CN110320220B - Device and method for analyzing short-range ordered structure and long-range ordered structure of material - Google Patents

Device and method for analyzing short-range ordered structure and long-range ordered structure of material Download PDF

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CN110320220B
CN110320220B CN201910666887.0A CN201910666887A CN110320220B CN 110320220 B CN110320220 B CN 110320220B CN 201910666887 A CN201910666887 A CN 201910666887A CN 110320220 B CN110320220 B CN 110320220B
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罗震林
刘志杰
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University of Science and Technology of China USTC
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/083—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the radiation being X-rays
    • G01N23/085—X-ray absorption fine structure [XAFS], e.g. extended XAFS [EXAFS]
    • G—PHYSICS
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    • G01N23/20083—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by using a combination of at least two measurements at least one being a transmission measurement and one a scatter measurement
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    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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    • G01—MEASURING; TESTING
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    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence

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Abstract

The technical scheme of the invention discloses a device and a method for analyzing a short-range ordered structure and a long-range ordered structure of a material, wherein a light beam of a continuous spectrum is emitted by a synchrotron radiation light source to irradiate a material sample to be tested on a bearing component, first optical information can be obtained by a plurality of energy dispersion detectors, an X-ray diffraction test of the sample to be tested can be carried out based on the first optical information, second optical information can be obtained by a position sensitive detector, and an X-ray absorption fine structure test of the sample to be tested can be carried out based on the second optical information. Therefore, the technical scheme of the invention can simultaneously and rapidly analyze the short-range ordered structure and the long-range ordered structure of the material.

Description

Device and method for analyzing short-range ordered structure and long-range ordered structure of material
Technical Field
The invention relates to the technical field of material analysis characterization, in particular to a device and a method for analyzing a short-range ordered structure and a long-range ordered structure of a material.
Background
In many material science researches, for example, structural evolution of lithium battery electrode materials under service conditions, real-time analysis under in-situ reaction conditions is required for short-range ordered structures (local structures) and long-range ordered structures of the materials, which puts high requirements on time resolution capability of analysis technology.
X-ray absorption fine structure (XAFS) and X-ray diffraction (XRD) are two important techniques for studying material structures, and XAFS can give structural information of short-range order and XRD gives structural information of long-range order, which are complementary to each other and are used in a large number of material studies. If these two techniques are combined, both local and long-range order structure analysis can be performed simultaneously.
Disclosure of Invention
In view of this, the technical solution of the present invention provides a device and a method for analyzing a short-range ordered structure and a long-range ordered structure of a material, which can simultaneously and rapidly analyze the short-range ordered structure and the long-range ordered structure of the material.
In view of this, the present invention provides the following technical solutions:
an apparatus for analyzing short range order and long range order structures of a material, comprising: the bearing assembly is used for loading a material sample to be tested;
the synchronous radiation light source is used for emitting light beams with continuous spectrums so as to irradiate the material sample to be detected;
the system comprises a plurality of energy dispersion detectors, a plurality of optical sensors and a plurality of optical sensors, wherein detection axes of the energy dispersion detectors have different angles with the irradiation direction of the light beam, and the energy dispersion detectors are used for detecting first optical information at positions; the first optical information is at least used for carrying out an energy dispersive X-ray diffraction test on the material sample to be tested;
the light splitting and converging component is positioned in the irradiation range of the light beam and is used for splitting the light beam transmitted by the material sample to be detected and irradiating the light beam to the position sensitive detector, and the position sensitive detector is positioned behind the light splitting and converging component and is used for detecting second optical information of the position where the position sensitive detector is positioned; the second optical information is used to perform an energy dispersive X-ray absorption fine structure test on the sample of material to be tested.
Preferably, in the above apparatus, the light splitting and converging means includes: and bending the spectroscopic crystal.
Preferably, in the above apparatus, further comprising: and the first slit is positioned between the light splitting and converging component and the bearing component and is used for removing scattered light.
Preferably, in the above apparatus, further comprising: and the second slit is positioned between the synchrotron radiation light source and the bearing component and used for blocking light to obtain an incident beam with a required size.
