Method and system for measuring diffusion element content distribution in grain boundary diffusion magnet in diffusion direction, electronic equipment and storage medium

By calibrating the ICP measurement value of the X-ray meter and combining the grain boundary diffusion heat treatment and dethickening treatment of the magnet sample, the problem of inaccurate diffusion depth measurement in the prior art is solved, and the accurate evaluation of the content distribution of diffusion elements in the magnet is achieved.

CN119595683APending Publication Date: 2025-03-11BEIJING ZHONG KE SAN HUAN HI TECH
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Patent Information

Application Number
CN202311161818.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-09-08
Publication Date
2025-03-11

AI Technical Summary

Technical Problem

In the prior art, the measurement and evaluation method of diffusion depth of diffusion elements in grain boundary diffusion process has the problem of inaccurate measurement, especially the scanning electron microscopy method is complicated to operate and the results are not fast enough. The relative value of the X-ray meter measurement results cannot accurately give the heavy rare earth element content distribution at different diffusion depths.

Method used

By calibrating the X-ray meter, using the ICP measurement value as a preset parameter, the element content of the calibration sample is measured multiple times, and the X-ray meter is calibrated based on the average value and the ICP measurement value. Then, the magnet sample was subjected to grain boundary diffusion heat treatment and dethickening treatment, and the content value of the target diffusion element of samples of different thicknesses was measured using a calibrated X-ray meter.

Benefits of technology

Through the calibration X-ray meter measurement, the concentration distribution of diffused elements can be obtained more accurately, and the effect of diffusion depth of the magnet grain boundary is evaluated, reducing the measurement inaccuracy problem caused by interference between other elements of the matrix other than diffused elements.

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Abstract

The invention discloses a method and system for measuring diffusion element content distribution in a grain boundary diffusion magnet in the diffusion direction, electronic equipment and a storage medium. The method for measuring the content distribution of the diffusion elements in the grain boundary diffusion magnet along the diffusion direction comprises the following steps: calibrating an X-ray instrument based on an ICP (Inductively Coupled Plasma) measured value of each element content of a calibration sample; performing grain boundary diffusion heat treatment on the film layer containing the diffusion elements attached to the surface of the magnet base material to obtain a magnet sample; performing thickness removal treatment on the magnet sample according to a preset thickness; and measuring the content values of the target diffusion elements on the to-be-measured surfaces of the magnet samples with different thicknesses through the calibrated X-ray instrument. According to the method, the X-ray instrument is calibrated through the ICP measured value of the content of each element of the calibration sample, so that the problem of inaccurate measurement caused by interference among other elements of a matrix except diffusion elements can be reduced; and the content values of the target diffusion elements of the magnet samples with different thicknesses are measured through the corrected X-ray instrument, so that the depth distribution of the content of the diffusion elements in the magnet can be accurately obtained, and the grain boundary diffusion depth effect can be evaluated.
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Description

Technical Field

[0001] The present application relates to the technical field of magnetic materials, and in particular to a method, system, electronic equipment and storage medium for measuring the content distribution of diffusion elements along a diffusion direction in a grain boundary diffusion magnet. Background Art

[0002] Sintered NdFeB material is an important magnetic functional material, which is widely used in electronic products (such as miniaturization and intelligence of electronic products), new energy vehicles and wind power generation. Grain boundary diffusion technology is an important technical means to prepare high-performance sintered NdFeB materials. It attaches a film layer containing diffusion elements (such as heavy rare earth elements Dy / Tb) on the surface of the substrate, and the grain boundary diffusion heat treatment allows the diffusion source elements to enter the interior of the NdFeB magnet along the grain boundary to improve the coercive force of the magnet substrate.

[0003] The diffusion depth of heavy rare earth elements Dy / Tb has a great influence on the performance of sintered NdFeB magnets. Therefore, it is necessary to analyze the grain boundary diffusion depth of sintered NdFeB magnets in order to make a qualitative analysis of the performance of sintered NdFeB magnets based on the depth of grain boundary diffusion.

