面向先进光源线站等大科学装置的低温X射线能谱仪原理及应用进展

张硕; 崔伟; 金海; 陈六彪; 王俊杰; 伍文涛; 吴秉骏; 夏经铠; 宋艳汝; 杨瑾屏; 翁祖谦; 刘志

doi:10.7498/aps.70.20210350

摘要

低温X射线能谱仪兼具高能量分辨率、高探测效率、低噪声、无死层等特点, 能量分辨率与X射线入射方向无关, 在暗弱的弥散X射线能谱测量方面具有明显优势. 基于同步辐射及自由电子激光的先进光源线站、加速器、高电荷态离子阱、空间X射线卫星这类大科学装置的快速发展对X射线探测器提出了更高要求, 因而低温X射线能谱仪被逐步引入到APS, NSLS, LCLS-II, Spring-8, SSNL, ATHENA, HUBS等大科学装置与能谱测量相关科学研究中. 本文从低温X射线能谱仪的工作原理及分类、能谱仪系统结构、主要性能指标以及国内外大科学装置研究现状及发展趋势等方面作简要综述.

关键词:

Abstract

Cryogenic X-ray spectrometers are advantageous in the spectrum research for weak and diffusive X-ray source due to their high energy resolution, high detection efficiency, low noise level and non-dead-layer properties. Their energy resolution independent of the incident X-ray direction also makes them competitive in diffusion source detection. The requirements for X-ray spectrometers have heightened in recent years with the rapid development of large scientific facilities where X-ray detection is demanded, including beamline endstations in synchrotron and X-ray free electron laser facilities, accelerators, highly charged ion traps, X-ray space satellites, etc. Because of their excellent performances, cryogenic X-ray detectors are introduced into these facilities, typical examples of which are APS, NSLS, LCLS-II, Spring-8, SSNL, ATHENA, HUBS. In this paper, we review the cryogenic X-ray spectrometers, from the working principle and classification, system structure, major performance characteristics to the research status and trend in large scientific facilities in the world.

Keywords:

作者及机构信息

1.
上海科技大学, 大科学中心, 上海　201210

2.
清华大学天文系, 北京　201203

3.
中国科学院理化技术研究所, 北京　100190

4.
中国科学院上海微系统与信息技术研究所, 上海　200050

通信作者: 刘志, liuzhi@shanghaitech.edu.cn

作者简介:

刘志, 教授, 上海科技大学大科学中心主任兼物质学院副院长. 1994年毕业于北京大学, 获得大气物理与大气环境专业理学学士, 在美国斯坦福大学获电子工程硕士、物理学博士. 回国前长期在斯坦福线性加速器国家实验室和美国劳伦斯伯克利国家实验室从事科学研究. 20多年来主要从事同步辐射原位谱学及其他相关技术的应用研究, 特别是近常压光电子能谱对催化和电化学体系表界面的原位表征测量. 受“国家特聘专家”资助, 2013年全职回国后, 主要从事同步辐射和自由电子激光原位表征研究和大科学装置建设, 主持完成了基金委国家重大科研仪器设备研制专项“基于上海同步辐射光源的能源环境新材料原位电子结构综合研究平台(SiP·ME2)研制”和国家重大科技基础设施“活细胞结构与功能成像等线站工程”. 目前参与领导十三五国家重大科技基础设施“上海硬X射线自由电子激光装置”的建设. 发表同行评议论文220余篇

基金项目: 国家自然科学基金国家重大科研仪器设备研制专项(批准号: 11927805)、国家自然科学基金青年科学基金(批准号: 12005134, 11803014)和上海市浦江人才计划(批准号: 20PJ1410900)资助的课题.

Authors and contacts

1.
Center for Transformative Science, Shanghai Tech University, Shanghai 201210, China

2.
Department of Astronomy, Tsinghua University, Beijing 201203, China

3.
Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190, China

4.
Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, Shanghai 200050, China

Corresponding author: Liu Zhi, liuzhi@shanghaitech.edu.cn

Funds: Project supported by the Special Fund for Research on National Major Research Instrument and Facilities of the National Natural Science Fundation of China (Grant No. 11927805), the Young Scientists Fund of the National Natural Science Foundation of China (Grant Nos. 12005134, 11803014), and the Shanghai Pujiang Program, China (Grant No. 20PJ1410900)

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施引文献

图 1 STJ由一个超导-非超导-超导的结构组成. 当X射线与超导层作用时打破库珀对准粒子. 准粒子在穿越非超导层时会形成电压信号, 通过电压信号幅度反推入射X射线的能量. 本图参考文献[38]绘制

