二维X射线衍射及其应用研究进展

介绍了三维、一维和二维X射线衍射的有关概念,给出二维X射线衍射的定义:在X射线衍射实验中使用二维探测器,并对由二维探测器记录的二维象、二维衍射花样的数据进行处理分析和解释的X射线衍射方法称为二维X射线衍射术。之后,分四部分综述二维X射线衍射(2D-XRD)和散射及其应用的进展。1)单晶样品的二维衍射包括经典的劳厄法定向和用二维探测器(带衰减底片组件、CCD和IP等)的劳厄法测定晶体结构的单晶样品现代二维衍射术;2)随后,评述多晶样品二维衍射的衍射几何、实验装置,以及在物相鉴定、应力测定和织构测定方面应用的方法和基本公式;3)二维小角散射(2D-SAXS)也作了简介。4)把一维和二维衍射术作了较全面的比较和综合评论。     

一维丝室气体探测器衍射像差的修正方法研究

一维位置灵敏单丝气体探测器采用单根镀金钨丝和200根阴极感应条的探测结构, X射线在阳极丝上产生的信号被多个阴极条感应, 利用重心法得到X射线的原初电离点的位置信息, 位置分辨率达到160 μm(半高全宽). 在同步辐射衍射实验中, X射线通过样品后会形成不同大小的衍射环, 本实验中测量得到11.148°和14.201°的两组衍射角位置信息; 通过平行移动一维探测器在衍射环范围内多次扫描, 可以重建得到二维衍射环. 由于一维探测器的气体厚度和入射窗宽度会给测量结果带来像差, 分析发现像差的影响大于一维探测器的位置分辨. 基于相应的物理分析对测量到的衍射位置进行修正, 修正后的衍射位置相比修正前的衍射位置的相对像差最大改善达到7%, 该方法实现了无像差二维衍射环的重建.     

二维点阵的软X射线衍射实验研究

以光刻胶作为探测器,用3.2nm的X射线进行了二维点阵测试样品的软X射线衍射实验,记录了探测器和样品间隔分别为0、2mm和80mm时的图像,并用光学显微镜放大观察。实验结果表明,探测器记录的图像与探测 和样品之间的距离有关,即随探测器和样品之间距离的变化而变化。这与理论模拟的结果一致。     

大尺寸LnBa_2Cu_3O_(7-δ)单晶的生长及其超导电性

本文报道大尺寸LnBa_2Cu_3O_(7-δ)(Ln=Y,Eu,Gd,Dy,Ho,Er,Tm,Yb,Lu)单晶生长及其超导电性,并讨论了(001)自然晶面的X射线多级衍射、劳厄相、旋进相等单晶鉴定法。     

纪念劳厄发现X射线衍射90周年学术报告会简讯

20 0 2年是劳厄 (MaxVonLaue)发现晶体X射线衍射 90周年 .劳厄的这一发现是 2 0世纪物理学的一件意义深远的大事 ,使物理学中关于物质结构和研究领域从宏观进入微观 ,从经典过渡到现代 ,发生了质的飞跃 .同时 ,X射线衍射的发现和研究对生物、材料科学和化学的发展起到了巨大的推动作用 .中国物理学会和中国晶体学会为纪念劳厄发现X射线衍射 90周年 ,由中国科学院物理研究所于 2 0 0 2年 12月 10日召开了学术报告会 ,会议邀请了部分院士、专家和广大同行 ,就X射线衍射的发现、发展历程 ,最新进展和研究展望以及在相关领域的应用进行了广泛…     

X射线衍射的发现

简单介绍了埃瓦尔德(Ewald P P)、劳厄(von Laue M)和布拉格父子(Bragg W H及Bragg W L)在1912年发现X射线衍射方面的贡献．1911年埃瓦尔德在索末菲的指导下在慕尼黑大学从事博士论文研究，劳厄在与他的讨论中了解到晶格的平移周期与X射线的波长属于同一量级，因此想到在二维光栅的两个衍射方程组中再加一个类似的方程，就可以描述X射线在三维晶体中的衍射．在此假设的指导下，Friedrieh W和Knipping P在1912年4月开始用CuSO4后来用闪锌矿(立方ZnS)进行实验，很快就得到X射线衍射的证据．这不但证明了X射线的波动性，还确定了晶体的三维周期性．老布拉格在1912年夏得知这个消息，与他儿子小布拉格一道尝试用X射线的粒子性解释它，并由小布拉格在剑桥大学重复这个实验．根据衍射斑点的椭圆形状和从Pope与Below那里学到的晶格理论(由此得知ZnS具有面心立方晶格)，小布拉格将X射线在晶体中的衍射看作是X射线从一些晶格平面的反射，从而推导出著名的布拉格方程．布拉格父子开拓了X射线晶体结构分析这门新兴学科，从简单的无机化合物和矿物，逐渐发展到有机化合物和生物大分子．劳厄和布拉格父子分别强调慕尼黑和剑桥的优良科学环境对发现X射线衍射的重要性．鉴于埃瓦尔德在发现X射线衍射的作用及他后来在倒易格子及动力学衍射理论方面的贡献，不少晶体学家认为他也应获得诺贝尔物理奖．     

