A method of discriminating a tungsten carbide treatment process

Abstract

This invention discloses a method for identifying tungsten carbide processing technology, comprising the following steps: First, the sample is subjected to phase and elemental composition analysis to determine whether the sample is tungsten carbide; second, the surface microstructure and micromorphological characteristics of the sample are analyzed, and the differences in microstructure and micromorphological characteristics are used to identify whether the tungsten carbide sample has undergone sintering treatment, and to identify whether the sample to be tested is spherical cast tungsten carbide or cast tungsten carbide; this invention proposes a rapid micromorphological analysis and identification method to address the differences in micromorphology of tungsten carbide processed by different processes. Due to the different tungsten carbide processing technology, the morphology of tungsten carbide particles varies significantly under the microscopic level. Microscopic analysis is performed using scanning electron microscopy and other methods, and conclusions are quickly drawn by comparing morphological differences.

Description

Technical Field

[0001] This invention belongs to the field of chemical analysis technology, and specifically relates to a method for identifying tungsten carbide processing technology. Background Technology

[0002] Tungsten carbide is an extremely important industrial raw material. Utilizing its ultra-high hardness, wear resistance, and other excellent properties, it is used to manufacture various tools, parts, and wear-resistant products. It is widely used in many fields such as industrial manufacturing, mining, petroleum, and military industry, and is the "teeth" and "armor" of modern industry.

[0003] Current analytical methods for tungsten carbide, including chemical composition analysis, are mainly used to detect whether the content of impurity elements exceeds the standard. These methods include inductively coupled plasma atomic emission spectrometry, X-ray fluorescence spectrometry, and atomic absorption spectrometry. These methods usually include chemical composition analysis to ensure purity, but they cannot identify the processing technology of tungsten carbide.

[0004] Currently, tungsten carbide is generally classified into four types based on different processing techniques: sintered tungsten carbide (hard alloy), unsintered tungsten carbide, spherical cast tungsten carbide, and cast tungsten carbide. There are currently no literature reports on methods for identifying these four types of tungsten carbide. Summary of the Invention

[0005] The purpose of this invention is to provide a method for identifying tungsten carbide processing technology, which can identify four types of tungsten carbide: sintered tungsten carbide, unsintered tungsten carbide, spherical cast tungsten carbide, and cast tungsten carbide.

[0006] The above-mentioned objective of this invention can be achieved through the following technical solution: a method for identifying tungsten carbide processing technology, comprising the following steps:

[0007] (1) Analysis of the main phases and elemental composition of the sample to be tested

[0008] X-ray fluorescence spectrometry was used to analyze the elemental composition of the sample and X-ray diffraction was used to analyze the phase composition of the sample to determine whether it is tungsten carbide.

[0009] (2) Analysis of the microscopic composition and microscopic morphology of the sample surface

[0010] If the result in step (1) is a tungsten carbide sample, then the surface micro-composition and micro-morphology characteristics of the tungsten carbide sample are analyzed by scanning electron microscopy and X-ray energy dispersive spectroscopy. The specific processing technology of the tungsten carbide sample is identified by the differences in surface micro-composition and micro-morphology characteristics. Specifically, the following are included:

[0011] (2.1) Microscopic composition analysis of the surface of the sample to be tested

[0012] Samples were prepared, and the scanning electron microscope (SEM) and its X-ray energy dispersive spectrometer (EDS) parameters were set. Energy dispersive spectrometry analysis was performed on the tungsten carbide sample to determine the surface microstructure of the tungsten carbide sample.

[0013] (2.2) Microscopic morphological characteristics analysis

[0014] Select the accelerating voltage, adjust the secondary electron image to be clear, and observe from low to high magnification to analyze the microscopic morphology of the tungsten carbide sample surface.

[0015] (2.3) Identification results

[0016] If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and in addition to tungsten, one or two metal elements, cobalt and nickel, are detected on the surface of the tungsten carbide microparticles, and the microscopic morphology of polygonal particles with straight edges is visible, then the sample to be tested is sintered tungsten carbide.

[0017] If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and only tungsten is detected on the surface of the tungsten carbide microparticles and regular spherical agglomerate particle morphology is visible at the microscopic level, then the sample to be tested is spherical cast tungsten carbide.

[0018] If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and only tungsten or oxygen is detected on the surface of the tungsten carbide microparticles, and irregular, angular blocky particle morphology is visible at the microscopic level, then the sample to be tested is cast tungsten carbide.

[0019] If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and only tungsten is detected on the surface of the tungsten carbide microparticles with irregular fine particles that have smooth edges, then the sample to be tested is unsintered tungsten carbide.

