Element detection device
By adjusting the light spot using a magnetized collimation module and collimator in a vacuum environment, combined with temperature control and a high-precision detector, the problems of weak detection signal and high scattering background in X-ray spectroscopy analysis devices were solved, enabling rapid and high-precision elemental composition detection.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- INST OF MICROELECTRONICS CHINESE ACAD OF SCI LTD
- Filing Date
- 2026-02-11
- Publication Date
- 2026-04-21
AI Technical Summary
Existing X-ray spectroscopy analysis devices face challenges in achieving high-precision and high-stability detection. Oxygen and nitrogen in the air strongly absorb low-energy characteristic X-rays, resulting in weak detection signals. The primary beam has a large divergence angle and a high scattering background, affecting the signal-to-noise ratio and spatial resolution. Heat accumulation in the detector leads to energy drift.
An element detection device was designed, which uses an X-ray generator, sample stage and detection components in a vacuum shell. A magnetic field is generated by a magnetized collimation module to prevent interference from ambient rays. The collimation plate adjusts the spot size and divergence angle. The temperature controller maintains stability. Combined with beryllium, diamond or silicon nitride windows and silicon drift detector, it can achieve rapid, high-precision non-destructive testing.
It enables rapid, high-precision, and non-destructive online detection of sample elemental composition, reduces environmental radiation interference, improves signal-to-noise ratio and spatial resolution, and ensures the stability of long-term quantitative analysis.
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Figure CN121899175A_ABST
Abstract
Description
Technical Field
[0001] This disclosure relates to the field of X-ray detection technology, and more specifically, to an element detection device. Background Technology
[0002] X-ray spectroscopy is an important non-destructive testing method for the composition of materials, and it has been widely used in materials science, geological exploration, environmental protection, and industrial production. X-ray spectroscopy utilizes high-energy X-rays or electron beams to irradiate a sample, exciting the inner-shell electrons of the atoms in the sample. When outer-shell electrons transition to fill inner-shell vacancies, they release characteristic X-rays with specific energies. By detecting and analyzing the energy and intensity of these characteristic X-rays, the types and amounts of elements in the sample can be determined.
[0003] However, existing X-ray spectroscopy analysis devices still face challenges in achieving high-precision and high-stability detection. Various components in the air, especially oxygen and nitrogen, exert a strong absorption effect on characteristic X-rays in the low-energy range, resulting in weak or even undetectable signals, severely limiting their ability to detect light elements. The primary beam generated by the X-ray tube has a certain divergence angle, producing a large spot on the sample and easily generating a significant scattering background, reducing the signal-to-noise ratio and spatial resolution of the analysis. Prolonged bombardment of the detector by high-energy particle beams also generates a large amount of heat; temperature fluctuations can cause energy drift, affecting the long-term stability of quantitative analysis. Summary of the Invention
[0004] To address at least one of the technical problems in the prior art, embodiments of this disclosure provide an element detection device capable of rapid, high-precision, and non-destructive online detection of elemental components in a sample.
[0005] This disclosure provides an element detection device, comprising: a housing having a first accommodating space with a vacuum inside, and a window disposed on the top of the housing; an X-ray generator disposed on the top of the housing, the X-ray generator being adapted to emit X-rays; a sample stage disposed within the first accommodating space and located below the window, the sample stage being adapted to hold a sample, the sample emitting target X-rays by receiving X-rays passing through the window; and a detection component disposed on the sample stage, adapted to receive the target X-rays and determine the elemental composition of the sample, the detection component comprising: a magnetization collimation module having a first opening in its center to allow the target X-rays to pass through, the magnetization collimation module being configured to generate a magnetic field by current supplied by an external power supply device to prevent interference from ambient radiation generated by reflection after the target X-rays irradiate the sidewall of the sample stage.
[0006] According to some embodiments of this disclosure, a second opening is provided at the top of the sample stage and below the window, and a collimator is detachably provided on the second opening to change the spot size and divergence angle of the X-rays from the X-ray generator.
[0007] According to some embodiments of this disclosure, the sample stage has a second accommodating space, and the second accommodating space is provided with: a first support plate extending along the height direction of the sample stage; a second support plate connected to one end of the first support plate and extending along the length direction of the sample stage; and a third support plate connected end to end to the first support plate and the second support plate, and a groove is provided on the third support plate at a position below the second opening to support the sample.
