用SAXS和XRD方法研究TiO2纳米颗粒微观结构

用溶胶-凝胶方法制备了TiO₂纳米样品,并对该样品在300℃到800℃温度区域进行了退火处理.应用同步辐射X射线粉末衍射(XRD)方法研究了经不同热处理温度的TiO₂纳米颗粒的结构相变.应用同步辐射小角X射线散射(SAXS)方法研究了TiO₂纳米颗粒的表面分形与界面特性.得到纳米颗粒粒度与退火温度的变化规律,讨论了表面界面特征与相变的关系. 关键词： X射线小角散射 X射线衍射 2纳米颗粒')" href="#">TiO₂纳米颗粒     

高温退火处理下SiNx薄膜组成及键合结构变化

采用等离子增强化学气相沉积法, 以氨气和硅烷为反应气体, p型单晶硅为衬底, 低温下(200 ℃)制备了非化学计量比氮化硅(SiN_x)薄膜. 在N₂氛围中, 于500–1100 ℃范围内对薄膜进行热退火处理. 室温下分别使用Fourier变换红外吸收(FTIR)光谱技术和X射线光电子能谱(XPS)技术测量未退火以及退火处理后SiN_x薄膜的Si–N, Si–H, N–H键键合结构和Si 2p, N 1s电子结合能以及薄膜内N和Si原子含量比值R的变化. 详细讨论了不同温度退火处理下SiN_x薄膜的FTIR和XPS光谱演化同薄膜内Si, N, H原子间键合方式变化之间的关系. 通过分析FTIR和XPS光谱发现退火温度低于800 ℃时, SiN_x薄膜内Si–H和N–H键断裂后主要形成Si–N键; 当退火温度高于800 ℃时薄膜内Si–H和N–H键断裂利于N元素逸出和Si纳米粒子的形成; 当退火温度达到1100 ℃时N₂与SiN_x薄膜产生化学反应导致薄膜内N和Si原子含量比值R增加. 这些结果有助于控制高温下SiN_x薄膜可能产生的化学反应和优化SiN_x薄膜内的Si纳米粒子制备参数. 关键词： x薄膜')" href="#">SiN_x薄膜 Fourier变换红外吸收光谱 X射线光电子能谱 键合结构     

基片温度与氧分压对磁控溅射制备氧化钒薄膜的影响

采用磁控溅射工艺制备了V₂O₅薄膜.通过改变制备工艺中基片温度和氧分压两个条件，研究了薄膜的晶相组成、表观形貌以及氧化物中钒和氧元素的化合价态.当基片温度升高时，V₂O₅薄膜中颗粒结晶由细长针状转变为平行于基片的片状，V⁵⁺状态保持不变，但723 K时氧结合能向高键能态移动.氧分压较低时，薄膜表面有部分V⁴⁺态存在，但存在较多的高键能氧，此时薄膜中晶粒尺寸较小.随着氧分压的提 关键词： 氧化钒 磁控溅射 相变薄膜 X射线光电子能谱     

C+注入a-SiNx：H薄膜的微结构及光发射的研究

常温下对低压化学气相沉积制备的纳米硅镶嵌结构的a-SiN_x:H薄膜进行低能量高剂量的C⁺注入后,在800~1200℃高温进行常规退火处理。X射线光电子能谱(XPS)及X射线光电子衍射(XRD)等实验结果表明,当退火温度由800℃升高到1200℃后,薄膜部分结构由SiC_xN_y转变成SiN_x和SiC的混合结构。低温下利用真空紫外光激发,获得分别来自于SiN_x、SiC_xN_y、SiC的,位于2.95,2.58,2.29 eV的光致发光光谱。随着退火温度的升高,薄膜的结构发生了变化,发光光谱也有相应的改变。     

前驱体和退火温度对Nd2O3薄膜组分影响的定量研究

采用Nd(thd)₃和O₃作为反应前驱体, 利用先进的原子层淀积方法在P型硅(100)衬底上制备了超薄Nd₂O₃介质膜, 并在N₂气氛下进行了退火处理. 采用X射线光电子能谱仪对薄膜样品组分进行分析. 研究结果表明, 淀积过程中将前驱体温度从175 ℃提高到185 ℃后, 薄膜的质量得到提高, O/Nd 原子比达到1.82, 更接近理想的化学计量比, 介电常数也从6.85升高到10.32.     