Preferably, in the above apparatus, the apparatus has 11 of the energy dispersion detectors, the angle is in the range of 16.98 ° to 68.27 °, and the interplanar spacing under X-ray diffraction test is in the range of
Figure BDA0002140396550000021
Preferably, in the above apparatus, further comprising: the host computer is respectively connected with the energy dispersion detector and the position sensitive detector and is used for carrying out energy dispersion X-ray diffraction test on the material sample to be tested based on the first optical information and carrying out energy dispersion X-ray absorption fine structure test on the material sample to be tested based on the second optical information.
Preferably, in the above apparatus, the host computer is further configured to perform an X-ray fluorescence test on the sample of the material to be tested based on the first optical information.
Preferably, in the above apparatus, the method for performing the X-ray fluorescence test on the sample of the material to be tested by the host computer includes:
plotting the energy and the intensity of the X-ray photons detected by at least two energy dispersion detectors;
and acquiring a fluorescence spectrum and a diffraction spectrum based on the characteristic that the X-ray fluorescence is not changed along with the detection angle and the detection result of the energy dispersion detector.
Preferably, in the above apparatus, the synchrotron radiation light source is: undulator light sources, or twister light sources, or bent iron light sources.
The invention also provides a method for analyzing the short-range ordered structure and the long-range ordered structure of the material, and the device of any one of the methods is used for analyzing the short-range ordered structure and the long-range ordered structure of the material.
As can be seen from the above description, in the device and method for analyzing a short-range ordered structure and a long-range ordered structure of a material provided in the technical scheme of the present invention, a light beam of a continuous spectrum emitted by a synchrotron radiation light source irradiates a sample of a material to be detected on a carrier assembly, first optical information can be obtained by a plurality of energy dispersion detectors, an X-ray diffraction test of the sample to be detected can be performed based on the first optical information, second optical information can be obtained by a position sensitive detector, and an X-ray absorption fine structure test of the sample to be detected can be performed based on the second optical information. Therefore, the technical scheme of the invention can simultaneously and rapidly analyze the short-range ordered structure and the long-range ordered structure of the material.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic diagram of a conventional apparatus for analyzing short-range order structures and long-range order structures of a material;
FIG. 2 is a schematic view of another conventional apparatus for analyzing short-range order structures and long-range order structures of a material;
FIG. 3 is a diagram illustrating an apparatus for analyzing short-range order structures and long-range order structures of a material according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of another apparatus for analyzing short-range order structures and long-range order structures of a material according to an embodiment of the present invention;
FIG. 5 is a graph of detector angle versus measured interplanar spacing provided in accordance with an embodiment of the present invention;
FIG. 6 is a graph illustrating the energy and intensity of detected X-ray photons provided by an embodiment of the present invention;
FIG. 7 is a graph of another detector angle versus measured interplanar spacing provided by an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Characterization of conventional XAFS requires energy scanning by continuously changing the angle of the monochromator, a process of mechanical movement that is typically slow. Currently, there are two more mature rapid XAFS characterization techniques: x-ray absorption spectroscopy by fast scan monochromator (QXAFS) and energy dispersive X-ray absorption spectroscopy (EDXAFS). QXAFS characterization time can be as low as on the order of tens of milliseconds, while EDXAFS is faster and characterization time can be as low as on the order of microseconds.
The main manifestation of the crystal structure of materials characterized by X-ray diffraction is the Bragg diffraction formula, namely:
2dhklsinθ＝λ (1)
where d ishklThe interplanar spacing, 2 θ is the angle of the included angle between the incident beam and the emergent beam, and λ is the wavelength of the incident X-rays. Diffraction occurs when the incident light, the emergent light, and the crystal plane simultaneously satisfy the reflection relationship and the Bragg diffraction formula (1). It is clear that there are two diffraction schemes, one is to fix the wavelength λ of the incident light, and different interplanar spacings dhklCorresponding to different diffraction angles theta, which is conventional angle dispersive X-ray diffraction (ADXRD); the other is to fix the diffraction angle theta, irradiate the sample by adopting white light X-rays and have different interplanar distances dhklDiffraction occurs for X-rays of different wavelengths λ in the incident beam, which is energy dispersive X-ray diffraction (EDXRD). Both diffraction modes can be used for rapid characterization, and the time resolution capability can be as low as microsecond or even lower, and is mainly determined by a detector; of course, ADXRD is better than EDXRD in terms of resolving power Δ d/d of interplanar spacing.