Fig. 1. STJ detector is composed of a superconducting/non-superconducting/superconducting structure. When the X-ray photon interacts with the superconducting layer, the Cooper pairs are broken, creating quasiparticle excitations. The tunneling of these quasiparticles through the non-superconducting layer gives rise to the voltage signal. By analyzing the amplitude of the voltage signal, the energy of incident X-ray can be calculated. Referenced from Ref. [38]

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图 2 (a)微量能器的核心芯片结构, 包含吸收体、热学弱连接G1、温度计、热学弱连接G2、热沉等结构; (b)温度计是区别微量能器的标志, 它决定了偏置电路以及信号放大器类型

Fig. 2. (a) Schematic of the core structure of the microcalorimeter chip, including structures like absorber, weak thermal connection-1, thermometer, weak thermal connection-2, heat sink and so on. (b) The thermometer is the sign distinguishing different microcalorimeters, which determines the bias circuit and the type of signal amplifier.

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图 3 先进光源线站上早期常用制冷机的结构图　(a) TES-X射线探测器的光敏面结构; (b) TES-X射线探测器的外形; (c)与制冷机冷头连接的探测鼻结构. 该制冷机的主体高度约1.2 m, 支撑结构与应用场景相关, 会进一步加大体积

Fig. 3. Structure diagram of early refrigerators for advanced beamline stations: (a) Structure of photosensitive surface of TES X-ray detector; (b) outlook of the TES-X-ray detector; (c) structure of the detector “snout” protrusion connected to the cold head of the refrigerator. The main body of the refrigerator is about 1.2 m high, and the supporting structure is determined by the application field, which will further increase the whole volume.

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图 4 XQC探空火箭上绝热去磁制冷机的结构图, 为了适应探空火箭环境, 该制冷机在机械结构强度以及体积方面做了特别设计. 同时, 探空火箭实验测量周期短, 因此该制冷机的液氦存储体积可以设计得比较小. 本图参考文献[51]绘制

Fig. 4. Structure diagram of the adiabatic demagnetization refrigerator (ADR) on the XQC sounding rocket. In order to adapt to the environment of the sounding rocket, the refrigerator is specially designed in terms of mechanical structure strength and volume. At the same time, the measurement period of the sounding rocket experiment is short, thus the storage volume of liquid helium of the refrigerator can be designed to be relatively small. Referenced from Ref. [51].

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图 5 应用于SEM上低温X射线能谱仪所用稀释制冷机的结构图, 该制冷机为了减小对SEM系统的振动干扰, 做了很多隔振结构, 整体高度约2 m. 本图参考自文献[52]

Fig. 5. Structure diagram of the dilution refrigerator (DR) used in the cryogenic X-ray spectrometer for SEM application. In order to reduce the vibration interference to the SEM system, the refrigerator has made many vibration-isolation structures with an overall height of about 2 m. Referenced from Ref. [52].

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图 6 STJ的结构图, 最外层的Ta用于X射线的吸收, 中间的Al-AlO_x-Al作为约瑟夫森结产生电压信号, 本图参考自文献[54]

Fig. 6. Structure diagram of the STJ detector, the outermost Ta layer is used for X-ray absorption, and the middle Al-AlO_x -Al structure is used as a Josephson Junction to generate voltage signals. Referenced from Ref. [54].

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图 7 三种微量能器的结构图, 他们的区别主要体现在温度计结构以及吸收体材质和厚度上

Fig. 7. Structure diagrams of three different kinds of microcalorimeter. They are mainly differed in the structure of the thermometer, and the material and thickness of the absorber.

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图 8 非复用SQUID的结构图, 右侧的单级SQUID将电流信号放大为电压信号, 左下侧的SQUID阵列将信号作进一步放大以降低在后端信号传输时杂散信号的干扰. 本图参考自文献[68]

Fig. 8. Structure diagram of the none-multiplexed SQUID. The single-stage SQUID on the right amplifies the current signal into a voltage signal, and the SQUID array on the lower left amplifies the signal further to reduce the interference of stray signals when the back-end signal is transmitted. Referenced from Ref. [68] .

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图 9 复用SQUID的原理图. 左上图为TDM-SQUID, 通过控制超导开关来决定读取哪一通道. 右上图为CDM-SQUID, 通过控制超导开关和后期反编码实现所有通道同时读取. 左下图为FDM-SQUID, 通过频谱移动区分和鉴别不同像素TES的信号. 右下图是RF-SQUID, 通过微波频段的频谱移动鉴别不同像素的信号

Fig. 9. Schematic diagram of multiplexed SQUID. The picture on the top left shows that TDM-SQUID, decides which channel to read by controlling the superconducting switch. The picture on the top right shows that CDM-SQUID, can read all channels at the same time by controlling the superconducting switch and post-reverse coding. The image below on the left shows that FDM-SQUID, distinguishes and discriminates the signals of different TES pixel through spectrum shift. The image below on the right shows RF-SQUID, distinguishes different pixels by the frequency spectrum shifting of the microwave band.