激光分子束外延BaTiO3薄膜最顶层表面原子平面与薄膜生长机理

用激光分子束外延技术在SrTiO₃(001)衬底上外延生长了高质量的BaTiO_{3< /sub>薄膜,薄膜的生长过程由反射式高能电子衍射仪(RHEED)原位实时监测,表明薄膜具有 二维层状生长模式.薄膜的晶体结构和表面形貌分别由X射线衍射和原子力显微镜表征,显示 该薄膜为完全c轴取向四方相晶体结构,其表面具有原子尺度光滑性.采用角分辨X射线光电 子谱技术(ARXPS),研究了BaTiO3薄膜表面最顶层原子种类和排列状况.结果表 明,BaTiO3 关键词： 激光分子束外延 3薄膜')" href="#">氧化物BaTiO3薄膜 最顶层表面 角分辨X射线光电子谱}     

ZnSb掺杂的Ge2Sb2Te5薄膜的相变性能研究

本文采用双靶(ZnSb靶和Ge₂Sb₂Te₅靶)共溅射制备了系列ZnSb掺杂的Ge₂Sb₂Te₅(GST)薄膜. 利用X射线衍射、透射电子显微镜、原位等温/变温电阻测量、X射线光电子能谱等测试研究了薄膜样品的非晶形态、电学及原子成键特性. 利用等温原位电阻测试表明ZnSb掺杂的Ge₂Sb₂Te₅薄膜具有更高的结晶温度. 采用Arrhenius 公式计算发现ZnSb掺杂的Ge₂Sb₂Te₅薄膜的十年数据保持温度均高于传统的Ge₂Sb₂Te₅薄膜的88.9℃. 薄膜在200, 250, 300和350℃ 下退火后的X射线衍射图谱表明ZnSb的掺杂抑制了Ge₂Sb₂Te₅薄膜从fcc态到hex态的转变. 通过对薄膜的光电子能谱和透射电镜分析可知Zn, Sb, Te原子之间键进行重组, 形成Zn–Sb 和Zn–Te 键, 且构成非晶物质存在于晶体周围. 采用相变静态检测仪测试样品的相变行为发现ZnSb掺杂的Ge₂Sb₂Te₅薄膜具有更快的结晶速度. 特别是(ZnSb)_24.3(Ge₂Sb₂Te₅)_75.7薄膜, 其结晶温度达到250℃, 十年数据保持温度达到130.1℃, 并且在70 mW激光脉冲功率下晶化时间仅～64 ns, 远快于传统Ge₂Sb₂Te₅薄膜的晶化时间～280 ns. 以上结果表明(ZnSb)_24.3(Ge₂Sb₂Te₅)_75.7薄膜是一种热稳定性好且结晶速度快的相变存储材料.     

Fe/ZnO (0001)体系界面相互作用中薄膜厚度效应的光电子能谱研究

利用同步辐射光电子能谱(SRPES)和X射线光电子能谱(XPS)技术,系统研究了室温下Fe/ZnO界面形成过程中Fe薄膜与氧结尾的ZnO(000 1 )衬底之间的相互作用,结果显示初始沉积的Fe明显被表面氧氧化为Fe²⁺离子,在Fe覆盖度为0—3 nm的范围内,分别观察到与界面电荷传输、化学反应以及薄膜磁性相关的三个有意义的临界厚度,这一结果将有助于基于Fe/ZnO界面的相关器件的设计和研发. 关键词： Fe/ZnO 界面作用 同步辐射光电子能谱 X射线光电子能谱     

La0.8Ca0.2MnO3/SrTiO3薄膜厚度对其结构及磁学性能的影响

采用多种X射线衍射技术和磁电阻测量技术研究了不同厚度的La_0.8Ca_0.2MnO₃/SrTiO₃ (LCMO/STO)薄膜的应变状态及其对磁电阻性能的影响.结果表明，在STO(001)单晶衬底上生长的LCMO薄膜沿［00l］取向生长.LCMO薄膜具有伪立方钙钛矿结构，随着薄膜厚度的增加，面内晶格参数增加，垂直于面内的晶格参数减小,晶格参数a和b相近，略小于c.LC 关键词： X射线衍射 微结构 应变 物理性能     

单晶Si表面离子束溅射沉积Co纳米薄膜的研究

采用离子束溅射沉积法，在单晶Si基片上制备了不同厚度(1—100nm)的Co纳米薄膜.利用原子力显微镜、X射线光电子能谱(XPS)仪和X射线衍射仪对不同厚度的Co纳米薄膜进行了分析和研究.结果表明：当薄膜厚度为1—10nm时，沉积颗粒形态随薄膜厚度增加将由二维生长的细长胞状过渡到多个颗粒聚集成的球状.当膜厚大于10nm时，小颗粒球聚集成大颗粒球，颗粒球呈现三维生长状态.表面粗糙度随膜厚的增加呈现先增加后减小的趋势，在膜厚为3nm时出现极值.XPS全程宽扫描和窄扫描显示：薄膜表面的元素成分为Co，化学态分别 关键词： 离子束沉积 纳米薄膜 X射线光电子能谱 X射线衍射     

