CN103175857B - Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device - Google Patents

Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device Download PDF

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CN103175857B
CN103175857B CN201310081613.8A CN201310081613A CN103175857B CN 103175857 B CN103175857 B CN 103175857B CN 201310081613 A CN201310081613 A CN 201310081613A CN 103175857 B CN103175857 B CN 103175857B
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CN103175857A (en
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谢亚宁
张静
张久昶
宋冬燕
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Institute of High Energy Physics of CAS
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Abstract

公开了一种专用于掠入射XAFS实验的装置及其调整方法,其中该装置包括:用于产生掠入射XAFS实验所需的X射线的装置;前狭缝,限定X射线的尺寸;第一升降台,使前狭缝在垂直方向上升降;样品架,承载样品;旋转台,使得样品架上的样品转动,以获得所需的X射线掠入射角度;第二升降台,使得旋转台在垂直方向上升降;后狭缝,限定全反射X射线的尺寸;第三升降台,使得所述后狭缝在垂直方向上升降;第一探测器,探测从样品发出的荧光信号;第二探测器,探测全反射X射线信号。采用该装置及方法,能够快速精确地设定样品初始位置,而且能够精确地调整样品角度,并以高信噪比获取样品的实验探测数据,获得高质量的掠入射XAFS实验谱。

Disclosed is a device dedicated to grazing incidence XAFS experiments and its adjustment method, wherein the device includes: a device for generating X-rays required for grazing incidence XAFS experiments; a front slit to limit the size of X-rays; a first lift The first lifting table makes the front slit vertically lift; the sample holder carries the sample; the rotating table makes the sample on the sample holder rotate to obtain the required X-ray grazing incidence angle; the second lifting table makes the rotating table vertically The rear slit limits the size of the total reflection X-ray; the third lifting platform makes the rear slit vertically ascending and descending; the first detector detects the fluorescent signal emitted from the sample; the second detector , to detect total reflection X-ray signals. By adopting the device and method, the initial position of the sample can be quickly and accurately set, and the angle of the sample can be adjusted precisely, and the experimental detection data of the sample can be obtained with a high signal-to-noise ratio, and a high-quality grazing incidence XAFS experimental spectrum can be obtained.

Description

专用于掠入射XAFS实验的装置及其调整方法Device and its adjustment method dedicated to grazing incidence XAFS experiments

技术领域technical field

本发明涉及现代物质结构分析方法-同步辐射实验方法,特别是涉及一种专用于掠入射X射线吸收精细结构(X-ray Absorption Fine Structure,XAFS)实验的装置及该装置的调整方法。The present invention relates to a modern material structure analysis method - synchrotron radiation experiment method, in particular to a device specially used for grazing incidence X-ray Absorption Fine Structure (X-ray Absorption Fine Structure, XAFS) experiment and an adjustment method of the device.

背景技术Background technique

同步辐射XAFS谱实验系统已经成为研究物质结构的一种有效手段,服务于多学科领域,例如,生命科学领域、新材料领域、环境健康领域和工业应用领域等。The synchrotron radiation XAFS spectrum experiment system has become an effective means to study the structure of matter, serving multidisciplinary fields, such as life sciences, new materials, environmental health, and industrial applications.

XAFS谱是利用双晶单色器通过光子能量扫描进行测定的。来自单色器的单能光束正入射到样品,对于不同能量的光子样品吸收变化,探测样品前后的光强随光子能量的变化即可以获得XAFS谱。对该XAFS谱进行分析即可以获得样品内的结构信息。XAFS spectra were determined by photon energy scanning using a twin crystal monochromator. The monoenergetic beam from the monochromator is incident on the sample, and the sample absorbs different photons with different energies, and the XAFS spectrum can be obtained by detecting the change of the light intensity before and after the sample with the photon energy. The structural information in the sample can be obtained by analyzing the XAFS spectrum.

随着能源、环境和新材料科学的发展及其相关科学研究的深入,人们需要知道各种功能的薄膜、器件表面、固体-固体和固体-液体界面的结构特性,然而,常规的XAFS实验系统无法获得样品表面的结构信息。于是,出现了掠入射XAFS(Grazing-incidence Absorption Fine Structure,GXAFS)谱实验系统。With the development of energy, environment and new material science and the deepening of related scientific research, people need to know the structural properties of thin films, device surfaces, solid-solid and solid-liquid interfaces with various functions. However, the conventional XAFS experimental system Structural information on the sample surface was not available. Thus, the grazing incidence XAFS (Grazing-incidence Absorption Fine Structure, GXAFS) spectrum experimental system appeared.

当X射线以极小的角度入射到物质表面时,其穿透深度急剧变小,当X射线的掠入射角小于一个材料相关的特定角度(例如临界角)时,入射的X射线被全部反射,仅与材料表层发生作用,这样出射的X射线中仅包含材料表层的结构信息。这种现象即是掠入射XAFS谱实验的物理基础。When the X-ray is incident on the material surface at a very small angle, its penetration depth becomes sharply smaller. When the grazing incidence angle of the X-ray is less than a material-related specific angle (such as the critical angle), the incident X-ray is completely reflected , only interact with the surface layer of the material, so that the emitted X-rays only contain the structural information of the surface layer of the material. This phenomenon is the physical basis of grazing incidence XAFS spectroscopy experiments.

国外的一些实验室,如日本的KEK(国家高能物理实验室)和SPRING-8、法国的ESRF(欧洲同步辐射机构)以及美国APS(美国物理学会)、ALS(先进光源同步辐射机构)和BNL(布鲁克黑文国家实验室),国内的实验室如合肥的国家同步辐射实验室和北京同步辐射实验室等陆续发展了多种薄膜试样的XAFS实验方法,获得了某些固体表面、界面和薄膜的结构,获得了表面催化和化学吸附、表面和界面原子结构重构、扩散和应力弛豫等特性。然而,在实验中,如何依据X射线源和探测器的特性来改进信噪比、减少杂散光或衍射峰的干扰仍然是极具挑战性的课题。Some foreign laboratories, such as KEK (National High Energy Physics Laboratory) and SPRING-8 in Japan, ESRF (European Synchrotron Radiation Facility) in France, APS (American Physical Society), ALS (Advanced Light Source Synchrotron Radiation Facility) and BNL in the United States (Brookhaven National Laboratory), domestic laboratories such as Hefei National Synchrotron Radiation Laboratory and Beijing Synchrotron Radiation Laboratory have successively developed XAFS experimental methods for various thin film samples, and obtained some solid surface, interface and The structure of the thin film has obtained properties such as surface catalysis and chemical adsorption, surface and interface atomic structure reconstruction, diffusion and stress relaxation. However, in experiments, how to improve the signal-to-noise ratio and reduce the interference of stray light or diffraction peaks according to the characteristics of X-ray sources and detectors is still a very challenging topic.

现有的通用方案是采用θ-2θ转角仪,其设置原理如图1所示。图1示意性示出现有技术中θ-2θ转角仪用于掠入射XAFS实验的示意图,经过单色器的X射线经过前电离室入射到样品上,样品台固定在轴座上,轴座本身可以绕测角台中心轴转动(θ转动)。探测器(一般为NaI闪烁探测器)则固定在轴臂上,轴臂也可以绕轴转动(2θ转动)。整个转台置于一个电动升降台上,以调整其垂直高度。在样品台上方的转台基座上固定一个荧光电离室以接收样品的荧光信号。The existing general solution is to use the θ-2θ angle meter, and its setting principle is shown in Figure 1. Figure 1 schematically shows the schematic diagram of the θ-2θ rotator used in the grazing incidence XAFS experiment in the prior art, the X-rays passing through the monochromator are incident on the sample through the front ionization chamber, the sample stage is fixed on the axle seat, and the axle seat itself It can rotate around the central axis of the goniometer (theta rotation). The detector (usually a NaI scintillation detector) is fixed on the shaft arm, and the shaft arm can also rotate around the axis (2θ rotation). The entire turntable is placed on an electric lifting platform to adjust its vertical height. A fluorescence ionization chamber is fixed on the turntable base above the sample stage to receive the fluorescence signal of the sample.