[0020] In the identification methods of the above-mentioned tungsten carbide processing technology:

[0021] Preferably, in step (1), an X-ray fluorescence spectrometer is used to analyze the elemental composition of the sample to be tested in accordance with GB / T 16597-2019.

[0022] Preferably, in step (1), an X-ray diffractometer is used to perform phase analysis on the sample to be tested in accordance with GB / T 30904-2014.

[0023] Preferably, the scanning electron microscope and its X-ray energy dispersive spectrometer described in step (2) meet the technical requirements of any one of the standards JY / T 0584-2020, GB / T17359-2023, GB / T 20726-2025 and GB / T 25189-2010.

[0024] Preferably, in step (2.1), the sample is prepared and the scanning electron microscope and its X-ray energy dispersive spectrometer parameters are set according to GB / T 17359-2023 or JY / T 0584-2020.

[0025] Preferably, the accelerating voltage in step (2.2) is set to 20-30kV.

[0026] Preferably, in step (2.2), the magnification of sintered tungsten carbide ranges from 900-1100 times to 7000-9000 times, the magnification of cast tungsten carbide and spherical cast tungsten carbide ranges from 400-600 times to 4000-6000 times, and the magnification of unsintered tungsten carbide ranges from 4000-5000 times to 14000-16000 times.

[0027] The present invention has the following advantages:

[0028] (1) This invention proposes a method for identifying tungsten carbide processing technology. Before the use of this method, there was no method for identifying tungsten carbide processing technology in the industry.

[0029] (2) The method of the present invention first uses X-ray diffraction and X-ray fluorescence spectrometry to analyze the phase and elemental composition of the sample to determine whether the sample is tungsten carbide; secondly, scanning electron microscopy and X-ray energy dispersive spectroscopy are used to further analyze the surface micro-composition and micro-morphology of the sample. The micro-composition analysis and the differences in micro-morphology characteristics are used to identify whether the tungsten carbide sample has been sintered, and to identify whether the sample to be tested is spherical cast tungsten carbide or cast tungsten carbide.

[0030] (3) The method of the present invention provides the optimal observation magnification range for four different tungsten carbide products, which can improve the detection efficiency for different tungsten carbide products;

[0031] (4) In general, this invention proposes a rapid analysis and identification of the microstructure of tungsten carbide under different processing techniques. Due to the different tungsten carbide processing techniques, the microstructure of tungsten carbide particles is significantly different. Microscopic analysis is performed using scanning electron microscopy and the morphological differences are compared to draw a conclusion quickly. Attached Figure Description

[0032] Figure 1 This is a computer-generated image of the sample to be tested in Example 1, where Tungsten Carbide is tungsten carbide.

[0033] Figure 2 The images show the scanning electron microscope (SEM) and X-ray energy dispersive spectroscopy (EDS) spectra of the sample to be tested in Example 1. The left image shows the microstructure, with the yellow box indicating the selected X-ray energy dispersive spectroscopy scanning area. The right image shows the elemental energy dispersive spectroscopy (EDS) spectra.

[0034] Figure 3 Here is a scanning electron microscope image of the sample to be tested in Example 1;

[0035] Figure 4 This is a computer-generated image of the sample to be tested in Example 2, where Tungsten Carbide is tungsten carbide.

[0036] Figure 5 The image shows the scanning electron microscope and X-ray energy dispersive spectroscopy (EDS) images of the sample to be tested in Example 2. The left image is a microscopic morphology image, with the yellow box indicating the selected X-ray energy dispersive spectroscopy scanning area. The right image is an elemental energy dispersive spectroscopy (EDS) image.

[0037] Figure 6 The image shows the scanning electron microscope (SEM) microstructure of the sample to be tested in Example 2.

[0038] Figure 7 This is a computer-generated image of the sample to be tested in Example 3, where Tungsten Carbide is tungsten carbide.

[0039] Figure 8 The image shows the scanning electron microscope and X-ray energy dispersive spectroscopy (EDS) images of the sample to be tested in Example 3. The left image is a microscopic morphology image, with the yellow box indicating the selected X-ray energy dispersive spectroscopy scanning area. The right image is an elemental energy dispersive spectroscopy (EDS) image.

[0040] Figure 9 The image shows the scanning electron microscope (SEM) microstructure of the sample to be tested in Example 3.

[0041] Figure 10 This is a computer-generated image of the sample to be tested in Example 4, where Tungsten Carbide is tungsten carbide.