For the XAFS-XRD combination, the characterization speed of the combination is determined by the XAFS part of the combination because the XRD testing speed is relatively high. One prior art approach to dynamic structural characterization by serial acquisition of QXAFS and ADXRD data is shown in fig. 1, where fig. 1 is a schematic diagram of a conventional apparatus for analyzing short-range order structures and long-range order structures of materials, comprising: a synchrotron radiation light source 11, a slit 12, a fast scanning monochromator 13, another slit 14, an incident light intensity monitor 15, a material sample 10 to be detected, a position sensitive detector 16 and a transmission X-ray detector 17.
In the manner shown in fig. 1, if the synchronous radiation beam passes through a slit 12 and then passes through a fast scanning monochromator 13 to generate a continuous spectrum, passes through another slit 14 and then passes through an incident light intensity detector 15 to irradiate the material sample 10 to be tested, and the transmitted beam strikes a rear X-ray detector 17, corresponding detection information can be obtained, and the detection information is used for performing an XAFS test on the material sample 10 to be tested to obtain XAFS data. When the XRD test is carried out alternately, the fast scanning monochromator 13 is controlled to enable emergent light to be monochromatic light at a fixed angle, scattered light of the monochromatic light after irradiating the material sample 10 to be tested is detected by the bent position sensitive detector 16, corresponding detection information can be obtained, and the detection information is used for carrying out the XRD test on the material sample 10 to be tested and obtaining XRD data.
According to the mode, a serial measurement mode is adopted to carry out XRD test and XAFS test on a material sample 10 to be tested respectively, QXAFS and ADXRD data acquisition can be carried out alternately by controlling a gate signal of a fast scanning monochromator, the standard period of the combined mode shown in figure 1 is shortened to 60ms, but for faster chemical kinetics and kinematics processes, the time resolution capability cannot meet the requirement, and a characterization technology with higher time resolution capability is required.
Compared with QXAFS, EDXAFS has higher time resolution capability which can reach microsecond order, so that the combination of EDXAFS and XRD technology is an effective method for improving the time resolution capability. However, in the conventional EDXAFS-ADXRD combination scheme, as shown in fig. 2, fig. 2 is a schematic view of another conventional apparatus for analyzing short-range order structure and long-range order structure of a material, including: a synchrotron radiation light source 21, a slit 22, a bending light splitting crystal 23, a movable slit 24, a material sample 20 to be detected, a position sensitive detector 25 and another position sensitive detector 26. In this way, the white light beam from the synchrotron radiation light source is reflected by the curved beam splitter crystal 23 and converged to the material sample 20 to be detected, and the light beam passing through the material sample 20 to be detected is incident on the rear position sensitive detector 26 to obtain corresponding detection information, and the detector information is used for performing the EDXAFS test on the material sample 10 to be detected, so as to obtain the EDXAFS data. When diffraction data needs to be collected, the movable slit 24 is moved to the back of the bent light splitting crystal 23, a beam with narrower energy bandwidth is clamped and irradiated to the material sample 20 to be detected, and the other position sensitive detector 25 positioned on the side surface of the material sample 20 to be detected is used for collecting diffraction signals, so that corresponding detection information can be obtained, and the detection information is used for carrying out ADXRD test on the material sample 20 to be detected and obtaining ADXRD data.
