化学气相沉积金刚石X射线探测器相对标定

利用神光Ⅱ激光装置,开展了化学气相沉积金刚石X射线探测器的相对标定技术研究。实验得到了金刚石X射线探测器与已绝对标定的平响应X射线二极管对X射线辐射的测量结果,计算得到金刚石X射线探测器平均灵敏度为1.19610-5 C/J,不同发次得到的灵敏度与平均值之间的偏差不大于13%。     

化学气相沉积金刚石X射线探测器相对标定

利用神光Ⅱ激光装置,开展了化学气相沉积金刚石X射线探测器的相对标定技术研究。实验得到了金刚石X射线探测器与已绝对标定的平响应X射线二极管对X射线辐射的测量结果,计算得到金刚石X射线探测器平均灵敏度为1.19610-5 C/J,不同发次得到的灵敏度与平均值之间的偏差不大于13%。     

X射线相位衬度成像

文章使用形象、生动、通俗、易懂的语言,介绍X射线相位衬度成像的基本概念,物理思想和方法,其中包括X射线的基本性质、光的波粒二象性、同步辐射X射线光源和常规非相干X射线光源的相位相干性,以及X射线相位衬度成像方法、三维成像的基本原理和相位衬度成像的最新进展,将抽象的相位、相位一阶导数和相位二阶导数概念与形象的光波阵面平移、倾斜和弯曲等形变联系在一起,着重介绍相位衬度成像发展中的创新思想,力图使读者能分享人类文明在这个学科发展中积累的精神财富.     

X射线相位衬度成像

文章使用形象、生动、通俗、易懂的语言,介绍X射线相位衬度成像的基本概念,物理思想和方法,其中包括X射线的基本性质、光的波粒二象性、同步辐射X射线光源和常规非相干X射线光源的相位相干性,以及X射线相位衬度成像方法、三维成像的基本原理和相位衬度成像的最新进展,将抽象的相位、相位一阶导数和相位二阶导数概念与形象的光波阵面平移、倾斜和弯曲等形变联系在一起,着重介绍相位衬度成像发展中的创新思想,力图使读者能分享人类文明在这个学科发展中积累的精神财富.     

同轴X射线相位衬度计算机X射线断层摄影术研究

基于北京同步辐射装置(BSRF)开展了同轴X射线相位衬度计算机X射线断层摄影术(CT)研究.利用北京同步辐射的14 keV单色X射线作为光源,以高分辨能力的X射线胶片作为探测器,分别开展吸收衬度和同轴相位衬度成像的比较研究以及相位衬度计算机X射线断层摄影术研究.相位衬度计算机X射线断层摄影术重建采用Bronnikov提出的算法.结果显示,与传统的吸收衬度图像相比,相位衬度图像具有更好的衬度和更高的空间分辨力;实验获得人工样品和蝗虫的相位衬度计算机X射线断层摄影术重建图像.重建图像中可见样品的一些结构细节.实验结果表明,相位衬度X射线成像更适合于研究弱吸收或吸收差异很小的材料;利用北京同步辐射开展同轴X射线相位衬度计算机X射线断层摄影术研究是可行的.     

X射线成像板衰退曲线标定

在实验室衍射仪平台上,开展了以富士公司SR-2025型成像板为样品的标定实验,获得了该样品随时间变化的信号强度衰退曲线.实验以铜靶X射线管为光源,经过三羟甲基甲胺晶体(Trihydroxymethylaminomethane,TAM)分光得到Cu-Kα单能特征辐射.在实验环境温度为(20±1)℃、光源稳定、成像板空间响应均匀、信号强度线性响应等条件下,在不同时刻对成像板上不同位置进行曝光,扫描后获得成像板对单能特征X射线的衰退曲线.对测到的衰退曲线进行数值拟合及不确定度分析,发现其与国外的研究结果符合得较好.实验数据表明,X射线光源的不稳定性为0.7%,成像板的空间非均匀性小于1%,并且对信号强度呈优异的线性响应;在Cu-Kα的8 027.84eV能点处,成像板的衰退曲线呈指数形式η(t)=0.368 84·exp(-t/159.647 56)+0.633 72缓慢衰减,在可见光屏蔽良好条件下曝光125min后X射线信号仍有80%的强度.     

