Method and device for characterizing crystallization degree of tungsten carbide powder with core-shell structure

Abstract

The invention relates to a core-shell structure tungsten carbide powder crystallization degree characterization method and device and computer equipment. The core-shell structure tungsten carbide powder crystallization degree characterization method comprises the steps that X-ray diffraction patterns of a core part and a shell part of core-shell structure tungsten carbide powder are obtained; determining a to-be-analyzed object phase and a corresponding diffraction peak in the X-ray diffraction pattern; judging whether the diffraction peak of the to-be-analyzed object phase has an overlapped peak region or not; selecting at least one preset crystal face diffraction peak when the diffraction peak of the to-be-analyzed object phase does not have the overlapping peak region; respectively obtaining the peak position and the full width at half maximum of each preset crystal face diffraction peak in the to-be-analyzed object phase; and determining the peak-to-valley ratio of the to-be-analyzed phase according to the peak position and the full width at half maximum of each preset crystal face diffraction peak. The method comprises the following steps: respectively acquiring X-ray diffraction patterns of a core part and a shell part of the tungsten carbide powder with the core-shell structure, and quantitatively characterizing the crystallinity of phases to be analyzed of the core part and the shell part of the tungsten carbide powder with the core-shell structure according to a peak-valley ratio.

Description

Technical Field

[0001] The invention relates to the technical field of X-ray diffraction spectrum analysis, and in particular to a method, a device and a computer device for characterizing the crystallinity of a core-shell structured tungsten carbide powder. Background Art

[0002] For many industrial products, the raw materials are mostly powder systems, including single-phase single-particle powder, multi-phase single-particle mixed powder, and multi-phase core-shell structure powder. Among them, the core-shell structure powder system refers to the particles in the powder having a core-shell structure, and each shell layer is single-phase or multi-phase.

[0003] The phase composition and corresponding crystal structure information of the powder are particularly important, which largely determines the organizational structure and related properties of the subsequent products. In the prior art, X-ray diffraction (XRD for short) is usually used to characterize the composition and corresponding crystal structure (such as crystallinity) of single-phase single-particle powders, but the XRD transmission depth is usually less than 10μm. When the shell thickness of the core-shell structure powder is greater than 10μm or the average particle size of the core-shell structure powder is greater than 20μm, the XRD transmission depth cannot cover the core of the core-shell structure powder, resulting in XRD being unable to fully characterize the crystallinity of the core-shell structure powder. The main component of the core of the core-shell structure tungsten carbide powder is W, and the main component of the shell is WC. The core or shell also includes a small amount of W2C. The core-shell structure tungsten carbide powder is the product of incomplete carbonization of tungsten powder. The degree of carbonization of tungsten powder determines the thickness of the tungsten carbide shell. How to use XRD to fully characterize the crystallinity of the core-shell structure tungsten carbide powder with a shell thickness of more than 10μm or an average powder particle size greater than 20μm is an urgent problem to be solved. Summary of the invention

[0004] In view of this, the present invention provides a method, device and computer equipment for characterizing the degree of crystallization of a core-shell structured tungsten carbide powder, which can characterize the crystallinity of different phases in the core and shell of a core-shell structured tungsten carbide powder system.

[0005] In the first aspect, the present invention provides a method for characterizing the degree of crystallization of a core-shell structured tungsten carbide powder, comprising the following steps: obtaining X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder; determining the phase to be analyzed and the corresponding diffraction peaks in the X-ray diffraction pattern; judging whether there is an overlapping peak region of the diffraction peaks of the phase to be analyzed; when there is no overlapping peak region of the diffraction peaks of the phase to be analyzed, selecting at least one crystal plane diffraction peak of a preset crystal plane; respectively obtaining the peak position and half-width at half-height of each crystal plane diffraction peak in the phase to be analyzed; and determining the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-width at half-height of each crystal plane diffraction peak.

[0006] The method for characterizing the degree of crystallinity of the core-shell structure tungsten carbide powder provided by the present invention determines the phase to be analyzed and the corresponding diffraction peak by obtaining the X-ray diffraction spectrum of the core and shell of the core-shell structure tungsten carbide powder, and determines whether there is an overlapping peak region in the diffraction spectrum of the phase to be analyzed. When there is no overlapping peak region in the phase to be analyzed, select at least one crystal plane diffraction peak of a preset crystal plane, obtain the peak position and half-height width of each crystal plane diffraction peak respectively, and determine the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-height width of each crystal plane diffraction peak. In this embodiment, by obtaining the X-ray diffraction spectrum of the core and shell of the core-shell structure tungsten carbide powder, the peak-to-valley ratio is obtained by analyzing the X-ray diffraction spectrum, and the peak-to-valley ratio can be used to characterize the crystallinity of different phases in the core and shell of the core-shell structure tungsten carbide powder system.

[0007] In an optional embodiment, determining the peak-to-valley ratio of the phase to be analyzed based on the peak position and half-width of the crystal plane diffraction peak of each preset crystal plane includes: respectively determining the back-to-bottom line, peak position and half-width of each crystal plane diffraction peak; determining the peak area dividing line of each crystal plane diffraction peak based on the peak position and half-width of each crystal plane diffraction peak; determining the first area and the second area of ​​each crystal plane diffraction peak based on the peak area dividing line of each crystal plane diffraction peak and the back-to-bottom line of each crystal plane diffraction peak; determining the peak-to-valley ratio of the phase to be analyzed based on the first area and the second area of ​​all crystal plane diffraction peaks.

[0008] In this way, the peak-to-valley ratio of different phases in the core and shell of the core-shell structured tungsten carbide powder can be accurately determined.

[0009] In an optional embodiment, the at least one preset crystal plane is selected from a first group of crystal planes or a second group of crystal planes, the first group of crystal planes includes a (220) crystal plane and a (310) crystal plane, the second group of crystal planes includes a (002) crystal plane and a (101) crystal plane, the diffraction peak of the (220) crystal plane or the (002) crystal plane corresponds to the first crystal plane diffraction peak, and the diffraction peak of the (310) crystal plane or the (101) crystal plane corresponds to the second crystal plane diffraction peak; the first crystal plane is determined according to the peak position and the half-height width of the first crystal plane diffraction peak. The peak area dividing line of the first crystal plane diffraction peak comprises: determining a first offset angle according to the half-height width of the first crystal plane diffraction peak, the first offset angle being smaller than the half-height width of the first crystal plane diffraction peak; taking the sum or difference of the peak position of the first crystal plane diffraction peak and the first offset angle as the abscissa of a first reference point on the X-axis in the X-ray diffraction spectrum; determining a first vertical line passing through the first reference point and perpendicular to the X-axis, and taking the intersection of the first vertical line and the first crystal plane diffraction peak as a second reference point; determining a vertical line passing through the second reference point and perpendicular to the back of the first crystal plane diffraction peak; a peak area dividing line of a first crystal plane diffraction peak that is parallel to the bottom line and intersects with the first crystal plane diffraction peak at a third reference point; determining the peak area dividing line of the second crystal plane diffraction peak according to the peak position and half-height width of the second crystal plane diffraction peak comprises: determining a second offset angle according to the half-height width of the second crystal plane diffraction peak, the second offset angle being greater than the half-height width of the second crystal plane diffraction peak and less than twice the half-height width of the second crystal plane diffraction peak; calculating a first difference between the half-height width of the second crystal plane diffraction peak and the half-height width of the first crystal plane diffraction peak, and calculating the second offset angle; The method comprises the following steps: determining a second difference between the angle and the first difference, and taking the third sum or the third difference between the peak position of the second crystal plane diffraction peak and the second difference as the abscissa of the fourth reference point on the X-axis in the X-ray diffraction pattern; determining a second vertical line passing through the fourth reference point and perpendicular to the X-axis, and taking the intersection of the second vertical line and the second crystal plane diffraction peak as the fifth reference point; determining a peak area dividing line of the second crystal plane diffraction peak passing through the fifth reference point and parallel to the back bottom line of the second crystal plane diffraction peak and intersecting the second crystal plane diffraction peak at the sixth reference point.

