CN115684224A - Test platform and use method thereof - Google Patents

Test platform and use method thereof Download PDF

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Publication number
CN115684224A
CN115684224A CN202110852762.4A CN202110852762A CN115684224A CN 115684224 A CN115684224 A CN 115684224A CN 202110852762 A CN202110852762 A CN 202110852762A CN 115684224 A CN115684224 A CN 115684224A
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Prior art keywords
sample
detector
tested
test platform
ray
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陈雨
高振华
储胜启
张贵凯
殷子
尹春霞
张静
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Institute of High Energy Physics of CAS
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Institute of High Energy Physics of CAS
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

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Abstract

The invention relates to a test platform and a using method thereof. The test platform comprises a sample bearing mechanism, an X-ray light source, a first signal acquisition mechanism and a second detector. The sample bearing mechanism is used for bearing a sample to be tested; the X-ray light source is used for emitting incident X-rays; the first signal acquisition mechanism comprises a first detector, the projections of the X-ray light source, the sample bearing mechanism and the first detector on the horizontal plane are sequentially arranged along a first direction, and the first detector is used for receiving an X-ray diffraction signal generated by a sample to be tested; the second detector is used for receiving the X-ray fluorescence signal generated from the sample to be tested. The test platform provided by the invention can obtain the information of the adjacent atomic structure and the long-range ordered structure of the same area of the sample by utilizing the incident X-ray emitted by the X-ray light source, thereby essentially revealing the influence mechanism of the evolution process of the atomic structure and the crystal structure of the surface layer of the material on the tissue performance.

Description

Test platform and use method thereof
Technical Field
The invention relates to the technical field of detection equipment, in particular to a test platform and a using method of the test platform.
Background
The synchrotron radiation light source has the advantages of extremely high brightness of the light source, wide frequency spectrum, high collimation, short pulse structure and the like, and has wide application in the basis and application research of physics, chemistry, life science, material science and the like. And with the rapid development of synchrotron radiation experimental technology, material scientists have obtained powerful tools for studying fine structures of substances on an atomic scale. The synchronous radiation X-ray diffraction (XRD) sensitivity is high, and the long-range ordered structure information of the crystal structure in the sample can be detected accurately; the synchrotron radiation X-ray absorption fine structure (XAFS) has the characteristic of short-range order sensitivity, can mainly obtain local short-range order structure information such as the type, the atomic distance, the coordination number, the disorder degree and the like of adjacent coordination atoms, combines the two technologies for application, can comprehensively obtain the short-range order structure information and the long-range order structure information of a substance, and provides technical support for establishing the incidence relation between the atomic distribution and the crystal structure of material elements.
In the prior art, the XRD technology and the XAFS technology are respectively utilized to research the change of a local structure around Co ions in the discharging process of a cathode catalyst of a borohydride fuel cell, in-situ XRD does not detect the generation of a new phase, in-situ XAFS detects the existence of an oxygen vacancy, and a new oxygen reduction reaction mechanism based on the oxygen vacancy is provided. But the in-situ XAFS and XRD are not completed in the same experiment, and all information of the sample in the state of the same position when the tissue structure is changed cannot be accurately obtained.
Meanwhile, the prior art discloses an experimental device capable of realizing synchronous radiation grazing incidence XAFS, which can collect XAFS information on the surface layers and at different depths of samples such as thin film samples, multilayer films, blocks and the like, but the device lacks synchronous representation of XRD signals.
Therefore, a test platform and a use method of the test platform, which are applicable to the combination of the XRD technology and the XAFS technology, are urgently needed to solve the technical problem that the long-range ordered structure information and the short-range ordered structure information when the tissue structure of the sample changes in the same position state cannot be accurately obtained.
Disclosure of Invention
The invention aims to provide a test platform to solve the technical problem that long-range ordered structure information and short-range ordered structure information when the organizational structure of a film sample is changed under the same position state cannot be accurately obtained.
