Graphitization degree characterization method, device, equipment, medium and program product

Abstract

The invention relates to the technical field of performance testing, and discloses a graphitization degree characterization method, device and equipment, a medium and a program product, and the method comprises the following steps: obtaining an X-ray diffraction pattern of a to-be-tested sample after X-ray scanning; determining a target peak position and a target full width at half maximum according to a diffraction peak corresponding to a preset crystal face in the X-ray diffraction pattern; calculating the peak volume ratio of the diffraction peak according to the target peak position and the target full width at half maximum, and representing the graphitization degree trend of the sample to be detected by the peak volume ratio. According to the method, the angle difference of the diffraction peaks can be converted into the peak-to-product ratio, accurate peak positions, peak dividing parameters and the like do not need to be considered, limitation caused when a Merging-Maire formula is adopted is avoided, the accuracy of graphitization trend judgment is improved, and therefore the reliability of product quality control or manufacturing process parameter adjustment is guaranteed.

Description

Technical Field

[0001] The present invention relates to the technical field of performance testing, and in particular to a method, device, equipment, medium and program product for characterizing the degree of graphitization. Background Art

[0002] Graphite is not meltable at high temperatures, has excellent electrical and thermal conductivity, and good chemical stability. It is widely used in metallurgy, chemical industry, aerospace and other industries. In industry, carbon raw materials (such as natural graphite, petroleum coke, asphalt coke, etc.) are often subjected to calcination, crushing, pressing, roasting, high-temperature heat treatment and other processes to obtain high-performance artificial graphite materials. The quality of artificial graphite has a great influence on the performance of subsequent carbon material products. Its "graphitization degree" must reach a certain value to ensure that the material has the best performance. Therefore, as a means of product quality control and a basis for adjusting manufacturing process parameters, the test of graphitization degree is very necessary.

[0003] The manufacturing process of artificial graphite is the process of carbon atoms changing from a disordered or two-dimensional (turbostratic structure) ordered arrangement to a three-dimensional ordered arrangement, that is, from amorphous carbon to graphite. The degree of transformation in this process is the "degree of graphitization", and the meaning of "degree of graphitization" is general. It is only a physical quantity used to judge the degree of growth of graphite crystals.

[0004] The judgment methods in the prior art include resistivity method, true specific gravity method, acid quantitative method, laser Raman spectroscopy, magnetoresistance method, X-ray diffraction method, etc. Among them, X-ray diffraction method, which is a means of directly obtaining crystal structure information, is the most commonly used. It mainly measures the value of the average interlayer spacing d002 and calculates the degree of graphitization using the Mering-Maire formula g=(0.3440-d002) / (0.3440-0.3354)×100%. Where g is the degree of graphitization, 0.3440 is the interlayer spacing of incompletely graphitized carbon, 0.3354 is the interlayer spacing of ideal graphitized crystals, and d002 is the interlayer spacing of the (002) crystal plane of the carbon material. However, the accurate determination of d002 is a problem at present, which will lead to inaccurate graphitization degree calculated using the Mering-Maire formula, thereby making the judgment of graphitization trend inaccurate, affecting the control of product quality or the adjustment of manufacturing process parameters. Summary of the invention

[0005] In view of this, the present invention provides a method, device, equipment, medium and program product for characterizing the degree of graphitization to solve the problem of inaccurate calculation of the degree of graphitization using the Mering-Maire formula.

[0006] In a first aspect, the present invention provides a method for characterizing the degree of graphitization, the method comprising:

[0007] Obtaining an X-ray diffraction pattern after X-ray scanning of the sample to be tested;

[0008] Determine the target peak position and target half-height width according to the diffraction peak corresponding to the preset crystal plane in the X-ray diffraction spectrum;

[0009] The peak area ratio of the diffraction peak is calculated according to the target peak position and the target half-height width, and the peak area ratio is used to characterize the graphitization degree trend of the sample to be tested.

[0010] The method for characterizing the degree of graphitization provided by the present invention performs X-ray scanning on the sample to be tested, determines the peak position and half-width according to the diffraction peak corresponding to the preset crystal plane in the obtained X-ray diffraction spectrum, calculates the peak-to-product ratio of the diffraction peak according to the peak position and half-width, and characterizes the graphitization trend of the sample to be tested by the peak-to-product ratio. The present invention can convert the angle difference of the diffraction peak into the peak-to-product ratio without considering the precise peak position, peak separation parameters, etc., avoids the limitations of the Mering-Maire formula, improves the accuracy of the judgment of the graphitization trend, and thus ensures the reliability of product quality control or manufacturing process parameter adjustment.

[0011] In an optional embodiment, the target peak position and target half-width are determined according to the diffraction peak corresponding to the preset crystal plane in the X-ray diffraction spectrum, including: determining the original peak top and the original peak height of the diffraction peak according to the peak shape of the diffraction peak; taking the horizontal coordinate corresponding to the original peak top in the X-ray diffraction spectrum as the target peak position of the diffraction peak, and determining the target half-width of the diffraction peak according to the original peak height.

[0012] The present invention directly determines the relevant information of the diffraction peaks. When the diffraction peaks are multi-peak mixtures, the angle difference can still be converted into a peak area ratio based on the relevant information of the diffraction peaks, thereby solving the problem that when there are components with different graphitization degrees, the calculation result of the Mering-Maire formula focuses on the graphite with the largest content, without considering the precise peak position, peak separation parameters, etc., thereby reducing the difficulty of characterizing the graphitization degree.

[0013] In an optional embodiment, the preset crystal planes include: (004) crystal plane and (110) crystal plane, the corresponding diffraction peaks include a first diffraction peak and a second diffraction peak, the target peak position includes a first target peak position and a second target peak position, and the target half-width includes a first target half-width and a second target half-width; the peak-to-product ratio of the diffraction peak is calculated according to the target peak position and the target half-width, including: determining whether to select the first diffraction peak or the first diffraction peak and the second diffraction peak according to the peak shape and intensity of the first diffraction peak and the second diffraction peak; if the first diffraction peak is selected, determining the first back baseline of the first diffraction peak, and determining a first parallel line parallel to the first back baseline according to the first target peak position and the first target half-width; calculating a first area below the peak of the first diffraction peak and above the first back baseline, and calculating a second area below the peak of the first diffraction peak and above the first parallel line; taking the ratio of the second area to the first area as the peak-to-product ratio.

