A tungsten carbide crystallinity determination method, device, electronic equipment and storage medium

Abstract

The application discloses a tungsten carbide crystallinity determination method and device, electronic equipment and storage medium. The tungsten carbide crystallinity determination method comprises the following steps: obtaining an X-ray diffraction spectrum of tungsten carbide; performing first differential characterization on the X-ray diffraction spectrum to obtain a completeness index; performing second differential characterization on the X-ray diffraction spectrum to obtain a coarsening index; and calculating the crystallinity index of the tungsten carbide according to the completeness index and the coarsening index. The WC crystallinity determination method can be used for detecting WC powder, and the crystallinity of the WC powder can be semi-quantitatively determined, so that the quality of the WC powder can be more comprehensively controlled.

Description

Technical Field

[0001] This invention relates to the field of X-ray diffraction pattern analysis technology, specifically to a method, apparatus, electronic device, and storage medium for determining the degree of crystallinity of tungsten carbide. Background Technology

[0002] As a raw material for cemented carbide production, the quality control of tungsten carbide (WC) powder is extremely important. Currently, the following testing methods are mainly used to control WC powder quality: ① Determining the average particle size and particle size distribution using the Fisher method and sieving; ② Observing the surface morphology of particles using scanning electron microscopy; ③ Observing the internal morphology of particles using ion thinning method; ④ Detecting free carbon and total carbon to control carbon content; ⑤ Determining W2C content and grain size using X-ray diffraction to control phase composition.

[0003] However, during the production process, it was found that for different batches of WC powder, even when the results of the above-mentioned test indicators were similar, the actual quality of the powder still differed. Specifically, this manifested as differences in the properties of the cemented carbide obtained under the same processing conditions. Therefore, it is evident that the current indicators for quality testing of WC powder are not comprehensive, and thus, it is necessary to conduct more precise characterization of WC powder. Summary of the Invention

[0004] In view of this, the present invention provides a method, apparatus, electronic device and storage medium for determining the degree of tungsten carbide crystallinity, so as to perform more accurate characterization of WC powder.

[0005] According to a first aspect, embodiments of the present invention provide a method for determining the degree of crystallinity of tungsten carbide, comprising the following steps: obtaining an X-ray diffraction pattern of tungsten carbide; performing a first differential characterization on the X-ray diffraction pattern to obtain an integrity index; performing a second differential characterization on the X-ray diffraction pattern to obtain a coarsening index; and calculating the crystallinity index of the tungsten carbide based on the integrity index and the coarsening index.

[0006] In conjunction with the first aspect, in the first embodiment of the first aspect, the step of performing a first differential characterization on the X-ray diffraction pattern to obtain an integrity index includes: performing micro-strain analysis on the X-ray diffraction pattern to obtain a micro-strain index; and, or; performing peak shape analysis on a first specified crystal plane of the X-ray diffraction pattern to obtain an α separation index.

[0007] In conjunction with the first embodiment of the first aspect, in the second embodiment of the first aspect, the step of performing micro-strain analysis on the X-ray diffraction pattern to obtain micro-strain indices includes: performing micro-strain analysis on the X-ray diffraction pattern using the WH method to obtain a first micro-strain index of a first group of crystal planes and a second micro-strain index of a second group of crystal planes; wherein, the first group of crystal planes belongs to the (h00) crystal plane family; and the second group of crystal planes belongs to the (00l) crystal plane family.

[0008] In conjunction with the first embodiment of the first aspect, in the third embodiment of the first aspect, the step of performing peak shape analysis on the first designated crystal plane of the X-ray diffraction pattern to obtain the α separation index includes: obtaining peak shapes in the first designated crystal plane of the X-ray diffraction pattern that are respectively related to K. α1 The corresponding first diffraction peak and K α2 The corresponding second diffraction peak; obtain the first lowest point between the first diffraction peak and the second diffraction peak; draw a first straight line parallel to a preset straight line through the first lowest point, the first straight line intersecting the first diffraction peak and the second diffraction peak to obtain a first intersection point and a second intersection point; calculate the peak area above the line connecting the first intersection point and the second intersection point to obtain a first area; calculate the total area of ​​the first diffraction peak and the second diffraction peak to obtain a second area; obtain the α separation index based on the first area and the second area.

[0009] In conjunction with the third embodiment of the first aspect, in the fourth embodiment of the first aspect, the first designated crystal plane is the (112) crystal plane.

[0010] In conjunction with the third embodiment of the first aspect, in the fifth embodiment of the first aspect, obtaining the α separation index based on the first area and the second area includes: calculating the α separation index using a preset first formula based on the first area and the second area; wherein the first formula is: D1=(S2-S1) / S2*100%, D1 represents the α separation index, S1 represents the first area, and S2 represents the second area.