[0010] In this way, the peak area dividing line of each crystal plane diffraction peak can be accurately determined.

[0011] In an optional embodiment, determining the first area and the second area of ​​each crystal plane diffraction peak according to the peak area dividing line of each crystal plane diffraction peak and the background line of each crystal plane diffraction peak includes: calculating the first area S1 below the peak top of the first crystal plane diffraction peak and above the background line, calculating the second area S2 below the peak top of the first crystal plane diffraction peak and above the peak area dividing line, calculating the first area S3 below the peak top of the second crystal plane diffraction peak and above the background line, and calculating the second area S4 below the peak top of the second crystal plane diffraction peak and above the peak area dividing line; determining the peak-to-valley ratio of the phase to be analyzed according to the first area and the second area of ​​all crystal plane diffraction peaks includes: calculating the sum D1 of S2 and S4, the sum D2 of S1 and S3, and taking the ratio of D1 to D2 as the peak-to-valley ratio.

[0012] This allows the peak-to-valley ratio of the phase to be analyzed to be accurately determined.

[0013] In an optional embodiment, the method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder further includes the following steps: when there are overlapping peak regions in the diffraction peaks of the phase to be analyzed, determining the lowest peak shape point between the diffraction peaks of the first overlapping peak region where the diffraction peaks of the (210) crystal plane, (003) crystal plane and (202) crystal plane are located in the X-ray diffraction spectrum; drawing a first straight line parallel to the back baseline of the diffraction peak of the first overlapping peak region through the lowest peak shape, the first straight line intersecting with the diffraction peak of the first overlapping peak region to obtain a first intersection point and a second intersection point; calculating the sum of the peak areas of the diffraction peaks of the (210) crystal plane, (003) crystal plane and (202) crystal plane above the back baseline in the first overlapping peak region to obtain a third area S; calculating the sum of the peak areas of the diffraction peaks of the (210) crystal plane, (003) crystal plane and (202) crystal plane above the line connecting the first intersection point and the second intersection point in the first overlapping peak region to obtain a fourth area S'; obtaining the peak-to-valley ratio of the multi-shell powder according to the ratio S of the fourth area S' to the third area.

[0014] Therefore, the method for characterizing the degree of crystallization of core-shell structured tungsten carbide powder can be applied to both the cases where the X-ray diffraction spectrum of the phase to be analyzed has overlapping peak regions and the cases where the X-ray diffraction spectrum does not have overlapping peak regions, and can fully characterize the degree of crystallization of core-shell structured tungsten carbide powder.

[0015] In an optional embodiment, obtaining the X-ray diffraction spectrum of the core-shell structure tungsten carbide powder includes: testing the sample of the core-shell structure tungsten carbide powder to be tested using an X-ray diffractometer to obtain the X-ray diffraction spectrum of the shell portion; obtaining the X-ray diffraction spectrum of the core-shell structure tungsten carbide powder also includes: testing the polished sample of the core-shell structure tungsten carbide powder to be tested using an X-ray diffractometer to obtain the X-ray diffraction spectrum of the core portion; wherein the polished sample of the core-shell structure tungsten carbide powder to be tested is prepared by the following method: filling the core-shell structure tungsten carbide powder into the empty groove on the glass slide, compacting and scraping it to the same level as the edge of the empty groove; dripping glue into the core-shell structure tungsten carbide powder in the empty groove and heating the glass slide, waiting for the core-shell structure tungsten carbide powder to solidify, peeling off the glass slide to obtain a powder block, inlaying it with bakelite and then polishing it to obtain the polished sample of the core-shell structure tungsten carbide powder to be tested.

[0016] The X-ray diffraction pattern thus obtained can better reflect the crystal structure information of the shell and core of the core-shell structure tungsten carbide powder; and the polished sample of the core-shell structure tungsten carbide powder is prepared by glue doping, so that when the core-shell structure tungsten carbide powder is polished and tested, there is no interference peak of copper introduced by the copper doping method during X-ray diffraction, and there is no interference of glue, and the sample preparation method is also simpler than the copper doping method.

[0017] In the second aspect, the present invention also provides a device for characterizing the degree of crystallization of a core-shell structured tungsten carbide powder, comprising an acquisition module, a confirmation module, a judgment module and a processing module; the acquisition module is used to obtain the X-ray diffraction spectrum of the core and shell of the core-shell structured tungsten carbide powder; the confirmation module is used to determine the phase to be analyzed and the corresponding diffraction peaks in the X-ray diffraction spectrum; the judgment module is used to determine whether there is an overlapping peak region of the diffraction peaks of the phase to be analyzed in the X-ray diffraction spectrum; the processing module is used to select the crystal plane diffraction peaks of at least one preset crystal plane of the phase to be analyzed when there is no overlapping peak region of the diffraction peaks of the phase to be analyzed; respectively obtain the peak position and half-height width of each crystal plane diffraction peak of the phase to be analyzed; determine the peak-to-valley ratio of the phase to be analyzed in the core-shell structured tungsten carbide powder according to the peak position and half-height width of each crystal plane diffraction peak.

[0018] In a third aspect, the present invention further provides a computer device, comprising a memory and a processor, the memory and the processor being communicatively connected to each other, the memory storing computer instructions, and the processor executing the method for characterizing the degree of crystallization of core-shell tungsten carbide powder according to the first aspect or any corresponding embodiment thereof by executing the computer instructions.

[0019] In a fourth aspect, the present invention further provides a computer-readable storage medium having computer instructions stored thereon, the computer instructions being used to enable a computer to execute the method for characterizing the degree of crystallization of a core-shell structured tungsten carbide powder according to the first aspect or any corresponding embodiment thereof.

[0020] In a fifth aspect, the present invention further provides a computer program product, comprising computer instructions, the computer instructions being used to enable a computer to execute the method for characterizing the degree of crystallization of core-shell structured tungsten carbide powder according to the first aspect or any corresponding embodiment thereof. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0022] Figure 1 is a flow chart of a method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder according to an embodiment of the present invention;

[0023] Figure 2 is a flow chart of another method for characterizing the crystallinity of core-shell structured tungsten carbide powder according to an embodiment of the present invention;

[0024] Figure 3 is a schematic diagram of a sample to be tested to be polished and prepared by using a glue-doping method according to an embodiment of the present invention;

[0025] Figure 4 3 is a schematic diagram of the peak area division of the core (220) crystal plane diffraction peak of the core portion of the core-shell structured tungsten carbide powder according to an embodiment of the present invention;

[0026] Figure 5 3 is a schematic diagram of the peak area division of the core (310) crystal plane diffraction peak of the core portion of the core-shell structured tungsten carbide powder according to an embodiment of the present invention;

[0027] Figure 6 is a flow chart of another method for characterizing the crystallinity of core-shell structured tungsten carbide powder according to an embodiment of the present invention;

[0028] Figure 7 Schematic diagram of the overlapping region of the shell X-ray diffraction spectrum of the core-shell structured tungsten carbide powder according to an embodiment of the present invention;

[0029] Figure 8 is a color image schematic diagram of an EBSD observation spectrum according to an embodiment of the present invention;

[0030] Fig. 9is a schematic diagram of a black and white image of an EBSD observation spectrum according to an embodiment of the present invention;

[0031] Fig.10 is a structural block diagram of a device for characterizing the degree of crystallinity of core-shell structured tungsten carbide powder according to an embodiment of the present invention;

[0032] Fig.11 It is a schematic diagram of the hardware structure of a computer device according to an embodiment of the present invention. DETAILED DESCRIPTION

[0033] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present invention.