[0004] At present, the grain boundary diffusion depth of the diffusing element is generally evaluated by scanning electron microscopy or X-ray instrument. However, the inventors of this application found that the scanning electron microscopy method has the problems of long sample preparation and observation process and cumbersome operation, which is not conducive to the rapid evaluation of the effect of grain boundary diffusion; the diffusion depth result obtained by the X-ray instrument is a relative value, which cannot give the content distribution of heavy rare earth at different diffusion depths, and has the problem of insufficient measurement accuracy.

[0005] Based on this, the inventors believe that the current method for measuring and evaluating the diffusion depth of diffusion elements in the grain boundary diffusion process needs to be improved. Summary of the invention

[0006] The present application provides a method, system, electronic device and storage medium for measuring the content distribution of diffusion elements along the diffusion direction in a grain boundary diffusion magnet, which are used to solve the problem of inaccurate measurement of diffusion depth evaluation methods of diffusion elements in the current grain boundary diffusion process.

[0007] According to one aspect of the present application, a method for measuring the content distribution of diffusion elements along the diffusion direction in a grain boundary diffusion magnet is provided, comprising: calibrating an X-ray instrument based on the ICP measurement values ​​of the contents of each element of a calibration sample; performing grain boundary diffusion heat treatment on a film layer containing the diffusion elements attached to the surface of a magnet substrate to obtain a magnet sample; performing a dethickening treatment on the magnet sample with a preset thickness; and measuring the content values ​​of the target diffusion elements on the test surfaces of the magnet samples with different thicknesses by the calibrated X-ray instrument.

[0008] According to some embodiments of the present application, calibrating an X-ray instrument based on the ICP measurement values ​​of the contents of each element of a calibration sample includes: determining the ICP measurement values ​​of the contents of each element of the calibration sample; inputting the ICP measurement values ​​into the X-ray instrument as preset parameters; measuring the X-ray instrument measurement values ​​of the contents of each element of the calibration sample multiple times by the X-ray instrument; and calibrating the X-ray instrument based on an average value of the multiple X-ray instrument measurement values ​​and the ICP measurement value.

[0009] According to some embodiments of the present application, a magnet sample is obtained by subjecting a magnet substrate having a film layer containing diffusion elements attached to its surface to grain boundary diffusion heat treatment, including: sputtering a metal target containing diffusion elements on the surface of the magnet substrate to form a film layer of target thickness, and subjecting the magnet sample to grain boundary diffusion heat treatment; or coating a film layer containing diffusion elements of target thickness on the surface of the magnet substrate, and subjecting the magnet sample to grain boundary diffusion heat treatment, wherein the coating means include screen printing, dipping, spraying, etc.

[0010] According to some embodiments of the present application, performing a dethickening treatment on the magnet sample to a preset thickness includes: performing an acid wash treatment on the magnet sample to obtain the preset thickness of the magnet sample.

[0011] According to some embodiments of the present application, measuring the content values ​​of target diffusion elements on the test surface of a magnetic sample with different thicknesses by a calibrated X-ray instrument includes: positioning the measurement area of ​​the test surface of the magnetic sample based on a positioning device; and measuring the content values ​​of the target diffusion elements in the measurement area by a calibrated X-ray instrument.

[0012] According to some embodiments of the present application, the diffusion element includes at least one of rare earth elements dysprosium, rare earth elements terbium, rare earth elements praseodymium, rare earth elements neodymium, rare earth elements cerium, rare earth elements holmium, copper, cobalt, and gallium.

[0013] According to some embodiments of the present application, in the measurement program of the X-ray instrument, the collimator aperture is set to 0.6 mm, and the primary filter is an aluminum sheet with a thickness of 500 μm.

[0014] According to some embodiments of the present application, after measuring the content value of the target diffusion element on the test surface of the magnet samples with different thicknesses by the calibrated X-ray instrument, the method further includes: measuring the magnetic properties of the magnet samples with different thicknesses.