[0014] The present invention converts the angle difference corresponding to the peak position into a peak area ratio, which can more easily distinguish the difference in diffraction peaks, thereby accurately judging the graphitization trend of the sample to be tested, reducing the difficulty of graphitization characterization, and providing a reliable reference for product quality control or manufacturing process parameter adjustment.

[0015] In an optional embodiment, the peak-to-area ratio of the diffraction peaks is calculated according to the target peak position and the target half-width, and also includes: if the first diffraction peak and the second diffraction peak are selected, the first back baseline of the first diffraction peak and the second back baseline of the second diffraction peak are determined, and a first parallel line parallel to the first back baseline is determined according to the first target peak position and the first target half-width, and a second parallel line parallel to the second back baseline is determined according to the second target peak position, the first target half-width and the second target half-width; a first area below the peak of the first diffraction peak and above the first back baseline is calculated, a second area below the peak of the first diffraction peak and above the first parallel line is calculated, a third area below the peak of the second diffraction peak and above the second back baseline is calculated, and a fourth area below the peak of the second diffraction peak and above the second parallel line is calculated; and the ratio of the sum of the second area and the fourth area to the sum of the first area and the third area is taken as the peak-to-area ratio.

[0016] The present invention analyzes the diffraction peaks of two crystal planes, can comprehensively analyze the angle differences of the diffraction peaks corresponding to the sample to be tested, and expresses them with the same peak area ratio, thereby further improving the accuracy of judging the trend of graphitization degree.

[0017] In an optional embodiment, a first parallel line parallel to the first back bottom line is determined according to the first target peak position and the first target half-width, including: determining a first deviation angle according to the first target half-width, the first deviation angle is smaller than the first target half-width, and taking the difference between the first target peak position and the first deviation angle as the horizontal coordinate of the 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 diffraction peak as the second reference point; determining a first parallel line passing through the second reference point, parallel to the first back bottom line, and intersecting with the first diffraction peak at a third reference point; determining a first parallel line passing through the second reference point, parallel to the first back bottom line, and intersecting with the first diffraction peak at a third reference point according to the second target peak position, the first target half-width and the second target half-width Determining a second parallel line parallel to the second back bottom line includes: determining a second deviation angle according to the second target half-width, the second deviation angle being less than twice the second target half-width, calculating a first difference between the first target half-width and the second target half-width, and calculating a second difference between the first deviation angle and the first difference, and using a third difference between the second target peak position and the second difference as the horizontal coordinate of a fourth reference point on the X-axis in the X-ray diffraction spectrum; determining a second vertical line passing through the fourth reference point and perpendicular to the X-axis, and using the intersection of the second vertical line and the second diffraction peak as a fifth reference point; and determining a second parallel line passing through the fifth reference point, parallel to the second back bottom line, and intersecting the second diffraction peak at a sixth reference point.

[0018] The present invention can convert the angle difference into a restriction condition in a mathematical formula by selecting a reference point for the diffraction peak, thereby dividing the diffraction peak area and identifying the angle difference by the ratio of the areas of different regions of the diffraction peak. There is no need for complex and cumbersome parameter determination, thus reducing the difficulty of graphitization degree characterization.

[0019] In some optional embodiments, after calculating the peak area ratio of the diffraction peak according to the target peak position and the target half-width, it also includes: correcting the peak area ratio according to the conversion coefficient to obtain the graphitization degree of the sample to be tested, and the conversion coefficient is determined based on the standard graphitization degree calculated in advance according to the standard sample and the Mellin formula and the pre-calculated standard peak area ratio.

[0020] The present invention can obtain a relatively accurate graphitization degree by correcting the peak area ratio, thereby solving the problem that the graphitization degree calculated by using the Mering-Maire formula is inaccurate due to the inability to accurately measure d002.

[0021] In a second aspect, the present invention provides a device for characterizing the degree of graphitization, the device comprising: a spectrum acquisition module, used to obtain an X-ray diffraction spectrum after an X-ray scan of a sample to be tested; a parameter determination module, used to determine a target peak position and a target half-width according to a diffraction peak corresponding to a preset crystal plane in the X-ray diffraction spectrum; a peak-to-area ratio calculation module, used to calculate the peak-to-area ratio of the diffraction peak according to the target peak position and the target half-width, and to characterize the graphitization trend of the sample to be tested with the peak-to-area ratio.

[0022] In a third aspect, the present invention provides a computer device, comprising: a memory and a processor, the memory and the processor are communicatively connected to each other, the memory stores computer instructions, and the processor executes the method for characterizing the degree of graphitization of the first aspect or any corresponding embodiment thereof by executing the computer instructions.

[0023] In a fourth aspect, the present invention 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 graphitization of the first aspect or any corresponding embodiment thereof.

[0024] In a fifth aspect, the present invention provides a computer program product, comprising computer instructions, wherein the computer instructions are used to enable a computer to execute the method for characterizing the degree of graphitization of the first aspect or any corresponding embodiment thereof. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] 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.

[0026] Figure 1 is a schematic diagram of XRD patterns of different carbon / carbon composite materials;

[0027] Figure 2 is a schematic flow chart of a method for characterizing the degree of graphitization according to an embodiment of the present invention;

[0028] Figure 3 It is a schematic diagram of a typical XRD pattern;

[0029] Figure 4 is a schematic diagram of a graphite emulsion XRD spectrum according to a method for characterizing the degree of graphitization according to an embodiment of the present invention;

[0030] Figure 5 is a schematic flow chart of another method for characterizing the degree of graphitization according to an embodiment of the present invention;

[0031] Figure 6 is a schematic diagram of diffraction peaks according to another method for characterizing the degree of graphitization according to an embodiment of the present invention;

[0032] Figure 7 is a schematic diagram of a (004) diffraction peak according to another method for characterizing the degree of graphitization according to an embodiment of the present invention;

[0033] Figure 8 2. It is a schematic diagram of comparison of graphite emulsion spectra of two batches according to another method for characterizing the degree of graphitization of an embodiment of the present invention;

[0034] Fig. 9 is a schematic flow chart of another method for characterizing the degree of graphitization according to an embodiment of the present invention;

[0035] Fig.10 is a schematic diagram of the (110) diffraction peak of another method for characterizing the degree of graphitization according to an embodiment of the present invention;

[0036] Fig.11 is a schematic diagram of comparison of graphite emulsion spectra of four batches according to another method for characterizing the degree of graphitization of an embodiment of the present invention;

[0037] Fig.12 is a structural block diagram of a device for characterizing the degree of graphitization according to an embodiment of the present invention;

[0038] Fig.13 It is a schematic diagram of the hardware structure of a computer device according to an embodiment of the present invention. DETAILED DESCRIPTION

[0039] 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.