天文观察用超软X射线探测器的标定

在北京同步辐射装置3W1B光束线上,对天文观测用超软X射线(0.2keV—3.5keV)正比计数管探测器进行了系统地标定.得到了正比计数管的死时间、计数率坪曲线、能量线性、能量分辨、窗材料透过比曲线;借助于已标定过的光电二极管探测器,测量了正比管探测器的能量响应效率,标定不确定度在10%—18%之间.另外,还对正比管系统在卫星上的六道记录和在实验室里的多道记录进行了对比,两种记录方式符合得很好.     

基于X射线衍射仪的X光晶体本征参量的标定

X光晶体本征参量的实验标定是准确鉴定X光晶体种类和品质,研制各种类型晶体谱仪,X光线谱定量测量和高分辨X光单能成像的基础.基于X射线衍射仪,通过制作平面晶体样品架,采取控制X射线管电源、滤波片选取和厚度控制等措施,极大地抑制了Cu-Kβ及韧致辐射,使X射线管光源Cu-Kα单能化,提出了用滤片作为光源单能化的判据.对X光线谱测量中常用的X光分光晶体季戊四醇的晶格常量2d和Cu-Kα能点的积分衍射效率R_c进行了标定方法研究,其标定值分别为(0.874 25±0.000 42)nm和(1.759±0.024)×10^-4 Rad.基于X射线衍射仪的X光晶体本征参量的精密实验标定方法既快速高效,且十分方便和灵活.通过更换衍射仪的X射线管靶材,采取类似方法,可以标定其它能点的晶体积分衍射效率,可为X光晶体的本征参量库提供更多的标定数据.     

基于X射线衍射仪的X光晶体本征参量的标定

X光晶体本征参量的实验标定是准确鉴定X光晶体种类和品质,研制各种类型晶体谱仪,X光线谱定量测量和高分辨X光单能成像的基础.基于X射线衍射仪,通过制作平面晶体样品架,采取控制X射线管电源、滤波片选取和厚度控制等措施,极大地抑制了Cu-KJ3及韧致辐射,使X射线管光源Cu-Kα单能化,提出了用滤片作为光源单能化的判据.对X光线谱测量中常用的X光分光晶体季戊四醇[PET(002)]的晶格常量2d和Cu-Ka能点的积分衍射效率R.进行了标定方法研究,其标定值分别为(0.87425±0.00042)nm和(1.759±0.024)×10-4 Rad.基于X射线衍射仪的X光晶体本征参量的精密实验标定方法既快速高效,且十分方便和灵活.通过更换衍射仪的X射线管靶材,采取类似方法,可以标定其它能点的晶体积分衍射效率,可为X光晶体的本征参量库提供更多的标定数据.     

航空胶片的X射线标定

利用光谱扩展的荧光型软X射线单色光源产生的多条谱线,通过时间递增和光强递增的方法首次标定了国产高速航空胶片在软X射线和超软X射线波段的响应特性,给出了这种胶片的响应特性曲线即光学密度与曝光量的关系和相对光谱灵敏度曲线.     

Linear polarization scans for resonant X‐ray diffraction with a double‐phase‐plate configuration

An in‐vacuum double‐phase‐plate diffractometer for performing polarization scans combined with resonant X‐ray diffraction experiments is presented. The use of two phase plates enables the correction of some of the aberration effects owing to the divergence of the beam and its energy spread. A higher rate of rotated polarization is thus obtained in comparison with a system with only a single retarder. Consequently, thinner phase plates can be used to obtain the required rotated polarization rate. These results are particularly interesting for applications at low energy (e.g. 4 keV) where the absorption owing to the phase plate(s) plays a key role in the feasibility of these experiments. Measurements by means of polarization scans at the uranium M₄ edge on UO₂ enable the contributions of the magnetic and quadrupole ordering in the material to be disentangled.     