这种设置存在如下问题:样品的初始位置难以精确定位。而且,这种设置中样品的转动角度难以精确调整。另外,这种设置的探测噪声大,采谱质量不高。This setup has the following problem: the initial position of the sample is difficult to locate precisely. Also, the angle of rotation of the sample in this setup is difficult to adjust precisely. In addition, the detection noise of this setup is large, and the quality of the spectrum is not high.

发明内容Contents of the invention

为了克服上述现有技术中存在的问题中的一个或多个,本申请实施例提供一种专用于掠入射XAFS实验的装置以及该装置的调整方法。In order to overcome one or more of the above-mentioned problems in the prior art, embodiments of the present application provide a device dedicated to grazing incidence XAFS experiments and an adjustment method for the device.

本申请实施例提供了一种专用于掠入射XAFS实验的装置,包括:The embodiment of the present application provides a device dedicated to grazing incidence XAFS experiments, including:

用于产生所述掠入射XAFS实验所需的X射线的装置;means for generating the x-rays required for said grazing incidence XAFS experiments;

前狭缝,用于限定所述X射线源发出的X射线的尺寸;a front slit for limiting the size of the X-rays emitted by the X-ray source;

第一升降台,用于安装所述前狭缝,并使所述前狭缝在与所述X射线的光轴方向垂直的方向上升降;a first lifting platform, used to install the front slit, and make the front slit lift in a direction perpendicular to the direction of the X-ray optical axis;

样品架,用于承载样品,所述样品的表面与从所述前狭缝出射的X射线相互作用;a sample holder for carrying a sample whose surface interacts with the X-rays emerging from the front slit;

旋转台,用于安装所述样品架,并使得所述样品架上的样品转动,以获得所需的X射线掠入射角度;A rotary table, used to install the sample holder, and make the sample on the sample holder rotate, so as to obtain the required X-ray grazing incidence angle;

第二升降台,用于安装所述旋转台,并使得所述旋转台在与所述X射线的光轴方向垂直的方向上升降;The second lifting platform is used to install the rotating platform, and make the rotating platform lift in a direction perpendicular to the direction of the X-ray optical axis;

后狭缝,用于限定与所述样品的表面相互作用后的全反射X射线的尺寸;a rear slit for defining the size of the totally reflected x-rays after interacting with the surface of the sample;

第三升降台,用于安装所述后狭缝,并使得所述后狭缝在与所述X射线垂直的方向上升降;a third lifting platform, used to install the rear slit, and make the rear slit move up and down in a direction perpendicular to the X-ray;

基座升降部,用于安装所述第一升降台、所述第二升降台和所述第三升降台,使得所述第一升降台、第二升降台和所述第三升降台在与所述X射线的光轴方向垂直的方向上升降;The base lifting part is used to install the first lifting platform, the second lifting platform and the third lifting platform, so that the first lifting platform, the second lifting platform and the third lifting platform are in contact with the third lifting platform The X-rays are raised and lowered in a direction perpendicular to the optical axis direction;

第一探测器,用于探测从所述样品发出的荧光信号;a first detector for detecting a fluorescent signal emitted from said sample;

第二探测器,用于探测从所述后狭缝出射的X射线信号。The second detector is used to detect the X-ray signals emitted from the rear slit.

在前述结构的基础上,还可以包括狭缝组件,设置在所述样品架与所述第一探测器之间;所述狭缝组件包括一组不平行的叶片并且具有焦点。并且所述样品的中线至所述旋转台的台面的距离为所述狭缝组件的焦点距离。On the basis of the foregoing structure, it may further include a slit assembly disposed between the sample holder and the first detector; the slit assembly includes a set of non-parallel blades and has a focal point. And the distance from the centerline of the sample to the table top of the rotating stage is the focal length of the slit assembly.

在前述实施例的基础上,所述第一探测器上可以设置有遮光罩。On the basis of the foregoing embodiments, a light shield may be provided on the first detector.

本申请实施例还提供了一种前述装置的调整方法,包括:The embodiment of the present application also provides a method for adjusting the aforementioned device, including:

调节基座升降部,使得所述基座升降部达到与准直光束相匹配的垂直高度;Adjusting the base lifting part so that the base lifting part reaches a vertical height matching the collimated beam;

打开前狭缝,移开样品,通过第三升降台调节所述后狭缝在与所述X射线的光轴垂直的方向上的高度,直到第二探测器的输出达到最大;Opening the front slit, removing the sample, and adjusting the height of the rear slit in the direction perpendicular to the optical axis of the X-ray through a third lift until the output of the second detector reaches the maximum;

调节前狭缝的缝宽,并通过第一升降台调节所述前狭缝在与X射线的光轴垂直的方向上的高度,直到第二探测器的输出达到最大;Adjust the slit width of the front slit, and adjust the height of the front slit in the direction perpendicular to the optical axis of the X-ray through the first lifting platform until the output of the second detector reaches the maximum;

将样品放置在样品架上,通过第二升降台调节所述样品架在与X射线的光轴垂直的方向上的高度,直到第二探测器的输出达到最大时的一半;然后驱动旋转台,直到第二探测器的输出达到最大;重复垂直调节所述样品架的步骤,直到所述第二探测器的输出达到最大时的一半,并且在顺时针和逆时针两个方向旋转所述旋转台时,所述第二探测器的输出均减小。The sample is placed on the sample holder, and the height of the sample holder in the direction perpendicular to the optical axis of the X-ray is adjusted by the second lifting platform until the output of the second detector reaches half of the maximum; then the rotary table is driven, until the output of the second detector reaches the maximum; repeat the steps of vertically adjusting the sample holder until the output of the second detector reaches half of the maximum, and rotate the turntable in both clockwise and counterclockwise directions When , the outputs of the second detectors all decrease.

在以上步骤的基础上,还可以包括:根据所需的掠入射角度旋转所述旋转台;设置所述后狭缝到所述样品架的距离,根据所述掠入射角度、所述后狭缝到所述样品架的距离,计算并设置所述后狭缝的垂直位置;转动所述旋转台,直到所述第二探测器的输出达到最大值。On the basis of the above steps, it may also include: rotating the turntable according to the required grazing incidence angle; setting the distance from the rear slit to the sample holder, according to the grazing incidence angle, the rear slit the distance to the sample holder, calculate and set the vertical position of the rear slit; rotate the turntable until the output of the second detector reaches the maximum value.

本申请实施例提供的专用于掠入射XAFS实验的装置,取代了常规的XAFS实验系统中的样品支架及探测部分的结构,可以与常规的XAFS实验系统结合构成具有实现掠入射XAFS实验功能的硬件环境。The device dedicated to the grazing incidence XAFS experiment provided by the embodiment of the present application replaces the structure of the sample holder and the detection part in the conventional XAFS experimental system, and can be combined with the conventional XAFS experimental system to form hardware with the function of realizing the grazing incidence XAFS experiment environment.

