Simulation of X-ray diffraction profiles in multilayers by direct wave summation: Application to asymmetric reflections

A novel algorithm for the simulation of the X-ray diffraction profiles in multilayers is developed, which can be applied to any multilayered structure, with no limitations. The simulation program in the MATLAB format is based on the direct summation of waves scattered by individual atomic planes. It takes into account the strain and concentration-induced fluctuations of interplanar spacings, interface roughness and buried amorphous layers, and enables adding the diffuse scattering contributions of the Gaussian or Lorentzian types.The summation over individual layers can be done coherently or incoherently, depending on the interface structure. In order to visualize the steps of the fitting procedure, the contribution of each layer can be plotted separately.In this paper the simulation routine is described with a focus on handling asymmetric reflections. We stress that in this case, the effective thickness of the layers, participating in the formation of diffraction signals, can be very different for low or high X-ray incidence angles. We also show that in contrast to symmetric reflections, when treating the asymmetric ones, an additional phase shift depending on the distance between the sample and detector, should be taken into account. The simulation program is applied to fit experimental diffraction profiles, symmetric and asymmetric, taken from the MOVPE-grown heterostructures and superlattices of practical importance, based on the InGaAsP/InP materials system.     

Structural properties of ferroelectric heterostructures using coherent bragg rod analysis

We investigated the crystal structure of SrRuO₃/BaTiO₃/SrRuO₃ (SRO/BTO/SRO) heterostructures grown on a SrTiO₃ (001) substrate using surface X-ray scattering. The interface structure of SRO/BTO/SRO heterostructures can decrease the critical thickness of ferroelectric BTO films reduced to 3.5 unit cells. Owing to weak intensity of ultrathin films, lab-source-based X-ray measurement cannot determine the atomic arrangement of the heterostructures and their lattice parameters. We introduced synchrotron-based X-ray scattering techniques combined with coherent Bragg rod analysis (COBRA) to resolve the details of the heterostructures. We obtained detailed crystal structural information based on the electron density profiles of the SRO/BTO/SRO heterostructures acquired from COBRA results, e.g., lattice parameters and atomic arrangements.     

Mo/Si多层膜小角X射线衍射结构表征

为了实现对Mo/Si多层膜的结构表征,测量了多层膜样品的小角X射线衍射谱。介绍了小角X射线衍射谱的分析方法,包括Bragg峰值拟合法,傅里叶变换法,反射谱拟合法。Bragg峰值拟合法和反射谱拟合法得到多层膜的周期厚度为7.09nm,两种模型的反射谱拟合法得到界面的粗糙度(扩散长度)为0.40～0.41nm(Si在Mo上),0.52～0.70nm(Mo在Si上),前者要比后者小,这与透射电镜法(TEM)得到的结果0.40nm(Si在Mo上),0.6～0.65nm(Mo在Si上)是一致的。通过基于扩散模型的反射谱拟合法得到的折射率剖面也与由高倍率透射电镜(HRTEM)积分得到的灰度值剖面在趋势上是一致的。通过X射线衍射谱和TEM图像对Mo/Si多层膜进行综合表征,得到了多层膜的精细结构信息,这对多层膜制备工艺的优化具有十分重要的意义。     

铌酸钾钠基无铅压电陶瓷的X射线衍射与相变分析

分析了斜方相、四方相铌酸钾钠基无铅压电陶瓷材料的结构和X射线衍射图谱的特点. 对于铌酸钾钠基压电材料斜方相结构, 从构成晶胞的一个单斜原胞进行分析, 计算出X射线衍射谱上每个衍射角附近的衍射峰数目和相对强度. 提出了2θ在20°—60°范围内根据(1 0 2)衍射峰(52°附近)和(1 2 1)衍射峰(57°附近)劈裂的数目区分斜方和四方相的新方法. 对于多晶陶瓷粉末, 可以更简便的由22°(或45°)附近前后峰的相对高低来判断斜方、四方相. 关键词： 铌酸钾钠 无铅压电陶瓷 X射线衍射 相变     