[0040] The embodiments of the present invention are applicable to application scenarios in which the degree of graphitization of samples to be tested is measured to control product quality or adjust manufacturing process parameters. The samples to be tested include industrial graphite emulsions for drawing hard wires such as tungsten and molybdenum, carbon / carbon composite materials for aviation brakes, carbon sheets for synthesizing diamonds in the superhard material industry, negative active materials for lithium-ion batteries, etc. The rapid quality judgment of graphite in graphite emulsions for wire drawing is taken as an example in the industrial field.

[0041] like Figure 1As shown in (a), in addition to the change in peak position of the (002) crystal plane of different carbon materials, the symmetry of the peak shape also changes continuously, which makes the peak shape fitting to determine the peak position and calculate d002 have great uncertainty. The reason is that during the graphitization process, a variety of crystal forms may be generated, and even if they belong to the same space group, there may be a variety of graphites with different degrees of graphitization in the powder, which increases the difficulty of peak shape fitting analysis. Therefore, in order to obtain a more accurate d002 value, various improvements and adaptive methods are proposed in the relevant technology. Such as: ① Accurate peak position, the peak position is obtained by adding Si powder internal standard or different fitting methods such as hanging line method, half-width method, peak top method, least squares method and first-order fitting method; ② Change the analysis object, do not use the (002) crystal plane for analysis, but use high-angle (004) crystal plane analysis to reduce errors, and then convert; ③ Multiple peak separation, such as Figure 1 As shown in (b), the (002) crystal plane or (004) crystal plane is divided into multiple diffraction peaks by the peak splitting method to calculate their respective d002 and graphitization degree and multiply their respective mass fractions by themselves; ④ According to the Mering-Maire formula, it is corrected. Some literatures have concluded that the maximum d002 of metallurgical coke should be Some literature uses the method of taking the derivative of d002 with respect to the stacking height Lc, and uses the intercept B of the relationship curve between the two on the d002 axis to replace the maximum value of d002 to obtain the graphitization degree of calcined petroleum coke; ⑤ Other methods are used to replace the Mering-Maire formula to characterize the graphitization degree. For example, some literature calculates the stacking probability of 2H and 3R graphite by Fourier analysis of the (10)(11) spectral line intensity of the chaotic layer structure; some literature proposes a "single layer" and "double layer" model, and uses the full spectrum fitting method to calculate the disorder degree P, P = 1-g; some literature uses the method of separating the half-width to calculate P and P by the half-width of (101)(102). AB +P ABC Indicators such as P AB and P ABC Characterize the disorder degree of hexagonal and rhombohedral graphite respectively.

[0042] The above-mentioned various improvements and adaptive methods have their own advantages, but they still have shortcomings. For example, the peak position method requires the addition of an internal standard, which is cumbersome, and the specific peak shape fitting method may not be applicable to all cases; the difficulty of the peak separation method lies in determining the number of phases and the peak shape parameters of each phase; the parameters of the full spectrum fitting and Fourier analysis in the alternative method are also applicable; the disorder degree P value in the separation half-width method is related to the length unit, and the (101)(102) crystal plane is often submerged in the diffraction peaks of rhombohedral graphite or other impurities in graphite emulsion and cannot be obtained. These are all disadvantageous for the rapid quality judgment of industrial graphite products.

[0043] Since the change of crystal structure caused by graphitization is continuous, "graphitization degree" cannot be simply regarded as the crystal ratio; and since "graphite" itself has different space group structures such as hexagonal and rhombohedral, it is impossible to give a clear definition of the crystal structure. Therefore, the meaning of "graphitization degree" is general, and it is only a physical quantity used to judge the growth degree of graphite crystals. Therefore, it can be considered and characterized from the perspective of crystallization degree, because the crystal growth degree changes or there are multiple components of graphite with different graphitization degrees at the same time, and the XRD (X-ray diffraction) spectrum lines will inevitably change. The embodiment of the present invention provides a method for characterizing the degree of graphitization, which converts the angle difference of the change of the diffraction peak shape into the peak area ratio to achieve the effect of accurately judging the trend of the degree of graphitization.

[0044] According to an embodiment of the present invention, an embodiment of a method for characterizing the degree of graphitization 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.

[0045] In this embodiment, a method for characterizing the degree of graphitization is provided, which can be used in mobile terminals, such as computers, etc. Figure 2 is a flow chart of a method for characterizing the degree of graphitization according to an embodiment of the present invention, such as Figure 2 As shown, the process includes the following steps:

[0046] Step S201, obtaining an X-ray diffraction pattern after performing X-ray scanning on the sample to be tested.

[0047] Specifically, in an embodiment of the present invention, a graphite dairy product is used as a sample to be tested, and a scanning spectrum of a specific area of ​​the graphite dairy product is obtained by X-ray diffraction. If the sample to be tested is in block form, it needs to be crushed and ground, and the powder is filled into the groove of the slide glass, and is scraped flat with a glass sheet to ensure that the surface of the sample to be tested is flat and flush with the edge of the groove. Then, an X-ray scan is performed on the sample to be tested based on the following test conditions: Co target, scanning angle 10-110°, step length 0.033°, dwell time 30s per step; divergence slit 1°, anti-scattering slit 6.6mm; the measuring instrument is PANalytical X-RAY DIFFRACTOMETERMODEL X'PERT PRO, so as to obtain the X-ray diffraction spectrum of the sample to be tested, which is only used as an example and is not limited to this.

[0048] Step S202, determining a target peak position and a target half-width according to a diffraction peak corresponding to a preset crystal plane in an X-ray diffraction spectrum.

[0049] Specifically, in the embodiment of the present invention, according to Figure 3The typical XRD pattern of the carbon material (Cu target) shown in FIG. 1 shows that when the carbon is an amorphous structure, the XRD pattern is as follows: Figure 3 As shown in (a), there is only (02) diffraction peak at this time; when carbon is a chaotic layer structure, the XRD spectrum is as follows Figure 3 As shown in (b), diffraction peaks (10), (04) and (11) have appeared. Figure 3 As shown in (c), it is mainly hexagonal and rhombohedral. The diffraction spectrum of graphite products for wire drawing is generally between (b) and (c). Figure 4 shown.