层状过渡金属硫代亚磷酸盐材料的磁性研究

采用化学气相输运的方法生长了一系列的MPS_3(M=Mn,Fe,Ni)单晶样品.X射线衍射和电子能谱测试结果表明生长出来的样品是纯相并且单晶质量较好.MPS_3单晶样品在低温下均为反铁磁性.当磁场平行于面内时,磁化率—温度曲线在奈尔点以上存在一个较宽的峰值,可能与准二维磁交换导致的短程序有关.这些现象表明MPS_3体系是一个很好的研究二维材料磁性的平台.此前理论与实验结果显示该体系具有宽带隙,电阻率也很大.因此,MPS_3体系在二维层状材料介电方面有很大的应用前景.     

多层膜劳厄透镜对8keV X射线的聚焦性能模拟研究

基于多层膜技术的劳厄(Laue)透镜能实现硬X射线纳米级聚焦,在X射线微纳分析领域具有重要的应用前景.基于衍射动力学理论,分析了X射线在多层膜劳厄透镜中的传播,计算了不同结构的多层膜劳厄透镜对8 keVX射线的聚焦性能.结果表明,最外层厚度为5 nm的倾斜多层膜劳厄透镜可获得5.7 nm的聚焦光斑和26%的平均衍射效率...     

合成氟金云母单晶缺陷的X射线研究

本文报道了人工合成大面积氟金云母单晶中缺陷的X射线研究结果。X射线劳厄法的研究表明,在合成云母中存在着较大程度的一维无序,并因而出现许多堆垛错排区及其亚晶界。X射线衍射形貌术的研究表明,合成云母中的亚晶界和位错线大部分是从晶种起源并向生长表面的法线方向延伸的。晶体的靠近表面的区域缺陷较密集,中心部分较少。探讨了合成云母与天然云母中缺陷分布的差别。对用于制作电容器的合成云母片的缺陷与性能的关系作了分析和讨论。 关键词：     

一种毛细管聚焦的微束X射线衍射仪

微区X射线衍射(micro-X-ray diffraction)分析在测量小样品或样品微区结构方面有着独特的优势.介绍了实验室自行研发的台式毛细管聚焦的微束X射线衍射仪(μ-Hawk),其主要由微焦斑X射线管、毛细管X光透镜、接收狭缝、SDD X射线探测器、q-q测角仪、三维样品台,以及在Lab VIEW语言环境下开发的计算机控制程序等部分组成.控制程序的主界面具备微区X射线衍射分析和微区能量色散X射线荧光分析两种分析模式.为了验证设备的可行性,分别对一枚人民币五角硬币上"角"字第一划中央处的微区和直径为140μm的铜质导线进行微区点分析;对苹果手机主板焊锡接触点上1.0 mm×0.6 mm区域内的物相分布进行二维扫描分析,具体方式为在二维待测区域内逐点自动执行q-q角度扫描,由程序控制的4个电机来实现此过程.分析结果表明,μ-Hawk所具备的微区能量色散X射线荧光分析模式,为物相结构的识别提供了元素种类的参考信息;与常规的X射线衍射仪相比较,μ-Hawk所采集的衍射图整体本底较低,并且所测得的衍射峰位置基本一致;μ-Hawk能适应小样品或样品微区物相结构的分析和物相分布的二维扫描分析,在材料科学、地球科学和文物保护等领域有着广泛的应用前景.     

On the Theory of X-Ray Diffractional Laue Focusing on Two Bent Crystals

The Laue focusing of a spherical x-ray wave onto dynamical diffraction by a double-bent crystal system is studied. The geometrical equations of two-dimensional Laue focusing and the intensity distribution formula are derived. A high sensitivity of the two-dimensional Laue focusing to the crystal thickness and bending radii difference is revealed. It is shown that this sensitivity can be used to control the crystal thickness with accuracy up to 100 and bending radii up to 10^-2 m. The focusing process of the spherical wave inside crystals as well as in vacuum is investigated. The possibility of using the two-crystal Laue system as a lens for x-ray microscopy is studied. The spectral characteristics of a twice-diffracted wave are discussed. The spectral resolution is demonstrated to be 10⁶.     