[0015] According to another aspect of the present application, a system for measuring the distribution of diffusion element content along the diffusion direction in a grain boundary diffusion magnet is also provided. The system includes an X-ray instrument calibration unit, a grain boundary diffusion processing unit, a magnet sample processing unit and a diffusion element content measurement unit. The X-ray instrument calibration unit calibrates the X-ray instrument based on the ICP measurement values ​​of the content of each element of the calibration sample; the grain boundary diffusion processing unit performs grain boundary thermal diffusion treatment on the film layer containing the diffusion element attached to the surface of the magnet substrate to obtain a magnet sample; the magnet sample processing unit performs a dethickening treatment on the magnet sample with a preset thickness; the diffusion element content measurement unit measures the content value of the target diffusion element of the magnet sample to be tested with different thicknesses through the calibrated X-ray instrument.

[0016] According to another aspect of the present application, the present application further provides an electronic device, which includes: one or more processors; and a storage device for storing one or more programs, so that when the one or more programs are executed by the one or more processors, the one or more processors can implement the method described above.

[0017] According to another aspect of the present application, the present application further provides a non-volatile computer-readable storage medium, wherein a computer program is stored on the storage medium, and the computer program can implement the method described above.

[0018] The present application calibrates the X-ray instrument by calibrating the ICP measurement values ​​of the content of each element of the calibration sample, which can reduce the problem of inaccurate measurement caused by interference between other elements in the matrix except the diffusion elements; and by measuring the content values ​​of the target diffusion elements in magnet samples of different thicknesses through the calibrated X-ray instrument, the concentration distribution of the diffusion elements can be obtained more accurately to evaluate the effect of the magnet grain boundary diffusion depth. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0020] Figure 1 A schematic diagram showing the principle of measuring element content using an X-ray instrument;

[0021] Figure 2 A flow chart of a method for measuring the distribution of diffusion element content along the diffusion direction in a grain boundary diffusion magnet according to an exemplary embodiment of the present application is shown;

[0022] Figure 3A flow chart showing another method for measuring the distribution of diffusion element content along the diffusion direction in a grain boundary diffusion magnet according to an exemplary embodiment of the present application;

[0023] Figure 4 An ICP measurement component diagram showing an exemplary embodiment of the present application;

[0024] Figure 5 A graph showing the relationship between the thickness of the Tb metal film layer and the magnetic properties of an exemplary embodiment of the present application;

[0025] Figure 6 A graph showing the relationship between Tb content and thickness of the dethickening according to an exemplary embodiment of the present application;

[0026] Figure 7 A schematic diagram showing a system according to an example embodiment of the present application.

[0027] Description of reference numerals:

[0028] System 1; X-ray instrument calibration unit 10; grain boundary diffusion processing unit 20; magnet sample processing unit 30; diffusion element content measurement unit 40. DETAILED DESCRIPTION

[0029] Example embodiments will now be described more fully with reference to the accompanying drawings. However, example embodiments can be implemented in many forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this application will be comprehensive and complete and will fully convey the concepts of the example embodiments to those skilled in the art. The same reference numerals in the figures represent the same or similar parts, and thus their repeated description will be omitted.

[0030] The described features, structures or characteristics may be combined in one or more embodiments in any suitable manner. In the following description, many specific details are provided to provide a full understanding of the embodiments of the present disclosure. However, those skilled in the art will appreciate that the technical solutions of the present disclosure may be practiced without one or more of these specific details, or other modes, components, materials, devices, etc. may be adopted. In these cases, known structures, methods, devices, implementations, materials or operations will not be shown or described in detail.

[0031] In addition, the terms "include" and "have" and any variations thereof are intended to cover non-exclusive inclusions. For example, a process, method, system, product or device that includes a series of steps or units is not limited to the listed steps or units, but may optionally include steps or units that are not listed, or may optionally include other steps or units that are inherent to these processes, methods, products or devices.

