Phase component measurement method, apparatus, device, storage medium, and program product

Abstract

The application relates to a phase component characterization method, device, equipment, storage medium and program product. The crystal lattice constant and phase content of each phase component in a to-be-detected powder are obtained, the atomic proportion of each element in each phase component is determined according to the crystal lattice constant corresponding to each phase component and a preset corresponding relationship between the atomic proportion of the first element and the crystal lattice constant, and then the mass proportion of each element in the to-be-detected powder is obtained according to the atomic proportion of each element in each phase component and the phase content of each phase component; wherein the to-be-detected powder is an infinite solid solution. The method can quickly and accurately calculate the mass proportion of each element in the to-be-detected powder by considering that the crystal lattice constant of each phase component in the to-be-detected powder changes with the change of the atomic proportion of the first element.

Description

Technical Field

[0001] This application relates to the field of materials testing technology, and in particular to a method, apparatus, equipment, storage medium, and program product for determining phase composition. Background Technology

[0002] Metal ceramics are composite structural materials composed of a ceramic hard phase and a metal / alloy binder phase. They mainly include two types of metal ceramics: TiC-based and Ti(C,N)-based. Due to the complexity of the phases in the finished products, the quality control of the raw materials is very important.

[0003] Taking Ti(C,N)-based cermets as an example, the main raw material is Ti(C,N) powder, and its phase composition has a significant impact on the machining performance of cutting tools. However, as an infinite solid solution alloy powder, Ti(C,N) powder may exist in different C / N ratios depending on the powder raw material preparation process or the stability of the preparation process; and the phase changes caused by these different C / N ratios will affect the process control of cermet sintered products. Therefore, it is necessary to study a stable and efficient characterization method for the Ti(C,N) phase composition.

[0004] In addition, traditional techniques typically use instruments such as inductively coupled plasma atomic emission spectrometers, energy dispersive spectroscopy analyzers, and fluorescence spectrometers to determine the content of elements in the solid solution phase. However, C and N are both light elements, and existing methods are not suitable for quickly and accurately determining their content. Summary of the Invention

[0005] Therefore, it is necessary to provide a method, apparatus, equipment, storage medium, and program product for determining phase composition, which can accurately determine the multiphase components and C / N content in Ti(C,N) powder, in response to the above-mentioned technical problems.

[0006] In a first aspect, this application provides a method for determining phase composition, the method comprising:

[0007] The lattice constants and phase contents of each phase in the powder to be tested are obtained; the powder to be tested is an infinite solid solution.

[0008] Based on the lattice constants corresponding to each phase composition and the pre-defined correspondence between the atomic percentage of the first element and the lattice constant, the atomic percentage of each element in each phase composition is determined.

[0009] The mass percentage of each element in the powder to be tested is obtained based on the atomic percentage of each element in each phase and the phase content of each phase.

[0010] In one embodiment, before obtaining the lattice constant and phase content corresponding to each phase component in the powder to be tested, the method further includes:

[0011] The content of a specified element in the powder to be tested is detected; the specified element refers to the element that affects the lattice constant of each phase composition in the powder to be tested.

[0012] If the content of a specified element is less than a preset threshold, the lattice constant and phase content of each phase component in the powder to be detected are obtained.

[0013] In one embodiment, the powder to be tested is Ti(C,N) powder.

[0014] In one embodiment, obtaining the lattice constant and phase content corresponding to each phase component in the powder to be detected includes:

[0015] Obtain the diffraction pattern of the powder to be tested under preset conditions;

[0016] A full-spectrum fitting analysis was performed on the diffraction pattern to obtain the fitting results;

[0017] Based on the fitting results, the lattice constants and phase contents of each phase component in the powder to be tested are obtained.

[0018] In one embodiment, the atomic percentage of each element in the phase composition is determined based on the lattice constant corresponding to the phase composition and the pre-defined correspondence between the atomic percentage of the first element and the lattice constant, including:

[0019] For any phase composition, obtain the adjacent lattice constants of the phase composition from the correspondence;

[0020] The atomic percentage of the first element in the phase composition is determined based on the adjacent lattice constants, the atomic percentage of the first element corresponding to the adjacent lattice constants, and the lattice constant of the phase composition.

[0021] The atomic percentage of each element in the phase composition is determined based on the atomic percentage of the first element in the phase composition.

[0022] In one embodiment, the method further includes:

[0023] Obtain the correspondence between the atomic percentage of the first element and the lattice constant from a standard database; and / or,

[0024] The relationship between the atomic percentage of the first element and the lattice constant was obtained through experiments.

[0025] Secondly, this application also provides a phase composition determination device, the device comprising:

[0026] The first acquisition module is used to acquire the lattice constant and phase content corresponding to each phase component in the powder to be tested; the powder to be tested is an infinite solid solution.

[0027] The second acquisition module is used to determine the atomic percentage of each element in each phase composition based on the lattice constant corresponding to each phase composition and the preset correspondence between the atomic percentage of the first element and the lattice constant.

[0028] The determination module is used to obtain the mass percentage of each element in the powder to be tested based on the atomic percentage of each element in each phase component and the phase content of each phase component.

[0029] Thirdly, embodiments of this application provide a computer device, including a memory and a processor. The memory stores a computer program, and the processor executes the computer program to implement the steps of any of the methods provided in the first aspect of the embodiments described above.

[0030] Fourthly, embodiments of this application provide a computer-readable storage medium having a computer program stored thereon, wherein the computer program, when executed by a processor, implements the steps of any of the methods provided in the first aspect of the embodiments described above.

[0031] Fifthly, embodiments of this application provide a computer program product, including a computer program that, when executed by a processor, implements the steps of any of the methods provided in the first aspect of the embodiments described above.

