An x-ray and electron beam combined testing apparatus
By designing a testing device that combines X-rays and electron beams, the combined use of XAFS and TEM was realized, solving the problem that existing technologies cannot simultaneously obtain the microscopic two-dimensional morphology image and local atomic coordination structure of the sample. This enables testing in the same time and space, obtaining the true two-dimensional morphology image and atomic local coordination structure information of the sample.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SHENZHEN ADVANCED LIGHT SOURCE RESEARCH INSTITUTE (HIGH-END SCIENTIFIC INSTRUMENT SHENZHEN BRANCH OF THE UNIVERSITY REGIONAL TECHNOLOGY TRANSFER & TRANSFORMATION CENTER)
- Filing Date
- 2023-06-25
- Publication Date
- 2026-05-01
AI Technical Summary
Current technologies have failed to achieve true integration of X-ray absorption fine structure spectroscopy (XAFS) and transmission electron microscopy (TEM), making it impossible to obtain microscopic two-dimensional morphology images and local atomic coordination structure information of samples in the same time and space.
Design an X-ray and electron beam coupled testing device, including a transmission electron microscope, an X-ray intensity detection device, an X-ray emitting device, and an X-ray fluorescence receiving device. By setting through holes and sample support components on the main body of the device, the X-ray and electron beam can be coupled to perform X-ray absorption fine structure spectroscopy testing and transmission electron imaging testing.
The X-ray absorption fine structure spectroscopy and transmission electron imaging tests of the sample were performed simultaneously in the same space and time, so as to obtain the true two-dimensional morphology image and atomic local coordination structure information of the sample.
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Figure CN116754593B_ABST
Abstract
Description
An X-ray and electron beam combined testing device Technical Field
[0001] This application relates to the field of testing equipment technology, and in particular to a testing device that combines X-rays and electron beams. Background Technology
[0002] Synchrotron radiation X-ray absorption fine structure spectroscopy (XAFS) is an important method for studying the local atomic coordination structure and chemical valence states of materials. Utilizing the advantages of synchrotron radiation's high brightness and continuously tunable energy source, tests that would take laboratory X-ray absorption spectrometers several hours to complete can be performed in seconds. Furthermore, XAFS offers irreplaceable advantages over X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Transmission electron microscopy (TEM) is an important method for studying the two-dimensional local morphology of materials. Using electron beams with wavelengths shorter than visible and ultraviolet light, it improves microscope resolution, achieving field-of-view imaging with a resolution of 0.2 nm, allowing for the analysis of elemental distribution in samples. It can be applied in research fields such as virology, materials science, nanotechnology, and semiconductor research.
[0003] Combining XAFS with TEM can simultaneously obtain the microscopic two-dimensional morphology and local atomic coordination structure of a sample, as well as the elemental distribution and valence states. However, to date, no scientist has truly achieved a combined XAFS and TEM technique. To meet the analytical needs of materials, environmental, energy, and biomedical fields for simultaneously obtaining two-dimensional morphology images and local atomic coordination structures of samples, there is an urgent need for a combined X-ray absorption spectroscopy and transmission electron microscopy (TEM) testing device to simultaneously perform XAFS and TEM tests on samples and obtain information such as morphology and elemental coordination. Summary of the Invention
[0004] In view of this, the purpose of this application is to overcome the shortcomings of the prior art and provide a testing device for X-ray and electron beam combined.
[0005] To address the aforementioned technical problems, this application provides:
[0006] An X-ray and electron beam coupled testing device includes:
[0007] A transmission electron microscope (TEM) apparatus, comprising a main body and a sample support assembly, wherein the main body has an inner cavity and a first through hole, a second through hole and a third through hole are spaced apart along the circumference of the main body, and a portion of the sample support assembly passes through the first through hole and is disposed within the inner cavity for mounting a sample;
[0008] An X-ray intensity detection device is provided, which includes a gas ionization chamber. The X-ray intensity detection device is disposed outside the main body of the device and faces the second through hole.
[0009] An X-ray emitting device emits X-rays that pass sequentially through the gas ionization chamber and the second through-hole and are directed toward the sample.