采用本申请实施例提供的专用于掠入射XAFS实验的装置及该装置的调整方法,在调整好前后狭缝的缝宽和垂直高度之后,将样品放置在样品架上,通过第二升降台调节样品架在垂直方向上的高度,然后驱动旋转台,直到第二探测器的输出达到最大;重复垂直调节样品架的步骤,直到第二探测器的输出达到最大时的一半,并且在顺时针和逆时针两个方向转动旋转台时,第二探测器的输出均减小。通过这样的调整方式,可以将样品调节到光束中心并且表面与光束平行,这样就实现了样品初始位置的快速精确设定,而且能够精确地调整样品角度,并以高信噪比获取样品的实验探测数据,获得高质量的掠入射XFAS实验谱。Using the device dedicated to grazing incidence XAFS experiments provided by the embodiment of the present application and the adjustment method of the device, after adjusting the slit width and vertical height of the front and rear slits, the sample is placed on the sample holder and adjusted by the second lifting platform. The height of the sample holder in the vertical direction, and then drive the rotary stage until the output of the second detector reaches the maximum; repeat the steps of adjusting the sample holder vertically until the output of the second detector reaches half of the maximum, and rotate clockwise and When the turntable is turned counterclockwise in both directions, the output of the second detector decreases. Through such an adjustment method, the sample can be adjusted to the center of the beam and the surface is parallel to the beam, so that the initial position of the sample can be quickly and accurately set, and the angle of the sample can be adjusted accurately, and the experiment of the sample can be obtained with a high signal-to-noise ratio Detect data and obtain high-quality grazing incidence XFAS experimental spectra.

在该装置中,采用了两种高灵敏度探测器,可以同时探测样品产生的荧光以及全反射X光信号。由于掠入射状态样品产生的X光信号强度比正入射状态样品产生的X光信号低,因而高灵敏度的探测器可以保证采谱质量。而且,第二探测器支持样品位置设定,以使得第二探测器与样品之间形成θ-2θ探测模式。另外,在该装置中,通过在荧光探测器(即第一探测器)的探测器口上设置遮光罩,减少了由于X光信号在空气中传播时发生散射而造成的散射背底,减小了探测噪声,提高了采谱质量。In this device, two high-sensitivity detectors are used, which can simultaneously detect the fluorescence generated by the sample and the total reflection X-ray signal. Since the intensity of the X-ray signal generated by the sample in the grazing incidence state is lower than that generated by the sample in the normal incidence state, the high-sensitivity detector can ensure the quality of the spectrum. Moreover, the second detector supports sample position setting, so that a θ-2θ detection mode is formed between the second detector and the sample. In addition, in this device, by setting a light shield on the detector port of the fluorescence detector (that is, the first detector), the scattering background caused by X-ray signal scattering when propagating in the air is reduced, reducing the Detect noise and improve the quality of spectrum acquisition.

在XAFS谱采谱过程中,样品的硅衬底会产生衍射峰,衍射峰的存在会破坏XAFS谱。衍射峰往往是由样品的前沿硅衬底暴露于X射线而激发产生的,通过应用本申请实施例提供的装置,微调样品的垂直位置,可以规避衍射峰的产生,从而解决了困扰半导体表面结构测试的问题。During the XAFS spectrum acquisition process, the silicon substrate of the sample will produce diffraction peaks, and the existence of the diffraction peaks will destroy the XAFS spectrum. Diffraction peaks are often excited by the exposure of the silicon substrate at the front of the sample to X-rays. By applying the device provided in the embodiment of this application and fine-tuning the vertical position of the sample, the generation of diffraction peaks can be avoided, thereby solving the problem of semiconductor surface structure. Test questions.

另外,由于旋转台的转动误差,有可能样品的位置在旋转台转动后没有达到准确的掠入射角度。采用本申请实施例提供的调整方法,根据所需的掠入射角度旋转旋转台后,设置后狭缝到样品架的距离,根据掠入射角度、后狭缝到样品架的距离结合θ-2θ关系,计算并设置后狭缝的垂直位置,然后转动旋转台,直到第二探测器的输出达到最大值。这样就消除了旋转台转动误差,实现了样品的转动角度的精确调整。In addition, due to the rotation error of the turntable, it is possible that the position of the sample does not reach the exact grazing incidence angle after the turntable turns. Using the adjustment method provided by the embodiment of the present application, after rotating the rotary stage according to the required grazing incidence angle, set the distance from the rear slit to the sample holder, and combine the θ-2θ relationship according to the grazing incidence angle, the distance from the rear slit to the sample holder , calculate and set the vertical position of the rear slit, and then turn the rotary table until the output of the second detector reaches the maximum value. In this way, the rotation error of the rotary table is eliminated, and the precise adjustment of the rotation angle of the sample is realized.

通过以下参照附图对优选实施例的说明,本发明的上述以及其它目的、特征和优点将更加明显。The above and other objects, features and advantages of the present invention will be more apparent through the following description of preferred embodiments with reference to the accompanying drawings.

附图说明Description of drawings

图1示意性示出现有技术中θ-2θ转角仪用于掠入射XAFS实验的示意图;Fig. 1 schematically shows the schematic diagram of the θ-2θ goniometry used in the grazing incidence XAFS experiment in the prior art;

图2示意性示出掠入射XAFS谱实验的基本原理;Figure 2 schematically shows the basic principle of grazing incidence XAFS spectroscopy experiment;

图3示意性示出本申请实施例的专用于掠入射XAFS实验的装置的侧视结构示意图;Fig. 3 schematically shows a side-view structure diagram of a device dedicated to grazing incidence XAFS experiments according to an embodiment of the present application;

图4示意性示出本申请实施例中的一种旋转台和样品的相对位置示意图;Figure 4 schematically shows a schematic diagram of the relative positions of a rotary table and a sample in an embodiment of the present application;

图5示意性示出带有该狭缝组件的荧光X射线探测器示意图;Fig. 5 schematically shows a schematic diagram of a fluorescent X-ray detector with the slit assembly;

图6示意性示出本申请实施例的专用于掠入射XAFS实验的装置的调整方法的流程图Figure 6 schematically shows the flow chart of the adjustment method of the device dedicated to grazing incidence XAFS experiments according to the embodiment of the present application

图7A和图7B示出了本申请实施例中样品初始位置的调整示意图;Figure 7A and Figure 7B show a schematic diagram of the adjustment of the initial position of the sample in the embodiment of the present application;

图8示意性示出本申请实施例的专用于掠入射XAFS实验的装置的机械结构图;FIG. 8 schematically shows a mechanical structure diagram of a device dedicated to grazing incidence XAFS experiments according to an embodiment of the present application;

图9示意性示出应用本申请实施例提供的装置和调整方法获得的掠入射XAFS谱。Fig. 9 schematically shows a grazing incidence XAFS spectrum obtained by applying the device and adjustment method provided by the embodiment of the present application.

具体实施方式Detailed ways

在描述本申请实施例的专用于掠入射XAFS实验的装置之前,先描述掠入射XAFS谱实验的基本原理。Before describing the device dedicated to the grazing-incidence XAFS experiment of the embodiment of the present application, the basic principle of the grazing-incidence XAFS spectrum experiment will be described first.

图2示意性示出掠入射XAFS谱实验的基本原理。使X射线11以略小于临界角的掠入射角度掠入射到样品S,入射的X射线11在样品S表面发生全发射,仅与样品S表面厚度为几纳米到几十纳米的物质作用(具体的穿透深度与X射线的能量以及材料本身等因素相关)。该表面产生的荧光13包含样品表面物质结构信息。在探测元素吸收边进行单能X射线扫描,同时通过荧光探测器FD接收荧光13,即可以获得样品的一定深度的表面XAFS谱。Figure 2 schematically shows the basic principle of grazing incidence XAFS spectroscopy experiments. The X-ray 11 is grazingly incident on the sample S at a grazing incidence angle slightly smaller than the critical angle, and the incident X-ray 11 is fully emitted on the surface of the sample S, and only interacts with the material on the surface of the sample S with a thickness of several nanometers to tens of nanometers (specifically The penetration depth is related to factors such as the energy of X-rays and the material itself). The fluorescence 13 generated on the surface contains the structural information of the material on the surface of the sample. The single-energy X-ray scanning is performed on the absorption edge of the detection element, and the fluorescence 13 is received by the fluorescence detector FD at the same time, so as to obtain the surface XAFS spectrum of a certain depth of the sample.

