An apparatus and method for combined analysis of internal fluorescence and diffraction of materials

Abstract

This invention discloses a combined fluorescence and diffraction analysis device and method for materials, relating to the field of non-destructive testing technology. The device includes an X-ray source, a three-dimensional motion stage, an incident collimator, an exit collimator, an energy-resolved detector, and a detector. The three-dimensional motion stage is used to place the sample. The X-ray source is located on one side of the three-dimensional motion stage, and the detector is located on the other side. The incident collimator is mounted on a first moving mechanism, and the exit collimator and energy-resolved detector are mounted on a second moving mechanism. In imaging mode, the X-ray source emits X-rays, which are then used to perform a CT scan of the sample by the detector. In fluorescence and diffraction modes, the incident collimator moves between the X-ray source and the three-dimensional motion stage via the first moving mechanism, and the exit collimator and energy-resolved detector can move via the second moving mechanism. This invention enables non-destructive testing of the chemical composition and crystal structure combination information within materials.

Description

Technical Field

[0001] This invention relates to the field of nondestructive testing technology, and in particular to a combined analysis device and method for internal fluorescence and diffraction of materials. Background Technology

[0002] Laboratory-grade X-ray fluorescence diffraction (XRF) systems can only acquire chemical composition and phase information at depths of a few micrometers to tens of micrometers on the surface of bulk metallic materials. To obtain information on the chemical composition and phase composition at millimeter-level depths within the internal material, the light source must possess either high photon flux (synchrotron radiation), strong penetrating power (neutron sources), or both (high-energy synchrotron radiation). However, several factors limit the widespread application of these experimental devices: firstly, synchrotron radiation and neutron sources are large-scale facilities with extremely high construction, operation, and maintenance costs, making them extremely scarce and expensive resources even globally; secondly, characterizing and analyzing certain toxic, hazardous, and highly radioactive samples requires complex environments and site conditions, the construction of which typically consumes enormous human and material resources, and is sometimes even impossible to achieve. Summary of the Invention

[0003] The purpose of this invention is to provide a combined fluorescence and diffraction analysis device and method for materials to solve the problems existing in the prior art and realize non-destructive detection of chemical composition and crystal structure information inside materials.

[0004] To achieve the above objectives, the present invention provides the following solution:

[0005] This invention provides a combined fluorescence and diffraction analysis device for materials, comprising an X-ray source, a three-dimensional motion stage, an incident collimator, an exit collimator, an energy-resolved detector, and a detector. The three-dimensional motion stage is used to place the sample. The X-ray source is located on one side of the three-dimensional motion stage, and the detector is located on the other side of the three-dimensional motion stage. The incident collimator is mounted on a first moving mechanism, and the exit collimator and the energy-resolved detector are mounted on a second moving mechanism. In imaging mode, the X-ray source emits X-rays, which are then used to perform a CT scan of the sample via the detector. In fluorescence and diffraction modes, the incident collimator moves between the X-ray source and the three-dimensional motion stage via the first moving mechanism, and the exit collimator and the energy-resolved detector can move via the second moving mechanism.

[0006] Preferably, it also includes a goniometer, which is used to measure the rotation angle of the outgoing collimator and the energy resolution detector.

[0007] Preferably, the detector is a flat panel detector or a line detector.

[0008] Preferably, both the incident collimator and the exit collimator are longitudinal collimators.

[0009] Preferably, the X-ray source is a heavy metal X-ray tube.

[0010] Preferably, after the X-ray emitted by the X-ray source passes through the emission collimator and the exit collimator, the width of the X-ray is 0.1 mm, the height is 20 mm, and the length is 140 mm.

[0011] The present invention also provides an analytical method using a combined internal fluorescence and diffraction analysis device for the material, comprising the following steps:

[0012] Step 1: Place the sample on a three-dimensional motion stage, use imaging mode, turn on the X-ray source, use a detector to perform a CT scan, and then perform three-dimensional reconstruction to identify and locate the inclusions inside the sample.

[0013] Step 2: In fluorescence mode, turn on the X-ray source, and rotate the energy-resolved detector and the output collimator around the center of the three-dimensional motion stage until they are at a 90° position with the X-rays emitted by the X-ray source to perform fluorescence analysis on the sample interior.

[0014] Step 3: Using a diffraction mode and a transmission method, the X-ray source is turned on, and the center of the three-dimensional motion stage of the energy-resolved detector and the output collimator rotates. The energy-resolved detector obtains the scattering signals of the sample at different angles, thereby obtaining the diffraction information inside the material.

[0015] The present invention achieves the following technical effects compared to the prior art:

[0016] This invention uses X-ray computed tomography to identify and locate inclusions inside a sample, and uses an energy-resolved detector to perform in-situ non-destructive fluorescence and diffraction analysis of the material inside the sample, thereby achieving non-destructive detection of the chemical composition and crystal structure combination information inside the material.