[0032] This application provides a method, apparatus, device, storage medium, and program product for determining phase composition. It obtains the lattice constant and phase content of each phase component in a powder to be tested. Based on the lattice constant of each phase component and the pre-defined correspondence between the atomic percentage of a first element and the lattice constant, the atomic percentage of each element in each phase component is determined. Then, based on the atomic percentage of each element in each phase component and the phase content of each phase component, the mass percentage of each element in the powder to be tested is obtained. The powder to be tested is an infinite solid solution. This method considers that the lattice constant of each phase component in the powder to be tested changes with the atomic percentage of the first element. Therefore, the atomic percentage of the first element can be determined based on the pre-defined correspondence between the atomic percentage of the first element and the lattice constant, thereby obtaining the atomic percentage of each element in each phase component in the powder to be tested. Finally, based on the atomic percentage of each element in each phase component in the powder to be tested and the phase content of each phase component, the mass percentage of each element in the powder to be tested is obtained. The detection method is simple, fast, and highly accurate. Attached Figure Description

[0033] Figure 1 This is a diagram illustrating the application environment of the phase composition determination method in one embodiment;

[0034] Figure 2 This is a schematic flowchart of a phase composition determination method in one embodiment;

[0035] Figure 3 This is a schematic diagram of the structure of NaCl crystals;

[0036] Figure 4 This is a schematic flowchart of a phase composition determination method in another embodiment;

[0037] Figure 5 This is a schematic flowchart of a phase composition determination method in another embodiment;

[0038] Figure 6 The diffraction pattern of Ti(C, N) in one embodiment is shown.

[0039] Figure 7 The diffraction pattern of Ti(C, N) in another embodiment;

[0040] Figure 8 This is a schematic flowchart of a phase composition determination method in another embodiment;

[0041] Figure 9 This is a schematic flowchart of a phase composition determination method in another embodiment;

[0042] Figure 10 This is a schematic flowchart of a phase composition determination method in another embodiment;

[0043] Figure 11 This is a structural block diagram of the phase composition determination device in one embodiment;

[0044] Figure 12 This is an internal structural diagram of a computer device in one embodiment. Detailed Implementation

[0045] To make the objectives, technical solutions, and advantages of this application clearer, the following detailed description is provided in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this application.

[0046] The phase composition determination method provided in this application embodiment can be applied to, for example... Figure 1 In the application environment shown, the detection device 102 communicates with the server 104. The data storage system can store the data that the function computing platform 104 needs to process. The data storage system can be integrated onto the server 104, or it can be located in the cloud or on other network servers. The detection device 102 can be, but is not limited to, an X-ray diffractometer or similar equipment. The server 104 can be a standalone server or a server cluster consisting of multiple servers.

[0047] In related technologies, when determining the phase composition of Ti(C,N) powder, if the analysis is carried out using traditional qualitative methods, it is difficult to solve the problem of overlapping peaks "splitting" in the diffraction pattern of Ti(C,N) powder. Due to the similar phase structure of Ti(C,N), Ti(C,N) with different C / N ratios mostly shows overlapping peaks in the diffraction pattern, and there are few cases of independent diffraction peaks.

[0048] Based on this, embodiments of this application provide a method, apparatus, device, storage medium, and program product for determining phase composition, which can characterize the multiphase components and C / N content ratio in Ti(C,N) powder.

[0049] It should be noted that the atomic percentage in this application is not limited to the sum of the atomic percentages of all elements in each phase being 1; it can also be 2, 3, or other values. Taking Ti(C) as an example... x N 1-x For example, C has an atomic percentage of x, but the total atomic percentage of all its elements is 2.

[0050] The following specific embodiments can be combined with each other, and the same or similar concepts or processes may not be described again in some embodiments. The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are some embodiments of this application, but not all embodiments.

[0051] In one embodiment, a phase composition determination method is provided for application in... Figure 1 Taking the application environment in the example, such as Figure 2 As shown, this embodiment involves obtaining the atomic percentage of each element in each phase component based on the lattice constant corresponding to each phase component and the pre-defined correspondence between the atomic percentage of the first element and the lattice constant, and obtaining the mass percentage of each element in the powder to be tested based on the atomic percentage of each element in each phase component and the phase content of each phase component. This embodiment includes the following steps:

[0052] S201, obtain the lattice constant and phase content corresponding to each phase component of the powder to be tested; the powder to be tested is an infinite solid solution.

[0053] In physics, a phase refers to a set of states of a macroscopic physical system, also known as a state of matter. Matter in a phase has a simple chemical composition and physical properties (such as density, crystal structure, refractive index, etc.). Based on the different forms and distributions of matter in the system, the system is divided into phases. The total number of phases in the system is called the phase number. Based on the different phase numbers, the system can be divided into single-phase systems and multi-phase systems.

[0054] A phase refers to an aggregate of homogeneous substances with identical physical and chemical properties and composition under the absence of external forces. An alloy phase containing other elements within the crystal lattice structure of one element is called a solid solution. In a solid solution crystal lattice, the chemical particles of each component are randomly and uniformly distributed, and its physical and chemical properties meet the requirements of phase homogeneity. Therefore, a solid solution formed between several substances constitutes a single phase.

[0055] Mixtures of different solids are multiphase systems, such as granite (composed of minerals like quartz, mica, and feldspar), or colorless, transparent diamond containing a small amount of black diamond. Under specified conditions, there are clear interfaces between phases; at these interfaces, changes in properties appear abrupt from a macroscopic perspective.

[0056] The crystals of ceramic materials are mainly single oxides (such as Al₂O₃, MgO) and composite oxides (such as spinel MgO·Al₂O₃, lead zirconate titanate Pb(Zr,Ti)O₃); in addition, non-oxide ceramic materials also contain crystals of corresponding components such as carbides, nitrides, borides, and silicides. The properties of ceramic materials are closely related to the type, quantity, distribution, and defect status of the phases; that is, the type and content of the phases affect the process control of sintered cermet products. Therefore, determining the phases and their contents in the material is crucial.

[0057] The powder to be tested is an infinite solid solution. Therefore, in one embodiment, the powder to be tested can be Ti(C,N) powder. Ti(C,N) powder is the main raw material for producing Ti(C,N) cermets. As an infinite solid solution alloy powder, Ti(C,N) may exist in different C / N ratios when the powder raw material preparation process is different or when it is affected by the stability of the preparation process. The type and content of these phases affect the process control of cermet sintered products.