[0011] In conjunction with the first aspect, in the sixth embodiment of the first aspect, performing a second differential characterization on the X-ray diffraction pattern to obtain a coarsening index includes: selecting a second lowest point between diffraction peaks in a second specified crystal plane region within a preset diffraction angle range of the X-ray diffraction pattern; drawing a second straight line parallel to a preset straight line through the second lowest point, the second straight line intersecting with the diffraction peaks in the region to obtain a third intersection point and a fourth intersection point; calculating the peak area above the preset straight line and within the diffraction angle range in the X-ray diffraction pattern to obtain a third area; calculating the peak area above the line connecting the third and fourth intersection points in the X-ray diffraction pattern to obtain a fourth area; obtaining the peak-to-valley ratio based on the third area and the fourth area, and using the peak-to-valley ratio as the coarsening index.

[0012] In conjunction with the sixth embodiment of the first aspect, in the seventh embodiment of the first aspect, the second designated crystal plane is crystal plane (210)(003)(202).

[0013] In conjunction with the sixth embodiment of the first aspect, in the eighth embodiment of the first aspect, obtaining the peak-to-valley ratio based on the third area and the fourth area includes: calculating the peak-to-valley ratio using a preset second formula based on the third area and the fourth area; wherein the second formula is: D2=(S3-S4) / S3*100%, where D2 represents the peak-to-valley ratio, S3 represents the third area, and S4 represents the fourth area.

[0014] In conjunction with the first embodiment of the first aspect, in the ninth embodiment of the first aspect, the step of calculating the crystallinity index of tungsten carbide based on the micro-strain index, the peak-to-valley ratio, and the α-separation index includes: calculating the crystallinity index of tungsten carbide using a preset third formula based on the micro-strain index, the peak-to-valley ratio, and the α-separation index; wherein the third formula is: A=[1-100*(σ1+σ2)+(1-D1)+(1-D2)]*100%, where A represents the crystallinity index of tungsten carbide, σ1 represents the first micro-strain index, σ2 represents the second micro-strain index, D1 represents the α-separation index, and D2 represents the peak-to-valley ratio.

[0015] According to a second aspect, the present invention also provides an apparatus for determining the degree of crystallinity of tungsten carbide, comprising an acquisition module, an integrity index determination module, a coarsening index determination module, and a calculation module, wherein the acquisition module is used to acquire an X-ray diffraction pattern of tungsten carbide; the integrity index determination module is used to perform a first differential characterization on the X-ray diffraction pattern to obtain an integrity index; the coarsening index determination module is used to perform a second differential characterization on the X-ray diffraction pattern to obtain a coarsening index; and the calculation module is used to obtain a crystallinity index of tungsten carbide based on the integrity index and the coarsening index.

[0016] According to a third aspect, the present invention also provides an electronic device, including a memory and a processor, wherein the memory and the processor are communicatively connected to each other, the memory stores computer instructions, and the processor executes the computer instructions to perform the method for determining the degree of tungsten carbide crystallization as described in the first aspect or any embodiment of the first aspect.

[0017] According to a fourth aspect, the present invention provides a computer-readable storage medium storing computer instructions for causing the computer to perform the tungsten carbide crystallization degree determination method described in the first aspect or any embodiment of the first aspect.

[0018] This invention discloses a method, apparatus, electronic device, and storage medium for determining the crystallinity of tungsten carbide (WC). The method includes: acquiring an X-ray diffraction pattern of tungsten carbide; performing a first differential characterization on the X-ray diffraction pattern to obtain an integrity index; performing a second differential characterization on the X-ray diffraction pattern to obtain a coarsening index; and calculating the crystallinity index of the tungsten carbide based on the integrity index and the coarsening index. In other words, this method rapidly characterizes WC powder from a crystal structure perspective in a semi-quantitative manner, enabling comprehensive quality testing of WC powder. Furthermore, this method requires no standard samples, exhibits good repeatability and high accuracy (RSD < 3% for medium-fine particle powder and RSD < 5% for coarse particle powder), and can simultaneously detect a large number of powder particles. Moreover, the use of two sub-indices, such as the integrity index and the coarsening index, during the crystallinity characterization process allows for the identification of the causes of differences in crystallinity, facilitating product quality tracking and comparison, and aiding in process adjustment. Attached Figure Description

[0019] The features and advantages of the invention will be more clearly understood by referring to the accompanying drawings, which are schematic and should not be construed as limiting the invention in any way. In the drawings:

[0020] Figure 1 This is a flowchart illustrating the method for determining the degree of crystallinity of tungsten carbide in Embodiment 1 of the present invention;

[0021] Figure 2 This is a schematic diagram of the detection process for tungsten carbide powder in Example 1 of the present invention;

[0022] Figure 3 A schematic diagram illustrating an example of the α separation index;

[0023] Figure 4 This is a schematic diagram illustrating an example of peak-to-valley ratio.

[0024] Figure 5 This is a schematic diagram of the tungsten carbide crystallization degree determination device in Embodiment 2 of the present invention;

[0025] Figure 6 This is a schematic diagram of the electronic device in Embodiment 3 of the present invention. Detailed Implementation

[0026] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0027] Example 1

[0028] S101: Obtain the X-ray diffraction pattern of tungsten carbide.

