蛋白质设施BL17B线站高次谐波抑制镜系统研制

卢兰露; 蒋罗震; 刘洋; 鲍康文; 李春宇; 吴婷婷; 朱中杰; 顾亦君; 唐健超; 肖清洁; 张禹浦; 张蔚哲; 周舒钰; 杨亚运; 姜政; 秦文明

doi:10.3724/j.0253-3219.2025.hjs.48.240498

您当前的位置：

首页 >

文章列表页 >

蛋白质设施BL17B线站高次谐波抑制镜系统研制

同步辐射技术及应用 | 更新时间：2025-11-27

- 蛋白质设施BL17B线站高次谐波抑制镜系统研制
- Development of a harmonic rejection mirror system at the NFPSS-BL17B beamline
- 核技术 2025年48卷第11期文章编号：110104
- 作者机构：
  
  1.中国科学院上海应用物理研究所上海 201800
  2.中国科学院上海高等研究院国家蛋白质科学研究上海设施上海 201210
  3.中国科学技术大学国家同步辐射实验室合肥 230029
  4.中国科学院大学北京 100049
  5.上海擎朗智能科技有限公司上海 201206
- 作者简介：
  
  卢兰露，女，1991年出生，2013年于中国科学院上海应用物理研究所获工程硕士学位，研究领域为X射线吸收谱学及其应用
  姜政，E-mail：jiangz@ustc.edu.cn
  秦文明，E-mail：qinwenming@sari.ac.cn
- 基金信息：
  
  中国科学院关键技术人才项目(2021000022)
- DOI：10.3724/j.0253-3219.2025.hjs.48.240498
  中图分类号： TL99
- 收稿：2024-12-05，
  
  修回：2025-03-10，
  
  纸质出版：2025-11-15
- 稿件说明：
移动端阅览
卢兰露,蒋罗震,刘洋等.蛋白质设施BL17B线站高次谐波抑制镜系统研制[J].核技术,2025,48(11):110104.

LU Lanlu,JIANG Luozhen,LIU Yang,et al.Development of a harmonic rejection mirror system at the NFPSS-BL17B beamline[J].NUCLEAR TECHNIQUES,2025,48(11):110104.
卢兰露,蒋罗震,刘洋等.蛋白质设施BL17B线站高次谐波抑制镜系统研制[J].核技术,2025,48(11):110104. DOI： 10.3724/j.0253-3219.2025.hjs.48.240498. CSTR： 32193.14.hjs.CN31-1342/TL.2025.48.240498.

LU Lanlu,JIANG Luozhen,LIU Yang,et al.Development of a harmonic rejection mirror system at the NFPSS-BL17B beamline[J].NUCLEAR TECHNIQUES,2025,48(11):110104. DOI： 10.3724/j.0253-3219.2025.hjs.48.240498. CSTR： 32193.14.hjs.CN31-1342/TL.2025.48.240498.

摘要

在低能区X射线吸收精细结构（X-ray Absorption Fine Structure，XAFS）实验中，高次谐波污染会导致数据振幅衰减和谱形失真，从而影响结构解析的可靠性。上海同步辐射光源（Shanghai Synchrotron Radiation Facility，SSRF）蛋白质设施（National Facility for Protein Science in Shanghai，NFPSS）BL17B线站在低能区XAFS实验中亦面临该问题。为此，本文基于BL17B的光学特性，研制了一种高次谐波抑制镜（Harmonic Rejection Mirror，HRM）系统，以提升实验数据的质量和可靠性。首先，采用XOP软件对BL17B的光学系统进行模拟，验证了HRM双平面反射镜结构设计的可行性，确定了Ni/Rh双镀层、固定5.8 mrad掠入射角以及镀层尺寸等关键参数。其次，通过精密机械结构设计，使HRM具备掠入射角调节、光路对准及镀层切换多维调节能力，以适应不同实验需求。在安装与调试阶段，采用全反射临界能量法解决掠入射角精准控制的难题，确保HRM达到设计要求。最后，结合单色器摇摆曲线测试和XAFS实验，对HRM的谐波抑制能力进行评估。实验结果表明，该HRM可将5~10 keV能区内的有效高次谐波含量抑制在10