[0017] This invention utilizes a heavy metal X-ray tube in a laboratory environment. Due to its high energy and high penetration, it enables the acquisition of information on the chemical composition and crystal structure of internal materials at a millimeter-level depth. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram (imaging mode) of the material internal fluorescence and diffraction combined analysis device of the present invention;

[0020] Figure 2 This is a schematic diagram of the material internal fluorescence and diffraction combined analysis device of the present invention (fluorescence mode);

[0021] Figure 3 This is a schematic diagram (diffraction mode) of the material internal fluorescence and diffraction combined analysis device of the present invention;

[0022] Figure 4 The image shows the fluorescence analysis of the internal cathode material of a ternary lithium battery using the combined internal fluorescence and diffraction analysis device and method of the present invention.

[0023] Figure 5 Fluorescence analysis diagram of the internal negative electrode material of a ternary lithium battery using the combined fluorescence and diffraction analysis device and method of the present invention;

[0024] Figure 6 This is a diffraction analysis diagram of the internal positive electrode material of a ternary lithium battery using the combined fluorescence and diffraction analysis device and method of the present invention.

[0025] Figure 7 This is a diffraction analysis diagram of the internal negative electrode material of a ternary lithium battery using the combined fluorescence and diffraction analysis device and method of the present invention.

[0026] Among them: 1-X-ray source, 2-three-dimensional motion stage, 3-incident collimator, 4-outcrystal collimator, 5-energy resolution detector, 6-flat panel detector, 7-sample, 8-frame. Detailed Implementation

[0027] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0028] The purpose of this invention is to provide a combined fluorescence and diffraction analysis device and method for materials to solve the problems existing in the prior art and realize non-destructive detection of chemical composition and crystal structure information inside materials.

[0029] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0030] Example 1

[0031] like Figures 1 to 3 As shown: This embodiment provides a combined fluorescence and diffraction analysis device for materials, including a frame 8 and an X-ray source 1 (heavy metal tungsten target or uranium target), a three-dimensional motion stage 2, an incident collimator 3, an exit collimator 4, an energy-resolved detector 5, and a detector mounted on the frame 8. The X-ray source 1 is a heavy metal X-ray tube. The three-dimensional motion stage 2 can rotate 360° and is used to place the sample 7. The X-ray source 1 is located on one side of the three-dimensional motion stage 2, and the detector is located on the other side of the three-dimensional motion stage 2. The incident collimator 3 is mounted on a first moving mechanism, and the exit collimator 4 and the energy-resolved detector 5 are mounted on a second moving mechanism. When the imaging mode is used, the X-ray source 1 emits X-rays, which are then used to perform a CT scan of the sample 7 by the detector. When the fluorescence and diffraction modes are used, the incident collimator 3 moves between the X-ray source 1 and the three-dimensional motion stage 2 via the first moving mechanism, and the exit collimator 4 and the energy-resolved detector 5 can move via the second moving mechanism.

[0032] This embodiment also includes a goniometer, which is used to measure the rotation angle of the outgoing collimator 4 and the energy resolution detector 5.

[0033] In this embodiment, the detector is a flat panel detector 6 or a linear array detector (i.e., it can measure the energy spectrum of multiple points at a time), and the energy resolution detector 5 is a dot array detector (i.e., it can only measure the energy spectrum of one point at a time). The energy resolution detector 5 can be selected as an X123 cadmium telluride detector.

[0034] In this embodiment, both the incident collimator 3 and the exit collimator 4 are longitudinal collimators. Both the incident collimator 3 and the exit collimator 4 are used to limit the horizontal divergence of the beam. After the X-ray emitted by the X-ray source 1 passes through the incident collimator and the exit collimator 4, the width of the X-ray is 0.1 mm, the height is 20 mm, and the length is 140 mm.

[0035] In this embodiment, the X-ray source 1 uses characteristic X-rays from a heavy metal target (such as a tungsten target) and performs energy-selective monochromatic processing on the detector. The energy-resolved detector 5 can both acquire fluorescence signals and rotate to detect fluorescence and diffraction signals inside the material. The incident collimator 3 and the exit collimator 4 are used to straighten the diffraction path and obtain better diffraction signals. The flat panel detector 6 can acquire a three-dimensional reconstructed image of the material's interior. The goniometer detects the angle of rotation of the energy-resolved detector 5 around the center of the sample 7, and the three-dimensional motion stage 2 can move up and down, left and right, and forward and backward.

[0036] This embodiment integrates the devices used in the three modes, utilizing the same light source. The imaging mode uses a flat panel detector 6, while the fluorescence and diffraction modes employ an energy-resolved detector 5. In a laboratory environment, based on a heavy metal X-ray tube, due to its high energy and high penetration characteristics, fluorescent X-rays can be excited from the substances inside the sample 7. The fluorescence and diffraction signals inside the sample 7 are then analyzed non-destructively using the energy-resolved detector 5.

[0037] Example 2

[0038] This embodiment provides an analytical method using the combined fluorescence and diffraction analysis device for materials according to Embodiment 1, including the following steps:

[0039] Step 1: Place sample 7 at the center of three-dimensional motion stage 2, adopt imaging mode, turn on X-ray source 1, use flat panel detector 6 to perform CT scan, and then perform three-dimensional reconstruction to identify and locate the inclusions inside sample 7.

