Parametrization of a tabletop micro-XRF system

A table-top micro X-ray fluorescence apparatus composed of a conventional X-ray tube with a polycapillary lens and a silicon drift X-ray detector was parametrized according to an independent parameter approach. The tube bremsstrahlung spectrum was calculated from the Bethe-Heitler equation, convoluted by the energy distribution of radiating electrons in the target. In this paper, we propose a simple analytical approximation for this energy distribution. An analytical approximation is also proposed for transmission of the lens composed of curved capillaries.     

A new film analysis method using polycapillary X-ray lens

Grazing emission X-ray fluorescence (GE-XRF) is a development of XRF related to total reflection XRF. This paper proposed a GE-MXRF setup involved a polycapillary X-ray lens. Polycapillary lens is an effective optics to obtain μm-size primary X-ray beam. Using this proposed setup, we applied it to the analysis of film samples, and the information of film thickness, composition and density can be acquired, which is very useful in semiconductor industry.     

Experimental evaluation of X‐ray optics applied for microanalysis

The performance of x‐ray capillary lenses has been evaluated. The tests were carried out using an x‐ray tube set‐up. A single glass capillary with tapered inner channel, a monolithic glass polycapillary, and an in‐house manufactured single metallic capillary with parabolic inner channel were characterized in terms of gain, spatial resolution, and element detection limits. The spatial resolution of a confocal set‐up utilizing a monolithic glass polycapillary and a polycapillary conical collimator has also been measured. The highest gain of about 2500 was observed for the glass polycapillary. The maximum gain achieved with the single glass capillary was equal to about 25, and the gain of the metallic capillary was only slightly greater than 1. For the glass capillary and polycapillary lenses, significant filtering of the higher‐energy photons (energy > 8 keV) was observed. The lowest relative detection limits were obtained with an ordinary cylindrical collimator and the polycapillary lens. Similar absolute detection limits were achieved with the use of the polycapillary and single capillary lenses. A relation between the ratios of the detection limits of elements achieved with different x‐ray lenses and the lens parameters (spatial resolution and gain) has been proposed and was verified experimentally. The monolithic polycapillary lens was found to be an optimum focusing device for an x‐ray tube‐based scanning spectrometer. This type of x‐ray lens can be coupled with a polycapillary conical collimator or a polycapillary half‐lens to make a confocal x‐ray microscope capable of depth profiling with a spatial resolution equal to about 30 micrometers. Copyright © 2008 John Wiley & Sons, Ltd.     

利用毛细管X光透镜共聚焦微束X射线荧光技术对单根头发中元素空间分布进行无损扫描分析

头发中的元素与人的饮食和健康状况有关,对头发中元素的分析,不仅可用于刑事物证鉴别,还可为疾病的预防和治疗提供依据,因此,如何检测头发中元素分布等信息倍受人们关注。本文利用基于毛细管X光透镜和实验室普通X射线光源的共聚焦微束X射线荧光技术对单根头进行了无损扫描分析,分析了单根头发中元素的空间分布。在该毛细管X光透镜共聚焦微束X射线荧光技术中,毛细管X光会聚透镜的出口焦斑和毛细管X光平行束透镜的入口焦斑处在共聚焦状态,从而形成共聚焦微元,探测器只能探测到来自该共聚焦微元中的X射线信号,降低了背底信号对X射线荧光谱的影响,从而有利于提高该共聚焦X射线荧光技术的分析精度。该共聚焦技术中采用了具有高功率密度增益的毛细管X光会聚透镜,降低了该共聚焦X射线荧光技术对X射线光源功率的要求,从而保证了该共聚焦技术可以采用实验室普通X射线光源,降低了实验成本。实验表明,毛细管X光透镜共聚焦微束X射线荧光技术在单根头发元素分布检测中具有应用价值。     

A simple calibration procedure of polycapillary based portable micro‐XRF spectrometers for reliable quantitative analysis of cultural heritage materials

Portable micro‐X‐ray fluorescence (micro‐XRF) spectrometers mostly utilize a polycapillary X‐ray lens along the excitation channel to collect, propagate and focus down to few tens of micrometers the X‐ray tube radiation. However, the polycapillary X‐ray lens increases the complexity of the quantification of micro‐XRF data because its transmission efficiency is strongly dependent on the lens specifications and the propagated X‐ray energy. This feature results to a significant and not easily predicted modification of the energy distribution of the primary X‐ray tube spectrum. In the present work, we propose a simple calibration procedure of the X‐ray lens transmission efficiency based on the fundamental parameters approach in XRF analysis. This analytical methodology is best suited for compact commercial and portable micro‐XRF spectrometers. The developed calibration procedure is validated through the quantitative analysis of a broad range of samples with archeological relevance such as glasses, historical copper alloys, silver and gold alloys offering an overall accuracy of less than 10%–15%. Copyright © 2015 John Wiley & Sons, Ltd.     