[0058] Optionally, by performing X-ray diffraction on the powder to be tested and fitting and analyzing its diffraction pattern, the lattice constant and phase content corresponding to each phase component in the powder to be tested can be obtained.

[0059] The powder to be tested is a raw material for producing a certain product, and is a substance whose phase composition needs to be detected. For example, if Ti(C,N) cermet is to be produced, then the powder to be tested is Ti(C,N) powder. The Rietveld method can be used to simulate and calculate different Ti(C) phase compositions. x N y The lattice constant and phase content of the phase; where phase content refers to the content of the phase composition.

[0060] The lattice constant (or lattice parameter) refers to the edge length of a unit cell, that is, the edge length of each parallelepiped unit. It is an important basic parameter of crystal structure. The lattice constant is the physical size of the unit cell in the crystal lattice. The unit cell is the basic repeating unit of the periodic arrangement in the crystal structure and is the smallest component that can represent the characteristics of the crystal structure.

[0061] It should be noted that the powder to be tested may contain one phase component or multiple phase components.

[0062] S202, based on the lattice constants corresponding to each phase component and the pre-defined correspondence between the atomic percentage of the first element and the lattice constant, determine the atomic percentage of each element in the phase component.

[0063] The atomic percentages of all remaining elements other than the preset first element must have a unique and definite value, and the preset first element is preferably a light element. In the powder to be tested, if the atomic percentage of the preset first element is determined, then the atomic percentages of each element in the phase composition are also determined.

[0064] Taking Ti(C,N) powder as an example, the crystal structure of Ti(C,N) powder is a face-centered cubic (FCC) phase similar to that of NaCl. Figure 3 As shown, Figure 3 This is a schematic diagram of the NaCl crystal structure; the components TiN and TiC also belong to the face-centered cubic phase structure, and the two can be miscible in any proportion to form Ti(C) x N y A solid solution phase in the form of ) where x and y are the atomic percentages of C and N, respectively (x < 1, y < 1; x + y = 1), can also be represented as Ti(C) x N 1-x In the form of ), the first element is pre-defined as C or N, preferably a C atom.

[0065] According to Vegard's law, the cell parameters of a solid solution phase are approximately linearly related to its constituent elements. Since Ti(C,N) is an infinite solid solution, the deviation from this relationship is minimal; therefore, theoretically, its lattice constant should increase with increasing TiC content, i.e., increase with increasing x. Thus, a linear relationship can be established between the atomic percentage of C and the lattice constant of the solid solution phase.

[0066] Based on the correspondence between the atomic percentage of element C and the lattice constant, and given the lattice constant corresponding to the phase composition, the atomic percentage of the first element C, i.e., x, can be calculated. Then, the atomic percentage of N, i.e., 1-x, can be calculated. The atomic percentage of Ti remains unchanged since its chemical formula is fixed, thus determining the atomic percentage of each element in the phase composition.

[0067] It should be noted that, given the knowledge of the first element in the powder to be tested, the atomic percentage of each element in each phase of the powder can be determined.

[0068] S203, based on the atomic percentage of each element in each phase component and the phase content of each phase component, the mass percentage of each element in the powder to be tested is obtained.

[0069] First, based on the atomic percentage of each element in the phase composition, the mass percentage of each element in the phase composition can be determined; then, based on the mass percentage of each element in the phase composition and the phase content of each phase composition, the mass percentage of each element in the powder to be tested can be obtained.

[0070] The conversion between atomic percentage and mass percentage can be shown in formula (1).

[0071]

[0072] Where, N i x represents the mass percentage of element i in a certain component. i Let X represent the atomic percentage of element i in a given composition, and let X represent the atomic weight of element i in that composition. j Let Y represent the atomic percentage of element j in a certain component, and Y represent the atomic weight of element j in a certain component. It should be noted that the ellipsis in formula (1) represents the product of the atomic percentage of other elements in a certain component and their corresponding atomic weights.

[0073] The conversion formula between atomic percentage and mass percentage can be: Mass (weight) percentage of a component = Atomic percentage of the component * Atomic weight of the component / (Atomic percentage of each component * Sum of atomic weights of each component).

[0074] Since the powder to be tested may contain multiple phase components, the mass percentage of each element in the powder to be tested is calculated based on the mass percentage of each element in each phase component and the phase content of each phase component. The mass percentage of each element in the powder to be tested can be calculated according to formula (2).

[0075]

[0076] Among them, Q wt W represents the mass percentage of element Q in the powder to be tested. i Q represents the phase content of the i-th phase component in the powder to be tested. i The expression represents the mass percentage of element Q in the i-th phase component of the powder to be tested, and n represents the number of phase components in the powder to be tested. Q can refer to any element in the powder to be tested. In this embodiment, Q is used only for illustration and does not represent any meaning.

[0077] It should be noted that the mass percentage of each element in the phase composition refers to the mass percentage of each element in its respective phase composition, the mass percentage of each element in the powder to be tested refers to the mass percentage of each element in the powder to be tested, and the phase content refers to the content percentage of the phase in the powder to be tested.

[0078] Continuing with the example of Ti(C,N) powder to be tested, the mass percentage of each element in the above phase composition is the mass percentage of C and N elements in the phase composition of Ti(C,N) powder. It can be calculated using formulas (3) and (4) based on the proportion of C and N atoms in the phase composition.

[0079]

[0080]

[0081] Among them, c i The percentage of C atoms in the phase composition, C z n is the atomic weight of a C atom. i The atomic percentage of N atoms in the phase composition, N z Ti is the atomic weight of N atoms, and ti is the atomic percentage of Ti atoms in the phase composition. z C is the atomic weight of Ti atoms. i The mass percentage of C atoms in the phase composition, N i This represents the mass percentage of N atoms in the phase composition.

[0082] Then, the mass percentages of C and N elements in Ti(C,N) powder can be calculated using formulas (5) and (6).