The arrangement shown in figure 2 requires the addition of a position sensitive detector 25 to detect the ADXRD signal on one side of the material sample 20 to be tested in the EDXAFS apparatus. The scheme can theoretically acquire EDXAFS data and ADXRD data at the same time, but because the energy bandwidth of incident light is too large (delta E/E-10%), the acquired diffraction signal peak width is large, the resolution of a d (interplanar spacing) value is low, and meanwhile, X-ray fluorescence also causes the diffraction background to be increased and the signal-to-noise ratio to be reduced. Therefore, in practical implementation of such a scheme, EDXAFS data and ADXRD data are typically acquired alternately in a serial manner; when ADXRD data is acquired, a slit 24 is moved into the optical path to capture a beam of light having a narrow energy bandwidth (FIG. 2). Obviously, the combined characterization speed is difficult to reduce to below tens of milliseconds due to the adoption of the moving mechanical slit.
Therefore, for the dynamic structure research of materials with higher time resolution requirements, a faster test scheme is also needed, in view of the above, the technical scheme of the embodiment of the invention combines EDXAFS and EDXRD, does not need moving mechanical parts, can break through the bottleneck of millisecond order and achieve microsecond time resolution, belongs to the field of material analysis characterization, and can be used for research of material science, relating to chemical, physical and material disciplines, and the like.
The technical scheme of the embodiment of the invention aims at the problem of dynamic structure research of materials, provides a device and a method for simultaneously measuring EDXAFS and EDXRD, improves the time resolution capability, and has important significance for the leading-edge basic research.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 3, fig. 3 is a device for analyzing a short-range order structure and a long-range order structure of a material, according to an embodiment of the present invention, the device including: a synchrotron radiation light source 31, a bearing component 33, a plurality of energy dispersion detectors 37, a light splitting and converging component 35 and a position sensitive detector 36.
The carrier assembly 33 is used for carrying the material sample 30 to be tested. The carrying component 33 may be a sample loading platform or a sample support, etc. based on the hardware configuration of the device, which is set according to the requirement, and the specific implementation manner of the carrying component 33 is not limited in the embodiment of the present invention.
The synchrotron radiation light source 31 is used for emitting continuous spectrum light beams to irradiate the material sample 30 to be measured. In the embodiment of the present invention, the light beam emitted from the synchrotron radiation light source 31 is synchrotron radiation light, which has a large wavelength coverage and has a continuous spectrum ranging from far infrared, visible light, ultraviolet to X-ray.
The detection axis of the energy dispersion detector 37 and the irradiation direction of the light beam have different angles 2 theta, and the energy dispersion detector 37 is used for detecting first optical information at the position; the first optical information is used at least for performing an energy dispersive X-ray diffraction (EDXRD) test on the material sample 30 to be tested, obtaining EDXRD data.
The light splitting and converging component 35 is located within the irradiation range of the light beam, and is used for splitting the light beam transmitted by the material sample 30 to be detected and irradiating the light beam to the position sensitive detector 36, and the position sensitive detector 36 is located behind the light splitting and converging component and is used for detecting second optical information of the position where the position sensitive detector is located; the second optical information is used for performing an energy dispersive X-ray absorption fine structure (EDXAFS) test on the material sample to be tested, and EDXAFS data is obtained.
Optionally, the light splitting and converging component 35 includes: the beam splitting crystal is bent to split the light rays with different wavelengths according to different exit angles, and the light rays are irradiated to the position sensitive detector 36. The device further comprises: a first slit 34 located between the light splitting and converging component 35 and the carrying component 33, wherein the first slit 34 is used for removing scattered light. The device further comprises: a second slit 32 located between the synchrotron radiation light source 31 and the carrier assembly 33, wherein the second slit 32 is used for card light to obtain an incident beam with a required size.
In the device according to the embodiment of the present invention, the device may be configured to have 11 energy dispersion detectors 27, the angle range is 16.98-68.27 °, and the interplanar spacing range of the X-ray diffraction test is 16.98 ° -68.27 °
Figure BDA0002140396550000081
Referring to fig. 4, fig. 4 is a schematic diagram of another apparatus for analyzing a short-range order structure and a long-range order structure of a material according to an embodiment of the present invention, where, based on the manner shown in fig. 3, the apparatus shown in fig. 4 further includes: a host computer 38, wherein the host computer 38 is connected with the energy dispersion detector 37 and the position sensitive detector 36 respectively, and is used for performing an energy dispersion X-ray diffraction test on the material sample 30 to be tested based on the first optical information and performing an energy dispersion X-ray absorption fine structure test on the material sample 30 to be tested based on the second optical information.
