基于单毛细管椭球镜的微束X射线荧光成像

X射线荧光成像是一种可无损获得样品内部元素空间分布信息的实验技术,可分为荧光mapping扫描成像与荧光CT成像,其空间分辨率由X射线聚焦束斑的大小决定。上海光源成像线站已建立X射线荧光成像系统并对用户开放,在多个领域取得较好的研究成果,该系统基于狭缝限束获取微束X射线,束斑为150μm,限制了该方法的广泛应用。椭球聚焦镜是反射面为椭球面的单次反射单毛细管光学元件,基于全反射原理,具有反射效率高、工作距离长、接收角宽、适用X射线能量范围宽、体积小等优点,已应用到X射线聚焦、全场纳米成像等领域。由于对面型精度的要求较高,制备椭球聚焦镜难度较大。为满足广大用户对微束荧光成像的需求,自行设计并成功研制了针对微束荧光成像系统的单毛细管椭球镜,并对其进行了X射线聚焦性能检测,结果显示可获得14μm聚焦光斑,焦点处增益可达255倍。基于自主研制的椭球镜,在上海光源BL13W搭建微束X射线荧光成像系统,并开展了微束荧光mapping成像与微束荧光CT实验研究:(1)对中风鼠脑切片的荧光mapping扫描成像,得到中风鼠脑中微量元素铜、铁、钙与锌的元素分布荧光光谱图;(2)对鼠脑及毛细管中浓度为0.5 mg·L~(-1)的标准砷溶液进行同步辐射微束X射线荧光CT成像,利用OSEM重构算法重构投影数据,获得了鼠脑中铜元素和毛细管中砷元素二维分布的切片图。两组实验表明,基于自行设计与研制的单毛细管椭球镜的微束X射线荧光成像系统,样品处的光通量密度增加,空间分辨率得到提高,单张荧光光谱的获取时间显著减少,同时也提高了系统的元素探测限。     

基于同步辐射的快速扫描X射线微束荧光成像方法

在上海光源硬X射线微聚焦光束线站(BL15U1)上, 基于EPICS软件平台, 集成运动控制, 光强探测, 荧光探测等功能, 实现了"飞行"模式 (on-the-fly) X射线扫描微束荧光成像方法. 用"飞行"扫描X射线荧光成像法获得了标准镍网, 以及微量元素Cu, Zn,K, Fe在样品老鼠脾内的分布图像, 结果显示该方法不但在速度上有了极大的提高, 而且获得的元素分布图像具有高质量. 关键词： 快速扫描X射线微束荧光成像 同步辐射 微量元素分布     

同步辐射微束荧光CT及其应用新进展

同步辐射微束X射线荧光CT（SR-XFCMT）是将传统的X射线荧光分析法和计算机断层成像（CT）技术有机结合发展起来的一种先进的分析技术．SR-XFCMT可以给出元素在样品内部的分布而不需要对样品进行破坏性的处理，现已成为很多研究领域的有力工具．文章简要介绍了同步辐射微束荧光CT技术及其应用的最新进展，阐述了同步辐射微束X射线荧光CT的关键问题及其发展的前景.     

毛细管X光透镜三维共聚焦微束X射线荧光技术在岩矿样品分析中的应用

利用毛细管X光透镜搭建了三维共聚焦微束X射线荧光谱仪,处在激发道的多毛细管X射线会聚透镜和处在探测道的多毛细管X射线平行束透镜处于共聚焦状态,该共聚焦结构降低了X射线荧光光谱的背底,从而有利于降低的X射线荧光分析技术的探测极限。在上述共聚焦结构中,多毛细管X射线会聚透镜和多毛细管X射线平行束透镜的焦斑重合形成共聚焦微元,探测器只能探测到来自该共聚焦微元内的X射线荧光信号,当该共聚焦微元在样品移动时,就可利用该共聚焦技术原位无损得到样品内部的三维X射线荧光信息。该共聚焦技术使用的多毛细管X射线会聚透镜具有103量级的功率放大倍数,从而降低了该共聚焦技术对高功率X射线源的依赖程度,即利用低功率普通X射线源就可以设计毛细管X光透镜共聚焦X射线荧光技术。利用上述共聚焦微束X射线荧光谱仪对两种岩矿样品进行三维无损分析,在其中一种岩石中发现：Fe浓度大的区域Cu的浓度也大,这在一定程度上反映了岩矿自然生长的机理。实验结果证明：该共聚焦X射线荧光技术可以在不破坏样品情况下分析岩矿样品中元素成分组成和元素三维分布情况。该共聚焦三维微束X射线荧光技术在矿石勘察、玉器选材和鉴别、石质食用器皿、“赌石”和家用石质地板检测等领域具有潜在的应用。     