高炉渣非晶态含量的定量分析方法研究

通过X-ray衍射方法对高炉渣中非晶态与晶态的含量进行了定量分析研究。定量分析过程包括标准样品制备、配样与衍射以及数据处理分析。数据处理包括非晶态衍射峰及晶态峰在一定衍射角度内的积分、线性拟合与定量系数确定。提出了X-ray衍射方法所用的高炉渣标准样品的制备方法,包括100％非晶态标样和100％晶态标样。提出了由100％非晶态和100％晶态为标准样品时,高炉渣中非晶态含量的测定方法,适用于非晶态含量较高(>80%)的高炉渣的定量分析。结合数学处理和X-ray衍射结果,可得到原始高炉渣中非晶态含量和晶态含量,以及相应的比例系数,适用于非晶态含量高的高炉渣(>90%)。     

Structural characterisation of GaAlN/GaN HEMT heterostructures

(GaN/GaAlN/GaN)//Al₂O₃(00.1) HEMT heterostructures have been studied by X-ray scattering techniques, transmission electron microscopy and atomic force microscopy. X-ray reflectometry has been used to determine with a high accuracy both the individual layer thicknesses and the interfacial roughness, in spite of the weak electronic density contrast between layers. From the Fourier inversion method and using a simulation software, the roughness of the interface corresponding to the two-dimensional electron gas location has been determined equal to 0.5 nm. Both high resolution X-ray diffraction and transmission electron microscopy experiments have shown the excellent crystallinity of the heterostructures. Finally, the surface morphology has been inferred using atomic force microscopy experiments.     

X射线衍射多相谱中某一物相点阵参数的直接求解方法

介绍了一种新的求解点阵参数的方法--不涉及结构的谱峰拟合方法.该方法适用于单一物相或多个物相衍射谱中某一物相点阵参数的直接求解,可以避免外推函数的不同选择而造成的差异,且快速准确.根据此方法编写的应用程序已在实际工作中得到应用.程序中还包括了调整样品表面离轴偏差和零度偏差以提高拟合精确度的功能. 关键词： X射线衍射 谱峰拟合 点阵参数     

nm量级薄膜厚度测量

 为了获得nm量级薄膜样品的精确厚度,采用软X射线反射率拟合方法、Bragg衍射方程方法和反射率Fourier变换方法分析了常规Cu靶X射线衍射数据及软X射线反射率数据。对厚度测量结果进行比较,3种方法得到的结果一致性很好。其中,软X射线反射率拟合和Bragg衍射方程方法精度很高,优于1 nm,Fourier变换方法精度稍低。对于单层W薄膜样品,3种方法获得厚度分别为(15.21±0.60) nm,(14.0±1.0) nm和(13.8±1.5) nm;对于双层W/C薄膜样品,W层厚度分别为(12.64±0.60) nm,(13.0±1.0) nm和(13.9±1.5) nm。这3种方法测量结果精度主要取决于反射率数据测量精度,而Fourier变换方法精度随着能量升高而提高,随着掠入射角范围增大而提高。     

Ⅱ-Ⅵ族应变层超晶格的X射线衍射分析

本文报导了用计算机控制的衍射仪(CuKα辐射)测量的金属有机化学汽相沉淀(MOCVD)方法生长的Ⅱ-Ⅵ族应变层超晶格的X射线衍射曲线,观察到了超晶格结构的多级卫星峰,且卫星峰的强度随角度呈周期性变化.对这种卫星峰形成包络的衍射曲线,用X射线运动学衍射理论进行了分析和讨论,这种讨论有助于理解X射线衍射曲线中卫星峰的形成.同时用光致发光和包络峰宽度的方法估算了样品的结构参数.     

一种点光源的自适应束斑X射线衍射仪的研制

为同时实现微米量级待测区域和毫米量级待测区域的物相分析,以及对表面不平整样品准确的物相分析,本实验室结合X射线衍射技术、CCD相机成像技术和毛细管微会聚X光调控技术,研制了一款能根据待测区域大小自适应调节照射X射线束斑直径的点光源X射线衍射仪Hawk-Ⅱ,其主要组成包括X射线源系统、六维联动运动系统、CCD相机、X射线探测系统和基于LabVIEW的软件控制系统.为验证设备的可行性,对表面不平整的人民币五角硬币进行分析,发现Hawk-Ⅱ测得的衍射图与标准PDF卡基本一致,而帕纳科X-Pert Pro MPD测得的衍射图最大偏移角度高达0.52°.对清代红绿彩瓷白釉和表面镀Cu,Fe的纳米材料采用不同直径的X射线束进行分析,发现白釉的晶体分布较为均匀,而纳米材料的表面镀膜不均匀.应用Hawk-Ⅱ分析一片西汉青铜,根据其锈蚀点的大小自适应调节照射X射线束斑直径,从而实现了物相的精确分析.由分析结果可知,Hawk-Ⅱ不仅拥有准确分析不规则样品的能力,而且拥有从微米级到毫米级待测区域的物相分析能力,并兼具能量色散X射线荧光分析功能,在诸多领域具有广泛的应用前景.     