-4

以下，同时保持基波通过率高于70%。全反射临界能量法实现了掠入射角0.01 mrad的校准精度，确保了HRM按设计运行。在5 keV条件下，HRM有效提高了光束的单色性，并显著改善了Ti箔的XAFS光谱质量，消除了谱形失真。该HRM的应用成功将BL17B XAFS实验的能量下限从10 keV拓展至5 keV，显著提升了低能区XAFS实验能力，并为同步辐射光源的高次谐波抑制提供了技术参考。

Abstract

Background

Harmonic contamination is a major issue in low-energy X-ray absorption fine structure (XAFS) experiments

leading to amplitude attenuation and spectral distortion

which compromise the reliability of structural analysis. The BL17B beamline

part of the National Facility for Protein Science in Shanghai (NFPSS) and operated within the Shanghai Synchrotron Radiation Facility (SSRF)

also faces this challenge in its low-energy XAFS experiments.

Purpose

This study aims to develop a Harmonic Rejection Mirror (HRM) system tailored to the optical characteristics of the BL17B beamline at SSRF to improve the quality and reliability of XAFS data.

Methods

Firstly

the simulation software XOP was applied to modelling the optical system of BL17B

confirming the feasibility of the HRM system based on a dual-plane mirror design. Key parameters

including the use of Ni and Rh coatings

a fixed grazing incidence angle of 5.8 mrad

and coating dimensions

were optimized accordingly. Then

a precise mechanical structure was designed

enabling multi-dimensional adjustments

including grazing incidence angle tuning

optical alignment

and coating switching to accommodate different experimental requirements. During installation and commissioning

the total reflection critical energy measurement method was employed to address the challenge of accurate grazing incidence angle control

ensuring the system met design specifications. Finally

the performance of HRM was evaluated by monochromator rocking curve measurements and XAFS experiments.

Results

Experimental results show that the HRM effectively suppresses effective harmonic contamination to below 10

-4

in 5~10 keV while maintaining a fundamental beam transmission above 70%. The total reflection critical energy measurement method achieves a grazing incidence angle calibration precision of 0.01 mrad

ensuring that the HRM operates as designed. At 5 keV

the HRM signi

ficantly enhances beam monochromaticity and improves Ti foil XAFS data quality by eliminating spectral distortions.

Conclusions

The implementation of the HRM in this study successfully extends the lower energy limit of XAFS experiments at BL17B from 10 keV to 5 keV

significantly enhancing the capability of low-energy XAFS experiments

providing a valuable technical reference for harmonic suppression in synchrotron radiation sources.

关键词

Keywords

references

杨予琪 , 张光颖 , 孙凡飞 , 等 . 钒调制钴-氮-碳催化剂氧还原反应性能 [J ] . 核技术 , 2021 , 44 ( 8 ): 080102 . DOI: 10.11889/j.0253-3219.2021.hjs.44.080102 http://dx.doi.org/10.11889/j.0253-3219.2021.hjs.44.080102 .

YANG Yuqi , ZHANG Guangying , SUN Fanfei , et al . Regulation of oxygen reduction reaction performance cobalt-based nitrogen-doped carbon catalysts by vanadium [J ] . Nuclear Techniques , 2021 , 44 ( 8 ): 080102 . DOI: 10.11889/j.0253-3219.2021.hjs.44.080102 http://dx.doi.org/10.11889/j.0253-3219.2021.hjs.44.080102 .

汪丽华 , 段辉平 , 朱剑 , 等 . 红绿彩瓷之釉上彩的XAFS研究 [J ] . 核技术 , 2010 , 33 ( 4 ): 246 ‒ 252 .

WANG Lihua , DUAN Huiping , ZHU Jian , et al . XAFS analysis of ancient Chinese porcelain of Honglvcai [J ] . Nuclear Techniques , 2010 , 33 ( 4 ): 246 ‒ 252 .

