晶向以及气敏特性都有所不同.利用X射线衍射(XRD)技术和薄膜气敏特性测试,分析了退火温度对薄膜气敏特性的影响.分析结果表明退火温度在500℃时,呈现锐钛矿结构,薄膜具有很好的选择性、很短的反应(恢复)时间.对TiO2薄膜表面进行修饰,发现此TiO2薄膜的最佳工作温度为370℃左右.薄膜的气敏机理也得到了讨论.     

磁控溅射制备纳米TiO2半导体薄膜的工艺研究与光谱分析

通过射频反应磁控溅射在玻璃基片上制备TiO2薄膜。采用X射线衍射仪和Raman光谱仪研究退火温度对薄膜晶体结构的影响;还探讨了磁控溅射氧分压对薄膜性能的影响。结果表明：磁控溅射制备的薄膜在不同温度下退火。300℃退火时薄膜没有结晶;400℃退火出现锐钛矿结构;500℃退火后薄膜锐钛矿结构更完善,（101）方向开始优先生长,是因为锐钛矿结构更完整。随着退火温度的升高晶粒长大拉曼光谱出现红移,拉曼光谱所反应的锐钛矿信息增强,500℃退火时197cm-1出现了Eg振动模式。和标准的单晶TiO2体材料相比,拉曼峰位置都略有红移是纳米量子尺寸效应造成的。氩氧比分别为9∶1、7∶3和6∶4溅射制备的薄膜通过400℃退火后的XRD衍射谱没有明显的区别,但拉曼光谱显示氩氧比为7∶3时结晶要完善些。     

生长温度对磁控溅射ZnO薄膜的结晶特性和光学性能的影响

采用反应射频磁控溅射方法，在Si (100) 基片上制备了具有高c轴择优取向的ZnO薄膜.利用 原子力显微镜、透射电子显微镜、X射线衍射分析、拉曼光谱等表征技术，研究了沉积温度 对ZnO薄膜的表面形貌、晶粒尺度、应力状态等结晶性能的影响；通过沉积温度对透射光谱 和光致荧光光谱的影响，探讨了ZnO薄膜的结晶特性与光学性能之间的关系.研究结果显示， 在室温至500℃的范围内，ZnO薄膜的晶粒尺寸随沉积温度的增加而增加，在沉积温度为500 ℃时达到最大；当沉积温度为750℃时，ZnO薄膜的晶粒尺度有所减小；在室温至750℃的范 围内，薄膜中ZnO晶粒与Si基体之间均存在着相对固定的外延关系；在沉积温度低于500℃时 ，制备的ZnO薄膜处于压应变状态，而750℃时沉积的薄膜表现为张应变状态.沉积温度的不 同导致ZnO薄膜的折射率、消光系数、光学禁带宽度以及光致荧光特性的变化，沉积温度对 紫外光致荧光特性起着决定性的作用.此外，探讨了影响薄膜近紫外光致荧光发射的可能因 素. 关键词： ZnO薄膜 表面形貌 微观结构 光学常数     

Ag/TiO2纳米材料的制备和光致变色性能研究

 采用光催化还原法在不同温度热处理的TiO2薄膜表面沉积Ag纳米颗粒,制备了Ag/TiO2纳米薄膜材料。通过UV-Vis吸收光谱表征对比了不同温度热处理的TiO2对Ag粒子光催化沉积的影响,发现500℃退火处理TiO2薄膜较利于Ag纳米粒子的光催化沉积;在650 nm红色激光照射下,500℃退火处理的Ag/TiO2样品具有明显的光致变色现象,对此变色过程中涉及的机理进行了讨论,且发现随着Ag纳米颗粒光催化沉积时间的增长,Ag/TiO2薄膜光致变色的响应速率提高,但Ag纳米颗粒过多会抑制Ag/TiO2薄膜的变色响应速率。     

Effects of depositing temperatures on structure and optical properties of TiO2 film deposited by ion beam assisted electron beam evaporation

TiO₂, which is high in refractive index and dielectric constant, plays an important role in the fields of optics and electronics. In this work, TiO₂ films were prepared on glass substrates by the technique of ion beam assisted electron beam evaporation. The films were deposited at 50, 150 and 300 °C, respectively. Then the as-deposited TiO₂ films were annealed at 450 °C for 1 h in vacuum atmosphere. Structures and optical properties of TiO₂ films were characterized by XRD, SEM, ellipsometry and spectrophotometer. As a result, the structure and the refractive index of films were improved by both the annealing and the increasing of the deposition temperature. The UV-vis transmittance spectra also confirmed that the deposition temperature has a significant effect on the transparency of the thin films. The highest transparency over the visible wavelength region of spectra was obtained at the deposition temperature of 300 °C. The allowed direct band gap at the deposition temperature ranging from 50 to 300 °C was estimated to be in the range from 3.81 to 3.92 eV.     