[0050] In some optional embodiments, for graphite emulsion, there are also overlapping regions of multiple diffraction peaks in the 48-58° region, but since other impurities such as lubricants also have diffraction peaks in this region, only other regions such as (004) and (110) diffraction peaks can be selected for characterization, and the changes in the degree of graphite crystallization can be characterized by simulating the changes in the overlapping peaks. For other graphite products, appropriate regions are selected for analysis according to actual conditions, and are not limited here. Although the diffraction peaks in other non-overlapping regions are essentially overlapping peaks of different graphite phases, especially hexagonal and rhombohedral, such as the commonly mentioned (002) diffraction peak, which is a diffraction mixed spectrum of the hexagonal (002) crystal plane and the rhombohedral (003) crystal plane, and the (004) diffraction peak, which is a diffraction mixed spectrum of the hexagonal (004) and rhombohedral (006) crystal planes, the difference between these two crystal forms mainly comes from whether the hexagonal grid planes of graphite are stacked in an ABAB... or ABCABC... manner, so no distinction is made. In summary, the embodiments of the present invention exclude interference from other impurities in the graphite emulsion, and select the (004) single crystal plane or a group of (004) and (110) crystal planes to evaluate the graphitization degree of the graphite emulsion. The more crystal planes analyzed, the more accurate the result. Therefore, when there are diffraction peaks corresponding to the (004) crystal plane and the (110) crystal plane in the diffraction spectrum, a group of (004) and (110) crystal planes are selected for analysis; when there is only a diffraction peak corresponding to the (004) crystal plane in the spectrum, or the diffraction peak intensity of the (110) crystal plane is not high and the interference is large, the (004) crystal plane is selected for analysis.

[0051] In some optional embodiments, after determining to select the (004) crystal plane, or selecting a group of crystal planes (004) and (110), the present invention determines the target peak position and target half-width of the corresponding diffraction peak based on the XRD spectrum, wherein the horizontal axis in the XRD spectrum is the angle information, the vertical axis is the diffraction intensity, the peak position is the horizontal axis corresponding to the highest point of the diffraction peak, and the half-width is the width corresponding to half the peak height of the diffraction peak.

[0052] Step S203, calculating the peak area ratio of the diffraction peak according to the target peak position and the target half-height width, and using the peak area ratio to characterize the graphitization degree trend of the sample to be tested.

[0053] Specifically, in an embodiment of the present invention, in the XRD spectrum, the spectrum line is located above the X-axis, and an area is formed below the spectrum line and above the X-axis, and different diffraction peaks correspond to different areas. Because the degree of crystal growth changes or there are multiple components of graphite with different degrees of graphitization at the same time, the spectrum line of the XRD spectrum changes, and the corresponding diffraction peaks will change due to the changes in the peak position of the abscissa and the diffraction intensity of the ordinate, and the peak shape will change, and then the area of ​​the area corresponding to the diffraction peak will be different. The embodiment of the present invention uses the background line of the diffraction peak as a reference to offset the peak position of the diffraction peak, thereby constructing a mathematical restriction condition, dividing the area corresponding to the diffraction peak, and characterizing the change of the peak shape according to the area ratio of different areas, which is equivalent to converting the angle difference of the diffraction peak into a peak-to-area ratio, and calculating the peak-to-area ratio obtained by comparing a single or multiple diffraction peaks by themselves to quantitatively characterize the degree of graphite crystallization, that is, the degree of graphitization. Among them, the background line is the midpoint line of the background noise point of the diffraction peak, and it is as straight as possible.

[0054] In some optional embodiments, the peak area ratio obtained in the embodiment of the present invention is an indicator for characterizing the trend of graphitization degree change. By analyzing different batches of graphite emulsions for wire drawing, users can obtain the graphitization degree trends of different batches of graphite emulsions for wire drawing. Therefore, using the peak area ratio as a means of product quality control and a basis for adjusting manufacturing process parameters, it is possible to accurately determine which batch of graphite emulsions for wire drawing has better quality or is more in line with the current manufacturing process, so that in the subsequent production process of carbon material products, by selecting a suitable graphite emulsion for wire drawing, it is ensured that the produced material has the best performance. The embodiment of the present invention uses the peak area ratio to characterize the trend of graphitization degree, does not need to add an internal standard to pursue accurate peak position, does not need to consider peak separation parameters, and does not need to consider the applicability of dmax when using the Mering-Maire formula. It can convert angle differences into peak area ratios, makes it easier to distinguish differences, and can solve the problem that when there are components with different degrees of graphitization, the calculation results of the Mering-Maire formula focus on the graphite with the largest content.

[0055] The method for characterizing the degree of graphitization provided by the present invention performs X-ray scanning on the sample to be tested, determines the peak position and half-width according to the diffraction peak corresponding to the preset crystal plane in the obtained X-ray diffraction spectrum, calculates the peak-to-product ratio of the diffraction peak according to the peak position and half-width, and characterizes the graphitization trend of the sample to be tested by the peak-to-product ratio. The present invention can convert the angle difference of the diffraction peak into the peak-to-product ratio without considering the precise peak position, peak separation parameters, etc., avoids the limitations of the Mering-Maire formula, improves the accuracy of the judgment of the graphitization trend, and thus ensures the reliability of product quality control or manufacturing process parameter adjustment.

[0056] In this embodiment, a method for characterizing the degree of graphitization is provided, which can be used in mobile terminals, such as computers, etc. Figure 5is a flow chart of a method for characterizing the degree of graphitization according to an embodiment of the present invention, such as Figure 5 As shown, the process includes the following steps:

[0057] Step S501, obtain the X-ray diffraction pattern after X-ray scanning of the sample to be tested. Figure 2 Step S201 of the illustrated embodiment will not be described in detail here.

[0058] Step S502, determining a target peak position and a target half-width according to a diffraction peak corresponding to a preset crystal plane in an X-ray diffraction spectrum.

[0059] Specifically, the above step S502 includes:

[0060] Step S5021, determining the original peak top and the original peak height of the diffraction peak according to the peak shape of the diffraction peak.

[0061] Specifically, in the embodiments of the present invention, the diffraction peaks of the crystal planes are generally symmetrical in the XRD spectrum. However, because graphites with multiple degrees of graphitization may exist in the same batch of graphite emulsions for wire drawing, the diffraction peaks corresponding to the same crystal plane in graphites with different degrees of graphitization may be different. When the different diffraction peaks are superimposed together, asymmetric diffraction peaks will appear in the XRD spectrum. Generally, the worse the symmetry, the more superimposed peaks there are, and the better the symmetry, the fewer superimposed peaks there are, or even only a single peak exists. In order to avoid the complexity of peak separation due to the superposition of multiple peaks, the embodiments of the present invention directly determine the target peak position and target half-width at half-height of the diffraction peaks corresponding to the crystal plane based on the diffraction peaks in the XED spectrum. Figure 6 As shown, it can be seen that the peak shape of the diffraction peak is asymmetric, and it is obviously a superposition of multiple peaks. The embodiment of the present invention directly determines the corresponding original peak top according to the peak shape of the diffraction peak, and determines the original peak height of the diffraction peak according to the vertical coordinate corresponding to the original peak top in the XRD spectrum, that is, the diffraction peak is not fitted or split.