Liu S , Wang Y , Zhao Y , et al . A nanozyme-based electrode for high-performance neural recording [J ] . Advanced Materials , 2024 , 36 ( 6 ): 2304297 . DOI: 10. 1002/adma.202304297 http://dx.doi.org/10.1002/adma.202304297 .

Koningsberger D C , Prins R . X-ray absorption: principles, applications, techniques of EXAFS, SEXAFS, and XANES [M ] . New York : Wiley , 1988 : 170 ‒ 175 . 10.1016/0160-9327(88)90177-9 http://dx.doi.org/10.1016/0160-9327(88)90177-9

Bunker G . Introduction to XAFS: A practical guide to X-ray absorption fine structure spectroscopy [M ] . Cambridge : Cambridge University Press , 2010 : 80 ‒ 85 . 10.1017/cbo9780511809194 http://dx.doi.org/10.1017/cbo9780511809194

Calvin S . XAFS for everyone [M ] . Boca Raton : CRC Press , 2013 : 48 ‒ 61 . 10.1201/b14843 http://dx.doi.org/10.1201/b14843

Giacovazzo C , Monaco H L , Artioli G , et al . Fundamentals of crystallography [M ] . Oxford : Oxford University Press , 2011 . 10.1093/acprof:oso/9780199573653.001.0001 http://dx.doi.org/10.1093/acprof:oso/9780199573653.001.0001

Pecharsky V K , Zavalij P Y . The powder diffraction pattern [M ] . Boston : Springer , 2009 .

陶鑫 , 赵贵 , 李玉楠 , 等 . 钯铋催化剂在乙炔加氢中的构效关系研究 [J ] . 核技术 , 2023 , 46 ( 5 ): 050101 . DOI: 10.11889/j.0253-3219.2023.hjs.46.050101 http://dx.doi.org/10.11889/j.0253-3219.2023.hjs.46.050101 .

TAO Xin , ZHAO Gui , LI Yunan , et al . Investigation of the structure activity relationship of palladium-bismuth catalyst in acetylene hydrogenation [J ] . Nuclear Techniques , 2023 , 46 ( 5 ): 050101 . DOI: 10.11889/j.0253-3219.2023.hjs.46.050101 http://dx.doi.org/10.11889/j.0253-3219.2023.hjs.46.050101 .

贺文雪 , 李红梅 , 陈炜 , 等 . 同步辐射研究高温氧化对金属-载体相互作用的影响 [J ] . 核技术 , 2022 , 45 ( 8 ): 080101 . DOI: 10.11889/j.0253-3219.2022.hjs.45.080101 http://dx.doi.org/10.11889/j.0253-3219.2022.hjs.45.080101 .

HE Wenxue , LI Hongmei , CHEN Wei , et al . Synchrotron radiation study of effects of high temperature oxidation on metal-support interactions in catalysts [J ] . Nuclear Techniques , 2022 , 45 ( 8 ): 080101 . DOI: 10.11889/j.0253-3219.2022.hjs.45.080101 http://dx.doi.org/10.11889/j.0253-3219.2022.hjs.45.080101 .

文青草 , 许子健 , 陈爱英 , 等 . 原位同步辐射技术在超级电容器中的应用进展 [J ] . 核技术 , 2025 , 48 ( 2 ): 020001 . DOI: 10.11889/j.0253-3219.2025.hjs.48.230032. CSTR: 32193.14.hjs.CN31-1342/TL.2025.48.230032 http://dx.doi.org/10.11889/j.0253-3219.2025.hjs.48.230032.CSTR:32193.14.hjs.CN31-1342/TL.2025.48.230032 .

WEN Qingcao , XU Zijian , CHEN Aiying , et al . Advances in applications of in situ synchrotron-based X-ray techniques in supercapacitor research [J ] . Nuclear Techniques , 2025 , 48 ( 2 ): 020001 . DOI: 10.11889/j.0253-3219.2025.hjs.48.230032. CSTR: 32193.14.hjs.CN31-1342/TL.2025.48.230032 http://dx.doi.org/10.11889/j.0253-3219.2025.hjs.48.230032.CSTR:32193.14.hjs.CN31-1342/TL.2025.48.230032 .