[0008] According to some embodiments of this disclosure, the third support plate is configured as a downwardly sloping surface so that X-rays passing through the collimator can irradiate the sample.
[0009] According to some embodiments of this disclosure, the sample stage includes a temperature controller adapted to regulate the temperature within the first accommodating space.
[0010] According to some embodiments of this disclosure, the detection assembly further includes: a frame, wherein a mounting groove is provided on the side of the frame facing the third support plate to accommodate the magnetization collimation module; a window, disposed in the mounting groove and located on the side of the magnetization collimation module closer to the sample; and a detector, disposed in the mounting groove and located on the side of the magnetization collimation module away from the sample, wherein the detector is adapted to determine the elemental composition of the sample based on target X-rays emitted from the magnetization collimation module.
[0011] According to some embodiments of this disclosure, the distance between the magnetization collimation module and the detector is not less than 1 mm.
[0012] According to some embodiments of this disclosure, the material of the above-mentioned window is any one of beryllium, diamond and silicon nitride; the thickness of the above-mentioned window is 1μm to 50μm.
[0013] According to some embodiments of this disclosure, the diameter of the first opening is 1 mm to 10 mm.
[0014] According to some embodiments of this disclosure, the element detection device further includes a shielding cover, which is fitted over the outside of the housing to shield against the influence of the magnetic field of the external environment.
[0015] According to an embodiment of the element detection apparatus of this disclosure, a first accommodating space with a vacuum is provided inside the housing, and a window is provided at the top of the housing. An X-ray generator is disposed at the top of the housing and is adapted to emit X-rays. A sample stage is disposed within the first accommodating space and located below the window. The sample stage is adapted to hold a sample, which receives X-rays passing through the window and excites target X-rays. A detection component is disposed on the sample stage and is adapted to receive the target X-rays and determine the elemental composition of the sample. The detection component includes a magnetization collimation module. A first opening in the middle of the magnetization collimation module is axially aligned with the detection surface of the detection component to allow the target X-rays to pass through. The magnetization collimation module can generate a magnetic field by providing current through an external power supply, thereby applying a Lorentz force to charged particles that pass through or approach, achieving trajectory deflection, thereby preventing interference from ambient radiation generated by reflection after the target X-rays irradiate the sidewall of the sample stage, and realizing rapid, real-time, high-precision, and non-destructive online detection of elemental composition in solid, powder, or compressed samples. Attached Figure Description
[0016] Figure 1 This is a first-view perspective perspective view of an element detection device according to an illustrative embodiment of the present disclosure;
[0017] Figure 2 This is a second-view perspective perspective view of an element detection apparatus according to an illustrative embodiment of the present disclosure;
[0018] Figure 3 This is a partial perspective view of a detection assembly according to an illustrative embodiment of the present disclosure, showing a window, a magnetization collimation module, and a detector;
[0019] Figure 4 This is a partial side view of a detection assembly according to an illustrative embodiment of the present disclosure, showing a window, a magnetization collimation module, and a detector.
[0020] The meanings of the reference numerals in the attached figure are as follows:
[0021] 1. Shell;
[0022] 11. Window;
[0023] 2. X-ray generator;
[0024] 3. Sample stage;
[0025] 30. Collimated film;
[0026] 31. First support plate;
[0027] 32. Second support plate;
[0028] 33. Third support plate;
[0029] 4. Sample;
[0030] 5. Detection components;
[0031] 51. Magnetization collimation module;
[0032] 510. The first opening;
[0033] 52. Frame;
[0034] 53. Window slats;
[0035] 54. Detector;
[0036] 6. Shielding cover. Detailed Implementation
[0037] The embodiments of the present disclosure will now be described with reference to the accompanying drawings. However, it should be understood that these descriptions are exemplary only and are not intended to limit the scope of the disclosure. In the following detailed description, numerous specific details are set forth to provide a thorough understanding of the embodiments of the present disclosure for ease of explanation. However, it will be apparent that one or more embodiments may be practiced without these specific details. Furthermore, descriptions of well-known structures and techniques are omitted in the following description to avoid unnecessarily obscuring the concepts of the present disclosure.
[0038] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit this disclosure. The terms “comprising,” “including,” etc., as used herein indicate the presence of the stated features, steps, operations, and / or components, but do not exclude the presence or addition of one or more other features, steps, operations, or components.
[0039] All terms used herein (including technical and scientific terms) have the meanings commonly understood by those skilled in the art, unless otherwise defined. It should be noted that the terms used herein are to be interpreted in a manner consistent with the context of this specification, and not in an idealized or overly rigid way.