[0042] Figure 11 The image shows the scanning electron microscope and X-ray energy dispersive spectroscopy (EDS) images of the sample to be tested in Example 4. The left image is a microscopic morphology image, with the yellow box indicating the selected X-ray energy dispersive spectroscopy scanning area. The right image is an elemental energy dispersive spectroscopy (EDS) image.

[0043] Figure 12 This is a scanning electron microscope image of the sample to be tested in Example 4. Detailed Implementation

[0044] The present invention will be further described below through specific embodiments, but this is not a limitation of the present invention. Those skilled in the art can make various modifications or improvements based on the basic idea of ​​the present invention, but as long as they do not depart from the basic idea of ​​the present invention, they are all within the scope of the present invention.

[0045] Unless otherwise mentioned, all reagents listed below are commercially available raw materials.

[0046] The following standards include, but are not limited to:

[0047] GB / T 16597-2019 General Rules for X-ray Fluorescence Spectrometry in Metallurgical Products Analysis;

[0048] GB / T 30904-2014 X-ray Diffraction Method for Crystal Structure Analysis of Inorganic Chemical Products;

[0049] GB / T 17359-2023 Microbeam analysis of elements with atomic number not less than 11 by energy dispersive spectroscopy for quantitative analysis;

[0050] JY / T 0584-2020 General Rules for Analytical Methods of Scanning Electron Microscopy;

[0051] GB / T 20726-2025 General Rules for Semiconductor Detectors and X-ray Energy Spectrometers;

[0052] GB / T 25189-2016 Method for setting quantitative analysis parameters for microbeam analysis scanning electron microscopy energy dispersive spectrometer.

[0053] Example 1

[0054] The identification method for tungsten carbide processing technology provided in this embodiment includes the following steps:

[0055] (1) Analysis of the main phases and elemental composition of the sample to be tested

[0056] The elemental composition of the externally submitted cemented carbide cutting tool tip was analyzed using X-ray fluorescence spectrometry according to GB / T 16597-2019. Tungsten elemental analysis was performed using standard-free semi-quantitative analysis software. The phase analysis of the sample was performed using X-ray diffraction according to GB / T 30904-2014 to determine whether it was tungsten carbide. The result was that it was a tungsten carbide sample.

[0057] (2) Analysis of the microscopic composition and microscopic morphology of the sample surface

[0058] The surface microstructure and morphology of tungsten carbide samples were analyzed using scanning electron microscopy and X-ray energy dispersive spectroscopy. The specific processing techniques used to process the samples were identified by analyzing the surface microstructure and morphology differences.

[0059] (2.1) Microscopic composition analysis of the surface of the sample to be tested

[0060] Samples were prepared according to JY / T 0584-2020. The scanning electron microscope and its X-ray energy dispersive spectrometer were set according to JY / T 0584-2020. Energy dispersive spectrometry analysis was performed on the sample to determine the microscopic composition of the sample surface.

[0061] (2.2) Microscopic morphological characteristics analysis

[0062] The accelerating voltage was set to 20kV, and the secondary electron image was adjusted to be clear. The microscopic morphology of the tungsten carbide sample surface was analyzed by observing the sample at magnifications from 1000x to 8000x.

[0063] (2.3) Identification results

[0064] The results are shown in Table 1 and... Figure 1-3 As shown, the main elemental component of the sample is tungsten, and the main phase is tungsten carbide. In addition to tungsten, cobalt metal was also detected on the surface of the tungsten carbide microparticles, and the microscopic morphology of polygonal particles with straight edges was visible. The sample is sintered tungsten carbide.

[0065] Table 1 Elemental analysis data of the samples to be tested

[0066] W 85.184 % Co 9.175 % Cr 3.815 % Ge 0.707 % Re 0.424 %

[0067] Example 2

[0068] The identification method for tungsten carbide processing technology provided in this embodiment includes the following steps:

[0069] (1) Analysis of the main phases and elemental composition of the sample to be tested

[0070] The externally submitted samples were analyzed for elemental composition using X-ray fluorescence spectrometry according to GB / T 16597-2019. Tungsten elemental analysis was performed using standard-free semi-quantitative analysis software. The phase composition of the samples was analyzed using X-ray diffraction according to GB / T30904-2014 to determine whether they were tungsten carbide. The result was that the samples were tungsten carbide.

[0071] (2) Analysis of the microscopic composition and microscopic morphology of the sample surface

[0072] Scanning electron microscopy and X-ray energy dispersive spectroscopy were used to analyze the surface micro-composition and micro-morphology of the samples. The specific processing technology of the samples was identified by analyzing the surface micro-composition and micro-morphology differences.