[0034] According to an embodiment of the present invention, an embodiment of a method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder is provided. It should be noted that the steps shown in the flowchart of the accompanying drawings can be executed in a computer system such as a set of computer executable instructions, and although a logical order is shown in the flowchart, in some cases, the steps shown or described can be executed in an order different from that shown here.

[0035] In this embodiment, a method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder is provided, which can be used in computer equipment. Figure 1 : is a flow chart of a method for characterizing the degree of crystallinity of core-shell structured tungsten carbide powder according to an embodiment of the present invention. Figure 1 As shown, the process includes the following steps:

[0036] Step S101: obtaining X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder.

[0037] In an optional embodiment, obtaining the X-ray diffraction spectrum of the shell of the core-shell structure tungsten carbide powder includes: using an X-ray diffractometer to test the sample of the core-shell structure tungsten carbide powder to obtain the X-ray diffraction spectrum of the shell. The sample of the core-shell structure tungsten carbide powder can be prepared by any preparation method in the prior art, but the sample is not polished, and the powder particle morphology is relatively complete. For example, the powder is filled into the sample slot, compacted, scraped, and the plane is flush with the edge of the slot; if the particles are large, they need to be shaken during filling to increase the powder filling density as much as possible.

[0038] In another optional embodiment, obtaining the X-ray diffraction pattern of the core of the core-shell tungsten carbide powder includes: using an X-ray diffractometer to test the polished sample of the core-shell tungsten carbide powder to obtain the X-ray diffraction pattern of the core of the core-shell tungsten carbide powder. After the core-shell tungsten carbide powder is polished, the core is exposed. The X-ray diffraction pattern thus obtained can better reflect the crystal structure information of the shell and core of the core-shell tungsten carbide powder.

[0039] Step S102: determining the phase of the substance to be analyzed and the corresponding diffraction peak in the X-ray diffraction spectrum.

[0040] Specifically, analysis software such as HighScore can be used to determine the physical phase and the corresponding diffraction peak.

[0041] Step S103: determining whether the diffraction peaks of the phase to be analyzed have overlapping peak regions.

[0042] Step S104: when the diffraction peaks of the phase to be analyzed do not have overlapping peak regions, selecting at least one crystal plane diffraction peak of a preset crystal plane.

[0043] Step S105: respectively obtaining the peak position and half-height width of each crystal plane diffraction peak in the phase to be analyzed.

[0044] Step S106: determining the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-height width of each crystal plane diffraction peak.

[0045] The method for characterizing the degree of crystallinity of the core-shell tungsten carbide powder provided in this embodiment is to obtain the X-ray diffraction patterns of the core and shell of the core-shell tungsten carbide powder, determine the phase to be analyzed and the corresponding diffraction peak, and judge whether there is an overlapping peak region in the diffraction pattern of the phase to be analyzed. When there is no overlapping peak region in the phase to be analyzed, select at least one crystal plane diffraction peak of a preset crystal plane, obtain the peak position and half-width of each crystal plane diffraction peak respectively, and determine the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-width of each crystal plane diffraction peak. In this embodiment, by obtaining the X-ray diffraction patterns of the core and shell of the core-shell tungsten carbide powder, the peak-to-valley ratio is obtained by analyzing the X-ray diffraction patterns, and the peak-to-valley ratio can be used to characterize the crystallinity of different phases in the core and shell of the core-shell tungsten carbide powder system.

[0046] In this embodiment, a method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder is provided, which can be used in computer equipment. Figure 2 FIG. 1 is a flow chart of another method for characterizing the crystallinity of core-shell structured tungsten carbide powder according to an embodiment of the present invention. Figure 2 As shown, the process includes the following steps:

[0047] Step S201: obtaining X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder.

[0048] In this embodiment, obtaining X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder includes: testing the polished sample of the core-shell structured tungsten carbide powder using an X-ray diffractometer to obtain an X-ray diffraction pattern.

[0049] Among them, the polished sample to be tested of the core-shell structure tungsten carbide powder can be prepared by copper doping, or by glue doping, and the physical phase of the glue used for glue doping has no diffraction peak in the XRD spectrum. Specifically, the copper doping method is to mix copper powder with the core-shell structure tungsten carbide powder, press and sinter to obtain a pseudo alloy, and then polish the pseudo alloy to obtain a polished sample to be tested. Preferably, the polished sample to be tested of the core-shell structure tungsten carbide powder is prepared by glue doping, so that the polished sample to be tested of the core-shell structure tungsten carbide powder does not have the interference peak of copper introduced by the copper doping method when performing X-ray diffraction, and there is no interference of glue, and the sample preparation method of glue doping is simpler, without pressing and sintering.

[0050] Specifically, the polished sample of the core-shell structure tungsten carbide powder to be tested can be prepared by the following method by mixing with glue: fill the core-shell structure tungsten carbide powder into the empty groove on the glass slide, compact and level it to the level of the edge of the empty groove; drip glue into the core-shell structure tungsten carbide powder in the empty groove and heat the glass slide, wait for the core-shell structure tungsten carbide powder to solidify, peel off the glass slide to obtain a powder block, inlay it with bakelite and then polish it to obtain the polished sample of the core-shell structure tungsten carbide powder to be tested.

[0051] For example, take a hollow glass trough and fit it to a glass slide, fill the powder in the trough, vibrate and scrape it flat. Take a few drops of glue A and glue B and dilute them with alcohol in a drying dish. Place the glass slide loaded with powder and the drying dish on a heating table. Pour the diluted glue A into the powder, and then pour glue B after it dries. After the powder is dry, repeat the process once. When the powder is finer, repeat the process 2-3 times. After heating on a heating table at 100°C for 8-12 hours, it can be solidified into a powder block. Take the powder block out from the glass slide, such as Figure 3 After being inlaid with bakelite, the sample was polished to expose the core phase, and the sample to be tested was obtained after polishing.

[0052] Among them, A glue and B glue are collectively called AB glue. AB glue is a two-component (two-part) chemical reaction adhesive, usually composed of a resin component (A component) and a hardener component (B component). When used, after the two are mixed in a certain proportion, a chemical reaction will occur and solidify, thereby forming a strong bond. The physical phase of the AB glue selected in this embodiment has no diffraction peak in the XRD spectrum.

[0053] In this embodiment, a conventional sample preparation method can be used to prepare a sample of core-shell structured tungsten carbide powder to be tested, and the peak-to-valley ratio obtained by analyzing the X-ray diffraction pattern obtained by the test can be called the shell crystallinity; the peak-to-valley ratio obtained by analyzing the X-ray diffraction pattern obtained by testing the polished sample of core-shell structured tungsten carbide powder can be called the core crystallinity.

[0054] Step S202: determining the phase of the substance to be analyzed and the corresponding diffraction peak in the X-ray diffraction spectrum.

[0055] The polished sample was tested to obtain an X-ray diffraction pattern. The specific test conditions are as follows: Co target, scanning angle 10-150°, step length 0.03°, and dwell time 20-50s per step. The measuring instrument is Panalytical X'Pert PRO X-ray diffractometer.

[0056] Step S203: determining whether the diffraction peaks of the phase to be analyzed have overlapping peak regions.