Optionally, the host computer 38 is further configured to perform an X-ray fluorescence test on the material sample 30 to be tested based on the first optical information. Specifically, the method for the host computer to perform the X-ray fluorescence test on the material sample to be tested includes: plotting the energy and the intensity of the X-ray photons detected by at least two energy dispersion detectors; based on the characteristic that the X-ray fluorescence does not change with the detection angle and the detection result of the energy dispersion detector 37, a fluorescence map and a diffraction map are obtained.
In the device according to the embodiment of the present invention, in order to ensure consistency of the light angle of the incident material sample 30 to be tested in the EDXRD test process, the device according to the embodiment of the present invention is different from the mode shown in fig. 2 in that the material sample 30 to be tested is placed in front of the incident light path, and the light beam irradiates the light splitting and converging part 35 after passing through the material sample 30 to be tested, so as to detect the second light information through the position sensitive detector 36, perform the EDXAFS test, and further obtain the EDXAFS data. In order to avoid the influence of the scattered light of the material sample 30 to be tested on the EDXAFS test, a first slit 34 is provided between the material sample 30 to be tested and the light splitting and converging part 35 for blocking off the scattered light. A series of X-ray energy dispersive detectors 37 are provided at specific angular 2 theta positions lateral to the optical path for detecting the diffraction data of EDXRD.
The light beam emitted from the synchrotron radiation light source 31 is a continuous spectrum, has a plurality of wavelength λ values, and different wavelength values correspond to different diffraction angles based on the bragg diffraction law, so a plurality of energy dispersion detectors 37 are provided in series, and correspond to different angles 2 θ respectively. Fig. 3 and 4 only show one energy dispersion detector 37 with a specific angle 2 θ, and the number of energy dispersion detectors 37 and the corresponding angle 2 θ may be set as required, which is not particularly limited in the technical solution of the present invention.
By analyzing the EDXRD test part, the calculation formula of EDXRD can be expressed as follows according to Bragg diffraction law:
Figure BDA0002140396550000091
wherein E is the incident X-ray photon energy, h is the Planck constant, c is the light beam, and 2 theta is the angle of the incident light and the emergent light, therefore, the energy dispersion detector 37 is placed at the position of the fixed angle 2 theta, and the energy E of the diffracted photons is collected, so that the corresponding structural information can be obtained.
According to the formula (2), when the diffraction angle 2 θ of the light is fixed, the energy E of the detected photon and the distance d between the mirror surfaces are determinedhklFor conventional EDXRD testing, due to the large energy bandwidth △ E of incident light, it is common to place the energy detector at an angle that has a large enough dhklA range of values. Then, when EDXAFS-EDXRD test is used in combination with synchrotron radiation, one angle-placed energy-dispersive detector 37 intelligently detects a partial range of interplanar spacing values due to the narrow beam energy bandwidth used in the EDXAFS test. Therefore, the energy dispersion detector 37 is placed in a plurality of angles in the device according to the embodiment of the invention, and the following brief calculation is performed based on the energy dispersion detector.
In the embodiment of the present invention, the synchrotron radiation light source 31 may be an undulator light source, a torsion pendulum light source, or a bent iron light source. Specifically, a continuous spectrum light beam is generated by an undulator light source, or a continuous spectrum light beam is generated by a torsion pendulum light source, or a continuous spectrum light beam is generated by a bent iron light source.