[0040] When using expressions such as "at least one of A, B, and C," the expression should generally be interpreted in accordance with the meaning commonly understood by a person skilled in the art (e.g., "a system having at least one of A, B, and C" should include, but is not limited to, systems having A alone, having B alone, having C alone, having A and B, having A and C, having B and C, and / or having A, B, and C, etc.). When using expressions such as "at least one of A, B, or C," the expression should generally be interpreted in accordance with the meaning commonly understood by a person skilled in the art (e.g., "a system having at least one of A, B, or C" should include, but is not limited to, systems having A alone, having B alone, having C alone, having A and B, having A and C, having B and C, and / or having A, B, and C, etc.).
[0041] Figure 1 This is a first-view perspective view of an element detection apparatus according to an illustrative embodiment of the present disclosure. Figure 2 This is a second-view perspective perspective view of an element detection apparatus according to an illustrative embodiment of the present disclosure.
[0042] An element detection device provided according to embodiments of this disclosure, such as Figure 1 and Figure 2 As shown, the elemental detection device includes a housing 1, an X-ray generator 2, a sample stage 3, and a detection assembly 5. The housing 1 has a first accommodating space with a vacuum, and a window 11 is provided at the top of the housing 1. The X-ray generator 2 is located at the top of the housing 1 and is used to emit X-rays. The sample stage 3 is located within the first accommodating space and below the window 11. The sample stage 3 is used to hold a sample 4, which emits target X-rays by receiving X-rays passing through the window 11. The detection assembly 5 is located on the sample stage 3 and is used to receive the target X-rays and determine the elemental composition of the sample 4. The detection assembly 5 includes a magnetization collimation module 51, which has a first opening 510 in its center to allow the target X-rays to pass through. The magnetization collimation module 51 is configured to generate a magnetic field through current supplied by an external power supply to prevent interference from ambient radiation reflected after the target X-rays irradiate the sidewalls of the sample stage 3.
[0043] In some illustrative embodiments, the element detection device is initialized before detection begins. Initialization includes vacuuming and temperature stabilization. This initialization is a crucial step to ensure accurate detection results. The external vacuum acquisition and maintenance system is activated to evacuate the pressure within the first containment space to a high vacuum state (≤1×10⁻⁶). -4 Pa), to minimize the scattering and absorption of low-energy X-rays by gas molecules.
[0044] In some illustrative embodiments, the magnetization collimation module 51 generates a magnetic field with a magnetic field strength of 0.3T to 0.5T through current supplied by an external power supply device.
[0045] In this implementation, the magnetization collimation module 51 can be configured as a ring or cylindrical structure surrounding the detection path. A first opening 510 in the center of the magnetization collimation module 51 is axially aligned with the detection surface of the detector 54 (which will be described in detail below) to allow the target X-rays to pass through. The magnetization collimation module 51 can be powered by an external power supply to drive its internal coils or permanent magnet array, generating a directional magnetic field with an intensity of not less than 0.1T. The magnetic field direction is set perpendicular to the axis of the magnetization collimation module 51, thereby applying a Lorentz force to the passing or approaching charged particles, achieving trajectory deflection. This prevents interference from ambient radiation reflected after the target X-rays irradiate the sidewall of the sample stage 3, enabling rapid, real-time, high-precision, and non-destructive online detection of elemental components in solid, powder, or tablet samples. This is suitable for precise elemental component detection in industrial testing, materials analysis, and other scenarios.
[0046] According to an embodiment of this disclosure, the diameter of the first opening 510 is 1 mm to 10 mm.
[0047] In some illustrative embodiments, the direction of the magnetic field is perpendicular to the axial direction of the first opening 510.
[0048] In some illustrative embodiments, the dimensions of the magnetization collimation module 51 can be configured according to detection requirements. The diameter of the first opening 510 can be selected between 1 mm and 10 mm, and the diameter of the first opening 510 is smaller than the effective detection area of the detector 54. The outer diameter of the magnetization collimation module 51 is greater than 10 mm and not less than the effective detection area of the detector 54, and the thickness of the magnetization collimation module 51 can be between 1 mm and 5 mm. Furthermore, the magnetization collimation module 51 can be detachable or replaceable, allowing for the replacement of different aperture sizes or magnetic field strengths to adapt to detection requirements of different energy ranges or spatial resolutions.