袁静 , 罗立强 . 同步辐射微区X射线荧光和吸收谱技术在大气、土壤和动植物分析中的应用 [J ] . 核技术 , 2014 , 37 ( 8 ): 080101 . DOI: 10.11889/j.0253-3219.2014.hjs.37.080101 http://dx.doi.org/10.11889/j.0253-3219.2014.hjs.37.080101 .

YUAN Jing , LUO Liqiang . Synchrotron μ-XRF and XAFS in element distribution and speciation of air, soil and biological samples [J ] . Nuclear Techniques , 2014 , 37 ( 8 ): 080101 . DOI: 10.11889/j.0253-3219.2014.hjs.37.080101 http://dx.doi.org/10.11889/j.0253-3219.2014.hjs.37.080101 .

Jiang M , Yang X , Xu H , et al . Shanghai synchrotron radiation facility [J ] . Chinese Science Bulletin . 2009 , 54 ( 22 ): 4171 ‒ 4181 . DOI: 10.1007/s11434-009-0689-y http://dx.doi.org/10.1007/s11434-009-0689-y .

Zhu Z , Lu L , Li C , et al . GIWAXS experimental methods at the NFPS-BL17B beamline at Shanghai Synchrotron Radiation Facility [J ] . Journal of Synchrotron Radiation , 2024 , 31 ( 4 ): 968 ‒ 978 . DOI: 10.1107/S1600577524004764 http://dx.doi.org/10.1107/S1600577524004764 .

梅丙宝 . 同步辐射高分辨XES和XAFS方法及其在电催化中的应用研究 [D ] . 上海 : 中国科学院大学（中国科学院上海应用物理研究所） , 2021 . DOI: 10.27585/d.cnki.gkshs.2021.000030 http://dx.doi.org/10.27585/d.cnki.gkshs.2021.000030 .

MEI Bingbao . Synchrotron radiation high-energy-resolution XES and XAFS methods and their application in the research of electrocatalysis [D ] . Shanghai : University of Chinese Academy of Sciences (Shanghai Institute of Applied Physics, Chinese Academy of Sciences) , 2021 . DOI: 10.27585/d.cnki.gkshs.2021.000030 http://dx.doi.org/10.27585/d.cnki.gkshs.2021.000030 .

刘泓舟 , 李季 , 顾颂琦 , 等 . 上海光源BL14W1线站透射XAFS数据采集系统升级 [J ] . 核技术 , 2022 , 45 ( 7 ): 070103 . DOI: 10.11889/j.0253-3219.2022.hjs.45.070103 http://dx.doi.org/10.11889/j.0253-3219.2022.hjs.45.070103 .

LIU Hongzhou , LI Ji , GU Songqi , et al . Upgrade of transmission XAFS data acquisition system upgrade of Shanghai Synchrotron Radiation Facility BL14W1 beamline station [J ] . Nuclear Techniques , 2022 , 45 ( 7 ): 070103 . DOI: 10.11889/j.0253-3219.2022.hjs.45.070103 http://dx.doi.org/10.11889/j.0253-3219.2022.hjs.45.070103 .

Lu L L , Qin W M , Jiang L Z , et al . XAFS platform at NFPS BL17B at SSRF: extending structural characterization from long-range to short-range orders [J ] . Nuclear Science and Techniques , 2025 , 36 : 197 . DOI: 10.1007/s41365-025-01774-5 http://dx.doi.org/10.1007/s41365-025-01774-5 .

Barnea Z , Mohyla J . Detection of the contribution of harmonics to the diffracted X-ray intensity [J ] . 1974 , 7 ( 2 ): 298 ‒ 299 . DOI: 10.1107/S0021889874009599 http://dx.doi.org/10.1107/S0021889874009599 .

Tran C Q , Barnea Z , de Jonge M D , et al . Quantitative determination of major systematics in synchrotron x-ray experiments: seeing through harmonic components [J ] . X-Ray Spectrometry , 2003 , 32 ( 1 ): 69 ‒ 74 . DOI: 10.1002/xrs.630 http://dx.doi.org/10.1002/xrs.630 .