[0010] An X-ray fluorescence receiving device, a portion of which is disposed within the inner cavity through the third through-hole and facing the sample, is used to receive characteristic X-rays excited by the sample.
[0011] In addition, the X-ray and electron beam combined testing equipment according to this application may also have the following additional technical features:
[0012] In some embodiments of this application, the X-ray and electron beam combined testing device further includes a light-transmitting element disposed within the second through hole, and the circumferential wall of the light-transmitting element abuts against the hole wall of the second through hole.
[0013] In some embodiments of this application, the X-ray and electron beam coupled testing device further includes a driving component, and the sample support assembly includes a sample rod and a sample holder. The sample holder is disposed in the inner cavity for mounting the sample. One end of the sample rod is connected to the output end of the driving component, and the other end passes through the first through hole and is connected to the sample holder.
[0014] In some embodiments of this application, the sample holder includes a holder body, a connecting component, and a sample stage. The holder body has a first mounting groove adapted to the connecting component and the sample stage, and a second mounting groove adapted to the sample rod. The sample stage is connected to the holder body through the connecting component.
[0015] In some embodiments of this application, the connecting assembly includes a connecting shaft, an elastic element, and a mating element. The groove wall of the first mounting groove has a mounting hole adapted to the connecting shaft. The elastic element and the mating element are both sleeved on the connecting shaft. One end of the mating element has a first abutting portion. The sample stage has a second abutting portion adapted to the first abutting portion. One end of the elastic element abuts against the support body, and the other end abuts against the side of the second abutting portion away from the first abutting portion.
[0016] In some embodiments of this application, the elastic element includes a spring body, a first torsion arm located at one end of the spring body, and a second torsion arm located at the other end of the spring body. The spring body is integrally formed with the first torsion arm and the second torsion arm. The spring body is sleeved on the connecting shaft. The first torsion arm supports and abuts against the bracket body. The second torsion arm supports and abuts against the side of the second abutment portion away from the first abutment portion.
[0017] In some embodiments of this application, the sample holder further includes a sample mounting component, the sample stage has a third mounting groove adapted to the sample mounting component, and the sample mounting component has a plurality of through holes arranged in an array.
[0018] In some embodiments of this application, the X-ray fluorescence receiving device includes an X-ray fluorescence detector and an information acquisition and analysis module. The probe of the X-ray fluorescence detector is disposed in the inner cavity through the third through hole and is oriented toward the sample. The information acquisition and analysis module is electrically connected to the X-ray fluorescence detector.
[0019] In some embodiments of this application, two X-ray fluorescence detectors are provided, and the two X-ray fluorescence detectors are arranged at intervals along the circumference of the main body of the device.
[0020] In some embodiments of this application, the transmission electron microscope apparatus further includes an electron generator and an imaging detector, both of which are disposed within the inner cavity and located on opposite sides of the sample support assembly. The electron generator emits an electron beam toward the sample, and the imaging detector receives the electron beam that passes through the sample.
[0021] Compared to existing technologies, the beneficial effects of this application are:
[0022] This application proposes an X-ray and electron beam coupled testing device, which includes a transmission electron microscope (TEM), an X-ray intensity detector, an X-ray emitting device, and an X-ray fluorescence receiver. The TEM includes a main body and a sample support assembly. The main body has an inner cavity, and the X-ray intensity detector has a gas ionization chamber. By creating a first through-hole, a second through-hole, and a third through-hole at circumferential intervals along the main body, and by inserting a portion of the sample support assembly through the first through-hole into the inner cavity, and mounting the sample on the sample support assembly, the sample is stably mounted within the inner cavity. By setting up the X-ray emitting device and placing the X-ray intensity detector outside the main body facing the second through-hole, the X-rays emitted by the X-ray emitting device can sequentially pass through the gas ionization chamber and the second through-hole to reach the sample. By inserting a portion of the X-ray fluorescence receiver through the third through-hole into the inner cavity and facing the sample, the characteristic X-rays excited by the sample are received, thereby enabling the X-ray absorption fine structure spectroscopy testing of the sample. Simultaneously, the transmission electron microscope (TEM) device can perform transmission electron imaging tests on the sample, realizing the function of conducting transmission electron imaging tests on the sample. The X-ray and electron beam coupled testing equipment provided in this application can perform X-ray absorption fine structure spectroscopy tests and transmission electron imaging tests on the sample at the same time and in the same space, thereby obtaining a true and corresponding two-dimensional morphological image and atomic local coordination structure information of the sample. Attached Figure Description
[0023] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.