[0057] Step S204: When there is no overlapping peak region in the X-ray diffraction spectrum, selecting a crystal plane diffraction peak of at least one preset crystal plane.

[0058] It should be noted that when there is no overlapping peak region in the X-ray diffraction pattern, the more crystal plane diffraction peaks are selected, the more accurate the peak-to-valley ratio is calculated.

[0059] For example, the tungsten carbide powder of the present invention is mainly composed of WC in the shell part and W in the core part due to incomplete carbonization, and the shell part or the core part also includes a small amount of W2C. Usually, there are no overlapping peaks in the XRD diffraction peaks of the W phase and the W2C phase, and there are overlapping peaks in the XRD diffraction peaks of the WC phase. The X-ray diffraction spectrum of the W phase in the core part does not have an overlapping peak area. In this case, two adjacent independent diffraction peaks can be selected for analysis, such as Figure 4 and Figure 5As shown, (220) crystal plane and (310) crystal plane are selected for analysis. It should be noted that the adjacent diffraction peaks can reduce the error, because the diffraction patterns in the low-angle and high-angle ranges are affected by different factors when the instrument is tested; for example, the low-angle X-ray irradiation area is large, and the high-angle irradiation area is relatively small, and the relative intensity of diffraction will be affected. There is no overlapping peak region in the X-ray diffraction spectrum of the W2C phase in the core or shell, and the (002) crystal plane and the (101) crystal plane are selected for analysis. Since the process of obtaining the peak-to-valley ratio of the (002) crystal plane diffraction peak is the same as the process of obtaining the peak-to-valley ratio of the (220) crystal plane diffraction peak, and the process of obtaining the peak-to-valley ratio of the (101) crystal plane diffraction peak is the same as the process of obtaining the peak-to-valley ratio of the (310) crystal plane diffraction peak, only the process of obtaining the peak-to-valley ratio of the (220) crystal plane diffraction peak and the peak-to-valley ratio of the (310) crystal plane diffraction peak will be described below, and the process of obtaining the peak-to-valley ratio of the (002) crystal plane diffraction peak and the peak-to-valley ratio of the (101) crystal plane diffraction peak will not be repeated.

[0060] Step S205: respectively obtaining the peak position and half-height width of each crystal plane diffraction peak in the phase to be analyzed.

[0061] like Figure 4 As shown in the figure, the peak position of the (220) crystal plane diffraction peak is θ1, and the half-maximum width is FWHM1. Figure 5 As shown, the peak position of the (310) crystal plane diffraction peak is θ2, and the half-width is FWHM2.

[0062] Step S206: determining the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-width at half maximum of each crystal plane diffraction peak.

[0063] In an optional embodiment, determining the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-height width of each crystal plane diffraction peak includes the following steps:

[0064] Step S2061: respectively determine the background line, peak position and half-height width of each crystal plane diffraction peak.

[0065] Step S2062: determining the peak area dividing line of each crystal plane diffraction peak according to the peak position and half-height width of each crystal plane diffraction peak.

[0066] For example, Figure 4 and Figure 5 As shown, at least one crystal plane includes a (220) crystal plane and a (310) crystal plane, and the diffraction peaks of the (220) crystal plane and the (310) crystal plane correspond to the first crystal plane diffraction peak and the second crystal plane diffraction peak, respectively.

[0067] like Figure 4As shown, determining the peak area dividing line of the first crystal plane diffraction peak based on the peak position and full width at half maximum of the first crystal plane diffraction peak includes: determining a first offset angle based on the full width at half maximum of the first crystal plane diffraction peak, the first offset angle being less than the full width at half maximum of the first crystal plane diffraction peak; using the sum or difference of the peak position of the first crystal plane diffraction peak and the first offset angle as the abscissa of the first reference point A on the X-axis in the X-ray diffraction pattern; determining a first perpendicular line passing through the first reference point A and perpendicular to the X-axis, and using the intersection point of the first perpendicular line and the first crystal plane diffraction peak as the second reference point B; determining the peak area dividing line of the first crystal plane diffraction peak that passes through the second reference point B and is parallel to the background bottom line of the first crystal plane diffraction peak and intersects the first crystal plane diffraction peak at the third reference point C.

[0068] That is to say, the peak position of the (220) crystal plane diffraction peak is θ1, the full width at half maximum is FWHM1, and the abscissa θ L = θ1 ± θ i1 , draw a perpendicular line through A to intersect the (220) crystal plane diffraction peak at point B, and draw a line parallel to the background bottom line through point B to intersect the (220) crystal plane diffraction peak at point C. Among them, the first offset angle θ i1 satisfies 0 < θ i1 < FWHM1. In Example 1 and Example 2, θ i1 = 0.5°

[0069] As Figure 5 shown, determining the peak area dividing line of the second crystal plane diffraction peak based on the peak position and full width at half maximum of the second crystal plane diffraction peak includes: determining a second offset angle based on the full width at half maximum of the second crystal plane diffraction peak, the second offset angle being greater than the full width at half maximum of the second crystal plane diffraction peak and less than twice the full width at half maximum of the second crystal plane diffraction peak; calculating a first difference between the full width at half maximum of the second crystal plane diffraction peak and the full width at half maximum of the first crystal plane diffraction peak, and calculating a second difference between the second offset angle and the first difference, and using the third sum or third difference between the peak position of the second crystal plane diffraction peak and the second difference as the abscissa of the fourth reference point D on the X-axis in the X-ray diffraction pattern; determining a second perpendicular line passing through the fourth reference point D and perpendicular to the X-axis, and using the intersection point of the second perpendicular line and the second crystal plane diffraction peak as the fifth reference point E; determining the peak area dividing line of the second crystal plane diffraction peak that passes through the fifth reference point E and is parallel to the background bottom line of the second crystal plane diffraction peak and intersects the second crystal plane diffraction peak at the sixth reference point F.

[0070] That is to say, the peak position of the (310) crystal plane diffraction peak is θ2, the full width at half maximum is FWHM2, and the abscissa θ R = θ2 ± [θ i2 - (FWHM2 - FWHM1)], draw a perpendicular line through D to intersect the (310) crystal plane diffraction peak at point E, and draw a line parallel to the background bottom line through E to intersect the (310) crystal plane diffraction peak at point F. Among them, the second offset angle θ i2Satisfy FWHM2<θ i2 <2FWHM2, in Example 1 and Example 2, θ i2 =1°.

[0071] Step S2063: determining the first area and the second area of ​​each crystal plane diffraction peak according to the peak area dividing line of each crystal plane diffraction peak and the background line of each crystal plane diffraction peak.

[0072] In an optional embodiment, determining the first area and the second area of ​​each crystal plane diffraction peak according to the peak area dividing line of each crystal plane diffraction peak and the back bottom line of each crystal plane diffraction peak includes the following steps: calculating the first area S1 below the peak top of the first crystal plane diffraction peak and above the back bottom line, calculating the second area S2 below the peak top of the first crystal plane diffraction peak and above the peak area dividing line, calculating the first area S3 below the peak top of the second crystal plane diffraction peak and above the back bottom line, and calculating the second area S4 below the peak top of the second crystal plane diffraction peak and above the peak area dividing line.

[0073] For example, Figure 4 As shown in , the peak area of ​​the first crystal plane diffraction peak above the background line is S1, and the peak area of ​​the first crystal plane diffraction peak above the peak area dividing line BC is S2. Figure 5 As shown, the peak area of ​​the second crystal plane diffraction peak above the back bottom line is S3, and the peak area of ​​the second crystal plane diffraction peak above the peak area dividing line EF is S4.