Chantler C T , Barnea Z , Tran C Q , et al . Precision X-ray optics for fundamental interactions in atomic physics, resolving discrepancies in the X-ray regime [J ] . Optical and Quantum Electronics , 1999 , 31 ( 5/7 ): 495 ‒ 505 . DOI: 10.1023/a:1006923329884 http://dx.doi.org/10.1023/a:1006923329884 .

Aquilanti G , Giorgetti M , Dominko R , et al . Operando characterization of batteries using X-ray absorption spectroscopy: advances at the beamline XAFS at synchrotron Elettra [J ] . Journal of Physics D: Applied Physics , 2017 , 50 ( 7 ): 074001 . DOI: 10.1088/1361-6463/aa519a http://dx.doi.org/10.1088/1361-6463/aa519a .

Newville M . Fundamentals of XAFS [J ] . Reviews in Mineralogy and Geochemistry , 2014 , 78 ( 1 ): 33 ‒ 74 . DOI: 10.2138/rmg.2014.78.2 http://dx.doi.org/10.2138/rmg.2014.78.2 .

Parratt L G , Hempstead C F , Jossem E L . "Thickness effect" in absorption spectra near absorption edges [J ] . Physical Review , 1957 , 105 : 1228 ‒ 1232 . DOI: 10.1103/PhysRev.105.1228 http://dx.doi.org/10.1103/PhysRev.105.1228 .

Stern E A , Kim K . Thickness effect on the extended-x-ray-absorption-fine-structure amplitude [J ] . Physical Review B , 1981 , 23 ( 8 ): 3781 ‒ 3787 . DOI: 10.1103/PhysRevB. 23.3781 http://dx.doi.org/10.1103/PhysRevB.23.3781 .

Chantler C T , Barnea Z , Tran C Q , et al . A step toward standardization: development of accurate measurements of X-ray absorption and fluorescence [J ] . Journal of Synchrotron Radiation , 2012 , 19 ( Pt 6 ): 851 ‒ 862 . DOI: 10.1107/S0909049512039544 http://dx.doi.org/10.1107/S0909049512039544 .

Abe H . XAFS spectral distortions related to optics issues [A ] //Chantler C T, Boscherini F, Bunker B. International Tables for Crystallography . I[M ] . Chester: Wiley, 2024 : 594 ‒ 599 . 10.1107/s1574870720003225 http://dx.doi.org/10.1107/s1574870720003225

Nomura M , Koike Y , Sato M , et al . A new XAFS beamline NW10A at the photon factory [J ] . AIP Conference Proceedings , 2007 , 882 ( 1 ): 896 ‒ 898 . DOI: 10.1063/1.2644697 http://dx.doi.org/10.1063/1.2644697 .

Liu H , Zhou Y , Jiang Z , et al . QXAFS system of the BL14W1 XAFS beamline at the Shanghai Synchrotron Radiation Facility [J ] . Journal of Synchrotron Radiation , 2012 , 19 ( 6 ): 969 ‒ 975 . DOI: 10.1107/S0909049512038873 http://dx.doi.org/10.1107/S0909049512038873 .

Glover C , McKinlay J , Clift M , et al . Status of the X-Ray Absorption Spectroscopy (XAS) Beamline at the Australian Synchrotron [J ] . AIP Conference Proceedings , 2007 : 882 : 884 ‒ 886 . DOI: 10.1063/1.2644692 http://dx.doi.org/10.1063/1.2644692 .

Caliebe W A , Murzin V , Kalinko A , et al . High-flux XAFS-beamline P64 at PETRA III [J ] . AIP Conference Proceedings , 2019 , 2054 ( 1 ): 060031 . DOI: 10.1063/1. 5084662 http://dx.doi.org/10.1063/1.5084662 .