[0029] Specifically, the phase composition of tungsten carbide powder was determined using an X-ray diffractometer (BB geometry, θ-θ scanning method) with a scanning angle of 33–151° and a Co target.

[0030] S102: Perform a first differential characterization on the X-ray diffraction pattern to obtain an integrity index;

[0031] Specifically, the integrity index includes at least one of the following: micro-strain index and α-separation index. Therefore, the integrity index can be obtained in the following three ways.

[0032] The first method is to perform micro-strain analysis on the X-ray diffraction pattern to obtain micro-strain indices.

[0033] Specifically, the microstrain analysis of the X-ray diffraction pattern to obtain the microstrain index can be performed using the following method: the Williamson-Hall (WH) method is used to perform microstrain analysis on the X-ray diffraction pattern to obtain the first microstrain index of the first group of crystal planes and the second microstrain index of the second group of crystal planes; wherein the first group of crystal planes belongs to the (h00) crystal plane family and the second group of crystal planes belongs to the (00l) crystal plane family.

[0034] For example, Jade software can be used to perform micro-strain analysis on X-ray diffraction patterns. Specifically, the analysis object is the (100)(200) crystal plane and the (001)(002)(003) crystal planes of WC. During the analysis, in the Jade software menu, go to "View" → "Reports" → "Size & strain plot", select the prepared instrument width correction curve, set the Origin to "3,2", and select "Size / Strain" or "Strain Only" to record the strain values ​​of the two crystal planes respectively. In particular, when the diffraction intensity I(101) / I(100) ≥ 1, select "Strain Only", and when I(101) / I(100) < 1, select "Size / Strain".

[0035] The second method is to perform peak shape analysis on the first designated crystal plane of the X-ray diffraction pattern to obtain the α separation index.

[0036] X-ray diffraction patterns are generally obtained from K. α1 and K α2 The mixed spectrum. K α1 and K α2 The wavelengths are very close, so the two sets of spectra obtained are almost overlapping. However, as the diffraction angle 2θ increases, the difference between 2θ1 and 2θ2 gradually increases. When the 2θ angle is greater than 90°, the two diffraction peaks can be separated. The degree of separation is affected by the instrument hardware, but theoretically it is related to the half-width at half-maximum (FWHM) of the diffraction peaks, that is, to the degree of crystal growth of the material.

[0037] Specifically, the peak shape analysis of the first designated crystal plane of the X-ray diffraction pattern to obtain the α separation index can be performed using the following method: Peak shapes with K are obtained from the first designated crystal plane of the X-ray diffraction pattern. α1 The corresponding first diffraction peak and K α2 The corresponding second diffraction peak; obtain the first lowest point between the first diffraction peak and the second diffraction peak; draw a first straight line parallel to a preset straight line through the first lowest point, the first straight line intersecting the first diffraction peak and the second diffraction peak to obtain a first intersection point and a second intersection point; calculate the peak area above the line connecting the first intersection point and the second intersection point to obtain a first area; calculate the total area of ​​the first diffraction peak and the second diffraction peak to obtain a second area; obtain the α separation index based on the first area and the second area.

[0038] Specifically, a straight line is preset as the background line. Therefore, before performing peak shape analysis on the first designated crystal plane of the X-ray diffraction pattern to obtain the α separation index, the background line of the X-ray diffraction pattern is also determined. This is because, for peak shape analysis, changes in the background line have a significant impact on the peak area or full width at half maximum (FWHM). In particular, if the powder has a low degree of crystallinity, the determination of the background line is especially important.

[0039] Specifically, the principle for determining the background line is as follows: Multiple fixed points are selected in the X-ray diffraction pattern, and these fixed points are connected to obtain the background line. When connecting multiple fixed points, the line connecting them should pass through the midpoint of the background noise point, and the line should be as straight as possible. This is because using fixed points helps avoid operational errors. For example, the fixed points to be used are: 34.5°, 35.1°, 38.3°, 39.0°, 39.5°, 43.7°, 49.2°, 51.8°, 54.2°, 59.8°, 72.0°, 82.0°, 97.0°, 106.0°, 114.2°, 119.9°, 129.9°, and 135.7°.

[0040] More specifically, the first designated crystal plane is the (112) crystal plane. This is because the selection principle for the first designated crystal plane is: ① the crystal plane is located in the high-angle region of the diffraction pattern, K α1 and K α2 The separation is obvious, which is beneficial for analysis; ② It is not affected by other crystal planes and there are no adjacent or overlapping diffraction peaks. In the diffraction pattern, the (112) crystal plane is the optimal solution of the first specified crystal plane.

[0041] More specifically, the α-separation index can be obtained based on the first area and the second area using the following method: the α-separation index is calculated using a preset first formula based on the first area and the second area; wherein the first formula is:

[0042] D1 = (S2 - S1) / S2 * 100%, where D1 represents the α separation index, S1 represents the first area, and S2 represents the second area.