[0062] Step S5022, taking the abscissa corresponding to the original peak top in the X-ray diffraction spectrum as the target peak position of the diffraction peak, and taking the original peak height as the target half-height width of the diffraction peak.

[0063] Specifically, in an embodiment of the present invention, the angle value of the horizontal coordinate corresponding to the original peak of the diffraction peak in the XRD spectrum is directly used as the target peak position of the diffraction peak, and the target half-height width of the diffraction peak is determined according to the horizontal coordinate corresponding to half of the peak height of the diffraction peak. Although the target peak position and target half-height width determined at this time do not have high accuracy, because the embodiment of the present invention converts the angle difference of the diffraction peak into a peak-to-product ratio, the determination of the peak position and the half-height width is only for the subsequent construction of mathematical constraints, and will not cause too much impact on the angle difference, so it is still possible to relatively accurately judge the graphitization trend of the graphite emulsion for wire drawing according to the peak-to-product ratio. The present invention can convert the angle difference into a peak-to-product ratio based on the relevant information of the diffraction peak when the diffraction peak is a multi-peak mixture, thereby solving the problem that when there are components with different graphitization degrees, the calculation result of the Mering-Maire formula focuses on the problem of graphite with the largest content proportion, without considering the precise peak position, peak separation parameters, etc., and reducing the difficulty of characterizing the graphitization degree.

[0064] Step S503, calculating the peak area ratio of the diffraction peak according to the target peak position and the target half-height width, and using the peak area ratio to characterize the graphitization degree trend of the sample to be tested.

[0065] Specifically, the above step S503 includes:

[0066] Step S5031, determining whether to select the first diffraction peak or the first diffraction peak and the second diffraction peak according to the peak shapes and intensities of the first diffraction peak and the second diffraction peak.

[0067] Specifically, in the embodiments of the present invention, in general, in the XRD spectrum, the diffraction intensity of the diffraction peak corresponding to the (004) crystal plane is generally higher than the diffraction intensity of the diffraction peak corresponding to the (110) crystal plane. Although the more crystal planes are analyzed, the more accurate the final judgment result is, it is still necessary to determine whether the (110) diffraction peak meets the requirements. If the peak shape and intensity of the (110) diffraction peak are analyzed to determine that the diffraction intensity is low or even that the (110) diffraction peak does not exist, or the (110) diffraction peak is highly disturbing, then only the (004) diffraction peak is selected for subsequent analysis.

[0068] Step S5032: if the first diffraction peak is selected, a first back baseline of the first diffraction peak is determined, and a first parallel line parallel to the first back baseline is determined according to the first target peak position and the first target half-width.

[0069] Specifically, in the embodiment of the present invention, if it is determined to select only the (004) diffraction peak, a mathematical restriction condition is constructed according to the background line, target peak position and target half-width of the (004) diffraction peak.

[0070] In some optional implementations, the above step S5032 includes:

[0071] Step a1, determining a first deviation angle according to the first target half-width, the first deviation angle is smaller than the first target half-width, and taking the difference between the first target peak position and the first deviation angle as the horizontal coordinate of the first reference point on the X-axis in the X-ray diffraction pattern.

[0072] Step a2, 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 diffraction peak as the second reference point.

[0073] Step a3, determining a first parallel line that passes through the second reference point, is parallel to the first background line, and intersects the first diffraction peak at a third reference point.

[0074] Specifically, in the embodiment of the present invention, Figure 7 As shown, the target peak position of the (004) diffraction peak is θ1, the target half-width is FWHM1, and the deviation angle is θ i1 , where 0<θ i1 <FWHM1, set θ according to actual operation i1 is 0.4, but not limited to this. L =θ1-θ i1 ,θ L It is the horizontal coordinate of point A on the X-axis in the X-ray diffraction spectrum. A vertical line from point A to the X-axis intersects the (004) diffraction peak at point C. The back baseline of the (004) diffraction peak is determined by software setting or manual point selection. At the same time, a parallel line parallel to the back baseline is drawn through point C. The parallel line intersects the (004) diffraction peak at point B.

[0075] Step S5033, calculating a first area below the first diffraction peak and above the first back baseline, and calculating a second area below the first diffraction peak and above the first parallel line.

[0076] Step S5034: taking the ratio of the second area to the first area as the peak-to-area ratio.

[0077] Specifically, in the embodiment of the present invention, the peak area below the peak of the (004) diffraction peak and above the back line is taken as S1, and the peak area below the peak of the (004) diffraction peak and above the parallel line BC is taken as S2. S1 and S2 are automatically calculated by software, and the peak area ratio D is defined as the ratio of S2 to S1, that is, D=S2 / S1*100%. The present invention can more easily distinguish the difference of the diffraction peak by converting the angle difference corresponding to the peak position into the peak area ratio, thereby accurately judging the graphitization trend of the sample to be tested, reducing the difficulty of graphitization characterization, and providing a reliable reference for product quality control or manufacturing process parameter adjustment.

[0078] In some optional embodiments, the present invention analyzes two batches of graphite emulsions, such as Figure 8 As shown in the figure, it can be seen that in the XRD spectra corresponding to the two batches of graphite emulsions, the (004) diffraction peak has good symmetry and high purity. Si powder was added as an internal standard and the (004) crystal plane was used for analysis. Figure 8 It can be seen that the peak positions of the two batches of samples are similar. The main difference is that the half-height width of 1#-02 is slightly larger than that of 1#-01, that is, theoretically, the grain size of 1#-02 is smaller or the stacking fault energy is larger, and the degree of crystallization is smaller. i1 Take 0.4°, and the calculation results are shown in the following table (the graphitization index in the table is calculated according to the Mellin formula, and the purpose of adding Si powder as the internal standard is also to facilitate the calculation of the Mellin formula). It can be seen that the peak area ratio index has the same trend as the graphitization index, which illustrates the accuracy of the new method:

[0079] Brand batch number Peak position (°) FWHM(°) Peak-to-area ratio index (%) Graphitization index (%) 1#-01 64.315 0.288 27.84 91.59 1#-02 64.311 0.304 26.68 91.37

[0080] In some optional embodiments, since the Mering-Maire formula sets the interplanar spacing value dmax of ideal graphite, the closer it is, the closer the value is to 100%, and the peak-to-area ratio obtained in the embodiment of the present invention is a trend indicator. If you want to compare it with the Mering-Maire formula, you can set a standard sample and correct the result. If the Mering-Maire calculated value of the standard sample is 90 and the peak-to-area ratio index is 40, then the conversion coefficient is set to 90 / 40. The peak-to-area ratios obtained by other samples are multiplied by the conversion coefficient for correction, so that they can be compared with the Mering-Maire formula. The present invention can obtain a more accurate degree of graphitization by correcting the peak-to-area ratio, and solve the problem of inaccurate degree of graphitization calculated using the Mering-Maire formula due to the inability to accurately measure d002.