[0024] Figure 1 shows a perspective view of an X-ray and electron beam combined testing device in some embodiments of this application;
[0025] Figure 2 shows an enlarged schematic diagram of the structure of part A in Figure 1;
[0026] Figure 3 shows a perspective view of the sample holder in some embodiments of this application;
[0027] Figure 4 shows a perspective view of the sample holder from another angle in some embodiments of this application.
[0028] Explanation of key component symbols:
[0029] 100 - X-ray and electron beam coupled testing equipment; 110 - Transmission electron microscope apparatus; 111 - Apparatus body; 1111 - Inner cavity; 1112 - First through hole; 1113 - Second through hole; 1114 - Third through hole; 112 - Sample support assembly; 1121 - Sample rod; 1122 - Sample holder; 11221 - Holder body; 112211 - First mounting groove; 1122111 - Mounting hole; 112212 - Second mounting groove; 11222 - Connecting assembly; 112221 - Connecting shaft; 112222 - Elastic element; 1122221 - Spring Main body; 1122222-First torsion arm; 1122223-Second torsion arm; 112223-Matching part; 1122231-First abutting part; 11223-Sample stage; 112231-Second abutting part; 112232-Third mounting slot; 11224-Sample mounting part; 112241-Through hole; 113-Electron generator; 114-Imaging detector; 120-X-ray intensity detection device; 121-Gas ionization chamber; 130-X-ray fluorescence receiving device; 131-X-ray fluorescence detector; 140-Light-transmitting element; 150-Driver. Detailed Implementation
[0030] The embodiments of this application are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this application, and should not be construed as limiting this application.
[0031] In the description of this application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application.
[0032] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this application, "multiple" means two or more, unless otherwise explicitly specified.
[0033] In this application, unless otherwise expressly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.
[0034] In this application, unless otherwise expressly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.
[0035] It should be noted that the related technology discloses an experimental method combining XAFS, TEM, Raman, IR, and GC-MS. This method involves sequentially performing in-situ electron microscopy, synchrotron radiation XAFS, IR, and Raman spectroscopy on an in-situ sample cell to obtain TEM, XAFS, Raman, and IR data for the same sample. Simultaneously, GC-MS is used to obtain changes in gas composition during the in-situ experiment, yielding information such as sample particle size, local coordination structure, crystal structure, and molecular adsorption characteristics under in-situ conditions. While this method can obtain in-situ structural information for the same sample, this information is not obtained simultaneously at the same time and location. Collecting different information requires repeated in-situ experiments under different conditions, which may lead to changes in the sample structure and distortion of structural information. Therefore, there is an urgent need to perform XAFS and TEM tests on the same sample simultaneously in the same space to obtain a true and corresponding two-dimensional morphology image and local coordination structure information.
[0036] As shown in Figure 1, an embodiment of this application provides an X-ray and electron beam combined testing device 100, which includes a transmission electron microscope device 110, an X-ray intensity detection device 120, an X-ray emitting device, and an X-ray fluorescence receiving device 130.
[0037] The transmission electron microscope (TEM) apparatus 110 includes an apparatus body 111 and a sample support assembly 112. The apparatus body 111 has an inner cavity 1111, and a first through hole 1112, a second through hole 1113 and a third through hole 1114 are spaced apart along the circumference of the apparatus body 111. A portion of the sample support assembly 112 passes through the first through hole 1112 and is disposed in the inner cavity 1111 for mounting a sample.
[0038] The X-ray intensity detection device 120 has a gas ionization chamber 121. The X-ray intensity detection device 120 is disposed outside the main body 111 of the device and faces the second through hole 1113. X-rays emitted by the X-ray emitting device pass sequentially through the gas ionization chamber 121 and the second through hole 1113 and are directed toward the sample. A portion of the X-ray fluorescence receiving device 130 is disposed within the inner cavity 1111 through the third through hole 1114 and faces toward the sample, for receiving the characteristic X-rays excited by the sample.