[0043] For example, such as Figure 3 As shown, take the (112) crystal plane K α1 With K α2 The lowest point C between them, the straight line passing through C and parallel to the back line and K α1 and K α2 The intersection points are C1 and C2. The area of ​​the peak above the back line (line 1) is S2, and the area of ​​the peak above the line C1C2 (line 2) is S1. Then D1 = (S2 - S1) / S2 * 100%.

[0044] In particular, when the powder has a low degree of crystallinity, the K of the (112) crystal plane... α1 With K α2 When it is impossible to distinguish between them and the α separation index cannot be calculated, its value can be set to 100%.

[0045] The third method is to perform micro-strain analysis on the X-ray diffraction pattern to obtain micro-strain indices; and simultaneously perform peak shape analysis on the first designated crystal plane of the X-ray diffraction pattern to obtain the α separation index.

[0046] It should be noted that the third method is a combination of the first and second methods. For the specific implementation of the third method, please refer to the first and second methods mentioned above, which will not be repeated here.

[0047] S103: Perform a second differential characterization on the X-ray diffraction pattern to obtain a coarsening index.

[0048] Specifically, the second differential characterization of the X-ray diffraction pattern to obtain the coarsening index can be performed using the following method: A second lowest point is selected between diffraction peaks in a second specified crystal plane region within a preset diffraction angle range of the X-ray diffraction pattern; a second straight line parallel to a preset straight line is drawn through the second lowest point, intersecting the diffraction peaks in the region to obtain a third and a fourth intersection point; the peak area above the preset straight line and within the diffraction angle range in the X-ray diffraction pattern is calculated to obtain a third area; the peak area above the line connecting the third and fourth intersection points in the X-ray diffraction pattern is calculated to obtain a fourth area; the peak-to-valley ratio is obtained based on the third and fourth areas, and this ratio is used as the coarsening index.

[0049] Specifically, the preset straight line is the back baseline.

[0050] More specifically, the second designated crystal plane is crystal plane (210)(003)(202). When the target material is a Co target, the preset diffraction angle range is 135°~150°.

[0051] Typically, when there are many nanocrystals, submicron phases, or fine grains in the powder, it will cause the diffraction peaks to broaden; in particular, it will cause the peak feet to extend and the area to increase; when adjacent diffraction peaks overlap, it can be manifested as a significant increase in the height between the line connecting the two at their boundary and the background line, and the overlapping area becomes larger. In the diffraction spectrum, the differential characteristics of the specified crystal planes in this preset region are the most significant: ① The diffraction peaks of the three specified crystal planes in this region are all adjacent, and the overlapping area is the largest. ② The diffraction intensity of the (003) crystal plane is small and is easily covered by the overlapping area. This significant differential characteristic makes the index obtained by this quantification extremely sensitive to the fluctuation of the grain size; for example, when the grain size of the powder increases, it can be directly observed from the pattern of this preset region that ① the overlapping area of ​​the specified crystal planes becomes smaller and ② the (003) crystal plane changes from unidentifiable to identifiable.

[0052] Furthermore, this diffraction angle range not only completely encompasses the three specified crystal planes but also takes into account the extension space of the diffraction peak feet, facilitating the delineation of the background line and preventing misjudgment. When other target materials are selected, their corresponding diffraction angle ranges can be calculated using analysis software.

[0053] More specifically, the peak-to-valley ratio obtained based on the third area and the fourth area can be calculated using the following method: the peak-to-valley ratio is calculated using a preset second formula based on the third area and the fourth area; wherein the second formula is:

[0054] D2 = (S3 - S4) / S3 * 100%, where D2 represents the peak-to-valley ratio, S3 represents the third area, and S4 represents the fourth area.

[0055] For example, such as Figure 4 As shown, the three diffraction peaks in the high-angle region of 135° to 150° are selected as the analysis object, and the lowest point between 140° and 145° is taken as B1; the intersection points of the straight line passing through B1 and parallel to the back baseline with the peak shape are B3 and B4. The peak area above the back baseline (line 3) is S3, and the peak area above the line B3B4 (line 4) is S4. Then the peak-to-valley ratio D2 = (S3 - S4) / S3 * 100%.

[0056] S104: The crystallinity index of the tungsten carbide is obtained based on the integrity index and the coarsening index.

[0057] Specifically, the crystallinity index of tungsten carbide can be obtained from the integrity index and the coarsening index using the following method: the crystallinity index of tungsten carbide is calculated using a preset third formula based on the micro-strain index, the peak-to-valley ratio, and the α-separation index.

[0058] The third formula is: A = [1 - 100 * (σ1 + σ2) + (1 - D1) + (1 - D2)] * 100%.

[0059] A represents the crystallinity index of the tungsten carbide, σ1 represents the first microstrain index, σ2 represents the second microstrain index, D1 represents the α separation index, and D2 represents the peak-to-valley ratio.

[0060] In Embodiment 1 of this invention, the crystallization index is calculated comprehensively from two aspects: "crystal structure integrity" and "coarsening degree". The first microstrain index σ1, the second microstrain index σ2, and the α-separation index D1 are used to characterize the degree of crystal structure integrity, while the peak-to-valley ratio D2 is used to characterize the size and uniformity of powder grains, i.e., coarsening degree. In reality, the peak-to-valley ratio D2 is also affected by the degree of crystal structure integrity, and the α-separation index D1 is also affected by the coarsening degree. However, considering that the crystallization index is only a comprehensive numerical representation and its influence is minimal, it is not differentiated.