[0032] The terms "first", "second" and the like in the specification and claims of this application and the above drawings are used to distinguish different objects rather than to describe a specific order.

[0033] The following is a clear and complete description of the technical solution of the present application in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present application.

[0034] Figure 1 The schematic diagram shows the principle of measuring element content by X-ray instrument. Figure 1 As shown, the principle of analyzing element content based on X-ray fluorescence method is: the high-intensity X-ray primary radiation generated by the X-ray tube or radioactive isotope passes through the primary filter or collimator, and then irradiates the sample surface to generate X-ray secondary fluorescence radiation.

[0035] After the X-ray secondary fluorescence radiation is received by the detector, it can be processed by software to obtain the characteristic energy spectrum corresponding to the elements contained in the magnet substrate. The measurement system can calculate the content of the elements in the sample based on the intensity of the characteristic energy spectrum.

[0036] However, the inventors have found that the existing method of analyzing element content based on X-ray fluorescence method may cause inaccurate measurement results due to mutual interference between elements.

[0037] For example, interference between elements includes the absorption-enhancement effect between matrix elements other than the measured element Dy or Tb, which will affect the measurement intensity of the measured element. For example, the matrix element absorbs the primary X-ray beam, which affects the excitation of the primary X-ray on the measured element (absorption effect); for another example, the matrix element absorbs the fluorescent X-ray beam of the measured element (absorption effect), which affects the excitation of the secondary fluorescence radiation of the X-ray; for another example, the fluorescent X-ray beam emitted by the matrix element is absorbed by the measured element on the short-wave side of the absorption limit of the measured element, which excites the characteristic spectrum line of the measured element (absorption effect) and affects the measurement result.

[0038] Interference between elements also includes overlapping interference of elements on spectral lines, such as the diffraction peak interference of other elements at the main diffraction peak spectral line position of Tb or Dy.

[0039] For example, according to the spectral lines, the two main peaks of Tb are in detector channel 194 (6.28keV) [the channel contains 65TbLη, 65TbLα1, 59PrLγ1, 61PmLβ2, 69TmLl, 58Ce Lγ3, 62SmLβ1, 26FeKα1] and channel 215 (6.97keV) [the channel contains 27CoKα1, 72HfLl, 65TbLβ1, 68ErLα1, 60NdLγ3, 61PmLγ1, 26FeKβ1, 68ErLη, 63EuLβ2].

[0040] The two main peaks of Dy are in detector channel 200 (6.48keV) [the channel contains 25MnKβ1, 66DyLα1, 63EuLβ1, 26FeKα1, 66DyLη, 70YbLI, 62SmLβ2, 60NdLγ1, 58CeLγ3] and channel 223 (7.23keV) [the channel contains 66DyLβ1, 61Pm Lγ3, 69TmLα1, 73TaLl, 62SmLγ1, 69TmLη, 64GdLβ2, 26FeKβ1].

[0041] Based on this, according to one aspect of the present application, the present application provides a method for measuring the content distribution of diffusion elements along the diffusion direction in a grain boundary diffusion magnet, which can solve the problem of inaccurate measurement caused by interference between elements.

[0042] Figure 2 A flow chart of a method for measuring the distribution of diffusion elements along the diffusion direction in a grain boundary diffusion magnet according to an exemplary embodiment of the present application is shown. Figure 2 As shown, the method includes steps S100 to S400. Exemplarily, the method may be performed by a measurement system for measuring the distribution of diffusion element content along the diffusion direction in a grain boundary diffusion magnet.

[0043] According to an example embodiment, in step S100 , the measurement system calibrates the X-ray instrument based on ICP measurement values ​​of the contents of various elements of the calibration sample.

[0044] For example, the calibration sample is a sintered NdFeB magnet selected according to actual needs. The ICP measurement value is the measured value of the content of each element in the sintered NdFeB magnet measured by ICP. The elements in the sintered NdFeB magnet include but are not limited to Dy, Tb, Nd, Pr, Fe, Co, Cu, Ga, Nb, Ho, Gd and Zr.