接下来描述本申请实施例的专用于掠入射XAFS实验的装置。Next, the device dedicated to the grazing incidence XAFS experiment of the embodiment of the present application will be described.

图3示意性示出本申请实施例的专用于掠入射XAFS实验的装置的侧视结构示意图,该装置包括:用于产生掠入射XAFS实验所需的X射线的装置201、前狭缝202、第一升降台203、样品架204、旋转台205、第二升降台206、后狭缝207、第三升降台208、第一探测器209和第二探测器210。Fig. 3 schematically shows a side-view structural diagram of a device dedicated to grazing incidence XAFS experiments according to an embodiment of the present application, the device includes: a device 201 for generating X-rays required for grazing incidence XAFS experiments, a front slit 202, The first lifting platform 203 , the sample holder 204 , the rotating platform 205 , the second lifting platform 206 , the rear slit 207 , the third lifting platform 208 , the first detector 209 and the second detector 210 .

其中,前狭缝202、第一升降台203、样品架204、旋转台205、第二升降台206、后狭缝207、第三升降台208、第一探测器209和第二探测器210可以都位于一个基座升降部上211,该基座升降部211用于安装第一升降台203、第二升降台206和第三升降台208,使得第一升降台203、第二升降台206和第三升降台208在与X射线的光轴方向垂直的方向上同时升降。X射线的光轴方向可以如图3中虚线F所示。Wherein, the front slit 202, the first lifting platform 203, the sample holder 204, the rotating platform 205, the second lifting platform 206, the rear slit 207, the third lifting platform 208, the first detector 209 and the second detector 210 can be All are located on a base lifting part 211, and the base lifting part 211 is used to install the first lifting platform 203, the second lifting platform 206 and the third lifting platform 208, so that the first lifting platform 203, the second lifting platform 206 and the The third elevating table 208 simultaneously elevates in a direction perpendicular to the X-ray optical axis direction. The direction of the optical axis of the X-rays may be shown by the dotted line F in FIG. 3 .

该基座升降部211可以包括安装基板211a和第四升降台211b,该安装基板211a用于安装第一升降台203、第二升降台206和第三升降台208,第四升降台211b用于安装安装基板211a,使得安装基板211a在与X射线的光轴方向垂直的方向上升降。第四升降台211b可以是手动或电动升降台。通过基座升降部211可以调整整个装置在垂直方向上的高度。The base lifting part 211 may include an installation base plate 211a and a fourth lift platform 211b, the installation base plate 211a is used for installing the first lift platform 203, the second lift platform 206 and the third lift platform 208, and the fourth lift platform 211b is used for The mounting substrate 211a is mounted such that the mounting substrate 211a is raised and lowered in a direction perpendicular to the X-ray optical axis direction. The fourth lifting platform 211b can be a manual or electric lifting platform. The height of the entire device in the vertical direction can be adjusted through the base lifting part 211 .

该基座升降部211可以固定在滑块212上,使得整个装置可以在平行于X射线光轴的方向上滑动。The base lifting part 211 can be fixed on the slider 212, so that the whole device can slide in a direction parallel to the X-ray optical axis.

在图3所示的装置中,用于产生掠入射XAFS实验所需的X射线的装置201可以具有各种结构。例如,该装置201可以包括同步辐射光源、双晶单色器等。同步辐射光源覆盖可见光到几百keV的硬X射线,具有高强度、高准直、发射角小、广谱、具有时间结构、有偏振性、有一定的相干性、可准确计算等一系列优点。根据布拉格公式,采用双晶单色器,可以实现掠入射XAFS实验所要求的单能可调X射线能量扫描。当然,装置201也可以采用其他的能够产生所需X射线的结构。In the apparatus shown in FIG. 3 , the apparatus 201 for generating X-rays required for grazing incidence XAFS experiments can have various structures. For example, the device 201 may include a synchrotron radiation light source, a twin-crystal monochromator, and the like. The synchrotron radiation light source covers visible light to hard X-rays of hundreds of keV, and has a series of advantages such as high intensity, high collimation, small emission angle, broad spectrum, time structure, polarization, certain coherence, and accurate calculation. . According to the Bragg formula, the single-energy adjustable X-ray energy scanning required by the grazing incidence XAFS experiment can be realized by using the double crystal monochromator. Of course, the device 201 may also adopt other structures capable of generating required X-rays.

前狭缝202用于限定用于产生掠入射XAFS实验所需的X射线的装置201发出的X射线的尺寸。前狭缝202的缝宽可以通过手动调节。The front slit 202 is used to limit the size of the X-rays emitted by the device 201 for generating X-rays required for grazing incidence XAFS experiments. The slit width of the front slit 202 can be adjusted manually.

第一升降台203设置在前狭缝202下方,用于使得前狭缝202在垂直方向上升降。第一升降台203可以采用日本骏河KZG06030-C这一型号的升降台,该升降台的调整精度为0.05μm,该升降台可以由DS102控制器(一种步进电机控制器)驱动,可以实现手动或自动控制。The first lifting platform 203 is disposed under the front slit 202 for making the front slit 202 vertically lift. The first lifting platform 203 can be a lifting platform of the type KZG06030-C from Suruga, Japan. The adjustment accuracy of the lifting platform is 0.05 μm. The lifting platform can be driven by a DS102 controller (a stepping motor controller). Realize manual or automatic control.

样品架204用于承载样品S。从前狭缝202出射的X射线与样品架204上的样品S相互作用,产生荧光和全反射光。The sample holder 204 is used to carry the sample S. The X-rays emitted from the front slit 202 interact with the sample S on the sample holder 204 to generate fluorescence and total reflection light.

旋转台205用于安装样品架204,并使得样品架204(也就是使得样品S)转动,以获得所需的X射线掠入射角度。旋转台205的旋转轴可以位于图3中的虚线F和L的交点处并且垂直于纸面。样品S表面也可以垂直于纸面。当旋转台205转动时,样品S转动,X射线的掠入射角度也改变。The rotating stage 205 is used to install the sample holder 204 and make the sample holder 204 (that is, make the sample S) rotate to obtain a desired X-ray grazing incidence angle. The rotation axis of the rotary table 205 may be located at the intersection of the dashed lines F and L in FIG. 3 and be perpendicular to the paper. The surface of the sample S can also be perpendicular to the paper. When the rotary table 205 rotates, the sample S rotates, and the grazing incidence angle of X-rays also changes.

样品架204的设计要点之一是使得旋转台205的转轴沿着样品S的表面延伸方向经过样品的表面,这样可以实现样品掠入射角度改变时不会发生垂直方向的移动。图4示意性示出本申请实施例中的一种旋转台和样品的相对位置示意图,该图中,旋转台205的转轴(如虚线所示)沿着样品S的表面延伸方向经过样品的表面。One of the design points of the sample holder 204 is to make the rotation axis of the rotating stage 205 pass the surface of the sample S along the extending direction of the surface of the sample S, so that the vertical movement of the sample will not occur when the grazing incidence angle of the sample changes. Fig. 4 schematically shows a schematic view of the relative position of a rotary table and the sample in the embodiment of the present application, in this figure, the rotation axis of the rotary table 205 (as shown by the dotted line) passes through the surface of the sample along the direction in which the surface of the sample S extends .

样品架204可以设计为可拆卸的结构,这样便于样品S的安装。The sample holder 204 can be designed as a detachable structure, which facilitates the installation of the sample S.

第二升降台206用于安装205旋转台,并使得旋转台205在与X射线的光轴方向垂直的方向上升降。该第二升降台206也可以采用日本骏河KZG06030-C这一型号的升降台。旋转台205可以采用日本骏河KRW04360这一型号的旋转台,调整精度为10角秒。旋转台205和第二升降台206这二者均可以由DS102控制器驱动,可以实现手动或自动控制。The second lifting platform 206 is used to install 205 the rotating platform, and make the rotating platform 205 rise and fall in a direction perpendicular to the direction of the X-ray optical axis. The second lifting platform 206 can also be a lifting platform of the model KZG06030-C from Suruga, Japan. The rotary table 205 can be a rotary table of the type KRW04360 from Suruga, Japan, and the adjustment accuracy is 10 arc seconds. Both the rotating platform 205 and the second lifting platform 206 can be driven by the DS102 controller, and can be controlled manually or automatically.