热处理引起3C-ZnS结构转变的X-射线衍射分析

为了论证层错是硫化锌晶体中交流电致发光的一个必要条件,我们把3C-ZnS单晶体在1100℃热处理后引入了层错.同时,我们对热处理前后的结构,用劳埃背反射法和文献[8、13]推导的公式进行了分析.结果表明,沿3C-结构<111>四个等价方向都可以产生无序、孪晶和2H-结构,而且当热处理时间足够长时,结构转变趋向于一个<111>方向.这些实验结果,在有关的文献中尚未见到.     

Dislocation-based plasticity model and micro-beam Laue diffraction analysis of polycrystalline Ni foil: A forward prediction

A physically-based, rate and length-scale dependent strain gradient crystal plasticity framework was employed to simulate the polycrystalline plastic deformation at the microscopic level in a large-grained, commercially pure Ni sample. The latter was characterised in terms of the grain morphology and orientation (in the bulk) by micro-beam Laue diffraction experiments carried out on beamline B16 at Diamond Light Source. The corresponding finite element model was developed using a grain-based mesh with the specific grain orientation assignment appropriate for the sample considered. Sample stretching to 2% plastic strain was simulated, and a post-processor was developed to extract the information about the local lattice misorientation (curvature), enabling forward-prediction of the Laue diffraction patterns. The ‘streaking’ phenomenon of the Laue spots (anisotropic broadening of two-dimensional (2D) diffraction peaks observed on the 2D detector) was correctly captured by the simulation, as constructed by direct superposition of reflections from different integration points within the diffraction gauge volume. Good agreement was found between the images collected from experiments and simulation patterns at various positions in the sample.     

1 kHz tabletop ultrashort hard x-ray source for time-resolved x-ray protein crystallography

We describe a compact, reliable, and high-average-power femtosecond x-ray source and its first application to diffraction on protein crystal. The setup relies on a homemade Ti: sapphire system delivering 12 mJ at a 1 kHz repetition rate, associated with a small vacuum chamber especially designed for laser-plasma interaction and x-ray applications. This device allows the generation of 5 x 10(9) photons/s/sr at 8 keV and optimized x-ray irradiation of the studied sample, which can be placed close to the source. We present the diffraction pattern of a protein crystal in a divergent beam geometry, which is a first step to a subpicosecond x-ray diffraction experiment.     

ZnS晶体3C⇔2H结构转变的LAUE衍射图中“奇异点”的标定

在ZnS晶体3C⇔2H结构转变的X—射线Laue衍射分析中,为了解释一维无序造成的异常衍射现象,本文推导了Laue衍射图曲线晶带的“奇异点”计算公式。并应用此公式,计算了ZnSLaue衍射照片上数条晶带上的“奇异点”,计算值与实验值完全吻合。另外,本文还对“奇异点”的形成、特点、标定的意义以及计算公式适用范围进行了讨论。     

Effect of neutron spin rotation at Laue diffraction in a deformed transparent crystal with no center of symmetry

The effect of neutron spin rotation at Laue diffraction in a noncentrosymmetric weakly deformed neutron-transparent crystal has been studied experimentally. The effect appears because of two phenomena: (i) the interaction of the magnetic moment of a moving neutron with the crystalline electric field and (ii) bending of trajectories of the neutron in a deformed crystal; as a result, the amplitudes of two waves excited at Laue diffraction, which propagate in the crystal in opposite electric fields, at the output of the crystal are not equal.     

Diffraction reflection of x-ray radiation with a two-dimensionally bounded wavefront from perfect crystals

The problem of dynamical diffraction of x-ray radiation with a two-dimensionally bounded wavefront is solved in the Bragg and Laue geometries in a crystal with an arbitrary thickness and an arbitrary reflection asymmetry parameter. An analysis of the wavefront deformation during the diffraction and subsequent propagation is carried out. It is shown that the most favorable conditions for the reflected beam to retain its shape are accomplished in a crystal whose thickness is less than the extinction depth.     

High pressure x-ray diffraction techniques with synchrotron radiation

This article summarizes the developments of experimental techniques for high pressure x-ray diffraction(XRD) in diamond anvil cells(DACs) using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, timeresolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF(Beijing Synchrotron Radiation Facility) and some results are also presented.     

Evidence for a 2D solid in intercalated graphite CsC24

In-plane x-ray diffraction experiments were carried out on stage-2 CsC₂₄ under hydrostatic pressure. We observed sharp Bragg rings which we claim as evidence for an orientationally unlocked two-dimensional (2D) solid on a single crystal graphite substrate. Annealing and time-dependent experiments suggest that the 2D solid may be thermodynamically stable.