[0083]

[0084]

[0085] Among them, C wt W represents the mass percentage of carbon (C) in the powder being tested. i C represents the phase content of the i-th phase component in the powder to be tested. i N represents the mass percentage of C element in the i-th phase component of the powder to be tested, n represents the number of phase components in the powder to be tested, and N represents the mass percentage of C element in the i-th phase component of the powder to be tested. wt This indicates the mass percentage of nitrogen (N) in the powder being tested. i This represents the mass percentage of N element in the i-th phase component of the powder to be tested.

[0086] It should be noted that the chemical formula of each infinite solid solution is fixed, with only one variable. Therefore, once the number of atoms of one element is determined, the number of other elements is also determined.

[0087] In the aforementioned method for determining phase composition, the lattice constant and phase content of each phase component in the powder to be tested are obtained. Based on the lattice constant of each phase component and the pre-defined correspondence between the atomic percentage of the first element and the lattice constant, the atomic percentage of each element in each phase component is determined. Then, based on the atomic percentage of each element in each phase component and the phase content of each phase component, the mass percentage of each element in the powder to be tested is obtained. The powder to be tested is an infinite solid solution. This method considers that the lattice constant of each phase component in the powder to be tested changes with the atomic percentage of the first element. Therefore, the atomic percentage of the first element can be determined based on the pre-defined correspondence between the atomic percentage of the first element and the lattice constant, thereby obtaining the atomic percentage of each element in each phase component in the powder to be tested. Finally, based on the atomic percentage of each element in each phase component in the powder to be tested and the phase content of each phase component, the mass percentage of each element in the powder to be tested is obtained. The detection method is simple, rapid, and highly accurate.

[0088] In one embodiment, such as Figure 4 As shown, before obtaining the lattice constant and phase content corresponding to the phase composition of the powder to be detected, this embodiment includes the following steps:

[0089] S401, Detect the content of a specified element in the powder to be tested; the specified element refers to the element that affects the lattice constant of each phase component in the powder to be tested.

[0090] Typically, the powder to be tested prepared by a certain method may contain a certain excess element. If there is too much of this element, it will directly affect the lattice constant of each phase component in the powder to be tested, resulting in an incorrect atomic ratio of each phase component in the tested powder. Therefore, it is necessary to test the content of a certain element before testing the powder to be tested.

[0091] Therefore, based on the preparation process of the powder to be tested, a designated element is determined. The designated element is an extra element that may be introduced into the powder during the preparation process. The designated element refers to the element that affects the lattice constant of each phase component in the powder to be tested.

[0092] The preparation of Ti(C,N) powder will be used as an example for illustration.

[0093] The main method for preparing Ti(C,N) powder is the direct carburization and nitridation method, which uses TiO2 as raw material and prepares it through a carbothermic reduction reaction in an N2 atmosphere. Under different reaction conditions, the powder may contain TiO2, free carbon, TiO(C,N) and Ti(C,N) in different C / N ratios, as shown in formulas (7) and (8).

[0094] TiO2 + C + N2 → Ti(C, N) + CO (7)

[0095] TiC-TiO+N2→TiC-TiO-TiN+CO (8)

[0096] Here, if oxygen (O) is also dissolved in Ti(C,N), the lattice constant of the solid solution phase changes; excessive O content affects the result determination. Therefore, before using this method to characterize the multiphase composition of Ti(C,N) powder, the O content of the Ti(C,N) powder needs to be determined to eliminate the influence of possible TiO(C,N) formation; however, if the O content is low, or its presence only results in TiO2 residue, this method can still be applied.

[0097] S402, if the content of a specified element is less than a preset threshold, then obtain the lattice constant and phase content corresponding to each phase component in the powder to be detected.

[0098] Therefore, based on the above analysis, if the content of a specified element in the powder to be tested exceeds the preset threshold, that is, is greater than or equal to the preset threshold, it means that the powder to be tested is not suitable for characterizing phase composition using this method.

[0099] Only when the content of a specified element in the powder to be tested is low, indicating that the lattice constant of each phase component in the powder to be tested is less affected, can the mass percentage of each element in the powder be obtained by the phase composition determination method in the embodiments of this application.

[0100] In the aforementioned method for determining phase composition, the content of a specified element in the powder to be tested is detected. The specified element refers to an element that influences the lattice constant of each phase component in the powder to be tested. If the content of the specified element is less than a preset threshold, the lattice constant and phase content corresponding to each phase component in the powder to be tested are obtained. This method ensures the accuracy of the atomic percentage of each element in each phase component of the powder to be tested by detecting whether the specified element is present in excess, further improving the accuracy of detecting the mass percentage of each element.

[0101] This application uses the Rietveld-assisted lattice constant method to determine the lattice constants and phase contents of each phase component in the powder to be tested. A detailed explanation of this method follows with an example. In one embodiment, such as… Figure 5 As shown, the lattice constants and phase contents corresponding to each phase component in the powder to be tested are obtained, including:

[0102] S501, Obtain the diffraction pattern of the powder to be tested under preset conditions.

[0103] In this embodiment, the lattice constant and phase content of each phase component in the powder to be tested are determined by the Rietveld characterization method. Specifically, when using TOPAS fitting parameters, the influence of peak position and peak shape is mainly considered, focusing on the fitting of lattice constant and grain size.

[0104] When obtaining the lattice constant and phase content corresponding to each phase component in the powder to be tested, the diffraction spectrum of the powder to be tested is first obtained by scanning under preset conditions.

[0105] Optionally, the diffraction pattern of the powder to be tested under preset conditions can be obtained by X-ray diffraction. For example, XRD diffraction pattern can be obtained by phase analysis of x-ray diffraction (XRD). The preset condition can be a preset angle. The XRD diffraction pattern is the diffraction pattern obtained by scanning at the preset angle, and the preset angle can be a low angle or a high angle. Specifically, the diffraction pattern of the powder to be tested at a low angle can be determined by low-angle diffraction of XRD technology, and the diffraction pattern of the powder to be tested at a high angle can also be determined by high-angle diffraction of XRD technology.