[0061] To verify the accuracy of the method for determining the degree of tungsten carbide crystallinity in Example 1 of the present invention, the following experiment was conducted.

[0062] The method for determining the degree of crystallinity of tungsten carbide described in Example 1 was verified using 9 samples. The 9 samples were labeled as 1-1#, 1-2#, 1-3#, 2-1#, 2-2#, 2-3#, 2-4#, 3-1#, and 3-2#, respectively.

[0063] Tungsten carbide powders 1-1#, 1-2#, and 1-3# were prepared by adding the same amount of grain inhibitor within a temperature range of 1350-1550℃. The processing temperature from lowest to highest is: 1-1# < 1-2# < 1-3#.

[0064] 2-1#, 2-2#, 2-3#, and 2-4# are tungsten carbide powders processed by different crushing methods for the same amount of time. Among them, 2-1# is the original powder, 2-2# is the tungsten carbide powder after ball milling, 2-3# is the tungsten carbide powder after stirring crushing, and 2-4# is the tungsten carbide powder after disc crushing.

[0065] 3-1# and 3-2# ​​are tungsten carbide powders prepared by adding different amounts of crystal inhibitors at the same process temperature. The amount of crystal inhibitor added to 3-1# is less than that added to 3-2#.

[0066] The test results for samples 1-1#, 1-2#, and 1-3# are shown in Table 1, with one additional parallel sample added for each sample. To verify some of the results, the average grain size was calculated using Maud software, and the results are listed in Table 2.

[0067] Table 1 Crystallization index A of WC powder at different process temperatures

[0068]

[0069]

[0070] Table 2 Average grain size of WC powder at different processing temperatures

[0071]

[0072] Theoretically, without additives or other influencing factors, the crystallinity of WC powder increases with increasing process temperature. Table 1 shows that the crystallinity index 1-1# < 1-2# < 1-3#, consistent with conventional understanding in this field. Looking at the sub-indices, 1-1# exhibits the lowest crystal integrity, the most crystal defects, the lowest coarsening, and the smallest grain size. Table 2 also confirms this.

[0073] The test results for samples 2-1#, 2-2#, 2-3#, and 2-4# are shown in Table 3, with two additional parallel samples added for each sample. To verify some of the results, the average grain size and distribution were calculated using Maud software, and the results are listed in Table 4.

[0074] Table 3. Crystallization Index A of WC Powder under Different Crushing Methods

[0075]

[0076] Table 4. Average grain size and distribution of WC powder under different crushing methods

[0077]

[0078]

[0079] Theoretically, as the degree of crushing increases, the grain size of WC powder decreases, the submicron phase increases, defects increase, and the degree of crystallinity decreases. Ball milling is generally considered the most efficient form of crushing. Table 3 shows that the crystallinity index 2-2# < 2-3# < 2-4# < 2-1#, consistent with conventional understanding in this field. Looking at the detailed indicators, compared to other crushing methods, ball milling produces the lowest integrity and the lowest coarsening, indeed demonstrating the highest efficiency. Table 4 also confirms this. Furthermore, looking at the detailed indicators, the difference in effect between stirred crushing and disc crushing is mainly reflected in the degree of coarsening; and in the parallel sample test results, stirred crushing exhibits greater fluctuations in coarsening. This is reflected in Table 4, where stirred crushing produces more fine grains with a more uneven grain size distribution.

[0080] The test results for samples 3-1# and 3-2# ​​are shown in Table 5, with one additional parallel sample added for each sample. To verify some of the results, the W2C solid solution content was measured and is shown in Table 6. The average grain size and distribution were calculated using Maud software, and the results are listed in Table 7.

[0081] Table 5 WC Powder Crystallization Index A

[0082]

[0083] Table 6. Results of W2C content test

[0084] Brand batch number Solid solution phase peak position (°) Solid solution ratio (%) 3-1# 46.41 0.03 3-2# 46.34 1.75

[0085] Table 7 Average grain size and distribution of WC powder

[0086]

[0087]

[0088] Theoretically, the addition of inhibitors should refine the WC powder grains and reduce its crystallinity. The amount of inhibitor can be roughly determined by the quantity of W2C solid solution in the powder. Table 6 shows that the amount of inhibitor added to 3-2# ​​is greater than that to 3-1#. Table 5 shows that the crystallinity index of 3-2# ​​is less than that of 3-1#, which is consistent with conventional understanding in this field. Looking at the detailed indicators, 3-2# ​​has lower integrity and less coarsening, which is also consistent with the results in Table 7.