[0081] The method for characterizing the degree of graphitization provided by the present invention performs X-ray scanning on the sample to be tested, determines the peak position and half-width according to the diffraction peak corresponding to the preset crystal plane in the obtained X-ray diffraction spectrum, calculates the peak-to-product ratio of the diffraction peak according to the peak position and half-width, and characterizes the graphitization trend of the sample to be tested by the peak-to-product ratio. The present invention can convert the angle difference of the diffraction peak into the peak-to-product ratio without considering the precise peak position, peak separation parameters, etc., avoids the limitations of the Mering-Maire formula, improves the accuracy of the judgment of the graphitization trend, and thus ensures the reliability of product quality control or manufacturing process parameter adjustment.

[0082] In this embodiment, a method for characterizing the degree of graphitization is provided, which can be used in mobile terminals, such as computers. Fig. 9 is a flow chart of a method for characterizing the degree of graphitization according to an embodiment of the present invention, such as Fig. 9 As shown, the process includes the following steps:

[0083] Step S901, obtain the X-ray diffraction pattern after X-ray scanning of the sample to be tested. Figure 5 Step S501 of the illustrated embodiment will not be described in detail here.

[0084] Step S902, determine the target peak position and target half-height width according to the diffraction peak corresponding to the preset crystal plane in the X-ray diffraction spectrum. Figure 5 Step S502 of the illustrated embodiment will not be described in detail here.

[0085] Step S903, calculating the peak area ratio of the diffraction peak according to the target peak position and the target half-height width, and using the peak area ratio to characterize the graphitization degree trend of the sample to be tested.

[0086] Specifically, the above step S903 includes:

[0087] Step S9031, if the first diffraction peak and the second diffraction peak are selected, the first back bottom line of the first diffraction peak and the second back bottom line of the second diffraction peak are determined, and the first parallel line parallel to the first back bottom line is determined according to the first target peak position and the first target half-width, and the second parallel line parallel to the second back bottom line is determined according to the second target peak position, the first target half-width and the second target half-width.

[0088] Specifically, in an embodiment of the present invention, if it is determined to select the (004) diffraction peak and the (110) diffraction peak for analysis, mathematical constraints are constructed according to the background line, target peak position and target half-height width corresponding to the (004) diffraction peak and the (110) diffraction peak. By analyzing the diffraction peaks of two crystal planes, the present invention can comprehensively analyze the angle differences of the diffraction peaks corresponding to the sample to be tested, and express them with the same peak-to-area ratio, thereby further improving the accuracy of judging the trend of graphitization degree.

[0089] In some optional implementations, the above step S9031 includes:

[0090] Step b1, determine the first deviation angle according to the first target half-height width, the first deviation angle is smaller than the first target half-height width, and use the difference between the first target peak position and the first deviation angle as the horizontal coordinate of the first reference point on the X-axis in the X-ray diffraction spectrum. Figure 5 Step S5032 of the illustrated embodiment will not be described in detail here.

[0091] Step b2, 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 diffraction peak as the second reference point. Figure 5 Step S5032 of the illustrated embodiment will not be described in detail here.

[0092] Step b3, determine a first parallel line that passes through the second reference point, is parallel to the first back bottom line, and intersects the first diffraction peak at a third reference point. Figure 5 Step S5032 of the illustrated embodiment will not be described in detail here.

[0093] Step b4, determining a second deviation angle based on the second target half-width, the second deviation angle being less than twice the second target half-width, calculating a first difference between the first target half-width and the second target half-width, and calculating a second difference between the first deviation angle and the first difference, and using a third difference between the second target peak position and the second difference as the horizontal coordinate of a fourth reference point on the X-axis in the X-ray diffraction pattern.

[0094] Step b5, 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 diffraction peak as the fifth reference point.

[0095] Step b6, determining a second parallel line that passes through the fifth reference point, is parallel to the second back bottom line, and intersects the second diffraction peak at a sixth reference point.

[0096] Specifically, in the embodiment of the present invention, Fig.10 As shown, the target peak position of the (110) diffraction peak is θ2, the target half-width is FWHM2, and the deviation angle is θ i2 , where 0<θ i2 <2FWHM2, set θ according to actual operation i2 is 0.4, but not limited to this. R =θ2-[θ i2 -(FWHM2-FWHM1)], θ R It is the horizontal coordinate of point E on the X-axis in the X-ray diffraction spectrum. A vertical line from point E to the X-axis intersects the (110) diffraction peak at point G. The back baseline of the (110) diffraction peak is determined by software setting or manual point selection. At the same time, a parallel line parallel to the back baseline is drawn through point G. The parallel line intersects the (110) diffraction peak at point F.

[0097] Step S9032, calculate the first area below the peak of the first diffraction peak and above the first back baseline, calculate the second area below the peak of the first diffraction peak and above the first parallel line, calculate the third area below the peak of the second diffraction peak and above the second back baseline, and calculate the fourth area below the peak of the second diffraction peak and above the second parallel line.

[0098] Step S9033: taking the ratio of the sum of the second area and the fourth area to the sum of the first area and the third area as the peak-to-area ratio.