位相恢复法重现软X射线同轴全息图

在物平面和全息平面上分别施加限制条件,实现了同轴全息图的位相恢复重现,基本消除了孪生像的干扰。提出了一种软Ｘ射线同轴全息实时成像的方案     

White‐beam X‐ray radioscopy and tomography with simultaneous diffraction at the EDDI beamline

A set‐up for simultaneous imaging and diffraction that yields radiograms with up to 200 frames per second and 5.6 µm effective pixel size is presented. Tomograms and diffractograms are acquired together in 10 s. Two examples illustrate the attractiveness of combining these methods at the EDDI beamline for in situ studies.     

利用边缘相位校正实现光束整形的高精度优化

提出利用边缘相位校正的新方法,校正用追迹法设计的产生环形光束的衍射光学元件的相位分布,从而实现光束整形中的高精度优化。通过将高斯光束整形为环形光束,将该方法、G-S(Gerchberg-Saxton)算法和改进的G-S算法设计得到的整形结果作了比较,结果表明,G-S算法的整形结果虽然衍射效率最大,但是均方根值和最大偏差也太大;改进的G-S算法可以有效的降低均方根值和最大偏差,但衍射效率也有较大的下降;而用边缘相位校正可以在衍射效率略微下降的情况下,更大的降低均方根值和最大偏差,其整形结果是综合了衍射效率、均方根值和最大偏差这三个评价指标以后得到的最优化结果,已接近理想的环形光束。     

Fabrication and testing of a newly designed slit system for depth‐resolved X‐ray diffraction measurements

A new system of slits called `spiderweb slits' have been developed for depth‐resolved powder or polycrystalline X‐ray diffraction measurements. The slits act on diffracted X‐rays to select a particular gauge volume of sample, while absorbing diffracted X‐rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range of diffraction angles, and work for X‐ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray‐tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X‐ray Powder Diffraction beamline at the National Synchrotron Light Source II.     

The power of in situ pulsed laser deposition synchrotron characterization for the detection of domain formation during growth of Ba0.5Sr0.5TiO3 on MgO

A highly sophisticated pulsed laser deposition (PLD) chamber has recently been installed at the NANO beamline at the synchrotron facility ANKA (Karlsruhe, Germany), which allows for comprehensive studies on the PLD growth process of dielectric, ferroelectric and ferromagnetic thin films in epitaxial oxide heterostructures or even multilayer systems by combining in situ reflective high‐energy diffraction with the in situ synchrotron high‐resolution X‐ray diffraction and surface diffraction methods. The modularity of the in situ PLD chamber offers the opportunity to explore the microstructure of the grown thin films as a function of the substrate temperature, gas pressure, laser fluence and target–substrate separation distance. Ba_0.5Sr_0.5TiO₃ grown on MgO represents the first system that is grown in this in situ PLD chamber and studied by in situ X‐ray reflectivity, in situ two‐dimensional reciprocal space mapping of symmetric X‐ray diffraction and acquisition of time‐resolved diffraction profiles during the ablation process. In situ PLD synchrotron investigation has revealed the occurrence of structural distortion as well as domain formation and misfit dislocation which all depend strongly on the film thickness. The microstructure transformation has been accurately detected with a time resolution of 1 s. The acquisition of two‐dimensional reciprocal space maps during the PLD growth has the advantage of simultaneously monitoring the changes of the crystalline structure as well as the formation of defects. The stability of the morphology during the PLD growth is demonstrated to be remarkably affected by the film thickness. A critical thickness for the domain formation in Ba_0.5Sr_0.5TiO₃ grown on MgO could be determined from the acquisition of time‐resolved diffraction profiles during the PLD growth. A splitting of the diffraction peak into two distinguishable peaks has revealed a morphology change due to modification of the internal strain during growth.     