[0106] XRD is a crystal detection method. When X-rays hit a crystal with periodically arranged atoms, they produce a diffraction pattern. The diffraction pattern reflects information about the arrangement of atoms inside the crystal. Different crystals have different atomic arrangements. Therefore, the type of crystal, phase composition, and a series of other information can be determined by the diffraction pattern.

[0107] It should be noted that 0-90 degrees can be defined as a low angle and 90-180 degrees as a high angle. The specific range of low and high angles is not limited in the implementation of this application.

[0108] The method for obtaining the powder to be tested can be as follows: after grinding the powder to be tested, spread it evenly on a glass slide, flatten it, use a Co target, scan at an angle of 20-120°, a step size of 0.033°, and a dwell time of 50s per step to obtain the scanning spectrum.

[0109] S502, perform full-spectrum fitting analysis on the diffraction pattern to obtain the fitting results.

[0110] First, based on the diffraction spectrum of the powder to be tested under preset conditions obtained above, phase pre-determination is performed, that is, the number of phases is determined by the diffraction spectrum, and then the full spectrum of the diffraction spectrum is fitted according to the determined number of phases to obtain the fitting result; the fitting result is further analyzed, and if the fitting result is inaccurate, the phase pre-determination of the diffraction spectrum is performed again, and then the full spectrum fitting is performed again on the pre-determined number of phases until the fitting result is accurate.

[0111] Taking Ti(C, N) powder as an example, such as Figure 6 and Figure 7 As shown, Figure 6 To obtain low-angle XRD diffraction patterns of Ti(C, N) obtained under different production processes, Figure 7The high-angle XRD diffraction patterns of Ti(C, N) obtained under different production processes show little difference between low-angle and high-angle diffraction patterns. It should be noted that phases with similar lattice constants tend to form overlapping peaks. Identifying the number of phases from high-angle diffraction peaks is more accurate; therefore, the number of phases can be predicted in advance based on the high-angle diffraction peaks.

[0112] One way to determine the number of phases based on the diffraction spectrum is by using an empirical method to determine the number of phases in the high-angle scan spectrum.

[0113] Then, based on the number of phases obtained from the above phase pre-determination, the diffraction spectrum is fully fitted to obtain the fit to be verified. Based on the obtained fit to be verified and the diffraction spectrum, the accuracy of the fit to be verified is analyzed. If the fit to be verified is accurate, it is determined as the fitting result of the diffraction spectrum.

[0114] Specifically, the error between the fitted spectrum to be verified and the scanning spectrum, as well as the grain size difference between different phases, are calculated.

[0115] When the error between the fitting to be verified and the diffraction spectrum meets the conditions, and the grain size difference between different phases also meets the conditions, it can be determined that the above-mentioned number of phases is correct, and the fitting to be verified is the fitting result.

[0116] If the error between the fitted sample and the diffraction spectrum does not meet the conditions, and / or the grain size difference between different phases does not meet the conditions, it can be determined that the number of the above phases is incorrect. In this case, the phase pre-judgment needs to be performed again. Then, based on the number of phases pre-judged, the diffraction spectrum is fitted to the whole spectrum until the error between the fitted sample and the scanning spectrum meets the conditions, and the grain size difference between different phases also meets the conditions. Then, the fitted sample can be determined as the fitting result.

[0117] Alternatively, the Rietveld method can be used to perform full-spectrum fitting of the diffraction pattern.

[0118] S503, based on the fitting results, obtain the lattice constant and phase content of each phase component in the powder to be tested.

[0119] Based on the fitting results obtained above, the lattice constants are refined to further determine the lattice constants and phase contents of each phase component in the powder to be tested.

[0120] In one embodiment, such as Figure 8 As shown, Figure 8The flowchart for determining lattice constants and phase contents using the Rietveld-assisted lattice constant method is as follows: First, XRD diffraction scanning of the powder to be tested is performed at high or low angles to obtain diffraction patterns. The number of phases present is determined by the high-angle diffraction patterns. Then, the determined number of phases is fitted with multiple standard models (standard scanning patterns) to calculate the fitting error between the diffraction patterns and the fitted scanning patterns to be verified, as well as the grain size difference of different phases. If both the fitting error and the grain size difference of different phases are less than the corresponding preset thresholds, the number of phases is correctly determined. The lattice constants are then further refined to determine the lattice constants and phase contents of each phase component in the powder to be tested. If either the fitting error or the grain size difference of different phases is not less than the corresponding preset threshold, it indicates that the number of phases is incorrect. The number of phases is then re-determined, and the fitting calculation is repeated with multiple standard models (standard scanning patterns) until both the fitting error and the grain size difference of different phases are less than the corresponding preset thresholds.

[0121] In the above-described method for determining phase composition, a diffraction spectrum of the powder to be tested is obtained by scanning under preset conditions. A full-spectrum fitting analysis is then performed on the diffraction spectrum to obtain the fitting results. Based on these results, the lattice constant and phase content of each phase component in the powder to be tested are obtained. This method improves the accuracy of determining the lattice constant and phase content of each phase component in the powder to be tested.

[0122] In one embodiment, such as Figure 9 As shown, the atomic percentage of each element in each phase is determined based on the lattice constants corresponding to each phase composition and the pre-defined correspondence between the atomic percentage of the first element and the lattice constants. This includes the following steps:

[0123] S901, for any phase composition, obtain the adjacent lattice constants of the phase composition's lattice constant from the correspondence.

[0124] Based on the preset correspondence between the atomic percentage of the first element and the lattice constant, the atomic percentage of the first element in each phase composition is determined. Specifically, for example, based on the lattice constant corresponding to the phase composition, the lattice constant of the phase composition can be found in the preset correspondence between the atomic percentage of the first element and the lattice constant, and the atomic percentage of the first element corresponding to the lattice constant of the phase composition is determined as the atomic percentage of the first element in that phase composition.