[0045] By setting preset parameters (ICP measurement values) in the X-ray instrument program and correcting the measurement results of the X-ray instrument according to the preset parameters, the problem of inaccurate measurement caused by interference between matrix elements other than the measured element Dy or Tb can be avoided.

[0046] Optionally, Figure 3 A flow chart of another method for measuring the distribution of diffusion elements along the diffusion direction in a grain boundary diffusion magnet according to an exemplary embodiment of the present application is shown. Figure 3 It can be seen that step S100 may include steps S110-S140.

[0047] In step S110 , the measurement system determines the ICP measurement values ​​of the contents of each element of the calibration sample.

[0048] In step S120, the measurement system inputs the ICP measurement value into the X-ray apparatus as a preset parameter.

[0049] In step S130 , the measurement system measures the X-ray instrument measurement values ​​of the content of each element of the calibration sample multiple times by means of the X-ray instrument.

[0050] In step S140, the measurement system calibrates the X-ray machine based on an average of a plurality of X-ray machine measurement values ​​and the ICP measurement value.

[0051] For example, at least three or more sintered NdFeB magnets are selected as calibration samples, and the contents of each element in the calibration samples are measured by ICP to obtain the ICP measurement values ​​of the calibration samples. For example, among the at least three or more calibration samples, the difference in Dy content of at least two calibration samples is greater than 1.5wt% and greater than 3.0wt%, and the difference in Tb content of at least two calibration samples is greater than 1.5wt% and greater than 3.0wt%, respectively.

[0052] Preset measurement programs for multiple elements in the measurement program of the X-ray instrument. For example, establish measurement programs for elements such as Dy, Tb, Nd, Pr, Fe, Co, Cu, Ga, Nb, Ho, Gd and Zr on the X-ray instrument. Enter the determined ICP measurement values ​​of the contents of each element in the measurement program of the X-ray instrument as preset parameters of the measurement program.

[0053] The measurement system starts the calibration function of the X-ray instrument, measures the X-ray instrument measurement values ​​of each element content of the calibration sample multiple times (e.g., at least three times or more), and completes the calibration of the X-ray instrument based on the average value of the X-ray instrument measurement values ​​measured multiple times and the preset parameters (ICP measurement values). This setting can prevent the calibrated X-ray instrument from inaccurate measurement problems caused by interference between elements during the measurement process.

[0054] Exemplarily, in the measurement program of the X-ray instrument, the collimator aperture is set to 0.6 mm, and the primary filter is an aluminum sheet with a thickness of 500 μm.

[0055] In step S200, the measurement system performs grain boundary diffusion heat treatment on a film layer containing diffusion elements attached to the surface of a magnet substrate to obtain a magnet sample.

[0056] According to an exemplary embodiment, the magnet substrate is described in detail below by taking a sintered NdFeB material as an example, but the present application is not limited thereto.

[0057] Optionally, the ICP method is also used to measure the content of each element in the magnet substrate to obtain the ICP measurement value of the magnet substrate. The magnet substrate is used as a sample to calibrate the X-ray instrument again. The calibration principle has been described above and will not be repeated here.

[0058] The measurement system can obtain the target magnet sample by performing grain boundary diffusion treatment on the magnet substrate.

[0059] Optionally, in step S200, the measurement system sputters a target material containing diffusion elements on the surface of the magnet substrate to form a film layer of target thickness, and performs grain boundary diffusion heat treatment to obtain a magnet sample.

[0060] For example, the measurement system uses metal Dy or metal Tb as a target material, forms a Dy metal film layer or a Tb metal film layer with a target thickness on the surface of the magnet substrate by sputtering, and obtains a grain boundary diffusion magnet sample to be measured after grain boundary diffusion heat treatment.

[0061] Optionally, in step S200, a film layer containing diffusion elements with a target thickness is coated on the surface of the magnet substrate, and a grain boundary diffusion heat treatment is performed to obtain a magnet sample.