[0089] Therefore, the method for determining the degree of crystallinity of tungsten carbide provided in Embodiment 1 of this invention rapidly characterizes WC powder from a crystal structure perspective in a defined manner, thereby enabling comprehensive quality testing of WC powder. Furthermore, this method requires no standard samples, exhibits good repeatability and high accuracy, with a relative standard deviation (RSD) of <3% for medium and fine-particle powders and <5% for coarse-particle powders; it can also simultaneously detect a large number of powder particles. Moreover, two sub-indices are used in the characterization of the degree of crystallinity, such as the integrity index and the coarsening index, which can identify the causes of differences in the degree of crystallinity, facilitating product quality tracking and comparison, and aiding in process adjustment.

[0090] Example 2

[0091] Corresponding to Embodiment 1 of the present invention, Embodiment 2 of the present invention provides a schematic diagram of the structure of a device for determining the degree of crystallinity of tungsten carbide. (See attached diagram.) Figure 5 As shown, the tungsten carbide crystallization degree determination device of Embodiment 2 of the present invention includes an acquisition module 20, an integrity index determination module 21, a coarsening degree index determination module 22, and a calculation module 23.

[0092] Specifically, module 20 is used to acquire the X-ray diffraction pattern of tungsten carbide;

[0093] The integrity index determination module 21 is used to perform a first differential characterization on the X-ray diffraction pattern to obtain the integrity index;

[0094] The coarsening index determination module 22 is used to perform a second differential characterization on the X-ray diffraction pattern to obtain a coarsening index;

[0095] The calculation module 23 is used to obtain the crystallinity index of the tungsten carbide based on the integrity index and the coarsening index.

[0096] The integrity index determination module 21 includes a micro-strain index determination unit and an α-separation index determination unit.

[0097] The micro-strain index determination unit is specifically used to: perform micro-strain analysis on the X-ray diffraction pattern using the WH method to obtain the first micro-strain index of the first group of crystal planes and the second micro-strain index of the second group of crystal planes; wherein, the first group of crystal planes belongs to the (h00) crystal plane family; and the second group of crystal planes belongs to the (00l) crystal plane family.

[0098] The α separation index determination unit is specifically used to: obtain the K-separation index from the first designated crystal plane of the X-ray diffraction pattern. α1 The corresponding first diffraction peak and K α2 The corresponding second diffraction peak; obtain the first lowest point between the first diffraction peak and the second diffraction peak; draw a first straight line parallel to a preset straight line through the first lowest point, the first straight line intersecting the first diffraction peak and the second diffraction peak to obtain a first intersection point and a second intersection point; calculate the peak area above the line connecting the first intersection point and the second intersection point to obtain a first area; calculate the total area of ​​the first diffraction peak and the second diffraction peak to obtain a second area; obtain the α separation index based on the first area and the second area.

[0099] More specifically, the α separation index determining unit is used to: calculate the α separation index based on the first area and the second area using a preset first formula; wherein, the first formula is: D1=(S2-S1) / S2*100%, D1 represents the α separation index, S1 represents the first area, and S2 represents the second area.

[0100] The roughness index determination module 22 is specifically used for: selecting the second lowest point between diffraction peaks of a second specified crystal plane region within a preset diffraction angle range of the X-ray diffraction pattern; drawing a second straight line parallel to a preset straight line through the second lowest point, the second straight line intersecting the diffraction peaks of the region to obtain a third intersection point and a fourth intersection point; calculating the peak area above the preset straight line and within the diffraction angle range of the X-ray diffraction pattern to obtain a third area; calculating the peak area above the line connecting the third and fourth intersection points of the X-ray diffraction pattern to obtain a fourth area; obtaining the peak-to-valley ratio based on the third area and the fourth area, and using the peak-to-valley ratio as the roughness index.

[0101] More specifically, the coarsening index determination module 22 is used to: calculate the peak-to-valley ratio based on the third area and the fourth area using a preset second formula; wherein, the second formula is: D2=(S3-S4) / S3*100%, D2 represents the peak-to-valley ratio, S3 represents the third area, and S4 represents the fourth area.

[0102] Specifically, the calculation module 23 is used to calculate the crystallinity index of tungsten carbide using a preset third formula based on the micro-strain index, the peak-to-valley ratio, and the α-separation index; wherein the third formula is: A=[1-100*(σ1+σ2)+(1-D1)+(1-D2)]*100%, where A represents the crystallinity index of tungsten carbide, σ1 represents the first micro-strain index, σ2 represents the second micro-strain index, D1 represents the α-separation index, and D2 represents the peak-to-valley ratio.

[0103] For specific details regarding the aforementioned tungsten carbide crystallinity determination device, please refer to the relevant documentation. Figures 1 to 4 The relevant descriptions and effects in the illustrated embodiments are for understanding purposes only and will not be repeated here.

[0104] Example 3

[0105] This invention also provides an electronic device, such as... Figure 6 As shown, the electronic device may include a processor 61 and a memory 62, wherein the processor 61 and the memory 62 may be connected via a bus or other means. Figure 6 Taking the example of a connection between China and Israel via a bus.