通过旋转台205和第二升降台206,可以进行样品S的垂直升降以及转动位置的设定。Through the rotating table 205 and the second elevating table 206, vertical lifting of the sample S and setting of the rotational position can be performed.

后狭缝207用于限定与样品S的表面相互作用后的全反射X射线的尺寸。后狭缝207是固定宽度的狭缝。可以选择不同缝宽的狭缝作为后狭缝207。The rear slit 207 is used to define the size of the totally reflected X-rays after interacting with the surface of the sample S. The rear slit 207 is a fixed width slit. Slits with different slit widths can be selected as the rear slit 207 .

第三升降台208用于安装后狭缝207,并使得后狭缝207在与X射线垂直的方向上升降。第三升降台208也可以采用日本骏河KZG06030-C这一型号的升降台。该第三升降台也可以由DS102控制器驱动,可以实现手动或电动控制。The third lifting table 208 is used to install the rear slit 207 and make the rear slit 207 rise and fall in a direction perpendicular to the X-ray. The third lifting platform 208 can also adopt the lifting platform of the model KZG06030-C of Suruga, Japan. The third lifting platform can also be driven by DS102 controller, which can realize manual or electric control.

第一探测器209是用于探测从样品S发出的荧光信号的荧光探测器。例如,可以采用型号为LYTLE型号的荧光探测器。该LYTLE荧光探测器的探头面垂直向下,以接收从样品S发出的荧光信号。荧光探测器209可以设置在探测器支架214上,探测器支架214可以设置在第二升降台206上,荧光探测器209与样品架204之间保持固定距离,并且探测器209与样品架204同步升降。The first detector 209 is a fluorescence detector for detecting fluorescence signals emitted from the sample S. For example, a fluorescence detector model LYTLE can be used. The probe face of the LYTLE fluorescence detector is vertically downward to receive the fluorescence signal emitted from the sample S. The fluorescence detector 209 can be arranged on the detector support 214, and the detector support 214 can be arranged on the second lifting platform 206, and a fixed distance is kept between the fluorescence detector 209 and the sample holder 204, and the detector 209 is synchronized with the sample holder 204 lift.

在荧光探测器209与样品架204之间可以设置有狭缝组件(图中未示出)。该狭缝组件可以包括一组不平行的叶片,并且具有焦点。样品S的中线(如图4中的点划线所示)至狭缝组件的距离为狭缝组件的焦点距离。具体而言,该狭缝组件可以采用EXAFS公司生产的荧光X射线探测器(Fluorescent x-raydetector)。图5示意性示出带有该狭缝组件的荧光X射线探测器示意图。在本申请的实施例中,将该公司提供的狭缝组件从荧光X射线探测器中分离出来单独使用,来实现本发明的目的。通过使用该狭缝组件,在焦点处各个方向的X射线均能被荧光探测器209接收到,从而将荧光探测器209接收到的X射线最大化。A slit assembly (not shown in the figure) may be provided between the fluorescence detector 209 and the sample holder 204 . The slot assembly may include a set of non-parallel blades and have a focal point. The distance from the midline of the sample S (as shown by the dotted line in Figure 4) to the slit assembly is the focal length of the slit assembly. Specifically, the slit assembly may use a fluorescent x-ray detector (Fluorescent x-ray detector) produced by EXAFS. Fig. 5 schematically shows a schematic diagram of a fluorescent X-ray detector with the slit assembly. In the embodiment of the present application, the slit assembly provided by the company is separated from the fluorescent X-ray detector and used alone to achieve the purpose of the present invention. By using the slit assembly, X-rays in all directions at the focal point can be received by the fluorescence detector 209 , thereby maximizing the X-rays received by the fluorescence detector 209 .

另外,荧光探测器209口可以设置遮光罩,以减少由于X光信号在空气中传播时发生散射而造成的散射背底。In addition, the mouth of the fluorescent detector 209 can be provided with a shading cover to reduce the scattering background caused by scattering of X-ray signals when propagating in the air.

第二探测器210用于探测从后狭缝207出射的X射线信号。该第二探测器210可以是光电二极管(PD),该光电二极管可以探测从后狭缝207出射的X射线的强度。第二探测器210可以与后狭缝207一起安装在第三升降台208上,这样,第二探测器210和后狭缝207均具有在垂直方向上的调整自由度。The second detector 210 is used to detect the X-ray signals emitted from the rear slit 207 . The second detector 210 can be a photodiode (PD), which can detect the intensity of X-rays emitted from the rear slit 207 . The second detector 210 can be installed on the third lifting platform 208 together with the rear slit 207 , so that both the second detector 210 and the rear slit 207 have a degree of freedom of adjustment in the vertical direction.

第三升降台208可以安装在以直线滑动台215上,通过该直线滑动台215,可以进行水平长距离手动调整。第三升降台208的滑动方向与X射线的光轴方向平行。由于后狭缝207和第二探测器210均是设置在第三升降台208上,这样,后狭缝207和第二探测器210也可以在水平方向上滑动。也就是说,后狭缝207和第二探测器210不仅具有垂直方向上的调节自由度,还具有水平方向上的调节自由度。通过在水平方向上滑动后狭缝207和第二探测器210,可以精确调节后狭缝207与样品S之间的水平距离。The third lifting platform 208 can be installed on the linear sliding platform 215, through which the linear sliding platform 215 can be manually adjusted horizontally and over a long distance. The sliding direction of the third lifting platform 208 is parallel to the optical axis direction of X-rays. Since both the rear slit 207 and the second detector 210 are arranged on the third lifting platform 208, the rear slit 207 and the second detector 210 can also slide in the horizontal direction. That is to say, the rear slit 207 and the second detector 210 not only have an adjustment degree of freedom in the vertical direction, but also have an adjustment degree of freedom in the horizontal direction. By sliding the rear slit 207 and the second detector 210 in the horizontal direction, the horizontal distance between the rear slit 207 and the sample S can be precisely adjusted.

另外,在图3所示的装置中,第一升降台203和第二升降台206均可以安装在垫块213上,这样便于调整第一、第二和第三升降台的垂直高度。In addition, in the device shown in FIG. 3 , both the first lifting platform 203 and the second lifting platform 206 can be installed on the spacer 213 , which is convenient for adjusting the vertical heights of the first, second and third lifting platforms.

下面来描述图3所示专用于掠入射XAFS实验的装置的调整方法。图6示意性示出本申请实施例的专用于掠入射XAFS实验的装置的调整方法的流程图。该方法包括如下步骤:The adjustment method of the device shown in Fig. 3 dedicated to grazing incidence XAFS experiments will be described below. FIG. 6 schematically shows a flow chart of an adjustment method of a device dedicated to grazing incidence XAFS experiments according to an embodiment of the present application. The method comprises the steps of:

步骤S31、调节基座升降部,使得基座升降部达到与准直光束相匹配的垂直高度。Step S31 , adjusting the base lifting part so that the base lifting part reaches a vertical height matching the collimated light beam.

调整过程是进行XAFS实验之前的准备工作,不需要装置201发出X射线,那么可以通过出光方向与X射线一致的准直光源来模拟X射线源进行调节。具体而言,可以用X光敏感纸在两点对X光曝光,通过两点光斑的空间位置来确定准直光源的光束方向。该准直光源可以采用准直激光。The adjustment process is the preparatory work before the XAFS experiment, and the device 201 does not need to emit X-rays, so the adjustment can be made by simulating the X-ray source through a collimated light source whose light output direction is consistent with that of the X-rays. Specifically, X-ray sensitive paper can be used to expose to X-rays at two points, and the beam direction of the collimated light source can be determined by the spatial positions of the two spots. The collimated light source can be a collimated laser.