[0049] As an example, the magnetization collimation module 51 can employ collimators with various aperture sizes. For applications requiring high spatial resolution for micro-area analysis, collimators of 1mm to 3mm should be used to obtain a smaller illumination spot. For applications involving the detection of uniform samples or requiring high count rates for rapid screening, collimators of 4mm to 10mm should be used.
[0050] In this implementation, the magnetization collimation module 51 is adapted to detect low-energy characteristic X-rays (0.108keV~1.74keV) of light elements. It applies a Lorentz force perpendicular to the direction of motion of the ambient rays (mainly stray electrons, secondary electrons and some scattered X-rays) that are incident on the side wall of the sample stage 3 and reflected by the directional magnetic field established inside it. This causes the trajectory of these charged particles to be deflected, thereby preventing the ambient rays from interfering with the target X-rays passing through the first opening 510 and optimizing the detection of low-energy characteristic X-rays.
[0051] According to an embodiment of this disclosure, a second opening is provided at the top of the sample stage 3 and below the window 11. A collimator 30 is detachably provided on the second opening to change the spot size and divergence angle of the X-rays from the X-ray generator 2.
[0052] As an example, the collimator 30 can be made with various aperture sizes. For applications requiring high spatial resolution for micro-area analysis, a collimator 30 of 1 mm to 3 mm should be used to obtain a smaller illumination spot. For applications involving the detection of homogeneous samples or requiring high count rates for rapid screening, a collimator 30 of 4 mm to 10 mm should be used.
[0053] In some illustrative embodiments, the collimator 30 can generate a directional magnetic field by the current provided by an external power supply device, which is used to directionally filter and collimate the primary and secondary high-energy X-rays emitted by the X-ray generator 2, forming a collimated beam that irradiates the sample 4 on the sample stage 3.
[0054] In some illustrative embodiments, the collimator 30 is installed in the second opening by means of threaded connection or snap-fit, so that the operator can quickly replace it according to the testing requirements.
[0055] In this implementation, X-rays from the X-ray generator 2 pass through the collimator 30 and irradiate the surface of the sample 4. A collimator 30 of 1 mm to 3 mm can reduce the spot size irradiated onto the surface of the sample 4, improving spatial resolution and making it suitable for micro-area analysis. A collimator 30 of 4 mm to 10 mm can allow more X-rays to pass through, increasing signal intensity and making it suitable for rapid screening or uniform sample detection. Simultaneously, the edges of the collimator 30 absorb scattered rays, reducing the scattering background and thus improving the signal-to-noise ratio and accuracy of the detection.
[0056] According to an embodiment of this disclosure, the sample stage 3 has a second accommodating space, within which a first support plate 31, a second support plate 32, and a third support plate 33 are disposed. The first support plate 31 is positioned along the height direction of the sample stage 3 (e.g., along the height direction of the sample stage 3). Figure 2 The second support plate 32 extends along the length of the sample stage 3 (as shown in the Y direction). One end of the second support plate 32 is connected to the first support plate 31, and the second support plate extends along the length of the sample stage 3 (as shown in the Y direction). Figure 2 Extending in the X direction (as shown). The third support plate 33 is connected end to end to the first support plate 31 and the second support plate 32. A groove is provided on the third support plate 33 at a position below the second opening to support the sample 4.
[0057] In some illustrative embodiments, a first support plate 31, a second support plate 32, and a third support plate 33 are disposed within the second accommodating space inside the sample stage 3. The first support plate 31 extends along the height direction of the sample stage 3, and the second support plate 32 is connected to one end of the first support plate 31 and extends along the length direction of the sample stage 3, forming an approximately L-shape. The third support plate 33 is connected end-to-end with the first support plate 31 and the second support plate 32 to form a stable closed frame. A groove is provided on the third support plate 33 at a position corresponding to the lower part of the second opening, and the groove is suitable for accommodating and positioning the sample 4 to be tested.
[0058] In some illustrative embodiments, a displacement stage can be disposed below the third support plate 33. The third support plate 33 can undergo at least one of three-dimensional translation, rotation, or tilting motion under the drive of the displacement stage. The displacement stage greatly enhances the detection flexibility. Through program control, it is possible to perform point-to-point analysis and line-scan analysis on sample 4, thereby obtaining the distribution information of elements at different locations on the sample. For non-uniform sample 4, multi-point measurement using the displacement stage can obtain more representative average composition results.