Als-Nielsen J , McMorrow D . Elements of Modern X-ray Physics [M ] . Singapore : Wiley , 2011 : 77 ‒ 80 . 10.1002/9781119998365 http://dx.doi.org/10.1002/9781119998365

Hou Z . Ray tracing study for a detuned nondispersed double crystal monochromator [J ] . Review of Scientific Instruments , 2005 , 76 ( 1 ): 013305 . DOI: 10.1063/1.1831251 http://dx.doi.org/10.1063/1.1831251 .

傅远 , 薛松 , 魏向军 , 等 . 上海光源XAFS光束线高次谐波抑制镜系统研制 [J ] . 核技术 , 2009 , 32 ( 10 ): 729 ‒ 732 .

FU Yuan , XUE Song , WEI Xiangjun , et al . The development of harmonic rejection mirror on XAFS beamline at SSRF [J ] . Nuclear Techniques , 2009 , 32 ( 10 ): 729 ‒ 732 .

郑雷 , 赵屹东 , 崔明启 , 等 . 北京同步辐射装置4B7A、4B7B光束线高次谐波抑制系统初步设计 [J ] . 核技术 , 2007 , 30 ( 9 ): 721 ‒ 724 .

ZHENG Lei , ZHAO Yidong , CUI Mingqi , et al . The primary design of higher-harmonics suppressor for Beamline 4B7A and 4B7B at Beijing Synchrotron Radiation Facility [J ] . Nuclear Techniques , 2007 , 30 ( 9 ): 721 ‒ 724 .

Polikarpov M , Snigireva I , Snigirev A . X-ray harmonics rejection on third-generation synchrotron sources using compound refractive lenses [J ] . Journal of Synchrotron Radiation , 2014 , 21 : 484 ‒ 487 . DOI: 10.1107/S1600577514001003 http://dx.doi.org/10.1107/S1600577514001003 .

Follath R , Flechsig U , Milne C , et al . Optical design of the ARAMIS-beamlines at SwissFEL [J ] . AIP Conference Proceedings , 2016 , 1741 ( 1 ): 020009 . DOI: 10.1063/1. 4952788 http://dx.doi.org/10.1063/1.4952788 .

Liu D G , Lee M H , Lu Y J , et al . Reducing the thermal deformation of InSb crystal by using double-bounce HHRMs in the TPS tender X-ray absorption spectroscopy beamline [J ] . Journal of Synchrotron Radiation , 2021 , 28 ( 4 ): 1202 ‒ 1209 . DOI: 10.1107/s1600577521003994 http://dx.doi.org/10.1107/s1600577521003994 .

Rae N A , Chantler C T , Barnea Z , et al . X-ray mass attenuation coefficients and imaginary components of the atomic form factor of zinc over the energy range of 7.2–15.2 keV [J ] . Physical Review A , 2010 , 81 ( 2 ): 022904 . DOI: 10.1103/PhysRevA.81.022904 http://dx.doi.org/10.1103/PhysRevA.81.022904 .

Barnea Z , Chantler C T , Glover J L , et al . Measuring the linearity of X-ray detectors: consequences for absolute attenuation, scattering and absolute Bragg intensities [J ] . Journal of Applied Crystallography , 2011 , 44 ( 2 ): 281 ‒ 286 . DOI: 10.1107/s0021889811004493 http://dx.doi.org/10.1107/s0021889811004493 .

Sainctavit P , Petiau J , Manceau A , et al . Two‐mirror device for harmonic rejection [J ] . Review of Scientific Instruments , 1989 , 60 ( 7 ): 2027 ‒ 2029 . DOI: 10.1063/1. 1140867 http://dx.doi.org/10.1063/1.1140867 .

Parratt L G . Surface studies of solids by total reflection of X-rays [J ] . Physical Review , 1954 , 95 ( 2 ): 359 ‒ 369 . DOI: 10.1103/PhysRev.95.359 http://dx.doi.org/10.1103/PhysRev.95.359 .

浏览量

下载量

CSCD

文章被引用时，请邮件提醒。

提交

工具集

关联资源

同步辐射TXRF用于细胞元素谱的初步研究

全反射X荧光分析技术的应用

光管穆斯堡尔实验