Effect of substrate temperature on the surface and interface oxidation of NiTi thin films

NiTi shape memory alloy thin films are deposited on pure Cu substrate at substrate ambient temperatures of 300 °C and 450 °C. The surface and interface oxidation of NiTi thin films are characterized by X-ray photoelectron spectroscopy (XPS). After a subsequent annealing treatment the crystallization behavior of the films deposited on substrate at different temperatures is studied by X-ray diffraction (XRD). The effects of substrate temperature on the surface and interface oxidation of NiTi thin films are investigated. In the film surface this is an oxide layer composed of TiO₂. The Ni atom has not been detected on surface. In the film/substrate interface there is an oxide layer with a mixture Ti₂O₃ and NiO in the films deposited at substrate temperatures 300 °C and 450 °C. In the films deposited at ambient temperature, the interface layer contains Ti suboxides (TiO) and metallic Ni.     

Structural and compositional stability of Co oxide grown on (001) bct Co

Room temperature (RT) adsorption of oxygen on the (001) surface of metastable, cubic Co film epitaxially grown on a Fe substrate results in the formation of about 7 monolayers (ML) crystalline CoO film, in the typical rocksalt structure 45° rotated with respect to the square unit mesh of the underlying Co film. We investigated the stability of this oxide layer upon annealing in the RT–620 K temperature range, by means of primary-beam diffraction modulated electron emission (PDMEE), and X-ray photoelectron spectroscopy (XPS). For temperatures up to 570 K, film thickness and local order are preserved, in spite of an increasing number of Co and O atoms bonded in sites of reduced coordination. For larger temperatures, thickness also reduces, but the oxide film is still characterized by a high degree of CoO-like local order.     

Impact of Al addition on the formation of Ni germanosilicide layers under different temperature annealing

Solid reactions between Ni and relaxed Si_0.7Ge_0.3 substrate were systematically investigated with different Al interlayer thicknesses. The morphology, composition, and micro-structure of the Ni germanosilicide layers were analyzed with different annealing temperatures in the appearance of Al. The germanosilicide layers were characterized by Rutherford backscattering spectrometry, cross-section transmission electron microscopy, scan transmission electron microscopy, and secondary ion mass spectroscopy. It was shown that the incorporation of Al improved the surface and interface morphology of the germanosilicide layers, enhanced the thermal stabilities, and retarded the Ni-rich germanosilicide phase to mono germanosilicide phase. With increasing annealing temperature, Al atoms distributed from the Ni/Si_0.7Ge_0.3 interface to the total layer of Ni₂Si_0.7Ge_0.3, and finally accumulated at the surface of NiSi_0.7Ge_0.3. We found that under the assistance of Al atoms, the best quality Ni germanosilicide layer was achieved by annealing at 700 ℃ in the case of 3 nm Al.     

Bismuth oxide thin films prepared by chemical bath deposition (CBD) method: annealing effect

Bismuth oxide thin films have been deposited by room temperature chemical bath deposition (CBD) method and annealed at 623 K in air. They were characterized for structural, surface morphological, optical and electrical properties. From the X-ray diffraction patterns, it was found that after annealing a non-stoichiometric phase, Bi₂O_2.33, was removed and phase pure monoclinic Bi₂O₃ was obtained. Surface morphology of Bi₂O₃ film at lower magnification SEM showed rod-like structure, however, higher magnification showed a rectangular slice-like structure perpendicular to substrate, giving rise to microrods on the surface. The optical studies showed the decrease in band gap by 0.3 eV after annealing. The electrical resistivity variation showed semiconductor behavior and from thermoemf measurements, the electrical conductivity was found to be of n-type.     

Surface characteristics and electrochemical behaviour of sputter-deposited NiTi thin film

Thin nanocrystalline amorphous NiTi film was deposited on Si substrate using DC magnetron sputtering. The as-deposited NiTi thin film was crystallized by heat treatment at 500 °C for 1 h. The crystal structure, surface morphology, microstructure and surface chemistry of the deposited films were studied using X-ray diffraction, atomic force microscopy, scanning electron microscopy and X-ray photoelectron spectroscopy (XPS), respectively. Corrosion behaviour was assessed in Ringer’s solution at 37 °C by open circuit potential (OCP), potentiodynamic polarization and electrochemical impedance spectroscopy as a function of exposure time. OCP values indicate that the tendency for the formation of a spontaneous oxide film is greater for the NiTi thin films than the bulk NiTi. Long time exposure to Ringer’s solution was found to have a great effect on the corrosion behaviour of the samples. Significantly low corrosion current density was obtained for the annealed NiTi film from the potentiodynamic polarization curves indicating a typical passive behaviour, but as-deposited film and bulk NiTi alloy exhibited breakdown of passivity at potentials approximately +1.4 V (vs. SCE). XPS showed that the oxide film formed on the annealed NiTi thin film mainly composed of Ti oxides, and no evidence of Ni was found up to 8.2 nm beneath the top surface, suggesting the excellent corrosion resistance of this sample in Ringer’s solution.     