[0059] In this implementation, the first support plate 31, the second support plate 32 and the third support plate 33 can ensure that the sample 4 is fixed on the central irradiation path of the X-ray, avoiding signal intensity fluctuations or spatial resolution reduction due to positional deviation, and ensuring the repeatability and accuracy of the detection process.
[0060] According to an embodiment of the present disclosure, the third support plate 33 is configured as a downwardly sloping surface to allow X-rays passing through the collimator 30 to irradiate the sample 4.
[0061] In some illustrative embodiments, the third support plate 33 is constructed as a downwardly sloping surface. The slope angle of this surface can be set to 30° to 60° with respect to the second support plate 32, and the specific slope angle is matched and calibrated according to the exit direction of the X-rays passing through the collimator 30 and the receiving orientation of the detection component 5.
[0062] In this implementation, the inclined arrangement of the third support plate 33 helps to direct the target X-rays excited by the sample 4 toward the receiving direction of the detection component 5 with a better path, reducing the absorption and scattering loss of X-rays inside the sample 4, thereby improving the intensity and quality of the detection signal, and ultimately improving the sensitivity and quantitative accuracy of element detection.
[0063] According to an embodiment of this disclosure, the sample stage 3 includes a temperature controller adapted to regulate the temperature within the first accommodating space.
[0064] In this implementation, the temperature controller actively regulates and maintains a stable temperature within the first accommodating space, keeping the operating temperature of the detection component 5 constant. This reduces thermal noise and energy drift caused by temperature fluctuations, ensuring stable energy spectrum peak positions and improving the long-term repeatability and accuracy of quantitative analysis. Simultaneously, a stable ambient temperature reduces minor geometric changes in the sample 4 due to thermal expansion and contraction, preventing X-ray beam shift. Furthermore, controlling the temperature within the first accommodating space helps maintain the stability of the vacuum environment, reducing scattering interference from residual gas molecules' thermal motion on low-energy X-rays. This, in turn, improves the accuracy and reliability of element detection from both the detection signal of the detection component 5 and the measurement environment.
[0065] Figure 3 This is a partial perspective view of a detection assembly according to an illustrative embodiment of the present disclosure, showing a window, a magnetization collimation module, and a detector. Figure 4 This is a partial side view of a detection assembly according to an illustrative embodiment of the present disclosure, showing a window, a magnetization collimation module, and a detector.
[0066] According to embodiments of this disclosure, such as Figure 2 , Figure 3 and Figure 4 As shown, the detection assembly 5 also includes a frame 52, a window 53, and a detector 54. The frame 52 has a mounting groove on its side facing the third support plate 33 to accommodate the magnetization collimation module 51. The window 53 is disposed in the mounting groove and located on the side of the magnetization collimation module 51 closest to the sample 4. The detector 54 is disposed in the mounting groove and located on the side of the magnetization collimation module 51 furthest from the sample 4. The detector 54 is suitable for determining the elemental composition of the sample 4 based on the target X-rays emitted from the magnetization collimation module 51.
[0067] According to embodiments of this disclosure, the window 53 is made of any one of beryllium, diamond, and silicon nitride. The thickness of the window 53 is 1 μm to 50 μm.
[0068] In some illustrative embodiments, the material and thickness of the window 53 are optimized for the detection of light elements. When detecting light elements such as beryllium, carbon, and aluminum, the window 53 is made of silicon nitride and has a thickness of 1 μm. The magnetic field parameters of the window 53 and the magnetization collimation module 51 are coordinated to reduce the absorption of low-energy characteristic X-rays and shield noise interference.
[0069] As an example, detector 54 can be a silicon drift detector (SDD), whose detection surface is made of any one of silicon, perovskite, germanium, zinc cadmium telluride, and cadmium telluride. Silicon drift detectors (SDDs) offer advantages such as high energy resolution, high count rate, and no need for liquid nitrogen cooling, making them suitable for online real-time detection. High energy resolution can effectively distinguish target X-ray peaks with similar energies, avoiding spectral line overlap interference and laying the foundation for accurate spectral interpretation and quantitative analysis.