[0062] For example, the measuring system uses a slurry containing metal Dy or metal Tb powder to coat a film layer of target thickness on the surface of the magnet substrate, and performs grain boundary diffusion heat treatment to obtain a magnet sample. The coating method includes but is not limited to screen printing, dipping, spraying, etc.

[0063] Optionally, the execution order of step S100 and step S200 is not limited in this application, that is, step S100 may be executed first and then step S200; or step S200 may be executed first and then step S100.

[0064] In step S300 , the measuring system performs a dethickening process on the magnet sample with a preset thickness.

[0065] In step S400, the measurement system measures the content values ​​of target diffusible elements on the test surfaces of magnet samples with different thicknesses by using a calibrated X-ray instrument.

[0066] The measurement system measures the content of the target diffusion element (such as heavy rare earth element) on the test surface of the magnet sample after the grain boundary diffusion treatment. After the magnet sample is subjected to the thickness reduction treatment, the measurement system determines the thickness change of the test surface and measures the composition of the test surface through the calibrated X-ray instrument.

[0067] Optionally, the measurement system performs a dethickening treatment on the magnet sample, including: performing an acid wash treatment on the magnet sample to remove the thickness of the magnet sample's test surface to a preset thickness; and may also include removing a diffusion element metal film layer remaining on the magnet surface after the diffusion heat treatment.

[0068] For example, the measurement system performs pickling treatment on the magnet sample with a preset thickness for multiple times to obtain the content values ​​of heavy rare earth elements on the surface of multiple magnet samples with different depths, so that the magnet grain boundary diffusion depth can be obtained based on the content values ​​of heavy rare earth elements.

[0069] Optionally, in step S400, the measuring system locates the measuring area of ​​the magnetic sample surface to be measured based on the positioning device, so that the measuring area each time can be the same as the heavy rare earth measuring area of ​​the magnetic sample surface to be measured, so as to measure the content of the target diffusible element of magnetic samples with different thicknesses.

[0070] Optionally, the target diffusion element includes at least one of rare earth elements dysprosium, rare earth elements terbium, rare earth elements praseodymium, rare earth elements neodymium, rare earth elements cerium, rare earth elements holmium, copper, cobalt, and gallium.

[0071] Example Embodiments

[0072] The present application is described below in conjunction with a specific example embodiment.

[0073] Figure 4 An ICP measurement component diagram showing an exemplary embodiment of the present application; Figure 5 A graph showing the relationship between the thickness of the Tb metal film layer and the magnetic properties of an exemplary embodiment of the present application; Figure 6 A graph showing the relationship between the Tb content and the thickness of the de-thickening according to an exemplary embodiment of the present application is shown.

[0074] Step 1: Select 14 sintered NdFeB magnets as calibration samples, and obtain the ICP measurement values ​​of the contents of each element in the sintered NdFeB magnets by ICP test (such as Figure 4 shown).

[0075] Step 2: Establish a measurement program on the X-ray instrument (Fisher XDV-SDD) for elements including Dy, Tb, Nd, Pr, Fe, Co, Cu, Ga, Nb, Ho, Gd, and Zr.

[0076] Step 3: Turn on the calibration function of the X-ray instrument, measure the X-ray instrument measurement values ​​of the content of each element of the sintered NdFeB magnet at least three times or more, and complete the calibration of the X-ray instrument based on the average value of the X-ray instrument measurement values ​​and the ICP measurement value measured multiple times.

[0077] Step 4: Select at least three magnets of the same type (such as N38SH brand, size 12*12*8mm) as magnet substrates, use ICP to measure the content of each element in one of the magnet substrates, and obtain the ICP measurement value of the magnet substrate. Use the other magnet substrates as samples to calibrate the X-ray instrument again.