[0039] The X-ray and electron beam combined testing equipment 100 provided in this application has a first through hole 1112, a second through hole 1113 and a third through hole 1114 spaced apart along the circumference of the main body 111 of the device, and a part of the sample support assembly 112 is disposed in the inner cavity 1112 through the first through hole 1112 and the sample is mounted on the sample support assembly 112, so as to achieve the function of stably mounting the sample in the inner cavity 1111.
[0040] By setting up an X-ray emitting device and an X-ray intensity detection device 120 facing the second through hole 1113 outside the main body 111, the X-rays emitted by the X-ray emitting device can pass through the gas ionization chamber 121 and the second through hole 1113 in sequence and be directed toward the sample. By inserting a part of the X-ray fluorescence receiving device 130 through the third through hole 1114 and setting it in the inner cavity 1111 and facing the sample, the device can receive the characteristic X-rays excited by the sample, thereby enabling the X-ray absorption fine structure spectrum test of the sample.
[0041] Simultaneously, the transmission electron microscope (TEM) device 110 can perform transmission electron imaging tests on the sample, realizing the function of performing transmission electron imaging tests on the sample. The X-ray and electron beam coupled testing equipment 100 provided in this application can perform X-ray absorption fine structure spectroscopy tests and transmission electron imaging tests on the sample at the same time and in the same space, thereby obtaining a true and corresponding two-dimensional morphological image and atomic local coordination structure information of the sample.
[0042] As shown in Figures 1 and 2, in one embodiment of this application, the X-ray and electron beam combined testing device 100 may optionally include a light-transmitting element 140, which is disposed in the second through hole 1113, and the circumferential wall of the light-transmitting element 140 abuts against the hole wall of the second through hole 1113.
[0043] In this embodiment, by providing a light-transmitting element 140 within the second through-hole 1113, X-rays emitted by the X-ray emitting device can sequentially pass through the gas ionization chamber 121, the light-transmitting element 140, and the second through-hole 1113 before reaching the sample. A sealed connection is achieved by having the circumferential wall of the light-transmitting element 140 abut against the wall of the second through-hole 1113, thereby facilitating the maintenance of a high vacuum environment within the inner cavity 1111.
[0044] For example, the material used for the light-transmitting element 140 may be beryllium, in order to reduce the absorption of X-rays by the light-transmitting element 140, increase the incident light flux, and thereby improve the signal-to-noise ratio.
[0045] As shown in Figures 1 and 2, in one embodiment of this application, optionally, the X-ray and electron beam coupled testing device 100 further includes a driving component 150, and the sample support assembly 112 includes a sample rod 1121 and a sample holder 1122. The sample holder 1122 is disposed in the inner cavity 1111 for mounting the sample. One end of the sample rod 1121 is connected to the output end of the driving component 150, and the other end passes through the first through hole 1112 and is connected to the sample holder 1122.
[0046] In this embodiment, one end of the sample rod 1121 is connected to the output end of the drive member 150, and the other end is passed through the first through hole 1112 and connected to the sample holder 1122. The drive member 150 drives the sample rod 1121 to rotate, so that the sample holder 1122 rotates synchronously with the sample rod 1121, thereby automatically adjusting the angle of the sample holder 1122, and thus realizing the function of automatically adjusting the angle of the sample, so as to perform X-ray absorption fine structure spectroscopy and transmission electron imaging tests on the sample.
[0047] For example, the drive unit 150 can be a rotary motor.
[0048] As shown in Figures 2, 3, and 4, in the above embodiments of this application, optionally, the sample holder 1122 includes a holder body 11221, a connecting component 11222, and a sample stage 11223. The holder body 11221 has a first mounting groove 112211 adapted to the connecting component 11222 and the sample stage 11223, and a second mounting groove 112212 adapted to the sample rod 1121. The sample stage 11223 is connected to the holder body 11221 through the connecting component 11222.
[0049] In this embodiment, a second mounting groove 112212 adapted to the sample rod 1121 is provided on the sample holder 1122 to achieve the function of connecting the sample rod 1121 and the sample holder 1122, so that the sample holder 1122 can rotate synchronously with the sample rod 1121. A first mounting groove 112211 adapted to the connecting component 11222 and the sample stage 11223 is provided on the holder body 11221, and the sample stage 11223 is connected to the holder body 11221 through the connecting component 11222 to achieve the function of connecting the sample stage 11223 and the holder body 11221.
