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压强是物质的基本热力学参数之一。高压可以有效改变物质内部的原子间距,调制相邻电子轨道的重叠、电子自旋以及电子与声子的相互作用,进而改变物质的电子状态、晶体结构、物理化学性质。在特定的高压条件下,半导体、绝缘体乃至分子固体材料均可以转化为金属态[1-6]。高压下的物质科学研究揭示了许多普通环境中无法观测到的新现象,是深入认识物质结构、性质及其变化规律的有效途径之一[7-10]。更进一步,高压技术结合高低温、磁场等原位条件为科学创新提供了更广阔的维度,有利于发现新现象、探索新问题、制备新材料[11-15]。
能够产生高压环境的实验技术主要有两种:动态高压实验技术(简称动高压)和静态高压实验技术(简称静高压)。动高压是利用爆炸或者高速撞击产生的冲击波使样品经受瞬时高温高压环境条件的实验技术[16],瞬时压力可以达到数千万大气压。静高压则是可以相对长时间维持较稳定的压力,目前最高压力可以达到数百万大气压。产生静高压的装置主要包括金刚石对顶砧(Diamond-anvil cell, DAC)[17-20]和大体积压机(Large-volume press, LVP)[21-26]。
DAC和LVP是高压实验研究中两种相辅相成、不可或缺的研究手段。每种技术均具有其独特的功能和应用范围。DAC能够产生几百万大气压的压力[20, 27-28],结合激光加热可以实现6 000~7 000 K的高温。为了获得超过百万大气压的实验压力,DAC中的试样通常只有几个到几十微米大小,压力梯度和温度梯度比较大。LVP的试样体积要大得多 (一般在毫米量级),并能够产生很高且均匀的温度 (3000 K以上),压力梯度也较小,但压力范围相对有限 (目前最高可达120 GPa)。这些特征使LVP成为用大体积试样精细研究材料 (尤其是多相系材料) 物性的理想工具,也方便同时使用多种原位探测技术[29-32]。
为了获得理想的高压条件,在实验中通常以减小样品体积为代价,而且将样品封闭在压腔内。这样能够有效保持试样与外界隔离,并保证了试样的纯度,同时要求与高压试样匹配的微探针。传统的实验室X射线光源受限于光强、能量及光斑尺寸,很难直接对高压样品进行测试。高亮度、高能量、低发射度的同步辐射X射线源为研究高压下微小样品提供了强力探针,并有效解决了在周围实验环境充满大量干扰物质的情况下探测微弱信号的问题[33-35]。同步辐射X射线与高压技术结合是原位研究物质在高温高压下物性和行为的有力手段,打开了高压研究领域的新纪元。
诸多基于同步辐射的X射线衍射实验方法中,同步辐射X射线衍射(XRD)是高压研究的重要技术,可用于测量单晶、多晶、纳米晶体和非晶材料的键长、密度、弹性及状态方程等诸多综合数据信息。与此同时,同步辐射X射线光谱学研究取得了重大进展。近年来,高压条件下的光谱分析技术逐渐成为一种重要的研究方法,光谱技术与高压技术的成功结合为探索高压力下丰富的物理和化学现象提供了强有力的工具,如:利用X射线吸收谱(XANES、XAFS)研究价态变化和原子近邻结构变化,利用成像方法研究形貌,利用非弹性散射(IXS) 研究电子结构、带隙变化等。
此外,以同步辐射为基础的XRD及光谱学技术连同激光加热和低温技术一起,为发现和拓展高压环境下的科学前沿问题提供了强有力的研究手段。最新发展的高分辨成像技术和快速时间分辨技术在高压X射线研究中发挥了越来越重要的作用。从原理上来讲,只要探针比样品尺寸小,同时探测效率比需要的时间分辨率高的情况下,任何X射线技术都可以被用来成像和进行时间分辨探测。因此,高压实验条件下探针大小和探测效率是设计中的关键。
目前,世界上主要的同步辐射光源均有进行高压研究的专用同步辐射光束线站,如:欧洲同步辐射光源(ESRF)的ID09A、ID27线站[36],英国钻石光源(Diamond)的I15线站,美国先进电子源(APS)的3ID、13BM、16ID线站[37-38],美国NSLSⅡ光源的X17C线站[39],日本SPring-8光源的BL04B1、BL10XU线站等[40]。我国同步辐射光源的高压研究应用始于20世纪90年代初期,北京同步辐射装置(BSRF)的4W2线站为国内首批高压用户提供支持,即使到了今天也依然满负荷运转,为我国高压研究领域作出了重要贡献[41]。2009年,作为世界先进的第三代同步辐射光源代表之一的上海同步辐射装置—上海光源(SSRF)建成开放,其中的硬X射线微聚焦及应用光束线站BL15U1由于光斑小、通量高,非常适合用于高压微束衍射实验。BL15U1线站于2010年开始服务于高压科学研究,目前超过一半的机时用于高压研究。近年来,国内外高压科学研究人员综合利用该线站以及世界上其他先进光源取得了一系列重要研究成果[42-45]。
BSRF的BL15U1线站拥有高通量、能量可调的单色硬X射线微束,空间分辨达到微米至亚微米量级,非常适合开展DAC高压研究。在建的SSRF二期线站工程中的超硬多功能线站(BL12SW) 配备了200 t和2 000 t的大压机,能量范围覆盖30~150 keV,是开展LVP实验的理想平台。本文将分别介绍SSRF适于开展高压研究的硬X射线微聚焦及应用光束线站BL15U1以及即将建成的超硬多功能线站BL12SW。
上海同步辐射光源高压相关线站概述
Application of Shanghai Synchrotron Radiation Source in High Pressure Research