[0074] Step S2064: determining the peak-to-valley ratio of the phase to be analyzed according to the first area and the second area of ​​all crystal plane diffraction peaks.

[0075] In an optional embodiment, determining the peak-to-valley ratio of the phase to be analyzed based on the first area and the second area of ​​all crystal plane diffraction peaks includes the following steps: calculating the sum D1 of S2 and S4, the sum D2 of S1 and S3, and taking the ratio of D1 to D2 as the peak-to-valley ratio. In other words, the peak-to-valley ratio can be calculated using the following formula: D = (S2 + S4) / (S1 + S3) * 100%.

[0076] In this embodiment, by obtaining the X-ray diffraction patterns of the core and shell of the core-shell tungsten carbide powder, the peak-to-valley ratio is obtained by analyzing the X-ray diffraction patterns, and the peak-to-valley ratio can be used to characterize the crystallinity of the different phases of the shell and core in the core-shell tungsten carbide powder system. Furthermore, the polished sample of the core-shell tungsten carbide powder is prepared by glue doping, so that the cross-sectional peak area dividing line of the core-shell tungsten carbide powder does not have the interference peak of copper introduced by the copper doping method when performing X-ray diffraction, and there is no interference from glue.

[0077] In this embodiment, a method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder is provided, which can be used in computer equipment. Figure 6 FIG. 1 is a flow chart of another method for characterizing the crystallinity of core-shell structured tungsten carbide powder according to an embodiment of the present invention. Figure 6 As shown, the process includes the following steps:

[0078] Step S601: Obtaining X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder.

[0079] Step S602: Determine the phase of the substance to be analyzed and the corresponding diffraction peak in the X-ray diffraction spectrum.

[0080] Step S603: Determine whether the diffraction peaks of the phase to be analyzed have overlapping peak regions. When the diffraction peaks of the phase to be analyzed do not have overlapping peak regions, proceed to step S604; when the diffraction peaks of the phase to be analyzed do have overlapping peak regions, proceed to step S607.

[0081] Step S604: selecting at least one crystal plane diffraction peak of a preset crystal plane.

[0082] Step S605: respectively obtaining the peak position and half-height width of the crystal plane diffraction peak of each preset crystal plane in the phase to be analyzed.

[0083] Step S606: determining the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-width at half maximum of each crystal plane diffraction peak.

[0084] Step S607: When there are overlapping peak regions of the diffraction peaks of the phase to be analyzed, determine the lowest point of the peak shape between the diffraction peaks in the first overlapping peak region where the diffraction peaks of the (210) crystal plane, (003) crystal plane and (202) crystal plane in the X-ray diffraction spectrum are located.

[0085] Specifically, when there are overlapping peak regions in the X-ray diffraction spectrum, the lowest point of the peak shape between the diffraction peaks in the designated crystal plane region is selected in the X-ray diffraction spectrum.

[0086] Step S608: Draw a first straight line through the lowest point of the peak shape and parallel to the back bottom line of the diffraction peak in the first overlapping peak region, and the first straight line intersects with the diffraction peak in the first overlapping peak region to obtain a first intersection point and a second intersection point.

[0087] Step S609: Calculate the sum of the peak areas of the diffraction peaks above the back bottom line, (210) crystal plane, (003) crystal plane and (202) crystal plane in the first overlapping peak region to obtain a third area S.

[0088] Step S610: Calculate the sum of the peak areas of the diffraction peaks of the (210) crystal plane, the (003) crystal plane, and the (202) crystal plane above the line connecting the first intersection and the second intersection in the first overlapping peak region to obtain a fourth area S'.

[0089] Step S611: obtaining the peak-to-valley ratio of the core-shell structured tungsten carbide powder according to the ratio S of the fourth area S' to the third area.

[0090] For example, Figure 7 As shown, the first overlapping peak region where the (210) crystal plane, (003) crystal plane and (202) crystal plane are located (when using Co target, corresponding to Figure 7 The lowest point of the peak in the 140° and 145° region is B1, and the intersection of the straight line passing through B1 and parallel to the back baseline and the peak is B3 and B4. The peak area above the back baseline is S, and the peak area above B3B4 is S'. The peak-to-valley ratio index D is defined as S' / S*100%.

[0091] Example 1

[0092] The core-shell structure WC powder of this embodiment is a coarse particle powder, denoted as sample 1#, with a powder particle size of 45-75μm, and the XRD transmission depth is ≤10μm, so the X-ray cannot irradiate and cover the core of the powder particles. The EBSD (Electron Backscatter Diffraction) results are as follows: Figure 8 and Fig. 9 As shown, the main phase component of the shell is WC, with a thickness of about 1-2μm, and the shell also includes a small amount of W2C phase. The main phase component of the core is W. Sample 1# was processed by different ball milling processes to obtain samples 1#-1 and 1#-2, among which the ball milling time of sample 1#-2 was longer. Since the shell thickness of sample 1# is much smaller than the XRD transmission depth, XRD can completely cover the shell and part of the core. The crystallinity of the WC phase and W2C phase of the shell can be characterized by the crystallinity of the shell.

[0093] Fill the powders of sample 1#, sample 1#-1 and sample 1#-2 into the sample slot respectively, shake, compact and flatten them, and make the plane level with the edge of the slot to obtain the test samples of 1#, 1#-1 and 1#-2 core-shell structure tungsten carbide powders; after obtaining the spectrum by XRD test, according to the crystallinity characterization method of the core-shell structure tungsten carbide powder of the present invention, the shell crystallinity of WC and W2C phases before and after ball milling is obtained respectively, and recorded in Table 1.

[0094] Table 1 Shell crystallinity of WC, W and W2C phases (%)

[0095]

[0096] As shown in Table 1. Theoretically, as the ball milling time increases, the powder grain size becomes smaller, the submicron phase increases, the defects increase, and the degree of crystallization decreases. As can be seen from Table 1, the shell crystallinity of WC and W2C decreases after ball milling. Since the ball milling time of 1#-2 is longer, the degree of crystallization decreases more, which is consistent with conventional cognition, indicating that it is feasible to use the peak-to-valley ratio index to characterize the trend change of the degree of crystallization of the phase. In addition, since the degree of crystallization of W2C also decreases after ball milling, it means that the WC shell of the particles has been destroyed after ball milling, which is also proved by observing the EBSD map.

[0097] Take sample 1# of core-shell structure tungsten carbide powder and fill it into the empty groove on the glass slide, vibrate and scrape it flat. Take a few drops of glue A and glue B and dilute them in alcohol in a drying dish. Place the glass slide loaded with powder and the drying dish on a heating table. Pour the diluted glue A into the powder, and then pour the glue B after drying. After the powder is dried, repeat the process once. After heating at 100°C on the heating table for 8-12 hours, it can be solidified into a powder block. The powder block is taken out from the glass slide, polished after bakelite inlay to expose the core phase, and samples 1#-3 are obtained after polishing. After obtaining the spectrum by XRD test, the core crystallinity after polishing of the W phase is obtained according to the characterization method of the degree of crystallization of the core-shell structure tungsten carbide powder of the present invention, and recorded in Table 2 together with the shell crystallinity obtained in Table 1 above.

[0098] Table 2W phase crystallinity (%)

[0099]

[0100] It can be seen from Table 2 that after polishing, the crystallinity of the core of the W phase is similar to that of the shell, indicating that the crystallinity of W in the particles is relatively uniform from the outside to the inside. After ball milling, the crystallinity of the shell of the W phase is much lower than that of the core, indicating that the grain integrity of the W phase has been severely damaged.