一款小角X射线散射测量专用样品旋转装置

在小角X射线散射实验中经常需要对各向异性结构样品进行旋转。针对传统样品架为固定方式,旋转调整困难的特点,本文设计了一款小角X射线散射专用的样品旋转装置。该装置主要由步进电机、高精度回转轴承、传动系统、样品架、控制器及配套软件等组成,它具有结构简单、回转精度高、可远程控制的特点。在北京同步辐射小角X射线散射实验站应用该样品旋转装置对石墨纤维样品进行了测试,验证了该装置的可行性。     

实验室光源的微束X射线荧光成像系统研制及应用研究

微束X射线荧光成像(μ-XRFI)是无损获取样品内部元素微区分布信息的重要方法,主要应用于微米量级区域内的元素分辨成像。同步辐射是μ-XRFI的理想光源,由于其装置庞大、造价高昂,用户机时紧张,并不适宜于常规应用。基于实验室X射线光管、多毛细管聚焦镜、高精度样品台及硅漂移探测器,研制了一套具有元素分辨的μ-XRFI系统,性能测试结果表明该系统可以测量分析元素含量为0.001%量级的溶液样品和优于20μm的空间分辨能力。基于该μ-XRFI系统开展了应用研究,获得了小鼠脑、芯片及古代陶瓷样品中的多种主要元素及微量元素的空间分布,结果表明该系统可满足μ-XRFI的需求,可为生物医学、电子元件检测、瓷器色彩成分鉴定等领域研究提供帮助。     

合肥同步辐射软X射线显微术研究

合肥国家同步辐射实验室首期建设的光束线之一用于软Ｘ射线显微成像研究。实验站现已装置初型的扫描透射Ｘ射线显微镜，并正在进行亲一代的扫描显微建设，同时还使同步辐射光进行接触软Ｘ射线呈微成像研究，并对选取的一些生物样品进行了成像试验。本文介绍了合肥同步辐射光源上软Ｘ射线显微术实验线站的建设及完成的一些实验结果。     

硬X射线微束掠入射实验的控制和数据采集系统及其应用

在国内发展了硬X射线微束掠入射实验方法,并将此具有微米级高空间分辨率的方法应用于纳米厚度薄膜的微区分析。该实验方法对分析样品表面或薄膜在微小区域的不均匀组分、结构、厚度、粗糙度和表面元素化学价态等信息具有重要意义。基于X射线全反射原理,以微聚焦实验站的高通量、能量可调的单色微束X射线为基础,通过集成运动控制、光强探测、衍射和荧光探测,设计了掠入射实验方法的控制和数据采集系统。此系统采用分布式控制结构,并基于Experimental Physics and Industrial Control System （EPICS）环境设计SPEC控制软件。通过建立SPEC和EPICS的访问通道,实现SPEC软件对EPICS平台上设备的控制和数据获取。在所设计的控制和数据采集系统中,运动控制系统控制多维样品台电机的运动,实现定位样品位置和调节掠入射角;光强探测系统则监测样品出射光强度,通过样品台运动控制和光强探测的联控,实现样品台的扫描定位控制;通过衍射和荧光探测系统获取不同入射深度下样品的衍射峰强度和荧光计数。此外,为准确控制掠入射角角度,必须确定样品平面与X射线平行的零角度位置,对此给出一种自动定位零角度的方法,编写了该方法的控制算法,设计了相应的控制软件。零角度自动化定位的扫描结果表明,实验系统微区分析的空间分辨率达到2.8 μm,零角度定位精度小于±0.01°。利用该系统在上海光源微聚焦实验站首次实现了具有自动化准确控制零角度的微束掠入射X射线衍射和荧光同步表征的实验方法,实验中被测样品为10 nm Au/Cr/Si薄膜材料,Si基底最上层为10 nm厚的Au薄膜,其间为一层很薄的Cr粘附层。在不同掠入射角下测量样品的衍射信号,获取不同入射深度下样品的衍射峰强度,并实现在同一掠入射角下,同步采集样品的荧光计数信号,从而确定了样品表层的相结构信息以及荧光信号强度与入射角关系,实现了对纳米厚度薄膜在微小区域的相结构和组分分析。此外,通过该技术能够选取荧光计数最大值对应的入射角度,有助于提高后续发展的低浓度样品掠入射X射线吸收近边结构实验方法的信噪比。     