X-ray microbeams based on Kumakhov polycapillary optics and its applications: Analytical consideration

Kumakhov polycapillary optics is based on the effective passage of X-ray radiation through bundles of monocapillaries of various configurations. The passage of radiation takes place because of the total external reflection of X-rays from the inner capillary walls. In this work, the basic characteristics of intense quasi-parallel X-ray polycapillary microbeams from a laboratory source with microfocus X-ray tube/polycapillary cylindrical structure are investigated theoretically (analytical consideration). The data generated from theoretical estimations are compared with the experimental results. Several new generations of X-ray analytical devices like, laboratory synchrotron, fluorescent spectrometers, reflectometers/refractometers, diffractometers, X-ray microscopes and combinations of several such devices, are developed based on polycapillary optics. Besides, a number of devices can be developed for the most modern research problems such as nanomateriology, namely, X-ray nanoscanner, portable X-ray nanothickness indicator etc. X-ray tubes and the radiators, specially developed for polycapillary optics as efficiently as possible, are used in all the devices mentioned above.     

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。     

Application of Three Dimensional Confocal Micro X-Ray Fluorescence Technology Based on Polycapillary X-Ray Lens in Analysis of Rock and Mineral SamplesSCIEI北大核心CSCD

Confocal three dimensional (3D) micro X-ray fluorescence (XRF) spectrometer based on a polycapillary focusing X-ray lens (PFXRL) in the excitation channel and a polycapillary parallel X-ray lens (PPXRL) in the detection channel was developed. The PFXRL and PPXRL were placed in a confocal configuration. This was helpful in improving the signal-to-noise ratio of the XRF spectra, and accordingly lowered the detection limitation of the XRF technology. The confocal configuration ensured that only the XRF signal from the confocal micro-volume overlapped by the output focal spot of the PFXRL and the input focal spot of the PPXRL could be detected by the detector. Therefore, the point-to-point information of XRF for samples could be obtained non-destructively by moving the sample located at the confocal position. The magnitude of the gain in power density of the PFXRL was 10(3). This let the low power conventional X-ray source be used in this confocal XRF, and, accordingly, decreased the requirement of high power X-ray source for the confocal XRF based on polycapillary X-ray optics. In this paper, we used the confocal 3D micro X-ray fluorescence spectrometer to non-destructively analyzed mineral samples and to carry out a 3D point-to-point elemental mapping scanning, which demonstrated the capabilities of confocal 3D micro XRF technology for non-destructive analysis elements composition and distribution for mineral samples. For one mineral sample, the experimental results showed that the area with high density of element of iron had high density of copper. To some extent, this reflected the growth mechanisms of the mineral sample. The confocal 3D micro XRF technology has potential applications in such fields like the analysis identification of ore, jade, lithoid utensils, "gamble stone" and lithoid flooring.     

一种快速测量共聚焦X射线分析装置探测微元尺寸方法

共聚焦X射线荧光技术是一种无损的三维光谱分析技术,在材料,生物,矿物样品分析,考古,证物溯源等领域具有广泛应用。共聚焦X射线荧光谱仪的核心部件为两个多毛细管X光透镜。一个为多毛细管X光会聚透镜（PFXRL）,其存在一后焦点,作用是把X光管所发出的发散X射线会聚成几十微米大小的高增益焦斑。另一透镜为多毛细管X光平行束透镜（PPXRL）,其存在一几十微米大小前焦点,置于X射线能量探测器前端,其作用是接收特定区域的X射线荧光信号。在共聚焦Ｘ射线荧光谱仪中,PFXRL的后焦点与PPXRL的前焦点重合,所形成的区域称作探测微元。只有置于探测微元区域的样品能够被谱仪检测到,使样品与探测微元相对移动,逐点扫描,便能够对样品进行三维无损的X射线分析。探测微元的尺寸决定共聚焦X射线荧光谱仪的空间分辨率,因此精确测量谱仪的探测微元的尺寸是非常重要的。如图1所示,谱仪探测微元可以近似为椭球体,其尺寸可以用水平方向分辨率X, Y,和深度分辨率Z表示。目前,常采用金属细丝或金属薄膜通过刀口扫描的方法测量谱仪探测微元尺寸。为了精确的从三个维度测量探测微元尺寸,金属细丝直径要小于探测微元尺寸。金属细丝和探测微元都是数十微米级别的尺寸大小,很难把金属靠近探测微元。为了得到探测微元在不同X射线能量下尺寸变化曲线,要采用多种金属细丝测量。采用单个金属细丝依次测量比较耗费时间。采用金属薄膜可以很方便地测量探测微元的深度分辨率Z,但是当测量水平分辨率X, Y时,难以准确测量。为了解决以上谱仪探测微元测量中存在的问题,本文提出采用多种金属丝平行粘贴在硬纸片上作为样品用于快速测量探测微元尺寸。附有金属细丝的硬纸片靠近谱仪探测微元,可以将探测微元置于硬纸片所在平面。由于硬纸片与金属细丝在同一水平面,在谱仪摄像头的协助下,可以把金属细丝迅速的靠近探测微元。靠近探测微元后,在全自动三维样品台的协助下,金属细丝沿两个方向对探测微元分别进行一次二维扫描。通过对二维扫描数据的处理便可以获得探测微元尺寸随入射X射线能量变化曲线。采用此方法对实验室所搭建的共聚焦X射线荧光谱仪的探测微元进行了测量。     