[0050] As shown in Figures 3 and 4, in the above embodiments of this application, optionally, the connecting assembly 11222 includes a connecting shaft 112221, an elastic element 112222, and a mating element 112223. The groove wall of the first mounting groove 112211 is provided with a mounting hole 1122111 adapted to the connecting shaft 112221. The elastic element 112222 and the mating element 112223 are both sleeved on the connecting shaft 112221. One end of the mating element 112223 has a first abutting portion 1122231. The sample stage 11223 has a second abutting portion 112231 adapted to the first abutting portion 1122231. One end of the elastic element 112222 abuts against the support body 11221, and the other end abuts against the side of the second abutting portion 112231 away from the first abutting portion 1122231.
[0051] In this embodiment, a mounting hole 1122111 adapted to the connecting shaft 112221 is formed in the groove wall of the first mounting groove 112211 to achieve the function of connecting the connecting shaft 112221 to the support body 11221. By sleeved on the connecting shaft 112221 with both the elastic member 112222 and the mating member 112223, and with one end of the elastic member 112222 abutting against the support body 11221 and the other end abutting against the side of the second abutting part 112231 away from the first abutting part 1122231, the second abutting part 112231 is clamped against the first abutting part 1122231 under the action of the elastic member 112222, thereby making the sample stage 11223 stably and detachably mounted on the support body 11221.
[0052] As shown in Figures 3 and 4, in the above embodiments of this application, optionally, the elastic element 112222 includes a spring body 1122221, a first torsion arm 1122222 located at one end of the spring body 1122221, and a second torsion arm 1122223 located at the other end of the spring body 1122221. The spring body 1122221 is integrally formed with the first torsion arm 1122222 and the second torsion arm 1122223. The spring body 1122221 is sleeved on the connecting shaft 112221. The first torsion arm 1122222 supports and abuts against the bracket body 11221. The second torsion arm 1122223 supports and abuts against the side of the second abutment portion 112231 away from the first abutment portion 1122231.
[0053] In this embodiment, by sleeved spring body 1122221 on connecting shaft 112221, and supporting and abutting the first torsion arm 1122222 with the bracket body 112221, and supporting and abutting the second torsion arm 1122223 with the side of the second abutting part 112231 away from the first abutting part 1122231, the second abutting part 112231 is clamped and abutted against the first abutting part 1122231 under the action of elastic member 112222, so that the sample stage 11223 is stably and detachably installed on the bracket body 11221. This not only improves the installation stability of the sample, but also allows the sample stage 11223 to be removed from the bracket body 11221 so that the operator can place the sample on the sample stage 11223, thus improving the convenience of sample installation.
[0054] As shown in Figures 3 and 4, in the above embodiments of this application, optionally, the sample holder 1122 further includes a sample mounting component 11224, the sample stage 11223 has a third mounting groove 112232 adapted to the sample mounting component 11224, and the sample mounting component 11224 has a plurality of through holes 112241 arranged in an array.
[0055] In this embodiment, a third mounting groove 112232 adapted to the sample mounting component 11224 is provided on the sample stage 11223 to realize the mounting function of the sample mounting component 11224. The sample mounting component 11224 is used to mount the sample, thereby realizing the mounting function of the sample. By providing multiple through holes 112241 arranged in an array on the sample mounting component 11224, the electron beam emitted by the transmission electron microscope device 110 is avoided, which is beneficial for performing transmission electron imaging tests on the sample.
[0056] As shown in Figures 1 and 2, in one embodiment of this application, optionally, the X-ray fluorescence receiving device 130 includes an X-ray fluorescence detector 131 and an information acquisition and analysis module. The probe of the X-ray fluorescence detector 131 is disposed in the inner cavity 1111 through the third through hole 1114 and is oriented towards the sample. The information acquisition and analysis module is electrically connected to the X-ray fluorescence detector 131.