[0099] Specifically, in the embodiment of the present invention, the (004) diffraction peak and the (110) diffraction peak are comprehensively considered, and the peak area below the top of the (004) diffraction peak and above the background line is taken as S1, the peak area below the top of the (004) diffraction peak and above the parallel line BC is taken as S2, the peak area below the top of the (110) diffraction peak and above the background line is taken as S3, and the peak area below the top of the (110) diffraction peak and above the parallel line GF is taken as S4. S1, S2, S3 and S4 are automatically calculated by software, and the corresponding addition of S2 and S4 and the corresponding addition of S1 and S3 are calculated, and the peak product ratio D is defined as the ratio of the sum of S2 and S4 to the sum of S1 and S3, that is, D=(S2+S4) / (S1+S3)*100%. The present invention can convert the angle difference into a restriction condition in a mathematical formula by selecting a reference point for the diffraction peak, thereby dividing the area under the diffraction peak and identifying the angle difference by the ratio of the areas of different regions under the diffraction peak. There is no need for complex and cumbersome parameter determination, thus reducing the difficulty of characterizing the degree of graphitization.

[0100] In some optional embodiments, the present invention analyzes four batches of graphite emulsions, such as Fig.11 As shown, the (004) crystal plane and (110) crystal plane are used for analysis. i1 and θ i2 The value is 0.4°, and the results are shown in the following table:

[0101] Brand batch number Peak-to-area ratio index (%) Graphitization index (%) 1# 33.73 87.19 2# 46.08 90.94 3# 71.05 92.86 4# 62.47 91.68

[0102] It can be seen that the peak area ratio and the graphitization degree have similar trends. However, the peak area ratios of different batches vary more. The reason is that the (004) diffraction peak is asymmetric, and there are components with different graphitization degrees in the graphite. The Mering-Maire formula results focus on the graphite with the largest content, so the new method is more accurate in characterizing the differences.

[0103] The method for characterizing the degree of graphitization provided by the present invention performs X-ray scanning on the sample to be tested, determines the peak position and half-width according to the diffraction peak corresponding to the preset crystal plane in the obtained X-ray diffraction spectrum, calculates the peak-to-product ratio of the diffraction peak according to the peak position and half-width, and characterizes the graphitization trend of the sample to be tested by the peak-to-product ratio. The present invention can convert the angle difference of the diffraction peak into the peak-to-product ratio without considering the precise peak position, peak separation parameters, etc., avoids the limitations of the Mering-Maire formula, improves the accuracy of the judgment of the graphitization trend, and thus ensures the reliability of product quality control or manufacturing process parameter adjustment.

[0104] In this embodiment, a device for characterizing the degree of graphitization is also provided, which is used to implement the above-mentioned embodiments and preferred embodiments, and will not be repeated hereafter. As used below, the term "module" can be a combination of software and / or hardware that implements a predetermined function. Although the devices described in the following embodiments are preferably implemented in software, the implementation of hardware, or a combination of software and hardware, is also possible and conceivable.

[0105] This embodiment provides a device for characterizing the degree of graphitization, such as Fig.12 As shown, including:

[0106] The spectrum acquisition module 1201 is used to acquire the X-ray diffraction spectrum after performing X-ray scanning on the sample to be tested.

[0107] The parameter determination module 1202 is used to determine the target peak position and the target half-height width according to the diffraction peak corresponding to the preset crystal plane in the X-ray diffraction spectrum.

[0108] The peak-to-area ratio calculation module 1203 is used to calculate the peak-to-area ratio of the diffraction peak according to the target peak position and the target half-height width, and to characterize the graphitization degree trend of the sample to be tested by the peak-to-area ratio.

[0109] In some optional implementations, the parameter determination module 1202 includes:

[0110] The peak shape determination unit is used to determine the original peak top and the original peak height of the diffraction peak according to the peak shape of the diffraction peak.

[0111] The target parameter determination unit is used to use the horizontal coordinate corresponding to the original peak top in the X-ray diffraction spectrum as the target peak position of the diffraction peak, and determine the target half-height width of the diffraction peak according to the original peak height.

[0112] In some optional embodiments, the preset crystal planes include: (004) crystal plane and (110) crystal plane, the corresponding diffraction peaks include a first diffraction peak and a second diffraction peak, the target peak position includes a first target peak position and a second target peak position, and the target half-width includes a first target half-width and a second target half-width; the peak-to-area ratio calculation module 1203 includes:

[0113] The diffraction peak selection unit is used to determine whether to select the first diffraction peak or the first diffraction peak and the second diffraction peak according to the peak shapes and peak intensities of the first diffraction peak and the second diffraction peak.

[0114] The first parallel line determining unit is used to determine the first background line of the first diffraction peak if the first diffraction peak is selected, and determine the first parallel line parallel to the first background line according to the first target peak position and the first target half-height width.

[0115] The first area calculation unit is used to calculate a first area below the first diffraction peak and above the first background line, and to calculate a second area below the first diffraction peak and above the first parallel line.

[0116] The first peak-to-area ratio calculation unit is used to take the ratio of the second area to the first area as the peak-to-area ratio.

[0117] In some optional implementations, the peak-to-area ratio calculation module 1203 further includes:

[0118] The second parallel line determination unit is used to determine the first back bottom line of the first diffraction peak and the second back bottom line of the second diffraction peak if the first diffraction peak and the second diffraction peak are selected, and determine the first parallel line parallel to the first back bottom line according to the first target peak position and the first target half-height width, and determine the second parallel line parallel to the second back bottom line according to the second target peak position, the first target half-height width and the second target half-height width.

[0119] The second area calculation unit is used to calculate the first area below the peak of the first diffraction peak and above the first back baseline, calculate the second area below the peak of the first diffraction peak and above the first parallel line, calculate the third area below the peak of the second diffraction peak and above the second back baseline, and calculate the fourth area below the peak of the second diffraction peak and above the second parallel line.

[0120] The second peak-to-area ratio calculation unit is used to take the ratio of the sum of the second area and the fourth area to the sum of the first area and the third area as the peak-to-area ratio.

[0121] In some optional implementations, the first parallel line determining unit includes:

[0122] The first reference point determination subunit is used to determine a first deviation angle according to the first target half-height width, the first deviation angle is smaller than the first target half-height width, and the difference between the first target peak position and the first deviation angle is used as the horizontal coordinate of the first reference point located on the X-axis in the X-ray diffraction pattern.

[0123] The second reference point determination subunit is used to determine a first vertical line passing through the first reference point and perpendicular to the X-axis, and to use the intersection of the first vertical line and the first diffraction peak as the second reference point.

[0124] The third reference point determination subunit is used to determine a first parallel line that passes through the second reference point, is parallel to the first background line, and intersects the first diffraction peak at the third reference point.