Design and application of a high‐temperature microfurnace for an in situ X‐ray diffraction study of phase transformation

Thermal treatment of mineral ores such as ilmenite can initiate phase transformations that could affect their activation or deactivation, subsequently influencing their ability to dissolve in a leaching agent. Most laboratory‐based X‐ray diffraction (XRD) studies were carried out ex situ in which realistic diffraction patterns could not be obtained simultaneously with occurring reactions and were time‐consuming. The availability of synchrotron‐radiation‐based XRD not only allows in situ analysis, but significantly shortens the data recording time. The present study details the design of a robust high‐temperature microfurnace which allows thermal processing of mineral ore samples and the simultaneous collection of high‐resolution synchrotron XRD data. In addition, the application of the manufactured microfurnace for in situ study of phase transformations of ilmenite ore under reducing conditions is demonstrated.     

A protocol for searching the most probable phase‐retrieved maps in coherent X‐ray diffraction imaging by exploiting the relationship between convergence of the retrieved phase and success of calculation

Coherent X‐ray diffraction imaging (CXDI) is a technique for visualizing the structures of non‐crystalline particles with size in the submicrometer to micrometer range in material sciences and biology. In the structural analysis of CXDI, the electron density map of a specimen particle projected along the direction of the incident X‐rays can be reconstructed only from the diffraction pattern by using phase‐retrieval (PR) algorithms. However, in practice, the reconstruction, relying entirely on the computational procedure, sometimes fails because diffraction patterns miss the data in small‐angle regions owing to the beam stop and saturation of the detector pixels, and are modified by Poisson noise in X‐ray detection. To date, X‐ray free‐electron lasers have allowed us to collect a large number of diffraction patterns within a short period of time. Therefore, the reconstruction of correct electron density maps is the bottleneck for efficiently conducting structure analyses of non‐crystalline particles. To automatically address the correctness of retrieved electron density maps, a data analysis protocol to extract the most probable electron density maps from a set of maps retrieved from 1000 different random seeds for a single diffraction pattern is proposed. Through monitoring the variations of the phase values during PR calculations, the tendency for the PR calculations to succeed when the retrieved phase sets converged on a certain value was found. On the other hand, if the phase set was in persistent variation, the PR calculation tended to fail to yield the correct electron density map. To quantify this tendency, here a figure of merit for the variation of the phase values during PR calculation is introduced. In addition, a PR protocol to evaluate the similarity between a map of the highest figure of merit and other independently reconstructed maps is proposed. The protocol is implemented and practically examined in the structure analyses for diffraction patterns from aggregates of gold colloidal particles. Furthermore, the feasibility of the protocol in the structure analysis of organelles from biological cells is examined.     

A plug‐and‐measure diagnostic tool for flux,resolution and beam size of a soft X‐ray beamline

A compact multi‐functional diagnostic tool has been installed for commissioning beamlines at the Taiwan Light Source. For a photon beam, the instrument can measure the photon flux, energy resolution and beam size, consecutively with a photodiode or gold mesh, a windowless gas cell and a movable fluorescence screen viewport. Two gratings with ruling densities of 350 and 1000 lines mm^?1 and dispersing photons of energies from 80 to 1200 eV were calibrated with a photon flux of 10¹¹ photon s^?1 at slit openings of 50 µm × 50 µm; a maximum resolving power of greater than 10000 was certified with an absorption spectra of gaseous samples. Pressure differences over four orders of magnitude were achieved between the ion chamber and the flux measurement chamber with a single capillary differential pumping stage. A sequence of beam profiles was measured by moving continuously in the vicinity of the nominal focal positions. This tool is useful in commissioning or trouble‐shooting at most beamlines in a synchrotron facility.