[0057] In this embodiment, the probe of the X-ray fluorescence detector 131 is disposed in the inner cavity 1111 through the third through hole 1114 and is positioned towards the sample so that the probe of the X-ray fluorescence detector 131 can receive the characteristic X-rays excited by the sample, thereby realizing the function of X-ray absorption fine structure spectrum testing of the sample.
[0058] By electrically connecting the information acquisition and analysis module to the X-ray fluorescence detector 131, the characteristic X-ray signals excited by the sample received by the X-ray fluorescence detector 131 can be sent to the information acquisition and analysis module for X-ray absorption fine structure spectrum testing and analysis, thereby realizing the function of X-ray absorption fine structure spectrum testing of the sample.
[0059] For example, the X-ray fluorescence detector 131 can be a silicon drift detector, and the information acquisition and analysis module can be composed of a multi-channel digital processor and spectral processing software, etc.
[0060] It should be noted that the X-ray and electron beam coupled testing equipment 100 uses a gas ionization chamber 121 and a silicon drift detector to perform X-ray absorption fine structure spectroscopy testing on the sample.
[0061] Specifically, first, the silicon drift detector and the gas ionization chamber 121 are turned on, and the incident X-ray intensity I0 in the gas ionization chamber 121 and the fluorescence intensity I of the sample elements in the silicon drift detector are recorded. f Using the formula μ=I f / I0 obtains the X-ray absorption coefficient μ of the target element in the sample, thus obtaining the absorption coefficient of X-rays at a specific energy of the element. By continuously changing the energy of the incident X-rays, the curve of the absorption coefficient as a function of the incident X-ray energy can be obtained, i.e., the fine structure spectrum of the sample's X-ray absorption.
[0062] As shown in Figures 1 and 2, in the above embodiments of this application, optionally, two X-ray fluorescence detectors 131 are provided, and the two X-ray fluorescence detectors 131 are arranged at intervals along the circumference of the device body 111.
[0063] In this embodiment, by setting the number of X-ray fluorescence detectors 131 to two and arranging the two X-ray fluorescence detectors 131 circumferentially spaced along the main body 111 of the device, the intensity of the characteristic X-ray signal excited by the sample received by the X-ray fluorescence detectors 131 is increased, thereby improving the accuracy and stability of the detection results, and further enhancing the function of X-ray absorption fine structure spectroscopy testing of the sample.
[0064] As shown in Figure 1, in some embodiments of this application, optionally, the transmission electron microscope (TEM) apparatus 110 further includes an electron generator 113 and an imaging detector 114. Both the electron generator 113 and the imaging detector 114 are disposed within the inner cavity 1111, and are located on opposite sides of the sample support assembly 112. The electron beam emitted by the electron generator 113 is directed towards the sample, and the imaging detector 114 receives the electron beam that passes through the sample. This enables the function of performing transmission electron imaging tests on the sample, thereby obtaining a true and corresponding two-dimensional morphological image of the sample. It should be noted that the TEM apparatus 110 also includes a circulating cooling system, a vacuum system, and a power supply system.
[0065] In summary, this application proposes an X-ray and electron beam coupled testing device 100, which includes a transmission electron microscope (TEM) apparatus 110, an X-ray intensity detection device 120, an X-ray emitting device, and an X-ray fluorescence receiving device 130. The TEM apparatus 110 includes a main body 111 and a sample support assembly 112. The main body 111 has an inner cavity 1111, and the X-ray intensity detection device 120 has a gas ionization chamber 121. By opening a first through hole 1112, a second through hole 1113, and a third through hole 1114 at circumferential intervals along the main body 111, and by passing a portion of the sample support assembly 112 through the first through hole 1112 within the inner cavity 1111, and by mounting the sample on the sample support assembly 112, the function of stably mounting the sample within the inner cavity 1111 is achieved. By setting up an X-ray emitting device and an X-ray intensity detection device 120 facing the second through-hole 1113 outside the main body 111, the X-rays emitted by the X-ray emitting device can pass through the gas ionization chamber 121 and the second through-hole 1113 sequentially and be directed towards the sample. A portion of the X-ray fluorescence receiving device 130 is inserted through the third through-hole 1114 and positioned within the inner cavity 1111, facing the sample, to receive the characteristic X-rays excited by the sample, thus enabling X-ray absorption fine structure spectroscopy testing of the sample. Simultaneously, the transmission electron microscope 110 can perform transmission electron imaging testing on the sample, achieving the function of transmission electron imaging testing. The X-ray and electron beam coupled testing equipment 100 provided in this application can perform X-ray absorption fine structure spectroscopy testing and transmission electron imaging testing on the sample simultaneously and in the same space, thereby obtaining a true and corresponding two-dimensional morphological image and atomic local coordination structure information of the sample.