[0101] Example 2

[0102] The core-shell structure WC powder of this embodiment is a coarse-grained powder, denoted as sample 2# and sample 3#. Sample 2# and sample 3# are obtained by carbonizing the same W powder raw material. The carbonization temperature of sample 3# is higher and the insulation time is longer. The particle size of the powder of sample 2# and sample 3# is 45-75μm, and the XRD transmission depth is ≤10μm, and the X-ray cannot irradiate and cover the core of the powder particles. The EBSD observation results show that the thickness of the outer shell WC is about 15μm. Since the shell thickness of sample 2# and sample 3# powder is much greater than the XRD transmission depth, XRD can only cover the WC phase of the outer shell of the powder particles, and cannot cover the W2C phase and W phase of the core. The crystallinity of the WC phase, W2C phase and W phase needs to be characterized in combination with the crystallinity of the shell and the crystallinity of the core.

[0103] Fill the powders of sample 2# and sample 3# into the sample groove respectively, shake, compact and flatten them, and make the plane level with the edge of the groove to obtain the test samples of core-shell structure tungsten carbide powder of sample 2# and sample 3#; after obtaining the spectrum by XRD test, according to the characterization method of the degree of crystallization of core-shell structure tungsten carbide powder of the present invention, the shell crystallinity of WC phase of sample 2# and sample 3# is obtained respectively.

[0104] After polishing the 2# and 3# samples by glue doping, the 2#-1 and 3#-1 samples to be tested were obtained. After obtaining the spectrum by XRD test, the WC phase, W2C phase and core crystallinity of the W phase after polishing of the 2#-1 and 3#-1 samples to be tested were obtained according to the characterization method of the degree of crystallization of the core-shell structure tungsten carbide powder of the present invention, and recorded in Table 3.

[0105] Table 3 Crystallinity of WC, W and W2C phases (%)

[0106]

[0107] As can be seen from Table 3, since sample 2# and sample 3# are obtained by carbonizing the same W powder raw material, the core crystallinity of sample 2#-1 W is similar to that of sample 3#-1, which is consistent with conventional cognition. Since the carbonization temperature of sample 3# is higher and the holding time is longer, the shell crystallinity of WC of sample 3# is greater than that of sample 2#, and the difference in the degree of crystallization between the shell and core of WC of sample 3# is small, which is consistent with conventional cognition, indicating the reliability of the method for characterizing the degree of crystallization of the core-shell structure tungsten carbide powder of the present invention.

[0108] In this embodiment, a device for characterizing the degree of crystallization of tungsten carbide powder with a core-shell structure is also provided, which is used to implement the above-mentioned embodiments and preferred embodiments, and the descriptions that have been made will not be repeated. As used below, the term "module" can implement a combination of software and / or hardware for a predetermined function. Although the device described in the following embodiments is preferably implemented in software, the implementation of hardware, or a combination of software and hardware, is also possible and conceived.

[0109] This embodiment provides a device for characterizing the crystallinity of core-shell tungsten carbide powder. Fig.10 As shown, including:

[0110] An acquisition module 1201 is used to obtain X-ray diffraction patterns of the shell and core of the core-shell structured tungsten carbide powder;

[0111] Confirmation module 1202, used to determine the phase of the substance to be analyzed and the corresponding diffraction peak in the X-ray diffraction spectrum;

[0112] A judgment module 1203 is used to judge whether there is an overlapping peak region of the diffraction peaks of the phase to be analyzed in the X-ray diffraction spectrum;

[0113] Processing module 1204 is used to select at least one preset crystal plane diffraction peak of the phase to be analyzed when there is no overlapping peak area of ​​the diffraction peak of the phase to be analyzed; obtain the peak position and half-height width of each crystal plane diffraction peak of the phase to be analyzed respectively; and determine the peak-to-valley ratio of the core-shell structure tungsten carbide powder phase to be analyzed according to the peak position and half-height width of each crystal plane diffraction peak.

[0114] In some optional embodiments, the processing module 1204 includes an acquisition unit, a peak area segmentation line determination unit, an area calculation unit, and a peak-to-valley ratio calculation unit. The acquisition unit is used to respectively determine the background line, peak position, and half-height width of each crystal plane diffraction peak; the peak area segmentation line determination unit is used to determine the peak area segmentation line of each crystal plane diffraction peak according to the peak position and half-height width of each crystal plane diffraction peak; the area calculation unit is used to determine the first area and the second area of ​​each crystal plane diffraction peak according to the peak area segmentation line of each crystal plane diffraction peak and the background line of each crystal plane diffraction peak; the peak-to-valley ratio calculation unit is used to determine the peak-to-valley ratio of the phase to be analyzed according to the first area and the second area of ​​all crystal plane diffraction peaks.

[0115] In some optional embodiments, at least one preset crystal plane is selected from the first group of crystal planes or the second group of crystal planes, the first group of crystal planes includes the (220) crystal plane and the (310) crystal plane, the second group of crystal planes includes the (002) crystal plane and the (101) crystal plane, the diffraction peak of the (220) crystal plane or the (002) crystal plane corresponds to the first crystal plane diffraction peak, and the diffraction peak of the (310) crystal plane or the (101) crystal plane corresponds to the second crystal plane diffraction peak. The peak area dividing line determination unit is specifically used to: determine a first offset angle according to the half-width at half height of the first crystal plane diffraction peak, the first offset angle being smaller than the half-width at half height of the first crystal plane diffraction peak; use the sum or difference of the peak position of the first crystal plane diffraction peak and the first offset angle as the horizontal coordinate of the first reference point on the X-axis in the X-ray diffraction pattern; determine a first vertical line passing through the first reference point and perpendicular to the X-axis, and use the intersection of the first vertical line and the first crystal plane diffraction peak as the second reference point; determine a peak area dividing line of the first crystal plane diffraction peak that passes through the second reference point and is parallel to the back bottom line of the first crystal plane diffraction peak and intersects with the first crystal plane diffraction peak at a third reference point. The peak area dividing line determination unit is also used to: determine a second offset angle according to the half-width at half height of the second crystal plane diffraction peak, the second offset angle being greater than the half-width at half height of the second crystal plane diffraction peak and less than twice the half-width at half height of the second crystal plane diffraction peak; calculate a first difference between the half-width at half height of the second crystal plane diffraction peak and the half-width at half height of the first crystal plane diffraction peak, and calculate a second difference between the second offset angle and the first difference, and use a third sum or a third difference between the peak position of the second crystal plane diffraction peak and the second difference as the horizontal coordinate of a fourth reference point on the X-axis in the X-ray diffraction pattern; determine a second vertical line passing through the fourth reference point and perpendicular to the X-axis, and use the intersection of the second vertical line and the second crystal plane diffraction peak as a fifth reference point; determine a peak area dividing line of the second crystal plane diffraction peak that passes through the fifth reference point and is parallel to the back bottom line of the second crystal plane diffraction peak and intersects with the second crystal plane diffraction peak at a sixth reference point.

[0116] In some optional embodiments, the area calculation unit is specifically used to: calculate a first area S1 below the peak of the first crystal plane diffraction peak and above the back baseline, calculate a second area S2 below the peak of the first crystal plane diffraction peak and above the peak area dividing line, calculate a first area S3 below the peak of the second crystal plane diffraction peak and above the back baseline, and calculate a second area S4 below the peak of the second crystal plane diffraction peak and above the peak area dividing line.

[0117] In some optional implementations, the peak-to-valley ratio calculation unit is specifically used to calculate a sum D1 of S2 and S4, a sum D2 of S1 and S3, and take the ratio of D1 to D2 as the peak-to-valley ratio.

