氧化物薄膜研制中的电子能谱技术

随着科学技术的不断发展，人们正在寻求更新的实用材料．金属氧化物，包括金属氧化物薄膜的各种实用材料，在工业界、信息产业界和能源开发等方面的应用前景，早已引起国内外学者的极大关注．例如，由于氧化物具有各种特殊的介电和光学性质，研究和开发基于氧化物薄膜的气敏材料非常热门．如何制备出有实用价值的各种薄膜材料，是科学家们一直关心和深入研究的课题．电子能谱技术在各种材料的基础研究和实际应用中起着重要的作用．本文以有序金属氧化物薄膜研制为例，简要评述了电子能谱技术（包括X射线光电子能谱（XPS），紫外光电子能谱（UPS），俄歇电子能谱（AES）和高分辨电子能量损失谱（HREELS）），以及低能电子衍射（LEED）等技术在氧化物薄膜材料制备和表征中的应用．     

注入在表面含氧的硼膜中氘的行为研究

硼是非常有潜力的聚变堆第一壁涂层材料。对氢同位素在硼膜中的滞留和释放性能已经作了大量研究。本文用X射线电子能谱（XPS）和热解释谱（TDS）方法研究了注入在表面含氧的硼膜中氘的行为。     

原子尺度上的异质催化

现实中的催化剂是个相当复杂的系统体系，且为粉末状，限制了多种表面科学表征手段的应用,科学家通过建立简化的催化剂模型，充分利用目前多种有力的科技分析手段，如扫描隧道显微镜（STM）、透射电镜（TEM）、光电子能谱（XPS）、傅里叶变换红外吸收谱（FTIR）、电子能量损失谱（EELS）等，直观地在原子尺度上研究催化反应的机理，从而使得人们能够设计出选择性能更高、催化性能更好的催化剂．     

固体金属二次电子发射的Monte-Carlo模拟

二次电子的发射在生产实践中有着广泛的应用,但其相关测量结果受实验环境和实验仪器的影响很大．在实验中难以精确测量．所以本文建立了一个包含二次电子激发、在固体内部传输和最后逸出固体表面的二次电子系统模型．采用Monte-Carlo的模拟方法仿真二次电子运动轨迹,定量分析二次电子的发射系数和能谱分布．并探讨它们与一次电子的入射角度和入射能量的关系．仿真结果表明：本文建立的二次电子系统模型能较好地反映实际情况．通过该模型仿真,可以定量得到二次电子发射系数和能谱分布与一次电子的入射能量和入射角度的关系．     

角分辨光电子能谱技术及其应用进展

角分辨光电子能谱（ARPES）是研究晶体表面电子结构,如能带,费米面,以及多体相互作用的重要工具。本文概述了光电子激发的一般过程和单粒子近似下的理论模型。详细讨论了角分辨光电子能谱的能带勾画（Energy Band Mapping）和费米面成像（Fermi Surface Mapping）技术,以及高分辨下的角分辨光电子能谱在强相关体系研究中的应用。文章最后简单介绍了当前角分辨光电子能谱研究的新进展,如研究宽禁带半导体材料的表面电子结构,有机功能材料与金属的界面,金属超薄膜中的量子阱态,以及高温超导机理研究等。     

分子束外延GaN薄膜的X射线光电子能谱和俄歇电子能谱研究

用XPS和AES电子能谱的方法对等离子体辅助分子束外延(MBE)生长的GaN薄膜进行了表面分析和深度剖析.发现红外分子束外延(RFMBE)生长的富镓GaN薄膜实际表面存在O和C吸附层,C主要为物理吸附,而O在GaN表面形成局域化学键产生氧络合物覆盖层,并形成一定的深度分布.杂质O在GaN带隙中导带底形成杂质带同时引入深受主能级,使得带隙变窄室温光吸收谱向低能方向移动,光致发光谱出现宽带发光峰.从而影响GaN薄膜的电学和光学性质 关键词： GaN薄膜 X射线光电子能谱 俄歇电子能谱 表面分析     