In order to achieve the above object, a first aspect of the present invention provides a test platform, comprising:
the sample bearing mechanism is used for bearing a sample to be tested;
an X-ray light source for emitting incident X-rays which can enter the sample to be tested;
the first signal acquisition mechanism comprises a first detector, the projections of the X-ray light source, the sample bearing mechanism and the first detector on the horizontal plane are sequentially arranged along a first direction, and the first detector is used for receiving an X-ray diffraction signal generated by the sample to be tested;
and the second detector and the sample bearing mechanism are arranged along a second direction, the first direction and the second direction form an included angle, and the second detector is used for receiving an X-ray fluorescence signal generated from the sample to be tested.
Optionally, the sample support mechanism comprises:
the sample stage is used for bearing the sample to be tested;
the first rotary driving part is connected with the sample stage and used for driving the sample stage to rotate so as to adjust an included angle between the incident X-ray and the surface of the sample to be tested.
Optionally, the sample support mechanism further comprises:
and the sample lifting adjusting piece is connected with the sample table and is used for adjusting the height of the sample table.
Optionally, the first signal collecting mechanism further includes:
and the second rotary driving part is connected with the first detector and is used for driving the first detector to rotate so as to enable the first detector to acquire X-ray diffraction signals at different positions in space.
Optionally, the rotation axis of the first detector is parallel to the second direction, and the rotation axis of the first detector coincides with the rotation axis of the sample stage.
Optionally, the first signal collecting mechanism further includes:
the second rotary driving piece and the first detector are connected through the connecting frame.
Optionally, the first signal collecting mechanism further includes:
and the balancing weight is connected with the second rotary driving part, and the balancing weight and the first detector are respectively positioned on two opposite sides of an output shaft of the second rotary driving part.
Optionally, the test platform further includes a supporting mechanism, and the supporting mechanism includes:
the sample bearing mechanism, the first signal acquisition mechanism and the second detector are all arranged on the rack;
the three-dimensional adjusting table is used for adjusting the position of the rack in the first direction and the vertical direction and driving the rack to rotate around the vertical direction.
The invention further aims to provide a using method of the test platform, so as to solve the technical problem that long-range ordered structure information and short-range ordered structure information when the tissue structure of a sample is changed in the same position state cannot be accurately obtained.
To achieve the purpose, the second aspect of the invention adopts the following technical scheme:
a method of using a test platform, for use with a test platform as described above; the using method comprises the following steps:
placing a sample to be tested on a sample bearing mechanism;
the X-ray light source emits X-rays, the first detector receives an X-ray diffraction signal generated by a sample to be tested, and meanwhile, the second detector receives an X-ray fluorescence signal generated by the sample to be tested.
Optionally, the test platform further comprises a sample stage, a first rotary driving member connected to the sample stage, and a second rotary driving member connected to the first detector;
the use method further comprises the following steps:
the first rotary driving piece drives the sample table to rotate so as to adjust an included angle between the surface of the sample to be tested and the incident X-ray;
when the surface of the sample to be tested and the incident X-ray keep the same included angle, the second rotary driving piece drives the first detector to rotate, so that the first detector collects X-ray diffraction signals at different positions in space.
Therefore, the test platform provided by the invention can simultaneously obtain the information of the adjacent atomic structure and the long-range ordered structure of the same area of the sample by utilizing the incident X-ray emitted by the X-ray light source, thereby essentially revealing the influence mechanism of the evolution process of the atomic structure and the crystal structure of the surface layer of the material on the tissue performance.
Drawings
FIG. 1 is a top view of a test platform provided by an embodiment of the present invention;
FIG. 2 is a front view of a test platform provided by an embodiment of the present invention;
FIG. 3 is a schematic diagram of a sample under test and incident X-rays according to an embodiment of the present invention;
FIG. 4 is a grazing incidence XRD diffraction pattern obtained using an experimental platform provided by an embodiment of the present invention;
FIG. 5 is an integral plot of grazing incidence XRD obtained using an experimental platform provided by an embodiment of the present invention;
fig. 6 is a grazing incidence XAFS spectrum obtained using the experimental platform provided by an embodiment of the present invention.