高温氢退火还原V2O5制备二氧化钒薄膜及其性能的研究

过渡金属氧化物二氧化钒(VO₂)在温度340 K附近会发生金属绝缘体的转变(metal-insulator transition, MIT). 基于金属绝缘体的转变性质, VO₂薄膜材料具有很好的应用前景. 本文首先采用脉冲激光沉积制备了高质量的V₂O₅薄膜, 再通过高温氢退火还原V₂O₅薄膜制备出VO₂多晶薄膜. 研究了不同的退火温度、退火时间、退火气氛对VO₂薄膜制备的影响, 采用X射线衍射、X射线光电子能谱、变温电阻特性测量等手段对样品进行分析, 发现在H₂(5%)/Ar退火气氛下, 在一定的退火温度范围内(500–525 ℃), 退火 3 h, 得到了B相和M相共存的VO₂薄膜, 具有M相的VO₂的MIT特性, 而相同退火温度下退火时间达到4.5 h, 薄膜完全变成B相的VO₂. 通过纯Ar气氛下对B相VO₂再退火, 得到了转变温度为350 K, 电阻突变接近4个数量级的M相的VO₂薄膜. 实现了VO₂的B相和M相的相互转变. 关键词： 2薄膜')" href="#">VO₂薄膜 金属绝缘体转变 氢退火     

Amorphous SiC film formation on Si(100) using electron beam excitation

The effect of electron impact on methylsilane (CH₃SiH₃) conversion to amorphous-Si_0.5C_0.5:H (a-Si_0.5C_0.5:H) films on Si(100) has been studied by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), temperature-programmed desorption (TPD), and low energy electron diffraction (LEED). It is found that electron impact greatly enhances CH₃SiH₃ decomposition on Si(100) at both 90 K and 300 K, resulting in a-Si_0.5C_0.5:H thin film formation. Thermal annealing of the film causes hydrogen desorption and amorphous silicon carbide (a-SiC) formation. Upon annealing to temperatures above 1200 K, the a-SiC film became covered by a thin silicon layer as indicated by AES studies. Ordered structures are not produced by annealing the a-SiC up to 1300 K.     

等离子增强原子层沉积低温生长AlN薄膜

采用等离子增强原子层沉积技术在单晶硅基体上成功制备了AlN晶态薄膜, 利用椭圆偏振仪、原子力显微镜、小角掠射X射线衍射仪、高分辨透射电子显微镜、 X射线光电子能谱仪对样品的生长速率、表面形貌、晶体结构、薄膜成分进行了表征和分析, 结果表明, 采用等离子增强原子层沉积制备AlN晶态薄膜的最低温度为200 ℃, 薄膜表面平整光滑, 具有六方纤锌矿结构与(100)择优取向, Al_2p与N_1S的特征峰分别为74.1 eV与397.0 eV, 薄膜中Al元素与N元素以Al-N键相结合, 且成分均匀性良好. 关键词： 氮化铝 等离子增强原子层沉积 低温生长 晶态薄膜     

Influences of annealing on structural and compositional properties of Al_2O_3 thin films grown on 4H–SiC by atomic layer deposition

Annealing effects on structural and compositional performances of Al_2O_3 thin films on 4H–Si C substrates are studied comprehensively. The Al_2O_3 films are grown by atomic layer deposition through using trimethylaluminum and H_2 O as precursors at 300?C, and annealed at various temperatures in ambient N_2 for 1 min. The Al_2O_3 film transits from amorphous phase to crystalline phase as annealing temperature increases from 750?C to 768?C. The refractive index increases with annealing temperature rising, which indicates that densification occurs during annealing. The densification and grain formation of the film upon annealing are due to crystallization which is relative with second-nearest-neighbor coordination variation according to the x-ray photoelectron spectroscopy(XPS). Although the binding energies of Al 2p and O 1s increase together during crystallization, separations between Al 2p and O 1s are identical between as-deposited and annealed sample, which suggests that the nearest-neighbour coordination is similar.