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图 10 一种高密度封装示意图, 主要包含高密度电缆、低温热沉、低温电路、转接插头、磁屏蔽、电磁屏蔽、红外遮光膜等结构

Fig. 10. Schematic diagram of a high-density package, which mainly includes high-density cables, low-temperature heat sink, low-temperature electronics, transfer plugs, magnetic filed shielding, electromagnetic shielding, infrared filter etc.

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图 11 一种用于半导体型微量能器的JFET放大器结构示意图. 本图参考自文献[73]

Fig. 11. Schematic diagram of the structure of a JFET amplifier for the semiconductor microcalorimeter. Referenced from Ref. [73].

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图 12 一个完整SQUID放大器结构示意图, SQUID 阵列一般置于4 K温区, 亦可根据实验需求将其放置于更低温区

Fig. 12. Complete schematic diagram of the SQUID amplifier structure. The SQUID array is generally placed in the 4 K temperature region, but also can be placed in the lower temperature region according to the experimental requirements.

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图 13 不同X射线能谱仪的能量分辨率对比图, 同时给出了不同元素K线及L线的本征展宽用于直观比较各能谱仪的性能差异. 本图摘自文献[3]

Fig. 13. Comparison diagram of energy resolution of different X-ray spectrometers. The natural line widths of K-line and L-line of different elements are given to directly compare the performance of different spectrometers. Referenced from Ref. [3].

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图 14 (a)能量分辨率、(b)探测效率及(c), (d)探测器种类对信噪比的影响, 图(c)和(d)为不同探测器在不同元素处性能比较. 本图参考自文献[2]

Fig. 14. (a) Effects of energy resolution, (b) detection efficiency and (c), (d) the type of detector on the signal-to-noise ratio. Panel (c) and (d) compare the performance of different detectors at different element positions. Referenced from Ref. [2].

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图 15 利用低温X射线能谱仪测量到的两种氮化物的XES. 本图摘自文献[3]

Fig. 15. Nitrogen X-ray emission spectrum (XES) of two kinds of nitrides measured by cryogenic X-ray spectrometer. Referenced from Ref. [3].

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图 16 利用低温X射线能谱仪测得的不同稀释浓度Fe元素样品的吸收谱

Fig. 16. XAS spectrum of Fe elements in different concentrations of samples, which were measured by cryogenic X-ray spectrometer.

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图 17 上海科技大学低温X射线能谱仪研制团队采集得到的PM2.5样品能谱

Fig. 17. Energy spectrum of PM2.5 samples collected by the Cryogenics X-ray Spectrometer Development team of Shanghai Tech University.

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图 18 利用低温X射线能谱仪与PIXE结合获得的超宽X射线谱. 本图引自文献[101]

Fig. 18. Ultra-wide X-ray spectrum obtained by the combination of cryogenic X-ray spectrometer and PIXE. Referenced from Ref. [101].

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图 19 利用MMC对不同核素进行标定的误差对比情况, 两家研发单位的MMC结构、制冷系统乃至数据分析均相互独立, 仍然得到了十分一致的标定效果. 本图摘自文献[65]

Fig. 19. Different MMC detectors from two research and development unit are used to compare the calibration errors of different nuclides. Both MMC structures, refrigeration systems and data analysis of these two research and development units are independent of each other, however still result in very consistent calibration results. Referenced from Ref. [65].

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表 1 针对软X射线波段几种X射线能谱仪的性能参数对比

Table 1. Comparison of performance parameters of several X-ray spectrometers in soft X-ray range.

Detector	Resolution $E_{\rm{FWHM}}$/eV	Count rate /cps	Efficiency (O)	P/B ratio
Ge (typical)	130	$3\times 10^5$	0.1	50∶1
Ge (best)	60	$3\times 10^4$	0.003	200∶1
STJ (typical)	20	$10^5$	$10^{-4}$	200∶1
STJ (best)	10	$10^6$	$10^{-3}$	1000∶1
Grating (typical)	0.5	$10^5$	$10^{-6}$	200∶1
Grating (best)	0.2	$10^6$	$10^{-5}$	1000∶1
Grating (best)	0.2	$10^6$	$3\times 10^{-4}$	200∶1

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表 2 安装于ATHENA卫星的低温X射线能谱仪关键参数

Table 2. Key parameters of cryogenic X-ray spectrometer installed on ATHENA satellite.

参数	设计指标	备注
能量范围/keV	0.2—12
能量分辨率	2.5 eV@7 keV
FOV/arcmin	5
像素尺寸/arcsc	< 5
单像素计数率/cps	0.25	保证80%的事例优于设计能量分辨率
非X射线背景/(cps·cm^-2)	$5^{-3}$

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