硅漂移电子温度测量系统的研制

在磁约束聚变装置中，对等离子体电子温度的测量一般采用电子回旋辐射法（ECE）、汤姆逊散射法以及软X射线能谱法。其中软X射线（1～20keV）能谱法是一种传统的方法，它比汤姆逊散射法的测量误差小，且有较好的时空分辨；与电子回旋辐射法（ECE）相比较，时空分辨能力相近，但可作绝对测量，并且受超热电子和逃逸电子的影响较ECE小。在软X射线能谱法的应用中，过去使用Si（Li）探测器来探测软X射线能谱，Si（Li）探测器体积大，能量分辨和量子效率低，并且需要使用液氮冷却，大体积的杜瓦（通常35L）使探测器体积庞大，     

高度离化的钼离子细致结构能谱测量

高度离化的中、高z元素激光等离子体辐射的细致结构能谱对惯性约束聚变等离子体诊断和原子结构理论计算等方面非常有用．在“神光Ⅱ”激光装置上，聚焦0．35μm激光束于真空室内的钼（Mo）元素固体靶上，产生Mo激光等离子体，用高分辨椭圆弯晶谱仪测量Mo激光等离子体辐射在0．32-0．58nm范围内的X射线细致结构能谱，并对实测能谱进行辨识和归类．辨识出了n=4—2，3—2系列离子共振跃迁和内壳层跃迁的能谱线，还有类氢、类氦离子共振线及伴线．另外，对谱线的半高全宽度（FWHM）值做了分析．在整个测量范围内，谱线精确波长值的绝对误差小于0．0005nm，与HFR方法得到的理论计算结果值比较，两者符合较好．此工作的结果对积累Mo元素离子谱线数据具有重要的意义．     

P2S5/NH4OH处理GaAs(100)表面的电子能谱研究

采用俄歇电子能谱(AES)和X射线光电子能谱(XPS)研究了P₂S₅/NH₄OH钝化液处理的GaAs(100)表面的微观特性。AES测量表明,在钝化膜和GaAs衬底之间的界面处无O组分,只有P和S组分。XPS测量分析指出,经过P₂S₅/NH₄OH溶液处理后,GaAs表面处Ga₂O₃和As₂O_{3关键词：}     

铀与表面铝薄膜界面反应的俄歇电子能谱分析

主要利用俄歇电子能谱（AES）研究了室温下铀、UO2与表面铝薄膜之间的界面反应，以及退火对界面反应的影响。在俄歇电子能谱仪超高真空室中，利用Ar^＋枪溅射铝靶，使其分别逐步沉积到铀基体与UO2表面上，然后利用电子枪适时采集表面俄歇电子能谱，研究膜基界面反应。     

Drying methods for XPS analysis of PureVision™, Focus Night&Day™ and conventional hydrogel contact lenses

The surface composition of hydrogel contact lenses that contain silicon-based monomers, PureVision™ (balafilcon A) and Focus^® Night&Day™ (lotrafilcon A), were investigated by X-ray photoelectron spectroscopy (XPS). Conventional and daily disposable hydrogel lenses based on hydroxyethyl methacrylate (HEMA) were also studied, with the commonly prescribed 1-day Acuvue^® lens (etafilcon A) used as a control. All the lenses were pre-washed and dehydrated by three different methods, including drying in air, drying in nitrogen or freezing with subsequent freeze-drying, before the XPS analysis. The lenses dried in air had more impurities on the surface, and the lenses that were freeze-dried lost transparency, suggesting that drying lenses in nitrogen is the preferred preparation method for XPS analysis. Surface compositions for all lens materials were obtained and this data can be used as a control/base-value for future analysis of the interactions of soft contact lens materials with chemicals such as drugs or tear components.     