Analysis of extended focal area of polycapillary lenses

The X-ray passage through a polycapillary lens and the formation of X-ray energy area in the focal area of the lens (i.e., in the space behind the output cross section of the lens) are studied.     

Measurement of X-ray and neutron sources with polycapillary optics

A new method to measure the anode of X-ray sources is suggested. Using this method, one can not only measure the size of an anode spot but also obtain a 3D intensity distribution in the anode. The anode spot measurement accuracy depends on the size of the focal spot of an X-ray polycapillary lens.     

一种毛细管聚焦的便携式微束X射线荧光谱仪

基于毛细管X光透镜技术的便携式能量色散X射线荧光分析因其无损分析等优点成为分析文物样品的有利工具。但由于文物样品的表面不平整或弧度以及毛细管X光透镜聚焦X射线的特点，导致在测量过程中样品测量点与毛细管X光透镜出端之间的距离产生变化，引起照射样品的X射线束斑大小发生改变，从而影响测量结果的准确性和元素区域扫描的分辨率。介绍了本实验室自行研发的一种新型便携式微束X射线荧光谱仪，此谱仪主要是由SDD X射线探测器、30 W低功率X射线管、毛细管X光透镜、CCD和一个新型闭环控制系统构成。该闭环控制系统是在激光位移传感器能够精确控制样品测量点到毛细管X光透镜出端距离的基础上，结合LabVIEW语言环境下开发的计算机控制程序以及步进电机、样品台等器件组成。基于此系统，该实验室研发的便携式微束X射线荧光谱仪在测量过程中可以时刻保证照射样品的X射线光斑大小固定不变。同时，该谱仪还可以通过调整样品测量点到透镜出端的距离来选择不同尺寸的X射线照射光斑。为了验证设备的可行性，使用该便携式微束X射线荧光谱仪在激活激光位移传感器和关闭激光位移传感器两种情况下测量了一块表面不平整古陶瓷样品釉彩层中K，Ca，Zn和Fe等元素的含量及分布，并将测量结果进行了对比。结果显示，在激活激光位移传感器的情况下测得的样品微区元素含量与真实值较接近，扫描区域元素分布图的分辨率更好，表明本谱仪基于激光位移传感器开发的自动调整样品测量点到透镜出口端距离的闭环控制系统能有效的减少由于样品表面不平整或弧度带来的测量误差，弥补了现有微束X射线荧光谱仪在此方面的不足。因此，本便携式微束X射线荧光谱仪在无损分析检测文物方面具有潜在的应用前景。     

整体X光透镜性能实验研究

利用高计数率探测器和低功率光源,在大的能量范围内,同时测量了整体X光透镜的传输效率和焦斑直径与能量的关系。实验结果表明：透镜的焦斑直径随着能量的升高而减小;对04-5-10-5透镜而言,在高于5．8keV的能量范围内,透镜的传输效率随着能量的升高而降低,在低于5．8keV的能量范围内,透镜的传输效率随着能量的升高而增加。通过测量不同能量的X射线在透镜会聚光束中的空间分布,研究了短出口焦距透镜的光晕现象,光晕会导致透镜焦斑直径增大和传输效率测量值的增加。利用轴向扫描法研究了整体X光透镜出口焦距和能量的关系,实验结果表明：会聚透镜的出口焦距随着X射线能量的升高而增加。     

X-ray focusing using an x-ray lens composed of multi-square polycapillary slices

A new type of x-ray lens composed of multi-square polycapillary slices(ASPXRL)used in focusing parallel x-ray beam was presented in this paper.Compared with conventional x-ray polycapillary lens,ASPXRL can provide smaller and brighter focus.The effects of the manufacturing imperfections on focusing quality of ASPXRL were evaluated with the values of transmission efficiency and discussed.It is suggested that ASPXRL has application prospects as a condenser lens for x-ray microscopy and flux collectors for x-ray analytical instruments.     