[0040] Step 2: Move the three-dimensional motion stage 2, adopt fluorescence mode, turn on the X-ray source 1, and rotate the energy-resolved detector 5 and the output collimator 4 around the center of the three-dimensional motion stage 2 to a position of 90° with the X-ray emitted by the X-ray source 1 to perform fluorescence analysis on the inside of the sample 7. Since the position of the inclusions inside the sample 7 was located by CT using the flat panel detector 6 in the early stage, the chemical element information of the inclusions inside the sample 7 is obtained by moving the position of the sample 7 by the three-dimensional motion platform. Because the X-ray emitted by the X-ray source 1 has passed through the 0.1mm slit of the front collimator and irradiated the center position of the sample 7, and the position of the inclusions inside the sample 7 has been located by CT scan, it is necessary to move the sample 7 by the three-dimensional motion platform in the later fluorescence analysis.

[0041] Step 3: Place sample 7 at the center of three-dimensional motion stage 2, adopt diffraction mode and transmission method, turn on X-ray source 1, energy resolution detector 5 and output collimator 4, rotate the center of three-dimensional motion stage 2, and obtain the scattering signal of sample 7 at different angles through goniometer and energy resolution detector 5, thereby obtaining diffraction information inside the material. In this embodiment, the phase information inside sample 7 can be detected by diffraction mode.

[0042] This embodiment establishes a combined analytical method integrating computed tomography, fluorescence analysis, and phase analysis. It combines X-ray computed tomography with characteristic X-ray diffraction analysis and X-ray fluorescence analysis. First, X-ray computed tomography is used to identify and locate inclusions inside sample 7. Then, in-situ non-destructive fluorescence and diffraction analysis of the internal materials of sample 7 is achieved, thereby improving the comprehensive analytical capabilities of computed tomography.

[0043] Application examples

[0044] The internal fluorescence and diffraction analysis device of Example 1 and the analysis method of Example 2 were used to perform non-destructive testing on the chemical composition and crystal structure of the ternary lithium battery. CT imaging technology was used to identify and locate the positive and negative electrode materials inside the ternary lithium battery. Fluorescence analysis revealed that the positive electrode material contained Mn, Co, and Ni, and the negative electrode material contained Ti. Diffraction analysis identified the positive electrode compound as MCN622 and the negative electrode compound as LTO(Li4Ti5O). 12 ).

[0045] This specification uses specific examples to illustrate the principles and implementation methods of the present invention. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of the present invention. Furthermore, those skilled in the art will recognize that, based on the ideas of the present invention, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. An analytical method employing a combined internal fluorescence and diffraction analysis device for materials, characterized in that: The combined fluorescence and diffraction analysis device for materials includes an X-ray source, a three-dimensional motion stage, an incident collimator, an exit collimator, an energy-resolved detector, and a detector. The three-dimensional motion stage is used to place the sample. The X-ray source is located on one side of the three-dimensional motion stage, and the detector is located on the other side. The incident collimator is mounted on a first moving mechanism, and the exit collimator and the energy-resolved detector are mounted on a second moving mechanism. In imaging mode, the X-ray source emits X-rays, which are then used to perform a CT scan of the sample via the detector. In fluorescence and diffraction modes, the incident collimator moves between the X-ray source and the three-dimensional motion stage via the first moving mechanism, and the exit collimator and the energy-resolved detector can move via the second moving mechanism. The analysis method includes the following steps: Step 1: Place the sample on a three-dimensional motion stage, use imaging mode, turn on the X-ray source, use a detector to perform a CT scan, and then perform three-dimensional reconstruction to identify and locate the inclusions inside the sample. Step 2: In fluorescence mode, turn on the X-ray source, and rotate the energy-resolved detector and the output collimator around the center of the three-dimensional motion stage until they are at a 90° position with the X-rays emitted by the X-ray source to perform fluorescence analysis on the sample interior. Step 3: Using a diffraction mode and a transmission method, the X-ray source is turned on, and the center of the three-dimensional motion stage of the energy-resolved detector and the output collimator rotates. The energy-resolved detector obtains the scattering signals of the sample at different angles, thereby obtaining the diffraction information inside the material.

2. The method of analysis according to claim 1, characterized in that: It also includes a goniometer, which is used to measure the rotation angle of the outgoing collimator and the energy resolution detector.

3. The analytical method using a combined internal fluorescence and diffraction analysis device according to claim 1, characterized in that: The detector is a flat panel detector or a line detector.

4. The analytical method using a combined internal fluorescence and diffraction analysis device according to claim 1, characterized in that: Both the incident collimator and the exit collimator are longitudinal collimators.

5. The analytical method using a combined internal fluorescence and diffraction analysis device according to claim 1, characterized in that: The X-ray source is a heavy metal X-ray tube.

6. The analytical method using a combined internal fluorescence and diffraction analysis device according to claim 1, characterized in that: The X-ray emitted by the X-ray source, after passing through the emission collimator and the exit collimator, has a width of 0.1 mm, a height of 20 mm, and a length of 140 mm.

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