在步骤S31中,进行的是一种粗调,以准直光束为基准,将整个装置升高到适当的高度。In step S31, a rough adjustment is performed, and the entire device is raised to an appropriate height based on the collimated light beam.

步骤S32、打开前狭缝,移开样品,通过第三升降台调节后狭缝在与X射线的光轴垂直的方向上的高度,直到第二探测器的输出达到最大。这时,表明后狭缝与准直光源的光束中心准直,也就是说,与X射线的光束中心准直。Step S32, open the front slit, remove the sample, and adjust the height of the rear slit in the direction perpendicular to the optical axis of the X-ray through the third lifting platform until the output of the second detector reaches the maximum. At this time, it indicates that the rear slit is collimated with the beam center of the collimated light source, that is, with the beam center of the X-ray.

步骤S33、调节前狭缝的缝宽,并通过第一升降台调节前狭缝在与X射线的光轴垂直的方向上的高度,直到第二探测器的输出达到最大。这时,表明前后狭缝均与准直光源的光束中心准直,也就是说,与X射线的光束中心准直。通过这样设置,前后狭缝之间的光束位置以及光束的截面尺寸均被限定。Step S33 , adjusting the slit width of the front slit, and adjusting the height of the front slit in the direction perpendicular to the optical axis of the X-ray through the first lifting platform until the output of the second detector reaches the maximum. At this time, it shows that both the front and rear slits are collimated with the beam center of the collimated light source, that is to say, with the beam center of the X-ray. By setting in this way, the position of the beam between the front and rear slits and the cross-sectional size of the beam are both limited.

步骤S34、将样品放置在样品架上,通过第二升降台调节样品架在与X射线的光轴垂直的方向上的高度,直到第二探测器的输出达到最大时的一半;然后驱动旋转台,直到第二探测器的输出达到最大;重复垂直调节样品架的步骤,直到第二探测器的输出达到最大时的一半,并且在顺时针和逆时针两个方向旋转旋转台时,第二探测器的输出均减小。这时,表明样品的表面与准直光束平行,而且样品位于光束中间。Step S34, the sample is placed on the sample holder, and the height of the sample holder in the direction perpendicular to the optical axis of the X-ray is adjusted through the second lifting platform until the output of the second detector reaches half of the maximum value; then the rotary table is driven , until the output of the second detector reaches the maximum; repeat the steps of adjusting the sample holder vertically until the output of the second detector reaches half of the maximum, and when the turntable is rotated clockwise and counterclockwise, the second detector The output of the device is reduced. This indicates that the surface of the sample is parallel to the collimated beam and that the sample is in the middle of the beam.

具体而言,如图7A和图7B所示,图7A和图7B示出了本申请实施例中样品初始位置的调整示意图。为了便于说明,图7A和图7B中对于准直光束的尺寸进行了放大。Specifically, as shown in FIG. 7A and FIG. 7B , FIG. 7A and FIG. 7B show a schematic diagram of adjusting the initial position of the sample in the embodiment of the present application. For ease of illustration, the size of the collimated beam is exaggerated in FIGS. 7A and 7B .

如果样品的表面没有与准直光束平行,而且样品没有位于准直光束中间,如图7A所示,则当转动旋转台使得样品逆时针旋转时,样品遮挡的准直光束截面增大,第二探测器的输出减小。而当转动旋转台使得样品顺时针旋转时,样品遮挡的准直光束截面变小,因而第二探测器的输出增大。If the surface of the sample is not parallel to the collimated beam, and the sample is not located in the middle of the collimated beam, as shown in Figure 7A, then when the rotating stage is rotated so that the sample rotates counterclockwise, the section of the collimated beam blocked by the sample increases, the second The output of the detector decreases. However, when the rotating stage is rotated so that the sample rotates clockwise, the cross-section of the collimated beam blocked by the sample becomes smaller, so the output of the second detector increases.

如果样品的表面与准直光束平行,而且样品位于准直光束的中间,如图7B所示,则当转动旋转台式的样品顺时针和逆时针旋转时,样品遮挡的准直光束截面均增大,第二探测器的输出均减小。If the surface of the sample is parallel to the collimated beam, and the sample is located in the middle of the collimated beam, as shown in Figure 7B, when the sample is rotated clockwise and counterclockwise, the cross section of the collimated beam blocked by the sample increases , the output of the second detector decreases.

步骤S34其实是一个“找零”的过程,通过步骤S34的调整,使得样品位于掠入射角为零的位置。Step S34 is actually a "recovery" process, through the adjustment of step S34, the sample is located at a position where the grazing incidence angle is zero.

经过了上述的步骤S31到步骤S34之后,即完成了样品初始位置的快速精确设置。After the above-mentioned steps S31 to S34, the rapid and accurate setting of the initial position of the sample is completed.

本申请实施例提供的调整方法还可以包括如下的步骤:The adjustment method provided in the embodiment of the present application may also include the following steps:

步骤S35、根据所需的掠入射角度(例如,0.15度)转动旋转台。Step S35 , rotating the rotary table according to the required grazing incidence angle (for example, 0.15 degrees).

步骤S36、设置后狭缝到样品架的距离,根据掠入射角度、后狭缝到样品架的距离并结合θ-2θ关系,计算并设置后狭缝的垂直位置。Step S36 , setting the distance from the rear slit to the sample holder, and calculating and setting the vertical position of the rear slit according to the grazing incidence angle, the distance from the rear slit to the sample holder and the relationship between θ-2θ.

根据θ-2θ的测量原理,当入射光线转动θ时,第二探测器需要变化2θ的角度。具体到如图3所示的装置,当步骤S34之后转动旋转台得到掠入射角度时,第二探测器的垂直位置发生变化。According to the measurement principle of θ-2θ, when the incident light rotates θ, the second detector needs to change the angle of 2θ. Specifically, for the device shown in FIG. 3 , when the rotary table is rotated to obtain a grazing incidence angle after step S34 , the vertical position of the second detector changes.

步骤S36相当于是通过理论计算计算出了后狭缝的垂直位置,并进行了设置。Step S36 is equivalent to calculating and setting the vertical position of the rear slit through theoretical calculation.

步骤S37、转动旋转台,直到第二探测器的输出达到最大值。Step S37, rotating the rotary table until the output of the second detector reaches the maximum value.

由于旋转台存在转动误差,因而经过步骤S35转动之后的掠入射角度可能不够准确。通过步骤S36设置完后狭缝的垂直位置之后,就获得了后狭缝的准确位置,通过转动旋转台使得透过后狭缝入射到第二探测器上的光信号最大,就可以实现样品掠入射角度的精确调整。Due to the rotation error of the rotary table, the grazing incidence angle after the rotation in step S35 may not be accurate enough. After the vertical position of the rear slit is set in step S36, the exact position of the rear slit is obtained. By rotating the rotary table, the optical signal transmitted through the rear slit and incident on the second detector is the largest, and the sample grazing incidence can be realized. Precise adjustment of the angle.

可以看出,上述步骤S35-S37实际上是起到了对掠入射角度进行核对的作用,进而保证了掠入射角度的精确调整。It can be seen that the above steps S35-S37 actually play a role of checking the grazing incidence angle, thereby ensuring the precise adjustment of the grazing incidence angle.

通过后移后狭缝和第二探测器这对组合,根据样品至后狭缝的距离以及后狭缝距离它初始位置的垂直距离,可以核算样品的掠入射角度。By moving back the combination of the rear slit and the second detector, the grazing incidence angle of the sample can be calculated according to the distance from the sample to the rear slit and the vertical distance of the rear slit from its initial position.