Anomalous scattering,transport, and spatial distribution of X-ray fluorescence at the exit of polycapillary structures

The angular distribution of the X-ray intensity at the exit of microchannel plates at grazing incidence of monochromatic radiation on the walls of microcapillaries has been investigated. The angles and energies of the primary radiation quanta at which the synchrotron beam excites X-ray fluorescence propagating inside polycapillary structures have been determined. The angular dependences of the intensity distribution of X-rays transmitted through the microcapillaries have been studied theoretically and experimentally for energies corresponding to the region of anomalous dispersion near the L _2,3 absorption edges of silicon. The propagation of waves in hollow polycapillary waveguides, the excitation of X-ray fluorescence, and the X-ray diffraction at the exit of microchannel plates have been modeled mathematically. The mathematical model takes into account the presence of a transition layer on the microchannel surface.     

原位微区X射线荧光分析在矿物学研究中的应用

从新疆采集了13件岩矿石样品,用于研究蚀变过程中矿物的元素含量变化特征。成都理工大学研制的IED-6000型原位微区X射线荧光分析仪被应用于获得蚀变过程中矿物的化学和物理数据。这种无损的微区X射线荧光分析仪主要是以低功耗X光管和电致冷Si-PIN半导体探测器为基础,采用毛细管X射线透镜实现微区测量的功能,并且能够集成到任何显微镜上进行测量,焦斑长轴直径约110 μm。通过微区X射线荧光测量,将黝铜矿更正为黄铁矿,提高了矿物鉴定的效率及准确性;在蚀变剖面研究中,矿化岩石样品的长石颗粒都富含Cu和Zn元素,可以作为找矿直接指示元素。Cr,Mn和Co等元素含量与矿化程度呈负相关。     

Polycapillary X-ray lens for the secondary focusing Beijing synchrotron radiation source

According to intensity distribution of the synchrotron radiation source focused by a toroidal mirror at the Beijing synchrotron radiation biological macromolecule station, theoretical modeling of the Beijing synchrotron radiation source is developed for capillary optics. Using this theoretical modeling, the influences of the configuration curve of the polycapillary X-ray lens on transmission efficiency and working distance are analyzed. The experimental results of the transmission efficiency and working distance at the biological macromolecule station are in good agreement with the theoretical results.     

Confocal depth‐resolved fluorescence micro‐X‐ray absorption spectroscopy for the study of cultural heritage materials: a new mobile endstation at the Beijing Synchrotron Radiation Facility

A confocal fluorescence endstation for depth‐resolved micro‐X‐ray absorption spectroscopy is described. A polycapillary half‐lens defines the incident beam path and a second polycapillary half‐lens at 90° defines the probe sample volume. An automatic alignment program based on an evolutionary algorithm is employed to make the alignment procedure efficient. This depth‐resolved system was examined on a general X‐ray absorption spectroscopy (XAS) beamline at the Beijing Synchrotron Radiation Facility. Sacrificial red glaze (AD 1368–1644) china was studied to show the capability of the instrument. As a mobile endstation to be applied on multiple beamlines, the confocal system can improve the function and flexibility of general XAS beamlines, and extend their capabilities to a wider user community.     

Characterization of homemade x‐ray polycapillaries

The possibilities of performing non‐destructive elemental microanalysis with synchrotron radiation by means of homemade polycapillary optics are described. Using fiber glass technology, monolithic polycapillary half‐lenses were made by drawing packages of glass capillaries at high temperature in a heating furnace. The performance of polycapillary half‐lenses with different geometries was evaluated. A gold knife‐edge scanned at the output of the lenses was used to determine the spot size at different distances. Measurements of photon flux impinging on the entrance end of the lenses and photon flux leaving the lenses were used to obtain the transmission efficiency. The polycapillary half‐lens made in our laboratory was used in a series of XRF microanalysis tests using white beam. The overall efficiency of the system was studied by means of establishing detection limits for various elements in an organic sample. Copyright © 2008 John Wiley & Sons, Ltd.     

Simulation of x-ray transmission through an ellipsoidal capillary

This paper develops a simulation program for x-ray transmission in an ellipsoidal capillary based on a ray-tracing method.The influence of the parameters of ellipsoidal capillary and x-ray energy on transmission efficiency,full width at half maximum and power density gain of x-ray beams through an ellipsoidal capillary was analysed by this program.It shows that the particular rules of the ellipsoidal capillary x-ray lens are different from the polycapillary lens.Furthermore,this analysis method can be applied to the optimized design of ellipsoidal capillary.