[0125] For example, if the lattice constant of a certain phase composition is Then, find the lattice constant in the correspondence. The atomic percentage of the first element is determined, and then the atomic percentage of each element in the phase composition is determined based on the atomic percentage of the first element. In the chemical formula of the solid solution phase, determining the atomic percentage of one element allows us to determine the atomic percentages of the other elements.

[0126] Before obtaining the adjacent lattice constants of the lattice constant from the correspondence, it is necessary to construct the correspondence between the atomic percentage of the first element and the lattice constant. In one embodiment, the correspondence between the atomic percentage of the first element and the lattice constant can be obtained from a standard database; and / or, the correspondence between the atomic percentage of the first element and the lattice constant can be obtained experimentally.

[0127] Specifically, the correspondence between the atomic percentage of the first element and its lattice constant can be a pre-constructed database of correspondences, the data of which can be obtained from standard databases and / or experimentally. Each data point contains two values: the atomic percentage of the first element and its corresponding lattice constant.

[0128] Taking Ti(C,N) powder as an example, the relationship between the atomic percentage of C and the lattice constant of the solid solution phase is shown in Table 1.

[0129] Table 1

[0130]

[0131] Table 1 shows data from both standard databases and experimental results. To ensure data reliability, experiments were conducted using a single Ti(C) solution as much as possible. x N y Therefore, during the experiment, a higher sintering temperature can be set to ensure that the obtained sample has the highest possible degree of crystallinity, thus avoiding broadening of the scanning spectrum peaks and causing misjudgment.

[0132] As can be seen from Table 1, as the carbon content increases, Ti(C) x N y The overall trend of the lattice constant is indeed increasing. In practical calculations, when deducing the atomic percentage of elements from known lattice constants, interpolation is used, taking the nearest neighbor function value for calculation, which can minimize errors to the greatest extent.

[0133] That is, based on the lattice constant of the phase composition, the adjacent lattice constants of the first element are obtained from the correspondence between the atomic percentage of the first element and the lattice constant. For example, if the lattice constant of the phase composition is 4.2600, then the adjacent lattice constants of 4.2600 are 4.2430 and 4.2644 obtained from the correspondence in Table 1.

[0134] S902, determine the atomic percentage of the first element in the phase composition based on the adjacent lattice constants, the atomic percentage of the first element corresponding to the adjacent lattice constants, and the lattice constant of the phase composition.

[0135] By comparing the corresponding relationships, the atomic percentage of the first element in the phase composition is calculated according to formula (9).

[0136]

[0137] Where x represents the atomic percentage of the first element in the phase composition, z1 and z2 represent the adjacent lattice constants of the phase composition, x1 and x2 represent the atomic percentage of the first element corresponding to two adjacent lattice constants, and z represents the lattice constant of the phase composition.

[0138] Therefore, by substituting the adjacent lattice constants, the atomic percentage of the first element corresponding to the adjacent lattice constants, and the lattice constant of the phase composition into formula (9), the atomic percentage of the first element in the phase composition can be obtained.

[0139] S903, determine the atomic percentage of each element in the phase composition based on the atomic percentage of the first element in the phase composition.

[0140] Taking Ti(Cx, Ny) as an example, if the atomic percentage of the first element C in the phase composition obtained above is 0.5, it can be directly determined that the atomic percentage of Ti is 1 and the atomic percentage of N is 0.5. That is, the phase composition of Ti(Cx, Ny) includes C, N and Ti elements.

[0141] In the aforementioned method for determining phase composition, adjacent lattice constants are obtained from a correspondence relationship. Based on these adjacent lattice constants, the atomic percentage of the first element corresponding to each adjacent lattice constant, and the lattice constant of the phase composition, the atomic percentage of the first element in the phase composition is determined. Then, based on the atomic percentage of the first element in the phase composition, the atomic percentage of each element in the phase composition is determined. This method, by using neighboring lattice constants for calculation, can minimize errors and improve the accuracy of the atomic percentage of each element in the phase composition.

[0142] In one embodiment, the Rietveld-assisted lattice constant method is used to rapidly and accurately characterize the phase composition of the Ti(C,N) solid solution phase. Multiple experiments demonstrate that the phase composition determination method of this application can rapidly determine the Ti(C,N) phases with different C / N ratios coexisting in Ti(C,N) powder. x N y The number and content of phases can be used to accurately deduce the actual C / N content of the powder without the need for additional chemical testing.

[0143] Regarding phase composition, a verification method is also provided to verify the accuracy of the phase composition in the embodiments of this application. In one embodiment, a certain number of powders to be tested are obtained, and the actual mass percentage of each element in the powders to be tested is known. The predicted mass percentage of each element in the powders to be tested is determined by the phase composition method in the embodiments of this application. By comparing it with the actual mass percentage, the accuracy of determining the mass percentage of each element in the powders to be tested in the phase composition method in the embodiments of this application can be determined.

[0144] Taking Ti(C,N) powder as an example for verification, several Ti(C,N) powders were selected, and the mass ratio of C / N elements in each Ti(C,N) powder was known. The mass ratio of C / N elements in the Ti(C,N) powder was determined by the phase composition method in this embodiment of the application. By comparing with the actual mass ratio of C / N elements, the error of determining the mass ratio of C / N elements in Ti(C,N) powder using the method in this embodiment of the application does not exceed 0.2%. The effectiveness of the phase composition method in this application was verified through the verification method in this embodiment.

[0145] In one embodiment, such as Figure 10 As shown, taking Ti(C, N) powder as an example, this embodiment includes the following steps:

[0146] S1001, construct a database of the correspondence between the atomic percentage of element C and the lattice constant.

[0147] S1002, Test the oxygen content of Ti(C,N) powder. If the oxygen content is less than the preset threshold, proceed to S1003.

[0148] If the oxygen content is less than the preset threshold, it means that the oxygen content is not exceeded and the content of C and N in Ti(C,N) powder is detected by the phase composition determination method in this application. If the oxygen content exceeds the standard, the phase composition determination method in this application cannot be used for detection.

[0149] S1003, the lattice constants and phase contents of each phase in Ti(C,N) powder were determined using the Rietveld-assisted lattice constant method.