大面积六硼化镧薄膜阴极制备及性能

 采用电子束蒸发方法在大面积玻璃基底和钽基底上沉积六硼化镧薄膜阴极。分别对玻璃基底上沉积的六硼化镧薄膜的生长取向、附着力与不同蒸发角度(0°, 30°,45°和60°)的关系进行了研究;对钽基底上沉积的六硼化镧薄膜阴极的逸出功进行了研究。结果表明:在基底温度为250 ℃时,制备的六硼化镧薄膜具有(100)晶面择优生长的特点;蒸发角度为45°时,六硼化镧薄膜(100)晶面的晶格常数与靶材相差最小,晶粒较小;根据优化的工艺制备的六硼化镧薄膜阴极的逸出功为2.56 eV。     

The structure and photocatalytic activity of TiO2 thin films deposited by dc magnetron sputtering

This paper seeks to determine the optimal settings for the deposition parameters, for TiO₂ thin film, prepared on non-alkali glass substrates, by direct current (dc) sputtering, using a ceramic TiO₂ target in an argon gas environment. An orthogonal array, the signal-to-noise ratio and analysis of variance are used to analyze the effect of the deposition parameters. Using the Taguchi method for design of a robust experiment, the interactions between factors are also investigated. The main deposition parameters, such as dc power (W), sputtering pressure (Pa), substrate temperature (°C) and deposition time (min), were optimized, with reference to the structure and photocatalytic characteristics of TiO₂. The results of this study show that substrate temperature and deposition time have the most significant effect on photocatalytic performance. For the optimal combination of deposition parameters, the (1 1 0) and (2 0 0) peaks of the rutile structure and the (2 0 0) peak of the anatase structure were observed, at 2θ ∼ 27.4°, 39.2° and 48°, respectively. The experimental results illustrate that the Taguchi method allowed a suitable solution to the problem, with the minimum number of trials, compared to a full factorial design. The adhesion of the coatings was also measured and evaluated, via a scratch test. Superior wear behavior was observed, for the TiO₂ film, because of the increased strength of the interface of micro-blasted tools.     

Effects of γ rays irradiation on structure and property of TiO2 thin films

TiO₂ thin films were deposited on a glass substrate by the radio frequency magnetron sputtering method, and annealed for 2 h at temperatures of 550°C. Then, ⁶⁰Co γ rays with different doses were used to irradiate the resulting TiO₂ thin films. The surface features of films before and after irradiation were observed by scanning electron microscope (SEM). Simultaneously, the crystal structure and optical properties of films before and after irradiation were studied by X-ray diffraction (XRD), UV–VIS transmission spectrum and Photoluminescence (PL) spectrum, respectively. The SEM analysis shows that the film is smooth with tiny particles on the film surface, and non-crystallization trend was clear after irradiated with γ rays. The XRD results indicated that the structure of the film at the room temperature mainly exists in the form of amorphous and mixed crystal at a sputtering power of 200 W, and non-crystallinity was more obvious after irradiation. Obvious difference can be found for the transmissibility of the irradiated and pre irradiation TiO₂ films by the UV-VIS spectra. The color becomes light yellow, and the new absorption edge also appeared at about 430 nm. PL spectra and photocatalysis experiments indicate that the photocatalysis degradation rate of the TiO₂ films on methylthionine chloride solution irradiated with the maximum dose can be increased to 90%.     