[0118] In some optional embodiments, the processing module 1204 is also used for: when there is an overlapping peak region of the diffraction peaks of the phase to be analyzed, determining the lowest point of the peak shape between the diffraction peaks of the first overlapping peak region where the diffraction peaks of the (210) crystal plane, (003) crystal plane and (202) crystal plane in the X-ray diffraction spectrum are located; drawing a first straight line parallel to the back baseline of the diffraction peak of the first overlapping peak region through the lowest point of the peak shape, the first straight line intersecting with the diffraction peak of the first overlapping peak region to obtain a first intersection point and a second intersection point; calculating the sum of the peak areas of the diffraction peaks of the (210) crystal plane, (003) crystal plane and (202) crystal plane above the back baseline in the first overlapping peak region to obtain a third area S; calculating the sum of the peak areas of the diffraction peaks of the (210) crystal plane, (003) crystal plane and (202) crystal plane above the line connecting the first intersection point and the second intersection point in the first overlapping peak region to obtain a fourth area S'; and obtaining the peak-to-valley ratio of the core-shell structure powder according to the ratio S of the fourth area S' to the third area.

[0119] In some optional embodiments, the acquisition module 1201 is specifically used for: testing the core-shell structure powder sample to be tested using an X-ray diffractometer to obtain an X-ray diffraction spectrum of the shell portion; testing the polished sample of the core-shell structure tungsten carbide powder to be tested using an X-ray diffractometer to obtain an X-ray diffraction spectrum of the core portion; wherein the polished sample of the core-shell structure tungsten carbide powder to be tested is prepared by the following method: filling the core-shell structure tungsten carbide powder into the empty groove on the glass slide, compacting and scraping it to the same level as the edge of the empty groove; dripping glue into the core-shell structure tungsten carbide powder in the empty groove and heating the glass slide, waiting for the core-shell structure tungsten carbide powder to solidify, peeling off the glass slide to obtain a powder block, inlaying it with bakelite and then polishing it to obtain the polished sample of the core-shell structure tungsten carbide powder to be tested.

[0120] The further functional description of each of the above modules and units is the same as that of the above corresponding embodiments and will not be repeated here.

[0121] The core-shell structure tungsten carbide powder crystallinity characterization device in this embodiment is presented in the form of a functional unit, where the unit refers to an ASIC (Application Specific Integrated Circuit) circuit, a processor and memory that executes one or more software or fixed programs, and / or other devices that can provide the above functions.

[0122] The embodiment of the present invention also provides a computer device having the above Fig.10 The device shown is used to characterize the crystallinity of the core-shell structured tungsten carbide powder.

[0123] See also Fig.11 , Fig.11 is a schematic diagram of the structure of a computer device provided by an optional embodiment of the present invention, such as Fig.11 As shown, the computer device includes: one or more processors 10, a memory 20, and interfaces for connecting various components, including high-speed interfaces and low-speed interfaces. Various components are connected to each other using different buses for communication, and can be installed on a common mainboard or installed in other ways as needed. The processor can process the instructions executed in the computer device, including instructions stored in or on the memory to display the graphical information of the GUI on an external input / output device (such as, a display device coupled to the interface). In some optional embodiments, if necessary, multiple processors and / or multiple buses can be used together with multiple memories and multiple memories. Similarly, multiple computer devices can be connected, and each device provides some necessary operations (for example, as a server array, a group of blade servers, or a multi-processor system). Fig.11 A processor 10 is taken as an example.

[0124] The processor 10 may be a central processing unit, a network processor or a combination thereof. The processor 10 may further include a hardware chip. The hardware chip may be a dedicated integrated circuit, a programmable logic device or a combination thereof. The programmable logic device may be a complex programmable logic device, a field programmable gate array, a general purpose array logic or any combination thereof.

[0125] The memory 20 stores instructions executable by at least one processor 10, so that at least one processor 10 executes the method shown in the above embodiment.

[0126] The memory 20 may include a program storage area and a data storage area, wherein the program storage area may store an operating system, an application required for at least one function; the data storage area may store data created according to the use of the computer device, etc. In addition, the memory 20 may include a high-speed random access memory, and may also include a non-transient memory, such as at least one disk storage device, a flash memory device, or other non-transient solid-state storage device. In some optional embodiments, the memory 20 may optionally include a memory remotely arranged relative to the processor 10, and these remote memories may be connected to the computer device via a network. Examples of the above-mentioned network include, but are not limited to, the Internet, an intranet, a local area network, a mobile communication network, and combinations thereof.

[0127] The memory 20 may include a volatile memory, such as a random access memory; the memory may also include a non-volatile memory, such as a flash memory, a hard disk or a solid state drive; the memory 20 may also include a combination of the above types of memory.

[0128] The computer device also includes an input device 30 and an output device 40. The processor 10, the memory 20, the input device 30 and the output device 40 may be connected via a bus or other means. Fig.11 The example of connecting through bus is taken in the following.

[0129] The input device 30 can receive input digital or character information, and generate key signal input related to the user settings and function control of the computer device, such as a touch screen, a keypad, a mouse, a track pad, a touch pad, an indicator bar, one or more mouse buttons, a trackball, a joystick, etc. The output device 40 may include a display device, an auxiliary lighting device (e.g., an LED) and a tactile feedback device (e.g., a vibration motor), etc. The above-mentioned display device includes but is not limited to a liquid crystal display, a light emitting diode, a display and a plasma display. In some optional embodiments, the display device can be a touch screen.

[0130] The embodiment of the present invention also provides a computer-readable storage medium. The method according to the embodiment of the present invention can be implemented in hardware, firmware, or can be implemented as a computer code that can be recorded in a storage medium, or can be implemented as a computer code that is originally stored in a remote storage medium or a non-temporary machine-readable storage medium and will be stored in a local storage medium through a network download, so that the method described herein can be stored in such software processing on a storage medium using a general-purpose computer, a dedicated processor, or programmable or dedicated hardware. Among them, the storage medium can be a magnetic disk, an optical disk, a read-only storage memory, a random access memory, a flash memory, a hard disk or a solid-state hard disk, etc.; further, the storage medium can also include a combination of the above types of memories. It can be understood that a computer, a processor, a microprocessor controller, or programmable hardware includes a storage component that can store or receive software or computer code. When the software or computer code is accessed and executed by a computer, a processor, or hardware, the method shown in the above embodiment is implemented.

[0131] A part of the present invention may be applied as a computer program product, such as a computer program instruction, which, when executed by a computer, can call or provide the method and / or technical solution according to the present invention through the operation of the computer. Those skilled in the art should understand that the existence of the computer program instruction in a computer-readable medium includes, but is not limited to, a source file, an executable file, an installation package file, etc., and accordingly, the way in which the computer program instruction is executed by the computer includes, but is not limited to: the computer directly executes the instruction, or the computer compiles the instruction and then executes the corresponding compiled program, or the computer reads and executes the instruction, or the computer reads and installs the instruction and then executes the corresponding installed program. Here, the computer-readable medium may be any available computer-readable storage medium or communication medium accessible to the computer.

[0132] Although the embodiments of the present invention have been described in conjunction with the accompanying drawings, those skilled in the art may make various modifications and variations without departing from the spirit and scope of the present invention, and such modifications and variations are all within the scope defined by the appended claims.

Claims

1. A method for characterizing the crystallinity of core-shell structured tungsten carbide powder, characterized in that: include: Obtaining X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder; Determining the phase of the substance to be analyzed and the corresponding diffraction peak in the X-ray diffraction spectrum; Determining whether the diffraction peaks of the phase to be analyzed have overlapping peak regions; When the diffraction peaks of the phase to be analyzed do not have overlapping peak regions, selecting at least one crystal plane diffraction peak of a preset crystal plane; Respectively obtaining the peak position and half-height width of each crystal plane diffraction peak in the phase to be analyzed; The peak-to-valley ratio of the phase to be analyzed is determined according to the peak position and half-height width of each crystal plane diffraction peak.