In the figure:
1. a sample carrying mechanism; 11. a sample stage; 12. a first rotary drive member; 13. a sample lifting adjusting piece;
2. a first signal acquisition mechanism; 21. a first detector; 22. a second rotary drive; 23. a connecting frame; 231. mounting a rod; 232. a compensation lever; 233. a slide bar; 234. a slider; 24. a balancing weight;
3. a second detector;
4. an X-ray light source;
5. a support mechanism; 51. a frame; 52. a three-dimensional adjusting table; 521. a diffractometer rotating table; 522. a diffractometer horizontal movement stage; 523. a diffractometer vertical mobile station;
6. a front ionization chamber; 7. incident X-rays;
10. and (5) testing the sample.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be further noted that, for the convenience of description, only some but not all of the elements associated with the present invention are shown in the drawings.
In the present invention, the directional terms such as "upper", "lower", "left", "right", "inner" and "outer" are used for easy understanding without making a contrary explanation, and thus do not limit the scope of the present invention.
In the present invention, unless expressly stated or limited otherwise, the recitation of a first feature "on" or "under" a second feature may include the recitation of the first and second features being in direct contact, and may also include the recitation that the first and second features are not in direct contact, but are in contact via another feature between them. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
In the description of the present invention, unless otherwise explicitly specified or limited, the terms "connected," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integral to one another; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The embodiment provides a test platform, which is used for accurately obtaining long-range ordered structure information and short-range ordered structure information when the tissue structure changes under the same position state of a sample.
As shown in fig. 1 and fig. 2, the testing platform provided in this embodiment includes a sample supporting mechanism 1, an X-ray light source 4, a first signal collecting mechanism 2, and a second detector 3, wherein the sample supporting mechanism 1 is used for supporting a sample 10 to be tested, the X-ray light source 4 is used for emitting incident X-rays 7, and the incident X-rays 7 can be emitted into the sample 10 to be tested. The first signal acquisition mechanism 2 comprises a first detector 21, and the first detector 21 is used for receiving an X-ray diffraction signal generated by the sample 10 to be tested, so as to acquire the long-range ordered structure information of the sample 10 to be tested. The second detector 3 is used for receiving the X-ray fluorescence signal generated from the sample 10 to be tested, so as to acquire the short-range ordered structure information of the sample 10 to be tested.
Specifically, the projections of the X-ray light source 4, the sample support mechanism 1, and the first detector 21 on the horizontal plane are sequentially arranged in the X direction (first direction), so that the first detector 21 collects an X-ray diffraction signal. The second detector 3 and the sample support mechanism 1 are arranged along the Y direction (second direction), and the X direction and the Y direction form an included angle, so that the second detector 3 collects X-ray fluorescence signals. Further, the angle between the X-direction and the Y-direction is substantially 90 deg.. It should be noted that the included angle between the X direction and the Y direction is not limited to be substantially 90 °, as long as the second detector 3 can acquire the X-ray fluorescence signal.
The use method of the test platform provided by the embodiment comprises the following steps:
placing a sample 10 to be tested on the sample bearing mechanism 1;
the X-ray source 4 emits X-rays, the first detector 21 receives an X-ray diffraction signal generated from the sample 10 to be tested, and the second detector 3 receives an X-ray fluorescence signal generated from the sample 10 to be tested.
The test platform provided by the embodiment can obtain the information of the adjacent atomic structure and the long-range ordered structure of the same region of the sample by using the incident X-ray 7 emitted by the X-ray light source 4, so that the influence mechanism of the evolution process of the atomic structure and the crystal structure of the surface layer of the material on the tissue performance is essentially disclosed.
It should be noted that the X-ray light source 4 provided in this embodiment may be a synchrotron radiation light source, but is not limited thereto, and may also be another form of X-ray light source 4 as long as it can emit rays.
The following mainly describes the specific structure of the sample support mechanism 1.
As shown in fig. 3, when the incident X-ray 7 enters the sample 10 to be tested, an included angle between the incident X-ray 7 and the surface of the sample 10 to be tested is a grazing incidence angle (α shown in fig. 3) of the incident X-ray 7, and the grazing incidence angle of the incident X-ray 7 determines a depth of the incident X-ray 7 penetrating through the sample, so that structural information of the sample 10 to be tested at different depths of the sample 10 to be tested can be obtained by changing the grazing incidence angle of the incident X-ray 7.