Structural characterisation of Sb-based heterostructures by X-ray scattering methods

Antimonide-based superlattices dedicated to the elaboration of opto-electronic devices have been studied by X-ray scattering techniques. In particular, specular and non-specular X-ray reflectometry experiments have been performed on two MBE-samples elaborated with different shutter sequences at the interfaces. The results have shown a limitation of the incorporation of Sb species in the subsequent InAs layer for one of the samples, as expected.Then, a study on a InGaAs-cap layer/(InGaAs/AlAsSb)_N superlattice grown on a InGaAs/InP buffer layer by both specular X-ray reflectometry and High resolution X-ray diffraction is reported. In particular, the results have revealed the presence of a highly disturbed thin-layer on top of the MOVPE-made GaInAs, whose presence has been explained by In-concentration modification during the desoxidation procedure at the surface of the MOVPE-made GaInAs.Beside the results on the Sb-based heterostructures, the use of X-ray scattering metrology as a routinely working non-destructive testing method has been emphasized.     

X-ray diffraction profiles of Si nanowires with trapezoidal cross-sections

Comparisons of the experimental and calculated X-ray diffraction profiles have been made for Si nanowires with trapezoidal cross-sections. Examined samples are periodically arranged nanowires prepared on a silicon-on-insulator wafer by electron-beam lithography, so that they are isolated from Si substrate. The nanowire periodicity gives rise to diffractions at additional reciprocal lattice points, which we employ to avoid the mixture of the diffraction from the Si substrate. The experimental diffraction profiles are found to be in good agreement with the square modulus of the Fourier transform of the trapezoidal cross-sections determined from transmission electron micrographs.     

Diffraction effects in low-energy electron emission

The origin of diffraction peaks in the energy distribution of intensity of low-energy (< 1000 eV) electron emission from crystals is discussed from the standpoint of the dynamical theory of diffraction. The emitted electrons are considered to originate at relatively incoherent point sources in the crystal. The two-beam approximation of dynamical theory is used. The theory accounts for the chief regularities of diffraction peaks: temperature-dependence of peak intensities like that for low-energy electron diffraction (LEED) peaks, correlation of peak energies with X-ray absorption fine structure, and correlation of peak energies with the energies of normal-incidence LEED peaks in specular reflection. It is shown that the conditions for diffraction peaks coincide with the conditions for emergence of Kikuchi lines. It is predicted that for energies just above those of diffraction peaks, such emergences should be observable in the angular distribution of emission as intensity minima for emission along low-index crystal axes. Theory of Kikuchi band profiles is developed in an Appendix.     

High Pressure X-Ray Absorption and Diffraction Study of InAs

We have performed X-ray absorption (XAS) and diffraction (XRD) measurements at high pressure on samples of powdered InAs, up to 50 and 80 GPa, respectively. In the lower pressure range, our data are consistent with the following structural sequence: Zincblende M NaCl M Cmcm . The first order transition from the semiconducting Zincblende phase to the metallic NaCl phase is clearly seen by the shift in the absorption onset at the As K-edge and the strong modifications of the extended X-ray absorption fine structure (EXAFS) due to the changes in the local structure from a 4-fold to a 6-fold coordinated environment. XAS shows the high pressure phase to be locally site-ordered. The diffraction data, analized by Rietveld fitting, gives a volume discontinuity of j V/V 0 ～0.18 for the first order transition. There is no apparent volume discontinuity associated to the NaCl M Cmcm transition.     