2. The method according to claim 1, characterized in that Determining the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-height width of each crystal plane diffraction peak includes: Respectively determine the background line, peak position and half-height width of each crystal plane diffraction peak; Determining a peak area dividing line of each crystal plane diffraction peak according to the peak position and half-height width of each crystal plane diffraction peak; Determine the first area and the second area of ​​each crystal plane diffraction peak according to the peak area dividing line of each crystal plane diffraction peak and the background line of each crystal plane diffraction peak; The peak-to-valley ratio of the phase to be analyzed is determined according to the first area and the second area of ​​all the crystal plane diffraction peaks.

3. The method according to claim 2, characterized in that The at least one predetermined crystal plane is selected from a first group of crystal planes or a second group of crystal planes, the first group of crystal planes includes a (220) crystal plane and a (310) crystal plane, the second group of crystal planes includes a (002) crystal plane and a (101) crystal plane, the diffraction peak of the (220) crystal plane or the (002) crystal plane corresponds to a first crystal plane diffraction peak, and the diffraction peak of the (310) crystal plane or the (101) crystal plane corresponds to a second crystal plane diffraction peak; Determining the peak area dividing line of the first crystal plane diffraction peak according to the peak position and half-height width of the first crystal plane diffraction peak includes: determining a first offset angle according to the half-height width of the first crystal plane diffraction peak, the first offset angle being smaller than the half-height width of the first crystal plane diffraction peak; using the sum or difference of the peak position of the first crystal plane diffraction peak and the first offset angle as the abscissa of a first reference point on the X-axis in the X-ray diffraction spectrum; determining a first vertical line passing through the first reference point and perpendicular to the X-axis, and using the intersection of the first vertical line and the first crystal plane diffraction peak as a second reference point; determining a peak area dividing line of the first crystal plane diffraction peak passing through the second reference point and parallel to the back bottom line of the first crystal plane diffraction peak and intersecting with the first crystal plane diffraction peak at a third reference point; Determining the peak area dividing line of the second crystal plane diffraction peak according to the peak position and half-width of the second crystal plane diffraction peak includes: determining a second offset angle according to the half-width of the second crystal plane diffraction peak, the second offset angle is greater than the half-width of the second crystal plane diffraction peak and less than twice the half-width of the second crystal plane diffraction peak; calculating a first difference between the half-width of the second crystal plane diffraction peak and the half-width of the first crystal plane diffraction peak, and calculating a second difference between the second offset angle and the first difference, and taking the third sum or the third difference between the peak position of the second crystal plane diffraction peak and the second difference as the abscissa of the fourth reference point on the X-axis in the X-ray diffraction pattern; determining a second vertical line passing through the fourth reference point and perpendicular to the X-axis, and taking the intersection of the second vertical line and the second crystal plane diffraction peak as the fifth reference point; determining a peak area dividing line of the second crystal plane diffraction peak that passes through the fifth reference point and is parallel to the back bottom line of the second crystal plane diffraction peak and intersects with the second crystal plane diffraction peak at a sixth reference point.

4. The method according to claim 3, characterized in that Determining the first area and the second area of ​​each crystal plane diffraction peak according to the peak area dividing line of each crystal plane diffraction peak and the background line of each crystal plane diffraction peak comprises: Calculate a first area S1 below the peak of the first crystal plane diffraction peak and above the back bottom line, calculate a second area S2 below the peak of the first crystal plane diffraction peak and above the peak area dividing line, calculate a first area S3 below the peak of the second crystal plane diffraction peak and above the back bottom line, and calculate a second area S4 below the peak of the second crystal plane diffraction peak and above the peak area dividing line; Determining the peak-to-valley ratio of the phase to be analyzed based on the first area and the second area of ​​all the crystal plane diffraction peaks includes: calculating the sum D1 of S2 and S4, the sum D2 of S1 and S3, and taking the ratio of D1 to D2 as the peak-to-valley ratio.

5. The method according to claim 1, characterized in that Also includes: When there are overlapping peak regions of the diffraction peaks of the phase to be analyzed, determining the lowest point of the peak shape between the diffraction peaks of the first overlapping peak region where the diffraction peaks of the (210) crystal plane, the (003) crystal plane and the (202) crystal plane in the X-ray diffraction spectrum are located; A first straight line is drawn through the lowest point of the peak shape and is parallel to the back bottom line of the diffraction peak of the first overlapping peak region, and the first straight line intersects with the diffraction peak of the first overlapping peak region to obtain a first intersection point and a second intersection point; Calculate the sum of the peak areas of the diffraction peaks of the (210) crystal plane, the (003) crystal plane, and the (202) crystal plane above the background line in the first overlapping peak region to obtain a third area S; Calculate the sum of the peak areas of the diffraction peaks of the (210) crystal plane, the (003) crystal plane, and the (202) crystal plane above the line connecting the first intersection point and the second intersection point in the first overlapping peak region to obtain a fourth area S'; The peak-to-valley ratio of the core-shell structured tungsten carbide powder is obtained according to the ratio S of the fourth area S' to the third area.

6. The method according to claim 1, characterized in that The method of obtaining the X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder comprises: The core-shell structured tungsten carbide powder sample is tested by using an X-ray diffractometer to obtain an X-ray diffraction spectrum of the shell portion; Using an X-ray diffractometer to test the polished sample of the core-shell structured tungsten carbide powder to obtain an X-ray diffraction spectrum of the core portion; Among them, the polished sample of the core-shell structure tungsten carbide powder to be tested is prepared by the following method: filling the core-shell structure tungsten carbide powder into the empty groove on the glass slide, compacting and leveling it to the level of the edge of the empty groove; dripping glue into the core-shell structure tungsten carbide powder in the empty groove and heating the glass slide, waiting for the core-shell structure tungsten carbide powder to solidify, peeling off the glass slide to obtain a powder block, inlaying it with bakelite and then polishing it to obtain the polished sample of the core-shell structure tungsten carbide powder to be tested.

7. A device for characterizing the crystallinity of core-shell tungsten carbide powder, characterized in that: include: An acquisition module is used to obtain X-ray diffraction patterns of the core and shell of the core-shell structured tungsten carbide powder; A confirmation module, used to determine the phase of the substance to be analyzed and the corresponding diffraction peak in the X-ray diffraction spectrum; A judgment module, used for judging whether the diffraction peaks of the phase to be analyzed have overlapping peak regions; A processing module is used to select at least one crystal plane diffraction peak of a preset crystal plane when there is no overlapping peak area in the diffraction peaks of the phase to be analyzed, and obtain the peak position and half-height width of each crystal plane diffraction peak in the phase to be analyzed; and determine the peak-to-valley ratio of the phase to be analyzed according to the peak position and half-height width of each crystal plane diffraction peak.

8. A computer device, characterized in that: include: A memory and a processor, wherein the memory and the processor are connected to each other for communication, the memory stores computer instructions, and the processor executes the method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder according to any one of claims 1 to 6 by executing the computer instructions.

9. A computer-readable storage medium, characterized in that: The computer-readable storage medium stores computer instructions, and the computer instructions are used to enable a computer to execute the method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder according to any one of claims 1 to 6.

10. A computer program product, characterized in that The method comprises computer instructions for causing a computer to execute the method for characterizing the degree of crystallinity of a core-shell structured tungsten carbide powder according to any one of claims 1 to 6.

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