As shown in fig. 1 and 2, in order to adjust the grazing incidence angle of the incident X-rays 7, the sample carrier mechanism 1 includes a sample stage 11 and a first rotary drive 12. The sample stage 11 is used for carrying a sample 10 to be tested. The first rotary driving part 12 is connected with the first rotary driving part 12 of the sample stage 11, and the first rotary driving part 12 is used for driving the sample stage 11 to rotate so as to adjust an included angle between the incident X-ray 7 and the surface of the sample 10 to be tested. Specifically, the rotation axis of the first rotary driver 12 is parallel to the Y direction, and the first rotary driver 12 may be any drive source such as a motor that can rotate the sample stage 11.
Alternatively, a first turntable may be connected to the output shaft of the first rotary drive element 12, and the sample stage 11 may be connected to the rotary drive element via the first turntable. Of course, in other embodiments, the first turntable may not be provided, as long as the first rotary driving member 12 is directly or indirectly connected to the sample stage 11 to drive the sample stage 11 to rotate around the Y direction.
Optionally, a clamp can be arranged on the sample stage 11, and the clamp can clamp and fix the sample to be tested 10; of course, the surface of the sample stage 11 may also be a flat surface, so that the sample 10 to be tested is fixed on the sample stage 11 by adhesion. It should be noted that, the present invention does not limit the specific structure of the sample stage 11, and the skilled person can set the structure according to the actual use requirement, and the change of the specific structure of the sample stage 11 does not depart from the basic principle of the present invention.
Because the incident X-rays 7 may not pass through the sample 10 to be tested due to different thicknesses of different samples, and the like, in order to ensure that the incident X-rays 7 do not be limited by other factors such as the height of the sample 10 to be tested and ensure that the incident X-rays 7 can pass through the sample in the Z direction (vertical direction), the sample loading mechanism 1 further includes a sample lifting adjusting part 13. The sample lifting adjusting piece 13 is connected with the sample table 11 and used for adjusting the height of the sample table 11.
After the sample 10 to be tested is fixed on the sample table 11, the horizontal position calibration and the grazing incidence angle adjustment of the sample 10 to be tested are realized by adjusting the first rotary driving piece 12 and the sample lifting adjusting piece 13.
Preferably, in this embodiment, the first rotary driving member 12 is connected to the sample stage 11 through the sample lifting and lowering adjusting member 13, that is, the output shaft of the first rotary driving member 12 is connected to the sample lifting and lowering adjusting member 13, and the output end of the sample lifting and lowering adjusting member 13 is connected to the sample stage 11. Of course, in other alternative embodiments, the sample lifting adjusting member 13 may be connected to the sample stage 11 via the first rotary driving member 12. The sample lifting adjusting part 13 may be a screw and nut mechanism, etc., and it should be noted that the present invention does not limit the specific structure of the sample lifting adjusting part 13, and the skilled person can set the sample lifting adjusting part according to the actual use requirement, as long as the lifting of the sample stage 11 can be realized, and the change of the specific structure of the sample lifting adjusting part 13 does not deviate from the basic principle of the present invention.
In the experiment, the surface of the sample 10 to be tested is leveled and centered on the incident X-ray 7 by repeatedly adjusting the first rotary driving member 12 and the sample elevation adjusting member 13. After the initial position of the sample 10 to be tested is adjusted, the grazing incidence angle required by the experiment is accurately set through the first rotary driving part 12, so that the accurate measurement of the structure information of different depths on the surface of the sample 10 to be tested is realized.
As shown in fig. 1 and 2, the specific structure of the first signal acquisition section 2 will be mainly described below.
Since the diffraction signals emitted from the sample 10 to be tested are distributed in a certain range of space and the diffraction signals at different positions are different, in order for the first detector 21 to acquire the diffraction signals at different positions, it is preferable that the first signal acquisition mechanism 2 further includes a second rotary drive 22. The second rotary driving element 22 is connected to the first detector 21, and the second rotary driving element 22 is configured to drive the first detector 21 to rotate, so that the first detector 21 collects X-ray diffraction signals at different positions in space. Specifically, the second rotary drive member 22 is any drive source such as a motor that can drive the first detector 21 to rotate.
