X射线衍射进展简介

100年前,劳厄等证明X射线对硫酸铜晶体具有衍射能力,揭开了X射线衍射分析晶体结构的序幕.100年的发展,X射线衍射已经成为自然科学乃至医学、考古、历史学等众多学科发展的必备技术.文章介绍了X射线衍射现象的发现历史,X射线运动学和动力学理论的发展概况,并举例说明了X射线衍射在粉末多晶体、单晶体和人工功能晶体以及人工薄膜材料中的具体应用情况,最后简要展望了X射线衍射技术的发展前景.     

掠入射X射线衍射研究Si覆盖层对Ge/Si量子点微结构的影响

利用掠入射X射线衍射和常规X射线衍射研究了Si(001)上的Ge量子点在不同厚度的Si覆盖层下微结构的变化,同时用AFM研究了其形貌变化.实验结果表明在小的覆盖度下,量子点中组分的变化已十分明显,同时量子点的形状也发生了明显的变化.     

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．     

X射线衍射的教学

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X射线和中子衍射研究进展

本文概述了近年来X射线和中子衍射方面的研究进展。最重要的进展是在生命科学和材料科学方面。同步辐射的应用大大推动了X射线衍射研究的发展，并由此出现了一系列新的研究领域。中子衍射在工业应用和基础研究方面均获得重要进展。在单晶和多晶的结构分析、数据处理及 晶体对称性研究方面也有突破性成果。     

薄膜结构分析中的低角X射线衍射方法

利用带折射修正的布喇格衍射定律和薄膜光学理论分析了低角Ｘ射线衍射谱中出现的一系列现象，导出了多层膜周期厚度和周期中不同材料间的配比率的计算公式，对多层膜的低角射线衍射谱中主峰间的次峰现象作出了解释，并对低角Ｘ射线衍射测量单层膜厚度进行了分析，给出了精确的测厚公式。     

X射线多重衍射的进展

若晶体具有多个（≥３）原子平面同时满足Ｂｒａｇｇ定律,并同时衍射一单色入射Ｘ射线光束,这就是多重衍射现象。本文介绍Ｘ射线多重衍射的基本原理,获得多重衍射花样的实验方法、衍射理论和若干应用。     

时间分辨的X射线衍射

详细论述了时间分辨X射线衍射探测原子动态过程和生物大分子瞬态结构的各种方法。介绍了多种超快X射线脉冲光源及其在材料和生化领域中的研究进展状况。材料方面:在皮秒时间尺度探测到了晶格间距毫埃的微小变化;在亚皮秒的时间尺度直接观测到晶体的超快熔化过程和晶体内的相干声子散射;生物化学方面:采用时间分辨X射线劳厄衍射方法探测了蛋白质大分子结构的变化和功能之间的关系;精确描述了有机分子在光作用下形态发生改变时分子键角的扭转角度,从结构上揭示了其动态机理。     

时间分辨的X射线衍射

详细论述了时间分辨X射线衍射探测原子动态过程和生物大分子瞬态结构的各种方法。介绍了多种超快X射线脉冲光源及其在材料和生化领域中的研究进展状况。材料方面:在皮秒时间尺度探测到了晶格间距毫埃的微小变化;在亚皮秒的时间尺度直接观测到晶体的超快熔化过程和晶体内的相干声子散射;生物化学方面:采用时间分辨X射线劳厄衍射方法探测了蛋白质大分子结构的变化和功能之间的关系;精确描述了有机分子在光作用下形态发生改变时分子键角的扭转角度,从结构上揭示了其动态机理。     

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,Friedrich　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Barlow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.     

Optical characterization of individual quantum dots

Optical characterization of single quantum dots (QDs) by means of micro-photoluminescence (μPL) will be reviewed. Both QDs formed in the Stranski–Krastanov mode as well as dots in the apex of pyramidal structures will be presented. For InGaAs/GaAs dots, several excitonic features with different charge states will be demonstrated. By varying the magnitude of an external electric or magnetic field and/or the temperature, it has been demonstrated that the transportation of carriers is affected and accordingly the charge state of a single QD can be tuned. In addition, we have shown that the charge state of the QD can be controlled also by pure optical means, i.e. by altering the photo excitation conditions. Based on the experience of the developed InAs/GaAs QD system, similar methods have been applied on the InGaN/GaN QD system.     

Utilizing broadband X‐rays in a Bragg coherent X‐ray diffraction imaging experiment

A method is presented to simplify Bragg coherent X‐ray diffraction imaging studies of complex heterogeneous crystalline materials with a two‐stage screening/imaging process that utilizes polychromatic and monochromatic coherent X‐rays and is compatible with in situ sample environments. Coherent white‐beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three‐dimensional reciprocal‐space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifying in situ chamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.     