[0106] Processor 61 can be a central processing unit (CPU). Processor 61 can also be other general-purpose processors, digital signal processors (DSPs), application-specific integrated circuits (ASICs), field-programmable gate arrays (FPGAs), or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components, or combinations of the above types of chips.

[0107] Memory 62, as a non-transitory computer-readable storage medium, can be used to store non-transitory software programs, non-transitory computer-executable programs, and modules, such as the program instructions / modules corresponding to the tungsten carbide crystallization degree determination method of this invention (e.g., Figure 5The acquisition module 20, integrity index determination module 21, coarsening index determination module 22, and calculation module 23 are shown. The processor 61 executes various functional applications and data processing by running non-transitory software programs, instructions, and modules stored in the memory 62, thereby realizing the tungsten carbide crystallization degree determination method in the above method embodiments.

[0108] The memory 62 may include a program storage area and a data storage area. The program storage area may store the operating system and applications required for at least one function; the data storage area may store data created by the processor 61, etc. Furthermore, the memory 62 may include high-speed random access memory and may also include non-transitory memory, such as at least one disk storage device, flash memory device, or other non-transitory solid-state storage device. In some embodiments, the memory 62 may optionally include memory remotely located relative to the processor 61, and these remote memories may be connected to the processor 61 via a network. Examples of such networks include, but are not limited to, the Internet, corporate intranets, local area networks, mobile communication networks, and combinations thereof.

[0109] The one or more modules are stored in the memory 62, and when executed by the processor 61, they perform the following: Figure 1-3 The method for determining the degree of tungsten carbide crystallinity in the illustrated embodiment.

[0110] For specific details regarding the aforementioned electronic devices, please refer to the relevant documentation. Figures 1 to 5 The relevant descriptions and effects in the illustrated embodiments are for understanding purposes only and will not be repeated here.

[0111] Those skilled in the art will understand that all or part of the processes in the methods of the above embodiments can be implemented by a computer program instructing related hardware. The program can be stored in a computer-readable storage medium, and when executed, it can include the processes of the embodiments of the methods described above. The storage medium can be a magnetic disk, optical disk, read-only memory (ROM), random access memory (RAM), flash memory, hard disk drive (HDD), or solid-state drive (SSD), etc.; the storage medium can also include combinations of the above types of memory.

[0112] Although embodiments of the invention have been described in conjunction with the accompanying drawings, those skilled in the art can make various modifications and variations without departing from the spirit and scope of the invention, and such modifications and variations all fall within the scope defined by the appended claims.

Claims

1. A method for determining the degree of crystallinity of tungsten carbide, characterized in that, include: Obtain the X-ray diffraction pattern of tungsten carbide; The X-ray diffraction pattern is subjected to a first differential characterization to obtain an integrity index; The X-ray diffraction pattern is subjected to a second differential characterization to obtain a coarsening index; The crystallinity index of the tungsten carbide is calculated based on the integrity index and the coarsening index. The first differential characterization of the X-ray diffraction pattern yields the following integrity indices: Microstrain analysis was performed on the X-ray diffraction pattern to obtain microstrain indices; and, or; Peak shape analysis was performed on the first designated crystal plane of the X-ray diffraction pattern to obtain the α separation index; The microstrain analysis of the X-ray diffraction pattern yields the following microstrain indices: Microstrain analysis was performed on the X-ray diffraction pattern using the WH method to obtain the first microstrain index of the first group of crystal planes and the second microstrain index of the second group of crystal planes. The first group of crystal planes belongs to the (h00) crystal plane family; the second group of crystal planes belongs to the (00l) crystal plane family. The peak shape analysis of the first designated crystal plane of the X-ray diffraction pattern to obtain the α separation index includes: Obtain the corresponding crystal planes in the first designated crystal plane of the X-ray diffraction pattern. The corresponding first diffraction peak and The corresponding second diffraction peak; Obtain the first lowest point between the first diffraction peak and the second diffraction peak; A first straight line parallel to a preset straight line is drawn through the first lowest point. The first straight line intersects the first diffraction peak and the second diffraction peak to obtain the first intersection point and the second intersection point. Calculate the peak area above the line connecting the first and second intersection points to obtain the first area; Calculate the total area of ​​the first diffraction peak and the second diffraction peak to obtain the second area; The α separation index is obtained based on the first area and the second area; The step of obtaining the α separation index based on the first area and the second area includes: calculating the α separation index using a preset first formula based on the first area and the second area; The first formula is: D1=(S2-S1) / S2*100%, where D1 represents the α separation index, S1 represents the first area, and S2 represents the second area. The X-ray diffraction pattern was subjected to a second differential characterization to obtain coarsening indices, including: The second lowest point between the diffraction peaks of the second specified crystal plane region is selected within the preset diffraction angle range of the X-ray diffraction pattern. A second straight line parallel to the preset straight line is drawn through the second lowest point. The second straight line intersects the diffraction peak of the region, resulting in a third intersection point and a fourth intersection point. Calculate the peak area above the preset straight line and within the diffraction angle range in the X-ray diffraction pattern to obtain the third area; Calculate the peak area above the line connecting the third and fourth intersection points in the X-ray diffraction pattern to obtain the fourth area; The peak-to-valley ratio is obtained based on the third area and the fourth area, and the peak-to-valley ratio is used as the coarsening index. The step of obtaining the peak-to-valley ratio based on the third area and the fourth area includes: calculating the peak-to-valley ratio using a preset second formula based on the third area and the fourth area; The second formula is: D2=(S3-S4) / S3*100%, where D2 represents the peak-to-valley ratio, S3 represents the third area, and S4 represents the fourth area. The step of calculating the crystallinity index of tungsten carbide based on the microstrain index, the peak-to-valley ratio, and the α-separation index includes: calculating the crystallinity index of tungsten carbide using a preset third formula based on the microstrain index, the peak-to-valley ratio, and the α-separation index; wherein the third formula is: A = [1 - 100 * (σ1 + σ2) + (1 - D1) + (1 - D2)] * 100%, where A represents the crystallinity index of the tungsten carbide, σ1 represents the first micro-strain index, σ2 represents the second micro-strain index, D1 represents the α-separation index, and D2 represents the peak-to-valley ratio.