Preferably, the rotation axis of the first detector 21 is parallel to the Y-direction, and the rotation axis of the first detector 21 coincides with the rotation axis of the sample stage 11. Namely, the motion trail of the first detector 21 is circular, the sample stage 11 is approximately located at the center of the circle, and when the first detector 21 rotates to different positions, the distance between the first detector 21 and the sample 10 to be tested does not change, so that the signal intensity detected by the first detector 21 is consistent, and the accuracy of the detection result is ensured. Preferably, the second rotary drive member 22 is disposed in the Y direction with the first rotary drive member 12.
As shown in fig. 2, the first signal collecting mechanism 2 further includes a connecting frame 23, and the second rotary driving member 22 and the first detector 21 are connected by the connecting frame 23, so that the first detector 21 can rotate around the output shaft of the second rotary driving member 22.
Optionally, the second rotary driver 22 and the first rotary driver 12 are electrically connected to a controller, and the controller can control the first rotary driver 12 and the second rotary driver 22 to work separately or in conjunction. In this embodiment, the controller may be centralized or distributed, for example, the controller may be a single-chip microcomputer or may be formed by a plurality of distributed single-chip microcomputers, and a control program may be run in the single-chip microcomputers to control the above-mentioned components to implement their functions.
Preferably, the attachment frame 23 comprises a mounting rod 231, the mounting rod 231 extending in a direction perpendicular to the axial direction of the output shaft of the second rotary drive member 22. The link frame 23 may further include a position adjusting portion including a slide bar 233 and a slider 234, the slide bar 233 being connected to the mounting bar 231 and being parallel to the mounting bar 231, the slider 234 being connected to the first detector 21. The sliding block 234 is provided with a sliding slot, and the sliding rod 233 is slidably disposed in the sliding slot. By sliding the first detector 21 along the slide bar 233, the spacing between the first detector 21 and the sample 10 to be tested can be adjusted to obtain the desired intensity of the X-ray diffraction signal.
Preferably, the mounting rod 231 and the sliding rod 233 can be connected through a compensation rod 232, and the compensation rod 232 can compensate the distance of the first detector 21 in the Y direction, so that the first detector 21 is opposite to the sample stage 11 in the X direction, and the strength of the signal detected by the first detector 21 is ensured to be strong. It should be noted that the compensating rod 232 may be a length-adjustable component or a length-fixed component, as long as it can satisfy that the first detector 21 and the sample stage 11 are opposite to each other in the X direction.
As shown in fig. 3, the first signal acquisition mechanism 2 may further preferably include a weight block 24. The counterweight 24 is connected to the second rotary drive member 22, i.e. the counterweight 24 is connected to the output shaft of the second rotary drive member 22. The weight block 24 and the first detector 21 are located on opposite sides of the output shaft of the second rotary driving member 22. The weight block 24 can reduce the load of the second rotary driving member 22, and improve the angle control accuracy of the first detector 21 and the position stability of the first detector 21. Preferably, the weight block 24 may be connected to the output shaft of the second rotary driving member 22 through the mounting rod 231 of the connecting frame 23, thereby balancing the total weight on the connecting frame 23. Of course, it should be noted that the weight 24 may also be directly connected to the output shaft of the second rotary driving member 22 or connected to the output shaft of the second rotary driving member 22 through other components.
Alternatively, the first detector 21 may be a Pilatis-100K two-dimensional detector with a minimum exposure time of 0.002S.
In the experiment, under the same grazing incidence angle, the first detector 21 is driven to rotate to different positions through the second rotary driving piece 22, diffraction signals of different positions are received, and then a grazing incidence XRD diffraction ring is obtained.
The contents of the second detector 3 are described below.
Preferably, the second detector 3 is arranged on the side of the sample along the Y direction, and the second detector 3 and the sample to be tested 10 are located on the same horizontal plane, so that interference of diffraction signals generated by a base material of the thin film type sample to be tested 10 can be effectively avoided, and the detection accuracy of the second detector 3 is ensured.
Furthermore, in order to enable the second detector 3 to ascend and descend along with the ascending and descending of the sample table 11, the testing platform may further include an ascending and descending driving member (not shown in the figure), and the ascending and descending driving member is used for driving the second detector 3 to ascend and descend so as to ensure that the second detector 3 and the sample 10 to be tested can be located on the same horizontal plane.