Preparation and photoelectrochemical performance of Ag/graphene/TiO2 composite film

By dipping-lifting in sol-gel solution and reducing process, the graphene/TiO₂ composite film on the glass plate was first prepared. Then, the Ag/graphene/TiO₂ composite film was fabricated by interface reaction with AgNO₃ and N₂H₄·H₂O on the surface of graphene/TiO₂ composite film. The characterization results show that the uniform porous TiO₂ film is made up of the anatase crystal, and the Ag/graphene/TiO₂ composite film is constructed by doping or depositing graphene sheets and Ag nanoparticles on the surface of TiO₂ film. The photoelectrochemical measurement results indicate that the Ag/graphene/TiO₂ composite film has an excellent photoelectrochemical conversion property.     

超高温度系数V0.97W0.03 O2多晶薄膜的制备研究

将V₂O₅粉体与WO₃粉体均匀混合并压制成靶，用离子束增强沉积加后退火技术在SiO₂衬底上制备掺钨VO₂多晶薄膜.X射线衍射表明，薄膜取向单一，为VO₂结构的［002］相,晶格参数d比VO₂粉晶增大约0.34%；薄膜从半导体相向金属相转变的相变温度约28；室温(300 K)时的电阻-温度系数(TCR)可大于10%/K，是目前红外热成像薄膜TCR的四倍.W离子的半径大于V离子的半径，W的掺入在薄膜中引入了张应力,使薄膜相变温度降低到室温附近，是IBED V_0.97W_0.03O₂薄膜的室温电阻温度系数提高的原因. 关键词： 二氧化钒薄膜 薄膜掺杂 离子束增强沉积     

Impact of substrate temperature and film thickness on the interfacial evolution during atomic layer deposition of HfO2 on InP

The effects of both the deposition temperature and the HfO₂ film thickness on the interfacial layer (IL) evolution were studied when tetrakis(ethylmethylamino)hafnium and H₂O based atomic layer deposition (ALD) was performed on InP substrates. While the self‐cleaning effect resulted in an IL‐free structure after formation of ～2 nm thick HfO₂ at 200 °C and 250 °C, substantial IL growth occurred at 300 °C, probably due to simultaneous InP oxidation. Following further growth to ～8 nm at 300 °C, the IL was almost removed and, in particular, a significant In incorporation into the HfO₂ film was observed, which was attributed to IL decomposition and subsequent out‐diffusion of the constituent elements. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

单斜相HfO2薄膜弹性常数的第一性原理计算

用电子束蒸发沉积在K9玻璃基底上镀制HfO2薄膜,沉积温度为200℃,蒸发速率为0.03nm/s。由X射线衍射谱可知薄膜出现明显结晶,且为单斜相和正交相混合结构,其中单斜相占明显优势。用Jade5软件分析得到单斜相HfO2的晶格常数a,b,c以及晶格矢量a和c之间的夹角β。基于得到的晶格常数建立了单斜相HfO2薄膜的晶体结构模型。同时建立固态单斜相HfO2的晶体结构模型进行对比。通过密度泛函理论(DFT)框架下的平面超软赝势法,采用两种不同的交换关联函数:局域密度近似(LDA)中的CA-PZ和广义梯度近似(GGA)中的质子平衡方程(PBE),计算了薄膜态和固态单斜晶相HfO2的弹性刚度系数矩阵Cij和弹性柔度系数矩阵Sij,Reuss模型、Voigt模型和Hill理论下的体积模量和剪切模量,材料平均杨氏模量和泊松比。此外还计算得到薄膜态和固态单斜晶相HfO2在不同方向上的杨氏模量。     

Low-temperature liquid phase deposited TiO2 films on stainless steel for photogenerated cathodic protection applications

The low-temperature synthesis of anatase TiO₂ films was an imperative requirement for their application to corrosion prevention of metals. In this paper, a liquid phase deposition (LPD) technique was developed to prepare TiO₂ films on SUS304 stainless steel (304SS) at a relatively low temperature (80 °C). The as-prepared films were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy and X-ray photon spectroscopy (XPS). It was observed that a dense and crack-free anatase TiO₂ film with a thickness about 300 nm was obtained. The film contained some fluorine and nitrogen elements, and the amounts of these impurities were greatly decreased upon calcination. Under the white light illumination, the electrode potential of TiO₂ coated 304SS rapidly shifted to a more negative direction. Moreover, the photopotential of TiO₂/304SS electrode showed more negative values with increased film thickness. In conclusion, the photogenerated cathodic protection of 304SS was achieved by the low-temperature LPD-derived TiO₂ film.