[0078] Step 5: Using metal Tb as the target, a Tb metal film layer with an average thickness of 3.2 μm, 6.5 μm and 13 μm was formed on the surface of multiple magnet substrates by magnetron sputtering, and then a diffusion treatment was performed at 900°C for 6 h. After a secondary tempering treatment (920°C for 2 h and 520°C for 4 h), the magnetic properties of magnet samples with different thicknesses were measured (such as Figure 5 shown).

[0079] Step 6: Remove the sputtered Tb metal film layer on the surface of the magnet substrate to obtain a magnet sample with the content distribution of the diffusion element to be measured along the diffusion direction. The surface thickness of the magnet sample is removed by pickling, and the thickness change of the surface to be measured is measured by a micrometer with a minimum resolution of 0.1μm. The thickness removed by pickling each time is set according to the demand, and the thickness removed is adjusted by the pickling time and the number of repeated pickling times, and the change can be controlled to be less than 0.5μm.

[0080] Step 7: Position the measurement area of ​​the surface to be measured of the magnet sample according to the positioning device, and measure the Tb content on the surface of the magnet samples of different thicknesses.

[0081] Step 8: Determine the relationship between the thickness of the magnet sample with different thicknesses of the Tb metal film layer and the Tb content (eg Figure 5 and Figure 6 shown).

[0082] Through the above-mentioned example embodiments, the present application calibrates the X-ray instrument by calibrating the ICP measurement values ​​of the contents of each element of the calibration sample, which can reduce the problem of inaccurate measurement caused by interference between other elements of the matrix except the diffusion elements; and by measuring the content values ​​of the target diffusion elements in magnet samples of different thicknesses through the calibrated X-ray instrument, the depth variation curve of the diffusion element content in the grain boundary diffusion magnet can be obtained more accurately, and the effect of the grain boundary diffusion depth of the magnet can be evaluated.

[0083] According to another aspect of the present application, the present application provides a system for measuring the distribution of diffusion element content along the diffusion direction in a grain boundary diffusion magnet, wherein the system is used to perform the method described above. Figure 7 A schematic diagram showing a system of an exemplary embodiment of the present application is shown as follows: Figure 7As shown, the system 1 for measuring the distribution of diffusion element content along the diffusion direction in a grain boundary diffusion magnet includes an X-ray instrument calibration unit 10 , a grain boundary diffusion processing unit 20 , a magnet sample processing unit 30 and a diffusion element content measurement unit 40 .

[0084] According to the exemplary embodiment, the X-ray instrument calibration unit 10 calibrates the X-ray instrument based on the ICP measurement values ​​of the contents of each element of the calibration sample. The grain boundary diffusion processing unit 20 performs grain boundary diffusion processing on the magnet substrate to obtain the magnet sample. The magnet sample processing unit 30 performs grain boundary diffusion processing on the magnet substrate to obtain the magnet sample, and performs a thickness reduction processing on the magnet sample with a preset thickness. The diffusion element content measurement unit 40 measures the content values ​​of the target diffusion elements of the magnet sample test surfaces with different thicknesses through the calibrated X-ray instrument.

[0085] The measuring principle of the system for measuring the distribution of the content of the diffusing elements along the diffusion direction in the grain boundary diffusion magnet has been described above and will not be repeated here.

[0086] The measurement system provided in the present application calibrates the X-ray instrument by calibrating the ICP measurement values ​​of the contents of each element in the sample, which can reduce the problem of inaccurate measurement caused by interference between other elements in the matrix except the diffusion elements; and by measuring the content values ​​of the target diffusion elements in magnet samples of different thicknesses through the calibrated X-ray instrument, the depth distribution of the diffusion element content in the magnet can be obtained more accurately to evaluate the effect of the diffusion depth of the magnet grain boundaries.

[0087] According to another aspect of the present application, the present application also provides an electronic device. The electronic device includes: one or more processors; a storage device for storing one or more programs, and when the one or more programs are executed by the one or more processors, the one or more processors can implement the method described above.