[0125] In some optional implementations, the second parallel line determining unit includes:

[0126] The fourth reference point determination subunit is used to determine the second deviation angle according to the second target half-width, the second deviation angle is less than twice the second target half-width, calculate the first difference between the first target half-width and the second target half-width, and calculate the second difference between the first deviation angle and the first difference, and use the third difference between the second target peak position and the second difference as the horizontal coordinate of the fourth reference point located on the X-axis in the X-ray diffraction pattern.

[0127] The fifth reference point determination subunit is used to determine a second vertical line passing through the fourth reference point and perpendicular to the X-axis, and to use the intersection of the second vertical line and the second diffraction peak as the fifth reference point.

[0128] The sixth reference point determination subunit is used to determine a second parallel line that passes through the fifth reference point, is parallel to the second back bottom line, and intersects the second diffraction peak at a sixth reference point.

[0129] In some optional embodiments, the device also includes: a correction module, which is used to correct the peak-to-area ratio according to a conversion coefficient to obtain the graphitization degree of the sample to be tested, and the conversion coefficient is determined based on a standard graphitization degree calculated in advance according to a standard sample and the Mellin formula and a pre-calculated standard peak-to-area ratio.

[0130] 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.

[0131] The graphitization degree 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.

[0132] The embodiment of the present invention also provides a computer device having the above Fig.12 The device for characterizing the degree of graphitization is shown.

[0133] See also Fig.13 , Fig.13 is a schematic diagram of the structure of a computer device provided by an optional embodiment of the present invention, such as Fig.13As 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.13 A processor 10 is taken as an example.

[0134] 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.

[0135] The memory 20 stores instructions executable by at least one processor 10, so that the at least one processor 10 executes the method shown in the above embodiment.

[0136] 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.

[0137] 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.

[0138] The computer device further comprises a communication interface 30 for the computer device to communicate with other devices or a communication network.

[0139] 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.

[0140] 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.

[0141] 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 degree of graphitization, characterized in that: The method comprises: Obtaining an X-ray diffraction pattern after X-ray scanning of the sample to be tested; Determining a target peak position and a target half-width according to a diffraction peak corresponding to a preset crystal plane in the X-ray diffraction spectrum; The peak area ratio of the diffraction peak is calculated according to the target peak position and the target half-height width, and the graphitization degree trend of the sample to be tested is characterized by the peak area ratio.

2. The method according to claim 1, characterized in that The step of determining the target peak position and the target half-width according to the diffraction peak corresponding to the preset crystal plane in the X-ray diffraction spectrum includes: Determining the original peak top and the original peak height of the diffraction peak according to the peak shape of the diffraction peak; The abscissa corresponding to the original peak top in the X-ray diffraction spectrum is used as the target peak position of the diffraction peak, and the target half-height width of the diffraction peak is determined according to the original peak height.

3. The method according to claim 1, characterized in that The preset crystal planes include: (004) crystal plane and (110) crystal plane, the corresponding diffraction peaks include a first diffraction peak and a second diffraction peak, the target peak positions include a first target peak position and a second target peak position, and the target half-width includes a first target half-width and a second target half-width; The step of calculating the peak-to-area ratio of the diffraction peak according to the target peak position and the target half-height width comprises: Determining whether to select the first diffraction peak or the first diffraction peak and the second diffraction peak according to the peak shapes and intensities of the first diffraction peak and the second diffraction peak; If the first diffraction peak is selected, a first background line of the first diffraction peak is determined, and a first parallel line parallel to the first background line is determined according to the first target peak position and the first target half-width; Calculate a first area below the first diffraction peak and above the first background line, and calculate a second area below the first diffraction peak and above the first parallel line; The ratio of the second area to the first area is taken as the peak-to-area ratio.

4. The method according to claim 3, characterized in that: The step of calculating the peak-to-area ratio of the diffraction peak according to the target peak position and the target half-height width further includes: If the first diffraction peak and the second diffraction peak are selected, a first back bottom line of the first diffraction peak and a second back bottom line of the second diffraction peak are determined, and a first parallel line parallel to the first back bottom line is determined according to the first target peak position and the first target half-width, and a second parallel line parallel to the second back bottom line is determined according to the second target peak position, the first target half-width and the second target half-width; Calculate a first area below the first diffraction peak and above the first background line, calculate a second area below the first diffraction peak and above the first parallel line, calculate a third area below the second diffraction peak and above the second background line, and calculate a fourth area below the second diffraction peak and above the second parallel line; The ratio of the sum of the second area and the fourth area to the sum of the first area and the third area is taken as the peak-to-area ratio.

5. The method according to claim 4, characterized in that The determining of a first parallel line parallel to the first back bottom line according to the first target peak position and the first target half-height width comprises: Determining a first deviation angle according to the first target half-width, the first deviation angle being smaller than the first target half-width, and taking the difference between the first target peak position and the first deviation angle as the abscissa of a 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 diffraction peak as a second reference point; Determine a first parallel line that passes through the second reference point, is parallel to the first background line, and intersects the first diffraction peak at a third reference point; The determining of a second parallel line parallel to the second back bottom line according to the second target peak position, the first target half-width and the second target half-width comprises: determining a second deviation angle according to the second target half width, the second deviation angle being less than twice the second target half width, calculating a first difference between the first target half width and the second target half width, calculating a second difference between the first deviation angle and the first difference, and using a third difference between the second target peak position and the second difference as the abscissa 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 diffraction peak as a fifth reference point; A second parallel line is determined which passes through the fifth reference point, is parallel to the second background line, and intersects the second diffraction peak at a sixth reference point.

6. The method according to claim 1, characterized in that After calculating the peak product ratio of the diffraction peak according to the target peak position and the target half-height width, the method further includes: The peak-to-area ratio is corrected according to a conversion coefficient to obtain the graphitization degree of the sample to be tested, wherein the conversion coefficient is determined based on a standard graphitization degree pre-calculated according to a standard sample and the Mellin formula and a pre-calculated standard peak-to-area ratio.

7. A graphitization degree characterization device, characterized in that: The device comprises: A spectrum acquisition module, used to obtain an X-ray diffraction spectrum after an X-ray scan of the sample to be tested; A parameter determination module, used to determine a target peak position and a target half-width according to a diffraction peak corresponding to a preset crystal plane in the X-ray diffraction spectrum; A peak-to-area ratio calculation module is used to calculate the peak-to-area ratio of the diffraction peak according to the target peak position and the target half-height width, and to characterize the graphitization degree trend of the sample to be tested by the peak-to-area ratio.

8. A computer device, characterized in that: include: 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 method for characterizing the degree of graphitization 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 graphitization 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 graphitization according to any one of claims 1 to 6.

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