[0150] S1004, obtain the adjacent lattice constants of the lattice constants of each phase component from the database of correspondence between the atomic percentage of C element and lattice constants.

[0151] S1005, based on the adjacent lattice constants, the atomic percentage of C element corresponding to the adjacent lattice constants, and the lattice constant of the phase composition, determine the atomic percentage of C element in each phase composition.

[0152] S1006, Determine the mass percentage of C and N elements in each phase component based on the atomic percentage of C element in each phase component;

[0153] Wherein, the mass (weight) percentage of C element = atomic percentage of C element * atomic weight of C element / (atomic percentage of C element * atomic weight of C element + atomic percentage of N element * atomic weight of N element + atomic percentage of Ti element * atomic weight of Ti element)

[0154] The mass (weight) percentage of nitrogen = the atomic percentage of carbon * the atomic weight of carbon / (atomic percentage of carbon * atomic weight of carbon + atomic percentage of nitrogen * atomic weight of nitrogen + atomic percentage of titanium * atomic weight of titanium)

[0155] S1007. Based on the phase content of each phase component, the mass percentage of C element and the mass percentage of N element, determine the mass percentage of C element and the mass percentage of N element in Ti(C,N) powder.

[0156] The specific limitations of the phase composition determination method provided in this embodiment can be found in the step limitations of each embodiment of the phase composition determination method above, and will not be repeated here.

[0157] It should be understood that although the steps in the flowcharts attached to the above embodiments are shown sequentially according to the arrows, these steps are not necessarily executed in the order indicated by the arrows. Unless explicitly stated herein, there is no strict order restriction on the execution of these steps, and they can be executed in other orders. Moreover, at least some of the steps in the figures attached to the above embodiments may include multiple steps or multiple stages. These steps or stages are not necessarily completed at the same time, but can be executed at different times. The execution order of these steps or stages is not necessarily sequential, but can be performed alternately or in turn with other steps or at least some of the steps or stages in other steps.

[0158] In one embodiment, such as Figure 11 As shown in the figure, this application embodiment also provides a phase composition determination device 1100, which includes: a first acquisition module 1101, a second acquisition module 1102, and a determination module 1103, wherein:

[0159] The first acquisition module 1101 is used to acquire the lattice constant and phase content corresponding to each phase component in the powder to be tested; the powder to be tested is an infinite solid solution.

[0160] The second acquisition module 1102 is used to determine the atomic percentage of each element in each phase composition based on the lattice constant corresponding to each phase composition and the preset correspondence between the atomic percentage of the first element and the lattice constant.

[0161] The determination module 1103 is used to obtain the mass percentage of each element in the powder to be tested based on the atomic percentage of each element in each phase component and the phase content of each phase component.

[0162] In one embodiment, the device 1100 further includes:

[0163] The detection module is used to detect the content of specified elements in the powder to be tested; the specified elements refer to the elements that affect the lattice constant of each phase composition in the powder to be tested.

[0164] The third acquisition module is used to acquire the lattice constant and phase content of each phase component in the powder to be detected if the content of a specified element is less than a preset threshold.

[0165] In one embodiment, the powder to be tested is Ti(C,N) powder.

[0166] In one embodiment, the first acquisition module 1101 includes:

[0167] The second acquisition unit is used to acquire the diffraction spectrum obtained by scanning the powder to be detected under preset conditions;

[0168] The analysis unit is used to perform full-spectrum fitting analysis on the diffraction spectrum and obtain the fitting results.

[0169] The third acquisition unit is used to acquire the lattice constant and phase content of each phase component in the powder to be detected based on the fitting results.

[0170] In one embodiment, the second acquisition module 1102 includes:

[0171] Obtain sub-units, used to obtain the adjacent lattice constants of the lattice constants of the phase composition from the correspondence for any phase composition;

[0172] The first determining subunit is used to determine the atomic percentage of the first element in the phase composition based on the adjacent lattice constants, the atomic percentage of the first element corresponding to the adjacent lattice constants, and the lattice constant of the phase composition.

[0173] The second determining subunit is used to determine the atomic percentage of each element in the phase composition based on the atomic percentage of the first element in the phase composition.

[0174] In one embodiment, the device 1100 further includes:

[0175] The fourth acquisition module is used to obtain the correspondence between the atomic percentage of the first element and the lattice constant from a standard database; and / or, to obtain the correspondence between the atomic percentage of the first element and the lattice constant through experiments.

[0176] Specific limitations regarding the phase composition determination apparatus can be found in the limitations of each step in the phase composition determination method described above, and will not be repeated here. Each module in the aforementioned phase composition determination apparatus can be implemented entirely or partially through software, hardware, or a combination thereof. These modules can be embedded in or independent of the target device in hardware form, or stored in the target device's memory in software form, so that the target device can invoke and execute the operations corresponding to each module.

[0177] In one embodiment, a computer device is provided, such as Figure 12 As shown, the computer device includes a processor, memory, communication interface, display screen, and input devices connected via a system bus. The processor provides computing and control capabilities. The memory includes non-volatile storage media and internal memory. The non-volatile storage media stores the operating system and computer programs. The internal memory provides an environment for the operation of the operating system and computer programs stored in the non-volatile storage media. The communication interface is used for wired or wireless communication with external terminals; wireless communication can be achieved through Wi-Fi, mobile cellular networks, NFC (Near Field Communication), or other technologies. When the computer program is executed by the processor, it implements a phase composition determination method. The display screen can be an LCD screen or an e-ink display screen. The input devices can be a touch layer covering the display screen, buttons, a trackball, or a touchpad on the computer device's casing, or an external keyboard, touchpad, or mouse.

[0178] Those skilled in the art will understand that Figure 12 The structure shown is merely a block diagram of a portion of the structure related to the present application and does not constitute a limitation on the computer device to which the present application is applied. Specific computer devices may include more or fewer components than those shown in the figure, or combine certain components, or have different component arrangements.

[0179] In one embodiment, a computer device is also provided, including a memory and a processor, wherein the memory stores a computer program, and the processor executes the computer program to implement the steps in the above method embodiments.