SiC表面C 1s谱最优拟合参数的研究

提出了一种新的,用未限定拟合峰位置、半高宽和峰面积的X射线光电子谱拟合方法,研究了拟合峰的数目、函数类型及背景对SiC表面C 1s谱拟合结果的影响,并与样品表面宽扫描X射线光电子谱和红外掠反射吸收谱相对照,确定了SiC表面C 1s谱的最优拟合参数,获得了与文献中数值相同的 C 1s束缚能. 为SiC及其他材料表面元素窄扫描X射线光电子谱的拟合和化学态结构的鉴定奠定了基础. 关键词： SiC X射线光电子谱 C 1s谱     

苝四甲酸二酐在Au(111)表面的取向生长及电子结构研究

利用X射线光电子能谱(XPS),同步辐射紫外光电子能谱(SRUPS),近边X射线吸收精细结构(NEXAFS)以及原子力显微镜(AFM)等技术研究了苝四甲酸二酐(PTCDA)与Au(111)的界面电子结构、PTCDA分子取向及有机薄膜的表面形貌.SRUPS价带谱显示,伴随PTCDA分子的微量沉积(0·5ML),位于费米能级附近Au的表面电子态迅速消失,但却观察不到明显的界面杂化态,这说明PTCDA分子和Au(111)界面间存在弱电子传输过程,但并没有发生明显的化学反应.角分辨NEXAFS以及SRUPS结果证明PTCDA分子是平铺在衬底表面.根据Au4f7/2和C1s峰积分强度随薄膜厚度的变化以及AFM图像可知,PTCDA分子在Au(111)表面是一种典型的Stranski-Krastanov生长模式,即先层状生长,再岛状生长,并且在层状生长到岛状生长的转变过程中,存在有机分子的去润湿过程.     

Protection of iron corrosion by stearic acid and stearic imidazoline self-assembled monolayers

A type of stearic imidazoline (IM) inhibitor was prepared using stearic acid (SA) and diethylenetriamine (DETA) as raw materials. The monolayers of IM and SA were assembled on the iron surface. The electrochemical characterization of stearic acid (SA) and stearic imidazoline (IM) on an oxide free iron surface had been studied. The monolayers of IM inhibitor were characterized by electrochemical impedance spectroscopy (EIS), electrochemical polarization curves, double layer capacitance, X-ray photoelectron spectroscopy (XPS) and molecular simulation. The results of electrochemical studies had illustrated that the inhibition efficiency of IM was higher than SA. XPS showed that the IM molecules adsorbed on the iron surface. The molecular simulation calculations showed that the IM molecules were tilted at an angle on the iron surface.     

Characterization and chemical behavior of submonolayer coverages of titania on a Pt foil

The interaction between submonolayer titania coverages and Pt foil has been studied by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), temperature programmed desorption (TPD) and high-resolution electron energy loss spectroscopy (HREELS). The submonolayer titania can be fully oxidized to TiO₂ at 923 K under 10⁻⁸ Torr O₂, and partially oxidized to TiO_x at lower oxidation temperatures. The oxidized surface can be reduced by annealing to 1000 K or higher, or by heating in H₂ at 823 K, or by interacting with surface carbon formed from acetone decomposition. Under certain conditions (e.g., hydrogen reduction at 923 K), the surface titania can be fully reduced to metallic Ti which diffuses into bulk Pt readily. The reduced metallic Ti can resurface when the surface is oxidized at 923 K. Both XPS and HREELS data indicate the existence of subsurface oxygen, which plays an important role for the diffusion of Ti into and out of the Pt foil. Although no special interfacial active sites were revealed by HREELS studies of adsorbed acetone and CO, some TPD and XPS data suggest the presence of sites active for acetone decomposition.     

Fibrinogen adsorption onto 316L stainless steel, Nitinol and titanium

Fibrinogen adsorption onto mechanically polished biomedical grade 316L stainless steel (316LSS), nickel titanium alloy (Nitinol) and commercially pure titanium (CpTi) surfaces were studied by measurements of adsorption isotherms and adsorption kinetics using an ex-situ wavelength dispersive spectroscopy technique (WDS). Surface composition, roughness and wettability of these materials were characterized by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and water contact angle (WCA) measurements. Adsorption isotherm results showed that surface protein concentration on these materials increased with increasing concentration of fibrinogen in phosphate buffer solution. The fibrinogen adsorption isotherms were modeled by both the monolayer Langmuir isotherm and the multilayer Brunauer-Emmett-Teller (BET) isotherm. The results strongly suggest that fibrinogen forms multilayer structures on these materials when the concentration in solution is high. Complementary measurements on the absorbed fibrinogen films by spectroscopic ellipsometry (SE) support this view.     

