Method for detecting uniformity of internal components of multilayer shielding particle radiation protection composite material

Abstract

The invention discloses a method for detecting the uniformity of internal components of a multi-layer shielding particle radiation protection composite material, which comprises the following steps of: S1, arranging micro-beam collimators in front of an X-ray tube and a detector, focusing X-rays to a micro-beam small focus, and realizing micro-beam fluorescence analysis in the depth direction of the composite material; s2, an automatic scanning area is set, and two-dimensional chemical element distribution characterization in the depth direction is achieved. The method comprises the following steps: performing point-by-point automatic control scanning on a three-dimensional plane of a multilayer shielding particle radiation protection composite film based on a heavy metal tungsten target or uranium target X-ray light tube in a laboratory environment to obtain the component distribution fluorescence intensity in the material, and analyzing the difference of the fluorescence intensity of each point of the two-dimensional plane along the depth direction; therefore, the distribution uniformity of the chemical components of the material in the two-dimensional plane along the depth direction is detected.

Description

Technical Field

[0001] The present invention relates to the technical field of composite material internal component detection technology, in particular to a method for detecting the uniformity of the internal components of a multi-layer shielding particle radiation protection composite material. Background Art

[0002] Currently, the internal compositional uniformity of multilayer shielding filler radiation protection composites is often tested destructively using liquid nitrogen quenching, followed by scanning electron microscopy-energy dispersive spectrometry (SEM-EDS) analysis of the composite cross-section. Although SEM-EDS is useful for determining elemental distribution in microscale samples, this technique requires removing the sample from the object, which is often impossible when using multilayer films. In this context, non-destructive analysis using X-rays, such as submicron computed tomography (CT) or synchrotron radiation-computed tomography (SR-CT), can be performed without sample collection. However, both techniques require complex and expensive facilities, and the microscopic analysis of specific points is not representative of the entire object under examination. Summary of the Invention

[0003] The present invention aims to solve the problem that the internal component uniformity detection of multi-layer shielding filler radiation protection composite materials often adopts destructive detection mode, and provides a method for detecting the internal component uniformity of multi-layer shielding particle radiation protection composite materials.

[0004] In order to achieve the above technical objectives, the technical solution provided by the present invention is: A method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material comprises the following steps: S1: Microbeam collimators are installed in front of the X-ray tube and detector to focus the X-rays to a small microbeam focus, enabling microbeam fluorescence analysis in the depth direction of the composite material; S2: Set up an automated scanning area to achieve two-dimensional characterization of chemical element distribution along the depth direction.

[0005] Furthermore, the X-ray tube adopts a high-energy heavy metal target X-ray tube.

[0006] Specifically, high-energy heavy metal target X-ray tubes offer high energy and high penetration, which can stimulate fluorescent X-rays from materials within a sample. The penetration depth of X-rays in a sample depends on the wavelength and sample composition: shorter wavelengths increase penetration depth, and X-rays from heavier elements penetrate deeper. The smaller the sample's average atomic number (higher light element content), the greater the penetration depth. Therefore, for the same sample, the shorter the target wavelength and the higher the energy, the greater the penetration depth.

[0007] Furthermore, the high-energy heavy metal target is a tungsten target or a uranium target.

[0008] Furthermore, the geometric size of the microbeam collimator is 0.1-0.5 mm×200 mm.

[0009] Furthermore, in S2, the automatic scanning device used for automatic scanning controls the three-dimensional movement of the sample left and right, up and down, and front and back, realizing two-dimensional fluorescence spectrum characterization in the depth direction with a repeatability of 0.001 mm.

[0010] Furthermore, in S2, the motion step is controlled to be 0.1-0.5 mm.

[0011] Furthermore, in S2, the acquisition time of the two-dimensional fluorescence spectrum was set to 10-60 s.

[0012] Furthermore, in S2, thousands of energy spectra are obtained through automated area scanning, and net peak area analysis is performed on the energy spectra. The elemental composition is related to the net peak area, so a two-dimensional distribution diagram of the elemental composition uniformity is drawn to characterize the elemental composition uniformity.

[0013] The present invention has the following beneficial effects: 1. For lossy micro-area detection, the present invention uses a high-energy heavy metal target X-ray tube to perform point-by-point automated control scanning of a two-dimensional plane of a multi-layer shielding particle radiation protection composite material film in a laboratory environment, obtains the fluorescence intensity of the component distribution inside the material, analyzes the difference in fluorescence intensity at each point on the two-dimensional plane, and thus detects the uniformity of the chemical composition distribution of the material within the two-dimensional plane.

[0014] 2. The present invention adopts a high atomic number tungsten target, which has the characteristics of high energy and high penetration, thereby obtaining the chemical composition information of the internal material at a depth of millimeters. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 Schematic diagram of automated detection of uniformity of fluorescence components within a material, where a is the X-ray tube, b is the front collimator, c is the composite material, d is a diagram showing uniform distribution of Bi elements in the flexible film, e is a fluorescence spectrum based on a tungsten target, and f is an energy-resolving detector. Figure 2 Fluorescence spectra based on tungsten target (a) and molybdenum target (b); Figure 3 Large-scale macroscopic X-ray fluorescence spectrometer (XRF) uniformity detection diagram, where (a), (b), and (c) show the uniform distribution of Bi, Sm, and Er elements in the flexible film, respectively; Figure 4 This is the intensity distribution of chemical elements in the depth direction. DETAILED DESCRIPTION

[0016] The following is a clear and complete description of the technical solution of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0017] In addition, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0018] Example 1 like Figure 1 As shown, a method for detecting the uniformity of the internal components of a multi-layer shielding particle radiation protection composite material comprises the following steps: S1: Microbeam collimators are installed in front of the X-ray tube and detector to focus the X-rays to a small microbeam focus, enabling microbeam fluorescence analysis in the depth direction of the composite material. In a specific implementation, the composite material is a Bi2O3-Sm2O3-Er2O3 / NR composite film.