[0073] (2.1) Microscopic composition analysis of the surface of the sample to be tested

[0074] Samples were prepared according to JY / T 0584-2020. The scanning electron microscope and its X-ray energy dispersive spectrometer were set according to JY / T 0584-2020. Energy dispersive spectrometry analysis was performed on the sample to determine the microscopic composition of the sample surface.

[0075] (2.2) Microscopic morphological characteristics analysis

[0076] Select an accelerating voltage of 20kV, adjust the secondary electron image to be clear, and observe it at magnifications from 500x to 5000x to analyze the microscopic morphology of the sample surface.

[0077] (2.3) Identification results

[0078] The results are shown in Table 2 and... Figure 4-6 As shown, the main elemental component of the sample to be tested is tungsten, and the main phase is tungsten carbide. Only tungsten is detected on the surface of the tungsten carbide microparticles, and regular spherical agglomerate morphology is visible at the microscopic level. Therefore, the sample to be tested is spherical cast tungsten carbide.

[0079] Table 2 Elemental analysis data of the samples to be tested

[0080] W 66.784 % Ni 31.612 % Ge 0.637 % Re 0.378 %

[0081] Example 3

[0082] The identification method for tungsten carbide processing technology provided in this embodiment includes the following steps:

[0083] (1) Analysis of the main phases and elemental composition of the sample to be tested

[0084] The externally submitted samples were analyzed for elemental composition using X-ray fluorescence spectrometry according to GB / T 16597-2019. Tungsten elemental analysis was performed using standard-free semi-quantitative analysis software. The phase analysis of the samples was performed using X-ray diffraction according to GB / T30904-2014 to determine whether they were tungsten carbide. The result was that the samples were tungsten carbide.

[0085] (2) Analysis of the microscopic composition and microscopic morphology of the sample surface

[0086] Scanning electron microscopy and X-ray energy dispersive spectroscopy were used to analyze the surface micro-composition and micro-morphology of the samples. The specific processing technology of the samples was identified by analyzing the surface micro-composition and micro-morphology differences.

[0087] (2.1) Microscopic composition analysis of the surface of the sample to be tested

[0088] Samples were prepared according to JY / T 0584-2020. The scanning electron microscope and its X-ray energy dispersive spectrometer were set according to JY / T 0584-2020. Energy dispersive spectrometry analysis was performed on the sample to determine the microscopic composition of the sample surface.

[0089] (2.2) Microscopic morphological characteristics analysis

[0090] The accelerating voltage was set to 20kV, the secondary electron image was adjusted to be clear, and the microscopic morphology of the tungsten carbide sample surface was analyzed by observing the image at magnifications from 500x to 5000x.

[0091] (2.3) Identification results

[0092] The results are shown in Table 3 and Figure 7-9 As shown, the main elemental component of the sample is tungsten, and the main phase is tungsten carbide. Tungsten and a small amount of oxygen were detected on the surface of the tungsten carbide microparticles. The sample is a cast tungsten carbide.

[0093] Table 3 Elemental analysis data of the samples to be tested

[0094] W 97.919 % Ge 0.853 % Re 0.431 % Ca 0.305 %

[0095] Example 4

[0096] The identification method for tungsten carbide processing technology provided in this embodiment includes the following steps:

[0097] (1) Analysis of the main phases and elemental composition of the sample to be tested

[0098] The externally submitted samples were analyzed for elemental composition using X-ray fluorescence spectrometry according to GB / T 16597-2019. Tungsten elemental analysis was performed using standard-free semi-quantitative analysis software. The phase analysis of the samples was performed using X-ray diffraction according to GB / T30904-2014 to determine whether they were tungsten carbide. The result was that the samples were tungsten carbide.

[0099] (2) Analysis of the microscopic composition and microscopic morphology of the sample surface

[0100] The surface microstructure and morphology of tungsten carbide samples were analyzed using scanning electron microscopy and X-ray energy dispersive spectroscopy. The specific processing techniques used to process the samples were identified by analyzing the surface microstructure and morphology differences.

[0101] (2.1) Microscopic composition analysis of the surface of the sample to be tested

[0102] Samples were prepared according to JY / T 0584-2020. The scanning electron microscope and its X-ray energy dispersive spectrometer were set according to JY / T 0584-2020. Energy dispersive spectrometry analysis was performed on the sample to determine the microscopic composition of the sample surface.

[0103] (2.2) Microscopic morphological characteristics analysis

[0104] Select an accelerating voltage of 20kV, adjust the secondary electron image to be clear, and observe it at magnifications from 5000x to 15000x to analyze the microscopic morphology characteristics of the sample surface.