Preferably, the second detector 3 employs a Lytle fluorescence detector.
Preferably, a front ionization chamber 6 is further arranged between the sample stage 11 and the X-ray light source 4, and a fluorescence signal generated by the action of the incident X-ray 7 passing through the front ionization chamber 6 and the sample 10 to be tested is received by the second detector 3, so that an XAFS spectrum of the sample can be obtained. The front ionization chamber 6 can make the incident X-ray 7 excite the working gas in the ionization chamber, and the polar plate collects the ionized electrons to form current (also the incident X-ray 7).
Preferably, the test platform further comprises a supporting mechanism 5, and the supporting mechanism 5 is used for supporting the sample carrying mechanism 1, the first signal acquisition mechanism 2 and the supporting mechanism 5 of the second detector 3. The support mechanism 5 will be mainly described below.
The support mechanism 5 includes a frame 51 and a three-dimensional adjustment table 52. The sample support mechanism 1, the first signal acquisition mechanism 2 and the second detector 3 are all arranged on the rack 51. The gantry 51 is provided on a three-dimensional adjustment stage 52, and the three-dimensional adjustment stage 52 is used to adjust the position of the gantry 51 in the X-direction and the Z-direction, and to drive the gantry 51 to rotate about the Z-direction, so as to accurately adjust the center of the first detector 21 to the center of the incident X-ray 7.
The three-dimensional adjusting stage 52 may include a diffractometer rotating stage 521, a diffractometer vertical moving stage 523, and a diffractometer horizontal moving stage 522 connected in sequence, wherein an output end of the diffractometer rotating stage 521 is connected to the frame 51 to drive the frame 51 to rotate in the Z direction, an output end of the diffractometer horizontal moving stage 522 is connected to the diffractometer rotating stage 521 to drive the diffractometer rotating stage 521 to move in the X direction, and an output end of the diffractometer vertical moving stage 523 is connected to the diffractometer horizontal moving stage 522 to drive the diffractometer horizontal moving stage 522 to move in the Z direction.
It should be noted that, a person skilled in the art can set the specific structures of the diffractometer rotating stage 521, the diffractometer vertical moving stage 523, and the diffractometer horizontal moving stage 522 according to actual use requirements, for example, the diffractometer vertical moving stage 523 and the diffractometer horizontal moving stage 522 may both be a screw-nut mechanism, and the diffractometer rotating stage 521 may be a motor, etc. The connection manner and connection sequence among the diffractometer rotating stage 521, the diffractometer vertical moving stage 523 and the diffractometer horizontal moving stage 522 can be set by those skilled in the art according to the actual use requirements, and these changes on the specific structure of the three-dimensional adjusting stage 52 do not depart from the basic principle of the present invention.
In conducting the experiment, the center of the first detector 21 is first precisely adjusted to the center position of the incident X-ray 7 by adjusting the diffractometer rotating stage 521, the diffractometer vertical moving stage 523, and the diffractometer horizontal moving stage 522 of the three-dimensional adjusting stage 52. The surface of the sample 10 to be tested is made horizontal and centered on the incident X-ray 7 by repeatedly adjusting the first rotary driving member 12 and the sample elevation adjusting member 13. After the initial position of the sample 10 to be tested is adjusted, the first rotary driving element 12 drives the sample stage 11 to rotate so as to adjust the included angle between the surface of the sample 10 to be tested and the incident X-ray 7, that is, the grazing incidence angle required by the experiment is accurately set, so that the second detector 3 receives the structure information of the sample 10 to be tested at different depths on the surface, and the XAFS spectrum of the sample is obtained.
Meanwhile, under the condition that the same grazing incidence angle is kept between the surface of the sample 10 to be tested and the incident X-ray 7, the second rotary driving piece 22 drives the first detector 21 to rotate, so that the first detector 21 collects X-ray diffraction signals at different positions in space, and a grazing incidence XRD diffraction ring is further obtained.