[0180] The implementation principles and technical effects of each step in this embodiment are similar to those of the phase composition determination method described above, and will not be repeated here.

[0181] In one embodiment, a computer-readable storage medium is provided having a computer program stored thereon that, when executed by a processor, implements the steps in the above method embodiments.

[0182] The implementation principles and technical effects of each step in this embodiment when the computer program is executed by the processor are similar to those of the phase composition determination method described above, and will not be repeated here.

[0183] In one embodiment, a computer program product is provided, including a computer program that, when executed by a processor, implements the steps in the above method embodiments.

[0184] The implementation principles and technical effects of each step in this embodiment when the computer program is executed by the processor are similar to those of the phase composition determination method described above, and will not be repeated here.

[0185] It should be noted that the user information (including but not limited to user device information, user personal information, etc.) and data (including but not limited to data used for analysis, data stored, data displayed, etc.) involved in this application are all information and data authorized by the user or fully authorized by all parties.

[0186] Those skilled in the art will understand that all or part of the processes in the methods of the above embodiments can be implemented by a computer program instructing related hardware. The computer program can be stored in a non-volatile computer-readable storage medium, and when executed, it can include the processes of the embodiments of the above methods. Any references to memory, databases, or other media used in the embodiments provided in this application can include at least one of non-volatile and volatile memory. Non-volatile memory can include read-only memory (ROM), magnetic tape, floppy disk, flash memory, optical memory, high-density embedded non-volatile memory, resistive random access memory (ReRAM), magnetic random access memory (MRAM), ferroelectric random access memory (FRAM), phase change memory (PCM), graphene memory, etc. Volatile memory can include random access memory (RAM) or external cache memory, etc. By way of illustration and not limitation, RAM can take many forms, such as Static Random Access Memory (SRAM) or Dynamic Random Access Memory (DRAM). The databases involved in the embodiments provided in this application may include at least one type of relational database and non-relational database. Non-relational databases may include, but are not limited to, blockchain-based distributed databases. The processors involved in the embodiments provided in this application may be general-purpose processors, central processing units, graphics processing units, digital signal processors, programmable logic devices, quantum computing-based data processing logic devices, etc., and are not limited to these.

[0187] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0188] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of this patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this application should be determined by the appended claims.

Claims

1. A phase component measurement method characterized by comprising: The method comprises: obtaining the lattice constant corresponding to each phase component in the to-be-detected powder and the phase content; the to-be-detected powder is an infinite solid solution; for any phase component, obtaining the adjacent lattice constant of the lattice constant of the phase component from the corresponding relationship; According to the adjacent lattice constant, the atomic proportion of the first element corresponding to the adjacent lattice constant, and the lattice constant of the phase component, the atomic proportion of the first element in the phase component is determined; wherein the atomic proportion x of the first element in the phase component is determined according to Determination; , respectively represent the adjacent lattice constant, , respectively represent the atomic proportion of the first element corresponding to the adjacent lattice constant, and z represents the lattice constant of the phase component. determining the atomic proportion of each element in the phase component according to the atomic proportion of the first element in the phase component; obtaining the mass proportion of each element in the to-be-detected powder according to the atomic proportion of each element in each phase component and the phase content of each phase component.

2. The method of claim 1, wherein, Before the obtaining the lattice constant corresponding to each phase component in the to-be-detected powder and the phase content, the method further comprises: detecting the content of a specified element in the to-be-detected powder; the specified element represents an element that has an impact on the lattice constant of each phase component in the to-be-detected powder; if the content of the specified element is less than a preset threshold, obtaining the lattice constant corresponding to each phase component in the to-be-detected powder and the phase content.

3. The method according to claim 1 or 2, characterized in that, The to-be-detected powder is Ti(C, N) powder.

4. The method according to claim 1 or 2, characterized in that, The obtaining the lattice constant corresponding to each phase component in the to-be-detected powder and the phase content comprises: obtaining a diffraction spectrum scanned by the to-be-detected powder under a preset condition; performing full-spectrum fitting analysis on the diffraction spectrum to obtain a fitting result; based on the fitting result, obtaining the lattice constant of each phase component in the to-be-detected powder and the phase content.

5. The method according to claim 1 or 2, characterized in that, The method further comprises: obtaining the corresponding relationship between the atomic proportion of the first element and the lattice constant from a standard database.

6. The method of claim 1 or 2, wherein, The method further comprises: obtaining the corresponding relationship between the atomic proportion of the first element and the lattice constant through experiments.

7. A phase component measuring device characterized by comprising: The device comprises: a first obtaining module, configured to obtain the lattice constant corresponding to each phase component in the to-be-detected powder and the phase content; the to-be-detected powder is an infinite solid solution; The second acquisition module is configured to, for any phase component, acquire a neighboring lattice constant of the lattice constant of the phase component from the correspondence relationship; and determine the atomic percentage of the first element in the phase component according to the neighboring lattice constant, the atomic percentage of the first element corresponding to the neighboring lattice constant, and the lattice constant of the phase component; wherein the atomic percentage x of the first element in the phase component is determined according to determining; 、 respectively represent the neighboring lattice constant, 、 respectively represent the atomic percentage of the first element corresponding to the neighboring lattice constant, and z represents the lattice constant of the phase component; and the atomic percentage of each element in the phase component is determined according to the atomic percentage of the first element in the phase component. a determining module, configured to obtain the mass proportion of each element in the to-be-detected powder according to the atomic proportion of each element in each phase component and the phase content of each phase component. 8.A computer device, comprising a memory and a processor, wherein the memory stores a computer program, and the computer device is configured to perform the method according to any one of claims 1-7. The processor executes the computer program to realize the steps of the method in any one of claims 1 to 6.

9. A computer readable storage medium having stored thereon a computer program, characterized in that, The computer program is executed by the processor to realize the steps of the method in any one of claims 1 to 6.

10. A computer program product comprising a computer program, characterized in that, The computer program is executed by the processor to realize the steps of the method in any one of claims 1 to 6.

Images