2. The method according to claim 1, characterized in that, The first designated crystal plane is the (112) crystal plane.

3. The method according to claim 1, characterized in that, The second designated crystal plane is crystal plane (210)(003)(202).

4. A device for determining the degree of tungsten carbide crystallization, characterized in that, include: The acquisition module is used to acquire the X-ray diffraction pattern of tungsten carbide; The integrity index determination module is used to perform a first differential characterization on the X-ray diffraction pattern to obtain the integrity index; The coarsening index determination module is used to perform a second differential characterization on the X-ray diffraction pattern to obtain the coarsening index; A calculation module is used to obtain the crystallinity index of the tungsten carbide based on the integrity index and the coarsening index; The integrity index determination module includes a micro-strain index determination unit and / or an α-separation index determination unit; The microstrain index determination unit is specifically used to: perform microstrain analysis on the X-ray diffraction pattern using the WH method to obtain the first microstrain index of the first group of crystal planes and the second microstrain index of the second group of crystal planes; wherein, the first group of crystal planes belongs to the (h00) crystal plane family; and the second group of crystal planes belongs to the (00l) crystal plane family. The α separation index determination unit is specifically used to: obtain the α separation index from the first designated crystal plane of the X-ray diffraction pattern, respectively. The corresponding first diffraction peak and The corresponding second diffraction peak; obtain the first lowest point between the first diffraction peak and the second diffraction peak; draw a first straight line parallel to a preset straight line through the first lowest point, the first straight line intersecting the first diffraction peak and the second diffraction peak to obtain a first intersection point and a second intersection point; calculate the peak area above the line connecting the first intersection point and the second intersection point to obtain a first area; calculate the total area of ​​the first diffraction peak and the second diffraction peak to obtain a second area; obtain the α separation index based on the first area and the second area; The α separation index determining unit is specifically used to: calculate the α separation index based on the first area and the second area using a preset first formula; wherein, the first formula is: D1=(S2-S1) / S2*100%, D1 represents the α separation index, S1 represents the first area, and S2 represents the second area; The roughness index determination module is specifically used for: selecting a second lowest point between diffraction peaks in a second specified crystal plane region within a preset diffraction angle range of the X-ray diffraction pattern; drawing a second straight line parallel to a preset straight line through the second lowest point, the second straight line intersecting the diffraction peaks in the region to obtain a third intersection point and a fourth intersection point; calculating the peak area above the preset straight line and within the diffraction angle range in the X-ray diffraction pattern to obtain a third area; calculating the peak area above the line connecting the third and fourth intersection points in the X-ray diffraction pattern to obtain a fourth area; obtaining the peak-to-valley ratio based on the third area and the fourth area, and using the peak-to-valley ratio as the roughness index; The coarsening index determination module is specifically used to: calculate the peak-to-valley ratio based on the third area and the fourth area using a preset second formula; wherein, the second formula is: D2=(S3-S4) / S3*100%, D2 represents the peak-to-valley ratio, S3 represents the third area, and S4 represents the fourth area; The calculation module is specifically used to: calculate the crystallinity index of tungsten carbide using a preset third formula based on the micro-strain index, the peak-to-valley ratio, and the α-separation index; wherein the third formula is: A=[1-100*(σ1+σ2)+(1-D1)+(1-D2)]*100%, where A represents the crystallinity index of tungsten carbide, σ1 represents the first micro-strain index, σ2 represents the second micro-strain index, D1 represents the α-separation index, and D2 represents the peak-to-valley ratio.

5. An electronic device, characterized in that, include: The system includes a memory and a processor, which are interconnected. The memory stores computer instructions, and the processor executes the computer instructions to perform the method for determining the degree of tungsten carbide crystallization as described in any one of claims 1 to 3.

6. A computer-readable storage medium, characterized in that, The computer-readable storage medium stores computer instructions for causing the computer to perform the method for determining the degree of tungsten carbide crystallinity as described in any one of claims 1 to 3.

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