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摘要: 同步辐射X射线与基于金刚石对顶砧(DAC)和大体积压机(LVP)的静高压技术的结合推动了高压科学的发展。上海同步辐射光源(SSRF)是性能指标达到世界一流的中能第三代同步辐射光源,其中的硬X射线微聚焦及应用光束线站(BL15U1)具备高通量、能量可调的单色微束X射线,空间分辨达到微米至亚微米量级,在开展DAC高压研究方面有相当大的优势。自2010年对从事高压科学研究的用户开放以来,国内外高压科学研究者综合利用BL15U1线站高压实验方法取得了一系列有影响力的成果。此外,在建的上海光源二期线站工程中的超硬多功能线站(BL12SW)中配备200 t和2 000 t大压机,将成为开展LVP原位高压实验的有力平台。为促进用户对SSRF高压研究相关线站的了解,更好地利用相关平台开展研究工作,并为后续线站建设和实验方法发展提出宝贵建议,本文对BL15U1和BL12SW线站的布局、性能指标、实验站主要设施以及相关实验方法等进行了较为完整的介绍。Abstract: The combination of synchrotron X-ray radiation and static high pressure technology based on diamond anvil cell (DAC) and large volume press (LVP) has fundamentally promoted the development of high pressure science. Shanghai Synchrotron Radiation Facility (SSRF) is one of the advanced third generation light sources in the world, the hard X-ray micro-focusing beamline (BL15U1) of SSRF provides a monochromatic micro X-ray beam with high flux and adjustable energy, whose spatial resolution reaches the order of micrometer to submicron, and it has considerable advantages in DAC high-pressure experiments. Since it provided beamline time to high-pressure researchers in 2010, a series of influential achievements have been produced by using the related high pressure experimental methods at BL15U1. Moreover, the ultra-hard X-ray multi-functional beamline (BL12SW) in SSRF phase II is equipped with 200 t and 2000 t of LVP, which is a powerful platform for LVP experiments. In order to promote high pressure researchers to have a full understanding of the high pressure beamline at SSRF and make better use of relevant platforms to carry out research work, as well as to put forward valuable suggestions for the follow-up beamline construction and the development of experimental methods. In this paper, the layout, beamline specifications, main facilities and related experimental methods of BL15U1 and BL12SW beamlines are introduced in detail.
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Key words:
- Shanghai synchrotron radiation /
- high pressure /
- beamlines /
- diamond anvil cell /
- large volume press /
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表 1 HXMF线站的主要指标
Table 1. Main parameters of HXMF beamline
Light source type Energy/
keVEnergy resolution
($ {\text{Δ}}E/E$ )Photon flux/[phs·s−1· $ {\text{μ}}{\rm{m}}$ −2·
(0.1%B.W.)−1]Beam size at sample/
(μm × μm)Divergence at sample/
(mrad × mrad)Undulator 5−20 < 2 × 10−4
Si (111)> 1012 < 2 × 2
(K-B mirrors)< 2 (H) × 1.5 (V)
(K-B mirrors)表 2 超硬多功能线站的技术指标
Table 2. Technical specification of super-hard multifunction station
Energy/keV Energy resolution ( $ {\text{Δ}}E/E$ )Photon flux/(phs·s−1@100 keV@25 μrad) Spot size at sample/(mm×mm) 30−150 < 9 × 10−3 2 × 1011 0.5 × 0.5(Focused mode);
Max:100 (H) × 30 (V)
(Non-focusing mode) -
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