[0019] S2: Set up an automated scanning area to achieve two-dimensional characterization of chemical element distribution along the depth direction.

[0020] In a specific implementation, the X-ray light source uses a high-energy heavy metal target X-ray tube with parameters of (150-200) kV and (1-3) mA. The high-energy heavy metal target X-ray tube has the characteristics of high energy and high penetration, thereby exciting fluorescent X-rays from the material inside the sample. The penetration depth of X-rays in the sample depends on the wavelength of the X-rays and the composition of the sample: the shorter the wavelength, the greater the penetration depth, and the X-rays generated by heavy elements penetrate deeper. The smaller the average atomic number of the sample (the higher the content of light elements), the greater the penetration depth.

[0021] In a specific implementation, the high-energy heavy metal target is a tungsten target or a uranium target. For the same sample, the shorter the wavelength of the target material, the higher the energy and the greater the penetration depth.

[0022] When X-rays penetrate the first and second layers of shielding fillers, there is an absorption fluorescence intensity attenuation effect. However, the thickness of each layer of filler is about 0.3-1 mm, which can be regarded as an infinite thickness substrate. In this way, even if the chemical composition of the first and second layers of shielding fillers is unevenly distributed, it will not affect the fluorescence intensity of the bottom layer.

[0023] In a specific implementation, the geometric size of the microbeam collimator is 0.1-0.5 mm×200 mm.

[0024] In a specific implementation, in S2, the automatic scanning device used for automatic scanning controls the three-dimensional movement of the sample left and right, up and down, and front and back to achieve a two-dimensional fluorescence spectrum representation in the depth direction, such as Figure 3 As shown, the repeatability is 0.001 mm.

[0025] In a specific implementation, in S2, the movement step is controlled to be 0.1-0.5 mm.

[0026] In the specific implementation, in S2, thousands of energy spectra are obtained through automated area scanning, and the net peak area analysis is performed on the energy spectra. The elemental composition is related to the net peak area, so as to draw a two-dimensional distribution map of the elemental composition uniformity to characterize the elemental composition uniformity.

[0027] In a specific implementation, in S2, the acquisition time of the two-dimensional fluorescence spectrum is 20 seconds per point (about 3.5 hours of measurement).

[0028] In a specific implementation, a high atomic number tungsten target is used.

[0029] In the test experiment of this embodiment, a 20×10mm 2 area. The sum of the XRF spectra of all irradiation points can be seen in the figure. Figure 2 (a), where the peaks show all elements identified in the movie, as compared to Figure 2 (b) Using a molybdenum target, only the fluorescence information of the surface element Bi can be observed.

[0030] like Figure 3 (a), (b), and (c) respectively indicate that Bi, Sm, and Er elements are evenly distributed in the flexible film, indicating that Bi2O3, Sm2O3, and Er2O3 particles are evenly distributed in NR.

[0031] like Figure 4 As shown, by automated scanning in the depth direction, the intensity distribution map of chemical elements in the depth direction can be obtained.

[0032] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

[0033] The above specific implementation methods are detailed descriptions of the present invention. It cannot be considered that the specific implementation methods of the present invention are limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, they can make several simple deductions and substitutions without departing from the concept of the present invention, which should be regarded as falling within the scope of protection of the present invention.

Claims

1. A method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material, characterized in that: The steps include: S1: Microbeam collimators are installed in front of the X-ray tube and detector to focus the X-rays to a small microbeam focus, enabling microbeam fluorescence analysis in the depth direction of the composite material; S2: Set up an automated scanning area to achieve two-dimensional characterization of chemical element distribution along the depth direction.

2. The method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material according to claim 1, characterized in that: The X-ray tube adopts a high-energy heavy metal target X-ray tube.

3. The method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material according to claim 2, characterized in that: The high-energy heavy metal target is a tungsten target or a uranium target.

4. The method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material according to claim 1, characterized in that: The microbeam collimator has an adjustable range of 0.1-0.5 mm.

5. The method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material according to claim 1, characterized in that: In S2, the automatic scanning device used for automatic scanning controls the three-dimensional movement of the sample left and right, up and down, and front and back, realizing two-dimensional fluorescence spectrum characterization in the depth direction with a repeatability of 0.001 mm.

6. A method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material according to claim 5, characterized in that: In S2, the motion step size is controlled to be 0.1-0.5 mm.

7. The method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material according to claim 5, characterized in that: In S2, the acquisition time of the two-dimensional fluorescence spectrum was set to 10-60 s.

8. The method for detecting uniformity of internal components of a multi-layer shielding particle radiation protection composite material according to claim 1, characterized in that: In S2, thousands of energy spectra are obtained through automated area scanning, and the net peak area analysis is performed on the energy spectra. The elemental composition is related to the net peak area, so a two-dimensional distribution map of the elemental composition uniformity is drawn to characterize the elemental composition uniformity.

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