本发明实施例中提供的以上调整方法,可以编制成通过计算机实现的程序软件,从而可以实现整个调整方法的自动化。The above adjustment methods provided in the embodiments of the present invention can be compiled into program software implemented by a computer, so that the automation of the entire adjustment method can be realized.

图8示意性示出本申请实施例的专用于掠入射XAFS实验的装置的机械结构图,请注意该图中省略了用于产生掠入射XAFS实验所需的X射线的装置。整个装置建立于升降安装板501之上,基座平台由手动升降台安装并调节整体装置的高度。手动升降台固定于滑块上,滑块可以在实验台轨道上沿光轴方向移动。该部分由AH长程平移台502、直线轴承组件510、内六角螺钉(GBT70.1-2000)526和525以及升降安装基板511实现。Fig. 8 schematically shows the mechanical structure diagram of the device dedicated to the grazing incidence XAFS experiment of the embodiment of the present application, please note that the device for generating X-rays required for the grazing incidence XAFS experiment is omitted in this figure. The whole device is built on the lifting installation plate 501, and the base platform is installed by a manual lifting platform to adjust the height of the whole device. The manual lifting platform is fixed on the slider, and the slider can move along the optical axis on the track of the test bench. This part is realized by AH long-distance translation stage 502, linear bearing assembly 510, hexagon socket screws (GBT70.1-2000) 526 and 525, and lifting installation base plate 511.

装置的最左边为前狭缝509,该狭缝的缝宽可以手动调节。前狭缝509通过角板508和垫块504固定于垂直电动升降台503上,则前狭缝509可以进行垂直位置调整。电动升降台503的型号为日本骏河KZG06030-C,其调整精度为0.05μm。电动升降台503由DS102控制器驱动,可以实现手动或自动控制。The leftmost part of the device is a front slit 509 whose width can be adjusted manually. The front slit 509 is fixed on the vertical electric lifting platform 503 through the corner plate 508 and the spacer 504, and then the front slit 509 can be adjusted in vertical position. The model of the electric lifting platform 503 is Japan Suruga KZG06030-C, and its adjustment accuracy is 0.05 μm. Electric lifting platform 503 is driven by DS102 controller, which can realize manual or automatic control.

前狭缝509之后是样品架514,样品架514固定于垂直电动升降台503和电动转台506之上,可以实现样品的垂直升降以及转动的空间位置设定。电动转台506的型号为日本骏河KRW04360,其调整精度为10角秒。电动转台506和垂直升降台503都是由DS102控制器驱动,可以实现手动或自动控制。电动转台506可以设置在转台安装台505上。Behind the front slit 509 is the sample rack 514, and the sample rack 514 is fixed on the vertical electric lifting table 503 and the electric turntable 506, which can realize the vertical lift and rotation spatial position setting of the sample. The model of the electric turntable 506 is Japan Suruga KRW04360, and its adjustment accuracy is 10 arc seconds. Both the electric turntable 506 and the vertical lifting platform 503 are driven by the DS102 controller, which can realize manual or automatic control. The motorized turntable 506 can be set on the turntable installation platform 505 .

样品架514设置在样品架安装板515上,样品架514具有样品板516。样品架514的设计要点之一是使得电动转台506的转轴沿着样品的表面延伸方向经过样品的表面。样品架514可拆卸,便于样品安装。A sample rack 514 is provided on a sample rack mounting plate 515 , and the sample rack 514 has a sample plate 516 . One of the design points of the sample holder 514 is to make the rotation axis of the motorized turntable 506 pass the surface of the sample along the extending direction of the surface of the sample. The sample rack 514 is detachable for easy sample installation.

样品架514上方安装有X射线荧光探测器513,该探测器的型号为LYTLE,该探测器的探头面垂直向下,以接收样品发出的荧光信号。该探测器513与样品架514之间保持固定距离。探测器513与样品架514之间还可以设置狭缝组件(图中未示出)。该探测器513的探测器口上可以设置遮光罩,以减少由于X光信号在空气中传播时发生散射而造成的散射背底。探测器513可以设置在探测器支架角板520上。An X-ray fluorescence detector 513 is installed above the sample holder 514, the model of the detector is LYTLE, and the probe surface of the detector is vertically downward to receive the fluorescence signal emitted by the sample. A fixed distance is maintained between the detector 513 and the sample holder 514 . A slit assembly (not shown in the figure) may also be provided between the detector 513 and the sample holder 514 . The detector port of the detector 513 may be provided with a shading cover to reduce the scattering background caused by scattering of the X-ray signal when propagating in the air. The detector 513 may be arranged on the corner plate 520 of the detector bracket.

样品架514后边是后狭缝518,后狭缝518具有固定缝宽,由角板517和压板519固定,可以有不同缝宽的狭缝可供选择安装。后狭缝518之后为光电二极管522,该光电二极管522安装在探测器安装板507上,用于探测通过后狭缝518的X射线强度。后狭缝518和光电二极管522都安装在垂直电动升降台521上,使得后狭缝518和光电二极管522都具有垂直调整自由度。垂直电动升降台521的型号为日本骏河KZG06030-C,其调整精度为0.05μm。该电动升降台521可以由DS102控制器驱动,可以实现手动或自动控制。The rear side of the sample holder 514 is a rear slit 518, which has a fixed slit width and is fixed by a corner plate 517 and a pressing plate 519, and slits with different slit widths can be selected for installation. Behind the rear slit 518 is a photodiode 522 mounted on the detector mounting plate 507 for detecting the intensity of X-rays passing through the rear slit 518 . Both the rear slit 518 and the photodiode 522 are installed on the vertical electric lifting platform 521, so that both the rear slit 518 and the photodiode 522 have vertical adjustment freedom. The model of the vertical electric lifting table 521 is Japan Suruga KZG06030-C, and its adjustment accuracy is 0.05 μm. The electric lifting platform 521 can be driven by the DS102 controller, and can realize manual or automatic control.

电动升降台521安装于一套直线滑动台上,包括滑板523和过渡板524,通过该直线滑动台可以进行水平长距离手动移动。后狭缝518和光电二极管522形成的组合不仅具有垂直方向的调整自由度,而且具有光轴方向上的调整自由度,因而可以在光轴方向上精确设定后狭缝518和光电二极管522与样品之间的距离。The electric lifting platform 521 is installed on a set of linear sliding platform, including a slide plate 523 and a transition plate 524, through which the linear sliding platform can carry out horizontal long-distance manual movement. The combination formed by the rear slit 518 and the photodiode 522 not only has an adjustment degree of freedom in the vertical direction, but also has an adjustment degree of freedom in the direction of the optical axis, so that the relationship between the rear slit 518 and the photodiode 522 can be precisely set in the direction of the optical axis distance between samples.

图8中的附图标记537为垫圈,538为六角螺母(GBT6170-2000M4),525-536为内六角螺钉(GBT70.1-2000)。Reference numeral 537 in FIG. 8 is a washer, 538 is a hex nut (GBT6170-2000M4), and 525-536 is a hexagon socket screw (GBT70.1-2000).

采用本申请的专用于掠入射XAFS实验的装置及其调节方法,至少能够获得如下效果之一。At least one of the following effects can be obtained by using the device and its adjustment method dedicated to grazing incidence XAFS experiments of the present application.

本申请实施例提供的专用于掠入射XAFS实验的装置,取代了常规的XAFS实验系统中的样品支架及探测部分的结构,可以与常规的XAFS实验系统结合构成具有实现掠入射XAFS实验功能的硬件环境。The device dedicated to the grazing incidence XAFS experiment provided by the embodiment of the present application replaces the structure of the sample holder and the detection part in the conventional XAFS experimental system, and can be combined with the conventional XAFS experimental system to form hardware with the function of realizing the grazing incidence XAFS experiment environment.