MBE[(GaAs)l(Ga1-λAlxAs)m]n/GaAS(001)一维超晶格的X射线双晶衍射测量

本文着重介绍了MBE[(GaAs)l(Ga1-xAlxAs)m]n/GaAs(001)一维超晶格的X射线双晶衍射测量方法。根据卫星峰的出现,证明超晶格的存在。基于超晶格的台阶模型和X射线衍射的运动学理论,推导出超晶格多结构参数的计算方法。并对X射线双晶给出的其他信息做了必要的讨论。     

质子交换LiNbO3光波导的特性研究

采用X射线衍射谱法和红外吸收光谱法对质子交换和退火质子交换LiNbO3光波导的特性进行了研究.研究结果表明:在LiNbO3晶体衬底X射线衍射主峰的左侧出现质子交换LiNbO3光波导的伴峰,则质子交换使光波导层Li1-xHxNbO3的晶格常数比衬底的晶格常数稍大,产生垂直于表面的应变,波导经过退火后,伴峰向主峰靠近,应变减少.质子交换波导中的OH-基团的红外吸收光谱在3 500和3 300 cm-1处存在特征峰,波导经过退火后,3 300 cm-1处的特征峰基本消失,而3 500 cm-1处的吸收强度基本不变.实验还表明,OH-在3 500 cm-1处吸收带的积分面积基本与交换时间的开方呈正比例关系.     

Thickness measurement of GaN epilayer using high resolution X-ray diffraction technique

In this paper we propose a new method for measuring the thickness of the GaN epilayer, by using the ratio of the integrated intensity of the GaN epilayer X-ray diffraction peaks to that of the sapphire substrate ones. This ratio shows a linear dependence on the GaN epilayer thickness up to 2 μm. The new method is more accurate and convenient than those of using the relationship between the integrated intensity of GaN epilayer diffraction peaks and the GaN thickness. Besides, it can eliminate the absorption effect of the GaN epilayer.     

Spectroscopic and structural studies of isochronally annealed cobalt oxide nanoparticles

X-ray absorption near edge structure (XANES) spectroscopy, X-ray photoelectron spectroscopy (XPS), and Synchrotron X-ray diffraction (SXRD) techniques are used to study as synthesized and isochronally annealed samples of cobalt oxide nanoparticles (NPs) grown using the wet chemical route. Quantitative phase composition determined using Linear Combination Fitting (LCF) on XANES data is found to be in reasonably good agreement with that obtained from Rietveld refinement on SXRD data. XPS data qualitatively indicate that Co₃O₄ concentration increases with increase in the annealing temperature, in confirmation with SXRD and XANES data. Larger shifts in the satellite peaks from the main peaks compared to these in bulk suggest larger crystal field splitting in nanoparticles as compared to the bulk.     

毛细管聚焦的X射线荧光光谱拟合软件的开发及应用

基于Python语言设计了一款毛细管聚焦的X射线荧光光谱拟合软件QMXRS(quantitative analysis of micro-energy dispersive X-ray fluorescence spectra)并实现其在毛细管聚焦的X射线荧光光谱拟合方面的应用。QMXRS具有小波降噪、本底扣除、能量刻度、元素特征峰的识别、分峰和拟合、能谱的批处理和元素分布成像等功能。毛细管聚焦的X射线荧光分析技术采用毛细管X光透镜对X射线源激发出的X射线束进行聚焦导致X射线荧光光谱分布发生改变。这一变化影响了毛细管聚焦的X射线荧光光谱本底分布。因此QMXRS利用本底预估模型对毛细管聚焦的X荧光光谱本底进行本底分布的修正;同时在全谱拟合过程中,利用半高宽与能量的关系对高斯峰半高宽进行约束,减少高斯峰模型中变量,在保证全谱拟合收敛的同时提高了拟合速度。为验证上述方法的可行性,分别利用QMXRS, PyMca(python multichannel analyzer)和QXAS(quantitative X-ray analysis system)三款软件分析NIST 610标准样品的毛细...     

Continuous Wavelet Transform to Improve Resolution of Overlapped Peaks Based on Curve Fitting

An improved curve fitting for the resolution of the overlapped peaks was proposed. The main work is to use the continuous wavelet transform (CWT) to sharpen peaks and get reasonable initial estimates for the parameters of each peak. As a result, the fitted condition was improved and accurate results could be acquired. To verify the suggested method, separation of several kinds of overlapping peaks simulated by computer and the experimental voltammogram have been performed and are discussed.