[0070] In some illustrative embodiments, the detector 54 can be fixed to the mounting slot by means of threads, snaps, or flanges to ensure optical alignment with the magnetization collimation module 51, so that the detection surface of the detector 54 can receive the target X-rays emitted by the magnetization collimation module 51. By reasonably setting the magnetic field strength and direction of the magnetization collimation module 51 and the position between the magnetization collimation module 51 and the detector 54, ambient rays can be deflected out of the detection path corresponding to the first opening 510, thereby preventing ambient rays from entering the detector 54 and interfering with signal acquisition, effectively reducing background noise in the energy spectrum, and improving the signal-to-noise ratio and detection accuracy of the target X-rays, especially when performing high-sensitivity analysis of light elements or low-energy rays.
[0071] In some illustrative embodiments, the X-ray spectrometer is electrically connected to the detector 54. The X-ray spectrometer is suitable for processing and analyzing the received target X-rays and determining the elemental composition of sample 4.
[0072] In this implementation, the window 53 is located on the side of the magnetization collimation module 51 closest to the sample 4, serving as a physical isolation layer. This allows the target X-rays to pass through, optimizing X-ray transmission efficiency and reducing signal attenuation. Simultaneously, it prevents contaminants in the second accommodating space from entering the detector assembly 5, protecting the magnetization collimation module 51 and the detector 54. The directional magnetic field generated by the magnetization collimation module 51 deflects stray electrons and other charged particles generated during the excitation of the sample 4, causing them to be blocked or absorbed before reaching the detector 54, thereby reducing the background noise of the energy spectrum. The filtered and collimated target X-rays are ultimately received by the detection surface of the detector 54 and converted into a detection signal (electrical signal). This layered filtering and reception, by combining the physical protection of the window 53 with the electromagnetic screening of the magnetization collimation module 51, effectively avoids the absorption of low-energy target X-rays. In particular, it improves the detection sensitivity and detection limit of light elements such as sodium (Na), magnesium (Mg), aluminum (Al), silicon (Si), phosphorus (P), and sulfur (S). The magnetization collimation module 51 collimates the divergent primary X-ray beam generated by the target X-rays excited by the sample 4 into a parallel or micro-beam, reducing the scattering background and beam divergence, improving the signal-to-noise ratio and spatial resolution of the detection, and enabling the detector 54 to obtain a purer target X-ray energy spectrum, providing a foundation for the subsequent energy spectrum analyzer to achieve accurate qualitative and quantitative elemental analysis.
[0073] According to embodiments of this disclosure, the distance between the magnetization collimation module 51 and the detector 54 is not less than 1 mm.
[0074] In this implementation, the magnetization collimation module 51 and the detection surface of the detector 54 are kept at least 1 mm apart, which can ensure that the deflected stray electrons and other charged particles have enough space to deflect out of the detection field of view.
[0075] According to embodiments of this disclosure, the element detection device further includes a shielding cover 6. The shielding cover 6 is fitted onto the outside of the housing 1 to shield against the influence of the magnetic field from the external environment.
[0076] As an example, shield 6 can be made of metal materials, such as stainless steel, aluminum alloy or lead.
[0077] In this embodiment, the shielding cover 6 can provide electromagnetic shielding and facilitate grounding. Furthermore, the inner wall of the shielding cover 6 can be coated or lined with lead plates or lead-containing polymers to enhance X-ray shielding protection.
[0078] In some alternative embodiments, the shield 6 may be made of a high-permeability material, such as permalloy or silicon steel sheet. The shield 6 made of a high-permeability material provides a low-resistivity bypass path for the magnetic field of the external environment (such as the geomagnetic field or stray magnetic field of the surrounding equipment), so that most of the external magnetic lines of force are guided and constrained within the wall of the shield 6, rather than penetrating into the first accommodating space within the housing 1.
[0079] Example 1: XRF Multi-Element Detection of Stainless Steel Alloys
[0080] For high-precision quantitative detection of Cr, Ni, Mn, and Fe elements in 304 stainless steel, a 304 stainless steel plate was selected and cut into 50 mm × 50 mm × 3 mm samples. The power was turned on, and the magnetization collimation module 51 used a collimator with a first opening 510, a diameter of 8 mm, an outer diameter of 15 mm, and a thickness of 3 mm. The magnetic field strength was 0.3 T, and the magnetic field direction was perpendicular to the collimation axis. The distance between the magnetization collimation module 51 and the detector 54 was maintained at 1.5 mm to filter out stray particles. The window 53 was made of diamond with a thickness of 1 μm, suitable for the characteristic X-ray energy ranges of Cr (5.41 keV), Ni (7.47 keV), and Mn (5.89 keV). The central beam emitted by the X-ray generator 2 irradiated the sample 4, with an operating voltage of 45 kV and an operating current of 1.2 mA to ensure sufficient excitation of medium- and high-energy elements. The sample 4 was fixed in the groove of the third support plate 33, keeping the sample stage 3 stationary for fixed-point measurement. X-ray generator 2 is activated. Primary X-rays pass through window 11 and collimator 30 and then irradiate the sample perpendicularly, exciting characteristic X-rays in sample 4. Detector 54 collects the characteristic X-rays and transmits them to the energy dispersive spectroscopy analyzer for spectral analysis and elemental content calculation.