掠入射式超环面反射镜组X射线显微镜设计（英文）

为了实现对激光惯性约束聚变中物理过程的诊断,建立了X射线显微成像系统。对该系统所采用的超环面镜成像特性、系统的光学设计、像差分析、公差分析和装调方法进行了研究。首先,以等离子体诊断的要求为依据确定了部分光学系统参数,设计了由U型排布的两个超环面镜和一个用于谱选择的平面镜构成的显微成像系统。根据消像散聚焦初步确定三个反射镜的结构参数,并利用光学设计软件进行了优化。接着,分析了X射线显微镜的球差、彗差、视场倾斜和像散。通过分析系统参数变化对成像质量的影响,根据系统精度要求确定了合理的公差。最后,针对离线超环面镜离轴掠入射装调问题,设计了一种辅助光学系统,并为在线高精度系统装调设计了一种双向双目交汇瞄准系统。实验结果表明:显微成像系统在物方视场500μm处的分辨率优于5μm,基本满足激光等离子体X射线成像的大视场和高分辨等要求。     

基于毛细管分光的同步辐射X射线立体成像

建立了一种基于同步辐射X射线的立体成像系统用于上海光源成像线站(BL13W)。该系统使用两个弯曲毛细管将同步辐射光引出并分为交叉的两束光,实验样品置于两束X射线交叉的位置,在其后一定距离处用成像探测器记录样品的两个投影。根据视差方程和相应算法计算出样品各组分的深度信息,得到样品的伪三维图像。与X射线计算机断层扫描技术相比,该方法成像的时间分辨率大大提升甚至接近单次曝光的时间,可以进行实时成像,并降低了样品受辐射的剂量。选用老鼠肝脏毛细血管的投影图像进行数值模拟,得到了理想的模拟效果。选取螺旋形金属丝在搭建的实验平台上进行立体成像,得到了初步的实验结果。螺旋形金属丝的立体信息可以清楚辨认。     

X射线同轴相衬成像的参数优化系统

通过对具有2维高斯型相位分布特征的物体的X射线同轴相衬成像技术进行理论分析,建立了成像系统参数优化系统。优化系统明确了图像衬度、信噪比、分辨力和探测器抽样数等成像质量评价参数对射线源能量、源焦斑尺寸、探测器分辨力、成像几何和物体结构特性等系统参数的依赖关系。采用数值模拟,分别对亚微焦点源、激光驱动微焦点源和同步辐射源3种X射线源下的成像系统相关参数进行了优化。结果表明,优化系统很好地完成了系统的优化工作。     

同步辐射X射线荧光光谱国内外研究进展

同步辐射光源是带电粒子在加速器储存环中以接近光速的速度运动时,沿轨道切线方向发射出的辐射,同步辐射X射线荧光分析(SR-XRF)是以同步辐射X射线作为激发光源的X荧光光谱分析技术.同步辐射X射线荧光分析包括了用于微区及微量元素分析的同步辐射XRF、用于表面及薄膜分析的同步辐射全反射X射线荧光(SR-TXRF)以及用于三...     

The first microbeam synchrotron X‐ray fluorescence beamline at the Siam Photon Laboratory

The first microbeam synchrotron X‐ray fluorescence (µ‐SXRF) beamline using continuous synchrotron radiation from Siam Photon Source has been constructed and commissioned as of August 2011. Utilizing an X‐ray capillary half‐lens allows synchrotron radiation from a 1.4 T bending magnet of the 1.2 GeV electron storage ring to be focused from a few millimeters‐sized beam to a micrometer‐sized beam. This beamline was originally designed for deep X‐ray lithography (DXL) and was one of the first two operational beamlines at this facility. A modification has been carried out to the beamline in order to additionally enable µ‐SXRF and synchrotron X‐ray powder diffraction (SXPD). Modifications included the installation of a new chamber housing a Si(111) crystal to extract 8 keV synchrotron radiation from the white X‐ray beam (for SXPD), a fixed aperture and three gate valves. Two end‐stations incorporating optics and detectors for µ‐SXRF and SXPD have then been installed immediately upstream of the DXL station, with the three techniques sharing available beam time. The µ‐SXRF station utilizes a polycapillary half‐lens for X‐ray focusing. This optic focuses X‐ray white beam from 5 mm × 2 mm (H × V) at the entrance of the lens down to a diameter of 100 µm FWHM measured at a sample position 22 mm (lens focal point) downstream of the lens exit. The end‐station also incorporates an XYZ motorized sample holder with 25 mm travel per axis, a 5× ZEISS microscope objective with 5 mm × 5 mm field of view coupled to a CCD camera looking to the sample, and an AMPTEK single‐element Si (PIN) solid‐state detector for fluorescence detection. A graphic user interface data acquisition program using the LabVIEW platform has also been developed in‐house to generate a series of single‐column data which are compatible with available XRF data‐processing software. Finally, to test the performance of the µ‐SXRF beamline, an elemental surface profile has been obtained for a piece of ancient pottery from the Ban Chiang archaeological site, a UNESCO heritage site. It was found that the newly constructed µ‐SXRF technique was able to clearly distinguish the distribution of different elements on the specimen.     