采用本申请实施例提供的XAFS谱测量装置,利用旋转台和第二升降台,将样品调节到光束中心并且表面与光束平行,这样就实现了样品初始位置的快速精确设定。Using the XAFS spectrum measurement device provided in the embodiment of the present application, the sample is adjusted to the center of the beam and the surface is parallel to the beam by using the rotating table and the second lifting table, so that the initial position of the sample can be quickly and accurately set.

本申请实施例的装置,样品台平面对于X射线的角度以及垂直位置可以进行精确的设定和读出,读出精度以及调整精度可以分别达到10角秒(0.003度)和0.05μm。In the device of the embodiment of the present application, the angle and vertical position of the sample stage plane to X-rays can be accurately set and read out, and the readout accuracy and adjustment accuracy can reach 10 arcseconds (0.003 degrees) and 0.05 μm, respectively.

在该装置中,采用了两种高灵敏度探测器,可以同时探测样品产生的荧光以及全反射X光信号。由于掠入射状态样品产生的X光信号强度比正入射状态样品产生的X光信号低,因而高灵敏度的探测器可以保证采谱质量。而且,这第二探测器的支持样品位置设定,以使得第二探测器与样品之间形成θ-2θ探测模式。另外,在该装置中,通过在荧光探测器的探测器口上设置遮光罩,减少了由于X光信号在空气中传播时发生散射而造成的散射背底,减小了探测噪声,提高了采谱质量。In this device, two high-sensitivity detectors are used, which can simultaneously detect the fluorescence generated by the sample and the total reflection X-ray signal. Since the intensity of the X-ray signal generated by the sample in the grazing incidence state is lower than that generated by the sample in the normal incidence state, the high-sensitivity detector can ensure the quality of the spectrum. Moreover, the position of the supporting sample of the second detector is set such that a θ-2θ detection mode is formed between the second detector and the sample. In addition, in this device, by setting a hood on the detector port of the fluorescence detector, the scattering background caused by the scattering of the X-ray signal when propagating in the air is reduced, the detection noise is reduced, and the spectrum acquisition is improved. quality.

在XAFS谱采谱过程中,样品的硅衬底会产生衍射峰,衍射峰的存在会破坏XAFS谱。衍射峰往往是由样品的前沿硅衬底暴露于X射线而激发产生的,通过应用本申请实施例提供的装置,微调样品的垂直位置,可以规避衍射峰的产生,从而解决了困扰半导体表面结构测试的问题。During the XAFS spectrum acquisition process, the silicon substrate of the sample will produce diffraction peaks, and the existence of the diffraction peaks will destroy the XAFS spectrum. Diffraction peaks are often excited by the exposure of the silicon substrate at the front of the sample to X-rays. By applying the device provided in the embodiment of this application and fine-tuning the vertical position of the sample, the generation of diffraction peaks can be avoided, thereby solving the problem of semiconductor surface structure. Test questions.

图9示意性示出应用本申请实施例提供的装置和调整方法获得的掠入射XAFS谱,该谱包含样品表面结构信息。该样品是硅衬底镀铂,具有100μm的膜,掠入射角度为0.15度。该图中横坐标是入射的单能X射线的光子能量,纵坐标是样品的吸收系数。Fig. 9 schematically shows the grazing incidence XAFS spectrum obtained by applying the device and the adjustment method provided by the embodiment of the present application, and the spectrum includes the surface structure information of the sample. The sample was a platinum-coated silicon substrate with a 100 μm film and a grazing incidence angle of 0.15 degrees. In the figure, the abscissa is the photon energy of the incident monoenergetic X-ray, and the ordinate is the absorption coefficient of the sample.

虽然已参照几个典型实施例描述了本发明,但应当理解,所用的术语是说明和示例性、而非限制性的术语。由于本发明能够以多种形式具体实施而不脱离发明的精神或实质,所以应当理解,上述实施例不限于任何前述的细节,而应在随附权利要求所限定的精神和范围内广泛地解释,因此落入权利要求或其等效范围内的全部变化和改型都应为随附权利要求所涵盖。While this invention has been described with reference to a few exemplary embodiments, it is to be understood that the terms which have been used are words of description and illustration, rather than of limitation. Since the present invention can be embodied in many forms without departing from the spirit or essence of the invention, it should be understood that the above-described embodiments are not limited to any of the foregoing details, but should be construed broadly within the spirit and scope of the appended claims. , all changes and modifications falling within the scope of the claims or their equivalents shall be covered by the appended claims.

Claims (7)

1. be exclusively used in the device that glancing incidence XAFS tests, comprise:
The device of the X ray needed for testing for generation of described glancing incidence XAFS;
Front slit, for limit described to test for generation of described glancing incidence XAFS needed for the size of X ray that sends of the device of X ray;
First lifting table, for installing described front slit, and makes described front slit be elevated on the direction vertical with the optical axis direction of described X ray;
Specimen holder, for carrying sample, the surface of described sample with interact from the X ray of described front slit outgoing;
Universal stage, for installing described specimen holder, and makes the sample on described specimen holder rotate, to obtain required X ray glancing incidence angles;
Second lifting table, for installing described universal stage, and makes described universal stage be elevated on the direction vertical with the optical axis direction of described X ray;
Rear slit, for limit with the surface interaction of described sample after the size of full-reflection X ray;
3rd lifting table, for installing described rear slit, and makes described rear slit be elevated on the direction vertical with described X ray;
Pedestal lifting unit, for installing described first lifting table, described second lifting table and described 3rd lifting table, makes described first lifting table, the second lifting table be elevated on the direction vertical with the optical axis direction of described X ray with described 3rd lifting table simultaneously;
First detector, for detecting the fluorescence signal sent from described sample;
Second detector, for detecting the X ray signal from described rear slit outgoing;
Wherein, the rotating shaft of described universal stage along the surperficial bearing of trend of described sample through the surface of described sample;
Described first detector is provided with light shield.
2. device according to claim 1, also comprises slit assembly, is arranged between described specimen holder and described first detector; Described slit assembly comprises one group of uneven blade and has focus.
3. device according to claim 2, wherein, the center line of described sample to the distance of the table top of described universal stage is the focal length of described slit assembly.
4. device according to claim 1, wherein, described second detector is arranged on described 3rd lifting table;
Described 3rd lifting table is arranged on linear slide platform, and the glide direction of described 3rd lifting table on described linear slide platform is parallel with the optical axis direction of described X ray.
5. the device according to claim arbitrary in claim 1-4, described pedestal lifting unit comprises:
Installation base plate, for installing described first lifting table, described second lifting table and described 3rd lifting table;
4th lifting table, for installing described installation base plate, makes described installation base plate be elevated on the direction vertical with the optical axis direction of described X ray.
6. a method of adjustment for the device as described in claim arbitrary in claim 1-5, comprising:
Adjusting base lifting unit, makes described pedestal lifting unit reach the vertical height matched with collimated light beam;
Open front slit, remove sample, regulate the height of described rear slit on the direction vertical with the optical axis of X ray, until the output of the second detector reaches maximum by the 3rd lifting table;
Before regulating, the seam of slit is wide, and regulates the height of described front slit on the direction vertical with the optical axis of X ray, until the output of the second detector reaches maximum by the first lifting table;
Sample is placed on specimen holder, regulates the height of described specimen holder on the direction vertical with the optical axis of X ray, until the half when output of the second detector reaches maximum by the second lifting table; Then universal stage is driven, until the output of the second detector reaches maximum; Repeated vertical regulates the step of described specimen holder, until the half when output of described second detector reaches maximum, and when clockwise and counterclockwise both direction rotates described universal stage, the output of described second detector all reduces.
7. method according to claim 6, also comprises:
Described universal stage is rotated according to required glancing incidence angles;
The distance of described rear slit to described specimen holder is set, according to described glancing incidence angles, described rear slit to the distance of described specimen holder, calculates and the upright position of described rear slit is set;
Rotate described universal stage, until the output of described second detector reaches maximal value.
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