Fig. 4-6 schematically illustrate grazing incidence XRD diffraction rings and grazing incidence XAFS spectra obtained using the assay platforms and methods of using the assay platforms provided by embodiments of the present application, the results including long range crystal structure and neighboring atomic structure information of the sample. The sample is FAPBBr3 perovskite nano-particles, and the grazing incidence angle is 2.5 degrees.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. A test platform, comprising:
the sample bearing mechanism (1) is used for bearing a sample (10) to be tested;
an X-ray light source (4) for emitting incident X-rays (7), said incident X-rays (7) being capable of entering said sample (10) to be tested;
the first signal acquisition mechanism (2) comprises a first detector (21), the projections of the X-ray light source (4), the sample bearing mechanism (1) and the first detector (21) on a horizontal plane are sequentially arranged along a first direction, and the first detector (21) is used for receiving an X-ray diffraction signal generated by the sample (10) to be detected;
the second detector (3) and the sample bearing mechanism (1) are arranged along a second direction, the first direction and the second direction form an included angle, and the second detector (3) is used for receiving an X-ray fluorescence signal generated by the sample (10) to be detected.
2. Test platform according to claim 1, characterized in that the sample carrier means (1) comprises:
the sample stage (11) is used for bearing the sample (10) to be tested;
the first rotary driving part (12) is connected with the sample stage (11), and the first rotary driving part (12) is used for driving the sample stage (11) to rotate so as to adjust an included angle between the incident X-ray (7) and the surface of the sample (10) to be tested.
3. Test platform according to claim 2, characterized in that the sample carrier (1) further comprises:
and the sample lifting adjusting piece (13) is connected with the sample table (11) and is used for adjusting the height of the sample table (11).
4. Test platform according to claim 2 or 3, characterized in that said first signal acquisition means (2) further comprise:
and the second rotary driving part (22) is connected with the first detector (21), and the second rotary driving part (22) is used for driving the first detector (21) to rotate so that the first detector (21) acquires X-ray diffraction signals at different positions in space.
5. Test platform according to claim 4, characterized in that the axis of rotation of the first detector (21) is parallel to the second direction and the axis of rotation of the first detector (21) coincides with the axis of rotation of the sample stage (11).
6. Test platform according to claim 4, characterized in that said first signal acquisition means (2) further comprise:
a connecting frame (23), the second rotary driving member (22) and the first detector (21) are connected through the connecting frame (23).
7. Test platform according to claim 4, characterized in that the first signal acquisition means (2) further comprise:
and the balancing weight (24) is connected with the second rotary driving part (22), and the balancing weight (24) and the first detector (21) are respectively positioned at two opposite sides of an output shaft of the second rotary driving part (22).
8. Test platform according to claim 1, characterized in that it further comprises a support mechanism (5), said support mechanism (5) comprising:
the sample bearing mechanism (1), the first signal acquisition mechanism (2) and the second detector (3) are all arranged on the frame (51);
a three-dimensional adjusting table (52), the frame (51) being disposed on the three-dimensional adjusting table (52), the three-dimensional adjusting table (52) being configured to adjust a position of the frame (51) in the first direction and the vertical direction and to drive the frame (51) to rotate around the vertical direction.
9. A method of using a test platform, for using a test platform according to any one of claims 1 to 8; the using method comprises the following steps:
placing a sample (10) to be tested on a sample bearing mechanism (1);
the X-ray light source (4) emits X-rays, the first detector (21) receives an X-ray diffraction signal generated by a sample (10) to be tested, and the second detector (3) receives an X-ray fluorescence signal generated by the sample (10) to be tested.
10. Method of use of a test platform according to claim 9, wherein the test platform further comprises a sample stage (11) and a first rotary drive (12) connected to the sample stage (11), and a second rotary drive (22) connected to the first detector (21);
the use method further comprises the following steps:
the first rotary driving part (12) drives the sample stage (11) to rotate so as to adjust an included angle between the surface of the sample (10) to be tested and the incident X-ray (7);
when the surface of the sample (10) to be tested and the incident X-ray (7) keep the same included angle, the second rotary driving piece (22) drives the first detector (21) to rotate, so that the first detector (21) collects X-ray diffraction signals at different positions in space.
CN202110852762.4A 2021-07-27 2021-07-27 Test platform and use method thereof Pending CN115684224A (en)

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