Currently, there are EDXAFS test line stations in the world, exemplified by ID24 line station for RSRF, which can provide an incident beam of energy bandwidth of about 1keV in a tap-undulator mode. Taking the energy battery material as an example, common elements include iron, cobalt, nickel, manganese, etc., for example, the K absorption edge of iron element is 7.111 keV. Based on this, assuming that the energy of incident photons is 7-8 keV when performing an EDXAFS-EDXRD combined experiment, a curve of interplanar distances that can be covered by placing the energy dispersion detector 37 at different angles 2 θ is drawn according to formula (2), as shown in fig. 5.
Referring to FIG. 5, FIG. 5 is a graph of the angle of a detector versus the measured interplanar spacing according to an embodiment of the present invention, and based on FIG. 5, this result shows that if coverage is desired
Figure BDA0002140396550000102
The detector D1-D11 needs to be placed at 11 angles, that is, a total of 11 energy dispersive detectors 37 corresponding to different angles 2 θ are needed, and the angle values and measurable interplanar spacing ranges for these detectors are listed in table 1.
TABLE 1 position and measurement method of X-ray energy dispersive detector
Figure BDA0002140396550000101
As can be seen from the above description, the apparatus according to the embodiment of the present invention can achieve microsecond time resolution; compared with the traditional EDXAFS test, the device disclosed by the embodiment of the invention has the advantages that the position of the material sample 30 to be tested is moved to the front of the focusing mirror, so that the interference of the scattered diffraction signals on the XAFS signals can be removed by using the first slit 34, the interference signals are difficult to remove when the material sample 30 to be tested is behind the focusing mirror, the energy bandwidth of the X-ray beam actually irradiating the material sample 30 to be tested is larger after the position of the material sample 30 to be tested is moved forwards, and the EDXRD test is facilitated.
Another benefit of EDXRD is that X-ray fluorescence (XRF) can be collected by energy-dispersive detector 37 at the same time that X-ray diffraction information is collected, and XRF can be used to determine elemental information in material sample 30. Since the XRF signal is emitted isotropically, while the EDXRD diffraction signal is closely related to the diffraction angle, the XRF signal and EDXRD can be distinguished by comparing the data collected by the detectors at different positions, and the implementation principle is shown in fig. 6.
Referring to fig. 6, fig. 6 is a graph of energy and intensity of X-ray photons detected according to an embodiment of the present invention, in which the detection results of two energy-dispersive detectors 37 with angles 2 θ being 30 ° and 2 θ being 50 ° are respectively placed, and the energy and intensity of the detected X-ray photons are plotted, as can be seen from the characteristic that X-ray fluorescence does not change with the detection angle, in fig. 6, F1、F2And F3The three peaks correspond to fluorescence spectrum signals, and the rest are diffraction peak signals. The peak position of the fluorescence spectrum does not change with the detection angle, and based on this characteristic, a fluorescence spectrum and a diffraction spectrum can be obtained according to the detection result of the energy dispersion detector 37.
As described above, since the energy bandwidth of the incident photons of the synchrotron radiation is insufficient, a plurality of energy-dispersive detectors 37 need to be provided. In this arrangement, the resolving power of the energy dispersive detector 37 is around 100 eV.
In the embodiment of the present invention, the light splitting and converging component 35 may be a curved light splitting crystal. By setting the position and the angle of the bent beam splitting crystal, part of optical wave bands suitable for XAFS test in the light beam can pass through, and the energy bandwidth of the light beam passing through the bent beam splitting crystal is narrowed so as to facilitate the XAFS test.
In other ways, the synchrotron radiation light source 31 may also be a synchrotron radiation wiggler (wiggler) light source, for example, a superconducting wiggler light source can provide a wider energy bandwidth, the energy range is 5-50keV, and the diffraction test can be performed more efficiently by using the light source, at this time, as shown in fig. 7, fig. 7 is another detector angle and measured interplanar spacing curve provided by the embodiment of the present invention, and when the 5-50keV light source is used, a detector can be covered only when placed at 20 ° and the measured interplanar spacing curve is used
Figure BDA0002140396550000111
The two or three detectors can be arranged in the vicinity of 20 degrees, the fluorescence signal and the diffraction signal can be distinguished, and the signal-to-noise ratio can be improved by correcting and then superposing the information collected by different detectors.