Sorption of Sb(III) on carbon steel surface in presence of molybdate and selenite in citric acid medium

Sorption of Sb(III) on carbon steel surface in aqueous medium (pH 2.8) in presence of different oxyanions like molybdate and selenite has been studied. It is observed that the presence of molybdate or selenite in solution reduced Sb(III) adsorption and surface precipitation to a great extent. The solution at different stages of the adsorption experiment has been analyzed by inductively coupled plasma-atomic emission spectroscopy technique. X-ray diffraction and X-ray photoelectron spectroscopy (XPS) techniques have been used to characterize the precipitate layer and the adsorbed layer. A detailed analysis of the XPS data reveals the mechanism involved in the two cases.     

Generation of oxygen vacancies in the surface of ferroelectric Pb(Nb,Zr,Ti)O3

Controlled generation of oxygen vacancies in the surface of ferroelectric thin films is crucial to study how surface reduction affects molecular adsorption and catalysis of gas-surface phenomena. We demonstrate the effective reduction in the surface of 4% niobium doped 20/80 PZT (PNZT) thin films. The sample was characterized by X-ray diffraction (XRD), Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM), and heated at 200, 250 and 300 °C in a high vacuum system at 10⁻⁵ T of H₂. Auger peak-to-peak intensities was used to study the elemental concentrations during the reduction experiment. High-resolution XPS spectra were acquired before and after reduction process for detecting the changes of the oxygen signal. Vacancies production rates as slow as 0.21% per minute were achieved and the temperature was not a key parameter in the process. Experiments at higher hydrogen pressures and lower temperatures might improve the control of the vacancies production.     

Application of XPS spectral subtraction and multivariate analysis for the characterization of Ar ion beam modified polyimide surfaces

This paper presents results of a detailed X-ray photoelectron spectroscopy (XPS) characterization of complex changes at a polyimide surface resulting from Ar⁺ ion beam modification. The changes in chemical composition in the surface layer lead to formation of a layer that can act as an alignment layer for liquid crystals. The goal of this paper is to report on the result of a combination of spectral subtraction and multivariate analysis for analysis of XPS spectra. Principal component analysis (PCA), applied to curve-fitting results of difference spectra and multivariate curve resolution (MCR), applied to raw spectra, provided consistent results, and allowed for extraction of chemical anisotropy, defining factor in the ion beam (IB) alignment mechanism. This study demonstrated that more detailed chemical information about complex systems can be obtained through application of multivariate analysis to XPS spectra and curve-fits. Further, this approach can be effectively used in the characterization of various complex materials to link chemical structure to their properties.     

Spectroscopic analysis of CIGS2/CdS thin film solar cell heterojunctions on stainless steel foil

This paper presents a spectroscopic analysis of the interface between a CuIn_1−xGa_xS₂ (CIGS2) absorber and a CdS buffer layer on stainless steel foil by Auger electron spectroscopy (AES), inverse photoemission spectroscopy (IPES) and photoelectron spectroscopy (PES) such as X-ray photoelectron spectroscopy (XPS), and ultraviolet photoelectron spectroscopy (UPS). By combining these spectroscopic techniques, detailed information about the electronic and chemical properties of the CIGS2 surface and the CdS/CIGS2 interface can be obtained. The gallium concentration in CIGS2 films was found to increase continuously towards the Mo back contact. XPS analysis showed the presence of KCO₃ on the surface of CdS, deposited on etched and un-oxidized samples indicating diffusion of potassium. No potassium was observed on oxidized as well as samples having thicker CdS (50 nm) indicating the effectiveness of oxidation and chemical bath deposition (CBD) process in cleaning the sample surface effectively. In addition, investigation of the electronic level alignment at the interface has been carried out by combining PES and IPES. Conduction band offset of −0.45 (±0.15) eV and a valence band offset of −1.06 (±0.15) eV were measured. These unfavorable conditions limit efficiency of CIGS2 thin film solar cells.