[0081] The test results showed that the elemental composition of Cr, Ni, Mn and Fe in 304 stainless steel was accurately measured and consistent with the actual parameters.
[0082] Example 2: EDS detection of Al, Mg, and Si light element distribution in aluminum alloys
[0083] Select an aluminum alloy welded workpiece and cut it into a sample 4 with dimensions of 15mm×15mm×5mm along the direction perpendicular to the weld.
[0084] Upon power-on, the vacuum acquisition and maintenance system evacuates the pressure in the first accommodating space to 1×10⁻⁶. -6 Pa, EDS electron beam excitation requires an ultra-high vacuum environment to avoid collision and scattering of the EDS electron beam with gas molecules, thus ensuring the integrity of the low-energy X-ray signal of light elements.
[0085] The magnetization collimation module 51 uses a collimator with a diameter of 3mm, an outer diameter of 12mm, and a thickness of 2mm for the first opening 510. This allows for both micro-area focusing and signal throughput. The magnetic field strength is set to 0.25T, and the magnetic field direction is perpendicular to the collimation axis. The distance between the magnetization collimation module 51 and the detector 54 is maintained at 1mm to enhance the filtering of stray electrons (secondary electrons generated by electron gun bombardment and backscattered electrons) and avoid interference with the characteristic signals of light elements.
[0086] Window 53 is made of ultrathin silicon nitride material with a thickness of 1μm to minimize the absorption loss of low-energy characteristic rays of Al (1.49keV), Mg (1.25keV), and Si (1.74keV).
[0087] The electron gun accelerates at 15kV, with a beam current of 40nA. The electron beam spot diameter is no greater than 2μm. It focuses on micro-region excitation to avoid interference from the base material composition around the weld. The electron beam bombardment point is aligned with the central axis of the magnetization collimation module 51 to ensure that the excited characteristic X-rays enter the detection optical path efficiently.
[0088] Detector 54 uses an SDD detector with an energy resolution of no more than 130 eV (@5.9 keV), and its low-energy response sensitivity is optimized to improve the ability to capture weak signals of light elements.
[0089] Open the sample chamber door of the first accommodating space, push the sample stage 3 with sample 4 fixed in place into the center of the first accommodating space, ensuring that the weld area is within the electron beam bombardment range, and close the chamber door. Start the sample stage line scan mode, set the scan path along the weld center to one side of the base material (scan length is 5mm), the scan step size is 30μm, and the detection time for each scan point is 100s. The electron gun emits a focused electron beam to bombard the sample scan point, exciting the characteristic X-rays of Al, Mg, and Si elements. After being filtered by window 53 and directionally screened by magnetization collimation module 51 (filtering out stray electrons and scattered rays), the characteristic X-rays are captured by detector 54 and converted into detection signals (electrical signals). The detection signals are transmitted to the X-ray energy dispersive spectroscopy analyzer, which interprets the spectrum in real time and records the elemental content data of each scan point. Linear distribution curves of Al, Mg, and Si elements are generated, clearly showing the elemental content in the central region of the weld. The relative standard deviations for the detection of each element were no greater than 0.4%, with the detection limits for Mg as low as 0.015%, Al at 0.01%, and Si at 0.012%.
[0090] Those skilled in the art will understand that the features described in the various embodiments and / or claims of this disclosure can be combined or combined in various ways, even if such combinations or combinations are not explicitly described in this disclosure. In particular, the features described in the various embodiments and / or claims of this disclosure can be combined and / or combined in various ways without departing from the spirit and teachings of this disclosure. All such combinations and / or combinations fall within the scope of this disclosure.
[0091] It should also be noted that the directional terms mentioned in the embodiments, such as "up," "down," "front," "back," "left," and "right," are only for reference to the directions in the accompanying drawings and are not intended to limit the scope of protection of this disclosure. Throughout the drawings, the same elements are represented by the same or similar reference numerals. Conventional structures or constructions will be omitted where they may cause confusion in understanding this disclosure, and the shapes and dimensions of the components in the drawings do not reflect actual size and proportion, but are only schematic representations of the embodiments of this disclosure.