On-line laser heating setup for ED-XAS at ID24: preliminary optical design and test results

Double-sided laser heating (LH) combined with synchrotron X-ray radiation for in situ studies in the diamond anvil cell (DAC) has been the most productive and widely used high-temperature–high pressure technique in the past two decades. In the framework of the UPBL11 project (upgrade of ID24 beamline of European Synchrotron Radiation Facility), we developed a new on-line LH system for DACs. The preliminary optical scheme of the system is presented and discussed. Varying the settings, we are able to shape and to size the beam on the surface of the sample in the DAC. First pilot applications to the Fe case are shown.     

ALBA Synchrotron Facility

ALBA is the Spanish synchrotron facility located in the area of Barcelona. It is a low-emittance, 3 GeV machine having, at present, seven state-of-the-art operating beamlines covering soft and hard X-rays. The hard X-ray beamlines comprise macromolecular crystallography, non-crystalline diffraction (SAXS and WAXS), high-resolution powder diffraction, and absorption spectroscopy. The soft X-ray beamlines include a photoemission beamline with two endstations—one devoted to photoelectron microscopy (PEEM) and the second to near ambient pressure photoemission (NAPP)—and another beamline devoted to XMCD and soft X-ray scattering. Both beamlines allow full control of the polarization of the beam, since they are equipped with helical undulators. An additional soft X-ray beamline, installed on a bending magnet port, is equipped with a full-field transmission X-ray microscope. Additional information may be found at http://www.albasynchrotron.es/en/beamlines.     

Radiation damage from EELS and NEXAFS in diesel soot and diesel soot extracts

Carbon NEXAFS and EELS spectra of soot, and NEXAFS spectra of soot extracts, are presented. The EELS spectra of solid soot particles from a TEM-EELS show fewer structures than the corresponding NEXAFS spectra obtained at two different synchrotron beamlines. We attribute radiation damage in the TEM-EELS to the failure at resolving structures of surface functional carbon groups in or on soot. NEXAFS spectra of soot extracts studied with a scanning transmission X-ray microscope show alterations during X-ray exposure, which can be explained by a simple chemical model where oxygen apparently reacts with the sample. When the same extract is studied in an ultrahigh-vacuum beamline, no such alterations are observed.     

Design,development and first experiments on the X‐ray imaging beamline at Indus‐2 synchrotron source RRCAT,India

A full‐field hard X‐ray imaging beamline (BL‐4) was designed, developed, installed and commissioned recently at the Indus‐2 synchrotron radiation source at RRCAT, Indore, India. The bending‐magnet beamline is operated in monochromatic and white beam mode. A variety of imaging techniques are implemented such as high‐resolution radiography, propagation‐ and analyzer‐based phase contrast imaging, real‐time imaging, absorption and phase contrast tomography etc. First experiments on propagation‐based phase contrast imaging and micro‐tomography are reported.     

Microscopic imaging and holography with hard X-rays using Fresnel zone-plates

The imaging properties of a Fresnel zone-plate (FZP) were used for magnified imaging of microobjects using hard X-rays. The experiments were done using 14 keV synchrotron radiation. The coherence properties of the radiation produced by an undulator allowed the recording of real images and holograms from an object in one single exposure. These images result from the positive and the negative first order diffracted beams respectively. The X-ray microscope worked at an X-ray magnification factor of 12 and could resolve structures of 0.3 μm in size. By going to slightly defocused conditions we obtained magnified images of the holographical nearfield diffraction pattern (in-line holograms) of the object.     

Confocal three-dimensional micro X-ray fluorescence based on synchrotron radiation for mineral analysis

The confocal three-dimensional micro X-ray fluorescence using polycapillary optics and a synchrotron radiation was applied to nondestructively analyze elemental compositions of minerals, and thereby obtain the three-dimensional distributions of elements in the minerals. Such confocal micro X-ray fluorescence had potential applications in the mineral prospecting, identification of jades, differentiation of stones.