[0105] (2.3) Identification results

[0106] The results are shown in Table 4 and Figure 10-12 As shown, the main elemental component of the sample to be tested is tungsten, and the main phase is tungsten carbide. Only tungsten is detected on the surface of the tungsten carbide microparticles, and the microscopic morphology of irregular fine particles with smooth edges is visible. The sample to be tested is unsintered tungsten carbide.

[0107] Table 4 Elemental Analysis Data of the Samples to be Tested

[0108] W 98.107 % Ge 0.879 % Re 0.449 % Ca 0.276 %

[0109] The above examples illustrate specific embodiments of the present invention. It is important to note that these specific embodiments are only for further explanation and do not constitute a limitation on the scope of protection of the present invention. Non-essential modifications and adjustments made by others based on the present invention still fall within the scope of protection of the present invention.

Claims

1. A method for identifying tungsten carbide processing technology, characterized in that, Includes the following steps: (1) Analysis of the main phases and elemental composition of the sample to be tested X-ray fluorescence spectrometry was used to analyze the elemental composition of the sample and X-ray diffraction was used to analyze the phase composition of the sample to determine whether it is tungsten carbide. (2) Analysis of the microscopic composition and microscopic morphology of the sample surface If the result in step (1) is a tungsten carbide sample, then the surface micro-composition and micro-morphology characteristics of the tungsten carbide sample are analyzed by scanning electron microscopy and X-ray energy dispersive spectroscopy. The specific processing technology of the tungsten carbide sample is identified by the surface micro-composition analysis and the characteristic differences of the micro-morphology of the tungsten carbide sample to be tested, specifically including: (2.1) Microscopic composition analysis of the surface of the sample to be tested Samples were prepared, and the scanning electron microscope (SEM) and its X-ray energy dispersive spectrometer (EDS) parameters were set. Energy dispersive spectrometry analysis was performed on the tungsten carbide sample to determine the surface microstructure of the tungsten carbide sample. (2.2) Microscopic morphological characteristics analysis Select the accelerating voltage, adjust the secondary electron image to be clear, and observe from low to high magnification to analyze the microscopic morphology of the tungsten carbide sample surface. (2.3) Identification results If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and in addition to tungsten, one or two metal elements, cobalt and nickel, are detected on the surface of the tungsten carbide microparticles, and the microscopic morphology of polygonal particles with straight edges is visible, then the sample to be tested is sintered tungsten carbide. If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and only tungsten is detected on the surface of the tungsten carbide microparticles and regular spherical agglomerate particle morphology is visible at the microscopic level, then the sample to be tested is spherical cast tungsten carbide. If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and only tungsten or oxygen is detected on the surface of the tungsten carbide microparticles, and irregular, angular blocky particle morphology is visible at the microscopic level, then the sample to be tested is cast tungsten carbide. If the main element of the sample to be tested is tungsten, the main phase is tungsten carbide, and only tungsten is detected on the surface of the tungsten carbide microparticles with irregular fine particle morphology that has smooth edge transition, then the sample to be tested is unsintered tungsten carbide.

2. The identification method for the tungsten carbide processing technology according to claim 1, characterized in that, In step (1), X-ray fluorescence spectrometry was used to analyze the elemental composition of the sample to be tested in accordance with GB / T 16597-2019.

3. The identification method for the tungsten carbide processing technology according to claim 1, characterized in that, In step (1), an X-ray diffractometer was used to perform phase analysis on the sample to be tested in accordance with GB / T 30904-2014.

4. The identification method for the tungsten carbide processing technology according to claim 1, characterized in that, The scanning electron microscope and its X-ray energy dispersive spectrometer mentioned in step (2) meet the technical requirements of any one of the standards JY / T 0584-2020, GB / T 17359-2023, GB / T 20726-2025 and GB / T25189-2010.

5. The identification method for tungsten carbide processing according to claim 1, characterized in that, In step (2.1), the sample is prepared and the scanning electron microscope and its X-ray energy dispersive spectrometer parameters are set according to GB / T 17359-2023 or JY / T 0584-2020.

6. The identification method for the tungsten carbide processing technology according to claim 1, characterized in that, In step (2.2), the accelerating voltage is set to 20-30kV.

7. The identification method for tungsten carbide processing according to claim 1, characterized in that, In step (2.2), the magnification of sintered tungsten carbide ranges from 900-1100 times to 7000-9000 times, the magnification of cast tungsten carbide and spherical cast tungsten carbide ranges from 400-600 times to 4000-6000 times, and the magnification of unsintered tungsten carbide ranges from 4000-5000 times to 14000-16000 times.

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