[0092] Unless otherwise stated, the numerical parameters in this specification and the appended claims are approximate values and can be varied according to desired characteristics derived from the content of this disclosure. Specifically, all figures used in the specification and claims to indicate composition, reaction conditions, etc., should be understood to be modified by the term "about" in all cases. Generally, this means that a specific amount may vary by ±10% in some embodiments, ±5% in some embodiments, ±1% in some embodiments, and ±0.5% in some embodiments.
[0093] The use of ordinal numbers such as "first," "second," "third," etc., in the specification and claims to modify the corresponding elements does not imply that the element has any ordinal number, nor does it represent the order of one element with another element, or the order of manufacturing methods. The use of these ordinal numbers is only to enable a named element to be clearly distinguished from another element with the same name.
[0094] Furthermore, unless specifically described or required to occur in a specific order, the order of the above steps is not limited to those listed above and can be varied or rearranged according to the desired design. Moreover, the above embodiments can be used in combination with each other or with other embodiments based on design and reliability considerations; that is, technical features from different embodiments can be freely combined to form more embodiments.
[0095] The embodiments of this disclosure have been described above. However, these embodiments are for illustrative purposes only and are not intended to limit the scope of this disclosure. Although various embodiments have been described above, this does not mean that the measures in the various embodiments cannot be used advantageously in combination. The scope of this disclosure is defined by the appended claims and their equivalents. Various substitutions and modifications can be made by those skilled in the art without departing from the scope of this disclosure, and all such substitutions and modifications should fall within the scope of this disclosure.
Claims
1. An element detection device, characterized in that, include: A housing having a first accommodating space with a vacuum inside, and a window provided at the top of the housing; An X-ray generator is disposed on the top of the housing, and the X-ray generator is adapted to emit X-rays; A sample stage is disposed within the first accommodating space and located below the window. The sample stage is suitable for carrying a sample, which receives X-rays passing through the window and excites target X-rays. A detection component, disposed on the sample stage, is adapted to receive the target X-rays and determine the elemental composition of the sample. The detection component includes: A magnetization collimation module has a first opening in the middle to allow the target X-rays to pass through. The magnetization collimation module is configured to generate a magnetic field through current supplied by an external power supply to prevent interference from ambient radiation generated by the reflection of the target X-rays after they irradiate the side wall of the sample stage.
2. The element detection device according to claim 1, characterized in that, A second opening is provided at the top of the sample stage and below the window. A collimator is detachably provided on the second opening to change the spot size and divergence angle of the X-rays from the X-ray generator.
3. The element detection device according to claim 2, characterized in that, The sample stage has a second accommodating space, and the second accommodating space is provided with: The first support plate extends along the height direction of the sample stage; The second support plate is connected to one end of the first support plate and extends along the length of the sample stage; The third support plate is connected end-to-end to the first support plate and the second support plate. A groove is provided on the third support plate at a position below the second opening to support the sample.
4. The element detection device according to claim 3, characterized in that, The third support plate is configured as a downward-sloping surface to allow X-rays passing through the collimator to irradiate the sample.
5. The element detection device according to claim 1, characterized in that, The sample stage includes: A temperature controller, suitable for regulating the temperature within the first accommodating space.
6. The element detection device according to claim 3, characterized in that, The detection component also includes: The frame has a mounting groove on the side facing the third support plate to accommodate the magnetization collimation module. A window is disposed in the mounting groove and located on the side of the magnetization collimation module closer to the sample; A detector, disposed in the mounting slot and located on the side of the magnetization collimation module away from the sample, is adapted to determine the elemental composition of the sample based on target X-rays emitted from the magnetization collimation module.
7. The element detection device according to claim 6, characterized in that, The distance between the magnetization collimation module and the detector is not less than 1 mm.
8. The element detection device according to claim 6, characterized in that, The window is made of any one of beryllium, diamond, and silicon nitride. The thickness of the window is 1μm to 50μm.
9. The element detection device according to claim 1, characterized in that, The diameter of the first opening is 1mm to 10mm.
10. The element detection device according to claim 1, characterized in that, Also includes: A shielding cover is fitted over the outside of the housing to shield against the influence of magnetic fields from the external environment.