X‐ray photon correlation spectroscopy in systems without long‐range order: existence of an intermediate‐field regime

Successful X‐ray photon correlation spectroscopy studies often require that signals be optimized while minimizing power density in the sample to decrease radiation damage and, at free‐electron laser sources, thermal impact. This suggests exploration of scattering outside the Fraunhofer far‐field diffraction limit d²/λR, where d is the incident beam size, λ is the photon wavelength and R is the sample‐to‐detector distance. Here it is shown that, in an intermediate regime d²/λ > Rdξ/λ, where ξ is the structural correlation length in the material, the ensemble averages of the scattered intensity and of the structure factor are equal. Similarly, in the regime d²/λ > Rdξ(τ)/λ, where ξ(τ) is a time‐dependent dynamics length scale of interest, the ensemble‐averaged correlation functions g₁(τ) and g₂(τ) of the scattered electric field are also equal to their values in the far‐field limit. This broadens the parameter space for X‐ray photon correlation spectroscopy experiments, but detectors with smaller pixel size and variable focusing are required to more fully exploit the potential for such studies.     

X‐ray focusing by the system of refractive lens(es) placed inside asymmetric channel‐cut crystals

An X‐ray one‐dimensionally focusing system, a refracting–diffracting lens (RDL), composed of Bragg double‐asymmetric‐reflecting two‐crystal plane parallel plates and a double‐concave cylindrical parabolic lens placed in the gap between the plates is described. It is shown that the focal length of the RDL is equal to the focal distance of the separate lens multiplied by the square of the asymmetry factor. One can obtain RDLs with different focal lengths for certain applications. Using the point‐source function of dynamic diffraction, as well as the Green function in a vacuum with parabolic approximation, an expression for the double‐diffracted beam amplitude for an arbitrary incident wave is presented. Focusing of the plane incident wave and imaging of a point source are studied. The cases of non‐absorptive and absorptive lenses are discussed. The intensity distribution in the focusing plane and on the focusing line, and its dependence on wavelength, deviation from the Bragg angle and magnification is studied. Geometrical optical considerations are also given. RDLs can be applied to focus radiation from both laboratory and synchrotron X‐ray sources, for X‐ray imaging of objects, and for obtaining high‐intensity beams. RDLs can also be applied in X‐ray astronomy.     

Silicon nitride transmission X‐ray mirrors

Transmission X‐ray mirrors have been fabricated from 300–400 nm‐thick low‐stress silicon nitride windows of size 0.6 mm × 85 mm. The windows act as a high‐pass energy filter at grazing incidence in an X‐ray beam for the beam transmitted through the window. The energy cut‐off can be selected by adjusting the incidence angle of the transmission mirror, because the energy cut‐off is a function of the angle of the window with respect to the beam. With the transmission mirror at the target angle of 0.22°, a 0.3 mm × 0.3 mm X‐ray beam was allowed to pass through the mirror with a cut‐off energy of 10 keV at the Cornell High Energy Synchrotron Source. The energy cut‐off can be adjusted from 8 to 12 keV at an angle of 0.26° to 0.18°, respectively. The observed mirror transmittance was above 80% for a 300 nm‐thick film.     

X‐ray dynamical diffraction Fraunhofer holography

An X‐ray dynamical diffraction Fraunhofer holographic scheme is proposed. Theoretically it is shown that the reconstruction of the object image by visible light is possible. The spatial and temporal coherence requirements of the incident X‐ray beam are considered. As an example, the hologram recording as well as the reconstruction by visible light of an absolutely absorbing wire are discussed.     

Coherent X‐ray scattering beamline at port 9C of Pohang Light Source II

The coherent X‐ray scattering beamline at the 9C port of the upgraded Pohang Light Source (PLS‐II) at Pohang Accelerator Laboratory in Korea is introduced. This beamline provides X‐rays of 5–20 keV, and targets coherent X‐ray experiments such as coherent diffraction imaging and X‐ray photon correlation spectroscopy. The main parameters of the beamline are summarized, and some preliminary experimental results are described.     

Simultaneous X‐ray fluorescence and scanning X‐ray diffraction microscopy at the Australian Synchrotron XFM beamline

Owing to its extreme sensitivity, quantitative mapping of elemental distributions via X‐ray fluorescence microscopy (XFM) has become a key microanalytical technique. The recent realisation of scanning X‐ray diffraction microscopy (SXDM) meanwhile provides an avenue for quantitative super‐resolved ultra‐structural visualization. The similarity of their experimental geometries indicates excellent prospects for simultaneous acquisition. Here, in both step‐ and fly‐scanning modes, robust, simultaneous XFM‐SXDM is demonstrated.