[0066] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.
[0067] Although embodiments of this application have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting this application. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of this application.
Claims
1. A testing device for X-ray and electron beam coupling, characterized in that, include: A transmission electron microscope (TEM) apparatus, comprising a main body and a sample support assembly, wherein the main body has an inner cavity and a first through hole, a second through hole, and a third through hole are spaced apart along the circumference of the main body; a portion of the sample support assembly passes through the first through hole and is disposed within the inner cavity for mounting a sample; and an X-ray intensity detection device having a gas ionization chamber, wherein the X-ray intensity detection device is disposed outside the main body and faces the second through hole. An X-ray emitting device emits X-rays that sequentially pass through the gas ionization chamber and the second through-hole towards the sample. An X-ray fluorescence receiving device, a portion of which is disposed within the inner cavity through the third through-hole and oriented towards the sample, is used to receive characteristic X-rays excited by the sample. The X-ray and electron beam coupled testing equipment also includes a driving component. The sample support assembly includes a sample rod and a sample holder. The sample holder is disposed within the inner cavity for mounting the sample. One end of the sample rod is connected to the output end of the driving component, and the other end passes through the first through-hole and connects to the sample holder. The sample holder includes a holder body, a connecting component, and a sample stage. The holder body has a first mounting groove adapted to the connecting component and the sample stage, and a second mounting groove adapted to the sample rod. The sample stage is connected to the support body via the connecting assembly. The connecting assembly includes a connecting shaft, an elastic element, and a mating element. The groove wall of the first mounting groove has a mounting hole adapted to the connecting shaft. The elastic element and the mating element are both sleeved on the connecting shaft. One end of the mating element has a first abutment portion, and the sample stage has a second abutment portion adapted to the first abutment portion. One end of the elastic element abuts against the support body, and the other end abuts against the side of the second abutment portion away from the first abutment portion. The elastic element includes a spring body, a first torsion arm located at one end of the spring body, and a second torsion arm located at the other end of the spring body. The spring body is integrally formed with the first torsion arm and the second torsion arm. The spring body is sleeved on the connecting shaft. The first torsion arm supports and abuts against the support body, and the second torsion arm supports and abuts against the side of the second abutment portion away from the first abutment portion.
2. The X-ray and electron beam combined testing equipment according to claim 1, characterized in that, The X-ray and electron beam combined testing equipment also includes a light-transmitting element, which is disposed in the second through hole, and the circumferential wall of the light-transmitting element abuts against the hole wall of the second through hole.
3. The X-ray and electron beam combined testing equipment according to claim 1, characterized in that, The sample holder also includes a sample mounting component. The sample stage has a third mounting groove that is adapted to the sample mounting component. The sample mounting component has multiple through holes arranged in an array.
4. The X-ray and electron beam combined testing equipment according to claim 1, characterized in that, The X-ray fluorescence receiving device includes an X-ray fluorescence detector and an information acquisition and analysis module. The probe of the X-ray fluorescence detector is disposed in the inner cavity through the third through hole and is oriented towards the sample. The information acquisition and analysis module is electrically connected to the X-ray fluorescence detector.
5. The X-ray and electron beam coupled testing equipment according to claim 4, characterized in that, Two X-ray fluorescence detectors are provided, and the two X-ray fluorescence detectors are arranged at intervals along the circumference of the main body of the device.
6. The X-ray and electron beam coupled testing apparatus according to any one of claims 1 to 5, characterized in that, The transmission electron microscope apparatus further includes an electron generator and an imaging detector, both of which are disposed within the inner cavity and located on opposite sides of the sample support assembly. The electron generator emits an electron beam toward the sample, and the imaging detector receives the electron beam that passes through the sample.
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