[0088] According to another aspect of the present application, a non-volatile computer-readable storage medium is provided, wherein a computer program is stored on the storage medium, and the computer program can implement the method described above.

[0089] Finally, it should be noted that the above is only a preferred embodiment of the present application and is not intended to limit the present application. Although the present application is described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions of the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A method for measuring the distribution of diffusion elements along the diffusion direction in a grain boundary diffusion magnet, characterized in that: include: Calibrate the X-ray instrument based on the ICP measurement values ​​of the content of each element of the calibration sample; A magnet sample is obtained by subjecting a film layer containing diffusion elements attached to the surface of a magnet substrate to a grain boundary diffusion heat treatment; Performing a dethickening process on the magnet sample with a preset thickness; The content values ​​of the target diffusion elements on the test surface of the magnet samples with different thicknesses are measured by a calibrated X-ray instrument.

2. The method according to claim 1, characterized in that The calibrating of the X-ray instrument based on the ICP measurement value of each element content of the calibration sample comprises: Determine the ICP measurement value of each element content of the calibration sample; inputting the ICP measurement value into the X-ray instrument as a preset parameter; The X-ray instrument measures the X-ray instrument measurement values ​​of the content of each element of the calibration sample for multiple times by the X-ray instrument; The X-ray machine is calibrated based on an average of a plurality of X-ray machine measurements and the ICP measurement.

3. The method according to claim 1, characterized in that The method of subjecting a magnet substrate having a film layer containing diffusion elements attached to its surface to grain boundary thermal diffusion treatment to obtain a magnet sample comprises: Sputtering a target material containing diffusion elements on the surface of the magnet substrate to form a film layer of target thickness, and performing grain boundary diffusion heat treatment to obtain the magnet sample; Alternatively, a film layer containing diffusion elements with a target thickness is coated on the surface of the magnet substrate, and a grain boundary diffusion heat treatment is performed to obtain the magnet sample.

4. The method according to claim 1, characterized in that: The step of performing a dethickening process on the magnet sample with a preset thickness includes: The magnet sample is pickled to obtain a preset thickness of the magnet sample.

5. The method according to claim 1, characterized in that The content values ​​of the target diffusion elements measured on the test surface of the magnet sample with different thicknesses by the calibrated X-ray instrument include: Positioning a measurement area of ​​the magnetic sample surface to be measured based on a positioning device; The content value of the diffusible element in the measurement area is measured by a calibrated X-ray instrument.

6. The method according to claim 1, characterized in that The target diffusion element includes at least one of rare earth elements dysprosium, rare earth elements terbium, rare earth elements praseodymium, rare earth elements neodymium, rare earth elements cerium, rare earth elements holmium, copper, cobalt, and gallium.

7. The method according to claim 1, characterized in that In the measurement program of the X-ray instrument, the collimator aperture is set to 0.6 mm, and the primary filter is an aluminum sheet with a thickness of 500 μm.

8. A system for measuring the distribution of diffusion element content along the diffusion direction in a grain boundary diffusion magnet, characterized in that: The system is used to execute the method according to any one of claims 1 to 7, and the system comprises: An X-ray instrument calibration unit, which calibrates the X-ray instrument based on the ICP measurement values ​​of the content of each element of the calibration sample; A grain boundary diffusion treatment unit is used to perform grain boundary diffusion heat treatment on a film layer containing diffusion elements attached to the surface of a magnet substrate to obtain a magnet sample; A magnet sample processing unit, for performing a thickness reduction process on the magnet sample with a preset thickness; The diffusible element content measurement unit measures the content value of the target diffusible element on the test surface of the magnet sample with different thicknesses through a calibrated X-ray instrument.

9. An electronic device, characterized in that: include: one or more processors; A storage device for storing one or more programs; When the one or more programs are executed by the one or more processors, the one or more processors implement the method according to any one of claims 1 to 7.

10. A non-volatile computer-readable storage medium having a computer program stored thereon, characterized in that: The computer program implements the method according to any one of claims 1-7.