Based on the foregoing embodiment, another embodiment of the present invention further provides a method for analyzing a short-range ordered structure and a long-range ordered structure of a material, in which the method uses the apparatus described in the foregoing embodiment to analyze the short-range ordered structure and the long-range ordered structure of the material.
The method provided by the embodiment of the invention adopts the device provided by the embodiment, and EDXAFS-EDXRD combined test can be realized.
The patent technology of the invention relates to a method for simultaneously and rapidly analyzing short-range order and long-range order structure information of a material. The invention designs an EDXAFS-EDXRD combined scheme, uses synchrotron radiation white light as a light source, adopts an EDXAFS technology to represent short-range ordered structure information of a material, and adopts EDXRD to represent long-range ordered structure information of the material. The method can realize the representation speed and the time resolution capability of microsecond magnitude, breaks through the bottleneck of the original millisecond magnitude, and provides a scheme for the representation of the dynamic evolution of the material structure.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The method disclosed by the embodiment corresponds to the device disclosed by the embodiment, so that the description is simple, and the relevant points can be described by referring to the corresponding part of the device.
It is further noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such article or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in an article or device that comprises the element.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. An apparatus for analyzing short range order and long range order structures of a material, comprising:
the bearing assembly is used for loading a material sample to be tested;
the synchronous radiation light source is used for emitting light beams with continuous spectrums so as to irradiate the material sample to be detected;
the system comprises a plurality of energy dispersion detectors, a plurality of optical sensors and a plurality of optical sensors, wherein detection axes of the energy dispersion detectors have different angles with the irradiation direction of the light beam, and the energy dispersion detectors are used for detecting first optical information at positions; the first optical information is at least used for carrying out an energy dispersive X-ray diffraction test on the material sample to be tested;
the light splitting and converging component is positioned in the irradiation range of the light beam and is used for splitting the light beam transmitted by the material sample to be detected and irradiating the light beam to the position sensitive detector, and the position sensitive detector is positioned behind the light splitting and converging component and is used for detecting second optical information of the position where the position sensitive detector is positioned; the second optical information is used to perform an energy dispersive X-ray absorption fine structure test on the sample of material to be tested.
2. The apparatus according to claim 1, wherein the light splitting and converging means comprises: and bending the spectroscopic crystal.
3. The apparatus of claim 1, further comprising: and the first slit is positioned between the light splitting and converging component and the bearing component and is used for removing scattered light.
4. The apparatus of claim 1, further comprising: and the second slit is positioned between the synchrotron radiation light source and the bearing component and used for blocking light to obtain an incident beam with a required size.
5. The apparatus of claim 1, wherein said apparatus has 11 of said energy-dispersive detectors, said angle is in the range of 16.98 ° -68.27 °, and the interplanar spacing of the X-ray diffraction test is in the range of
Figure FDA0002467286630000011
6. The apparatus of any of claims 1-5, further comprising: the host computer is respectively connected with the energy dispersion detector and the position sensitive detector and is used for carrying out energy dispersion X-ray diffraction test on the material sample to be tested based on the first optical information and carrying out energy dispersion X-ray absorption fine structure test on the material sample to be tested based on the second optical information.
7. The apparatus of claim 6, wherein the host computer is further configured to perform an X-ray fluorescence test on the sample of material to be tested based on the first optical information.
8. The apparatus of claim 7, wherein the host computer performs an X-ray fluorescence test method with respect to the sample of material to be tested, comprising:
plotting the energy and the intensity of the X-ray photons detected by at least two energy dispersion detectors;
and acquiring a fluorescence spectrum and a diffraction spectrum based on the characteristic that the X-ray fluorescence is not changed along with the detection angle and the detection result of the energy dispersion detector.
9. The apparatus of claim 1, wherein the synchrotron radiation light source is: undulator light sources, or twister light sources, or bent iron light sources.
10. A method for analyzing short-range order structures and long-range order structures of a material, characterized in that the short-range order structures and long-range order structures of the material are analyzed using the apparatus according to any one of claims 1 to 9.
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