Sample preparation method suitable for hard alloy cobalt phase structure X-ray diffraction method test

A cemented carbide and X-ray technology, which is applied in the field of cemented carbide material detection, can solve the problems affecting the measurement accuracy and achieve the effect of quantitative testing, eliminating the need for instrument condition selection tests, and simple configuration

Pending Publication Date: 2022-08-09
ZIGONG CEMENTED CARBIDE CORP
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Problems solved by technology

[0006] Aiming at problems such as the electropolishing process that exists in the existing cobalt phase structure determination technology that changes the cobalt phase structure on the alloy surface and thus affects the measurement accuracy, the purpose of the present invention is to provide an X-ray diffraction method suitable for testing the cobalt phase structure of cemented carbide. The sample preparation method does not use electrolytic polishing or electrolytic extraction equipment, directly uses chemical reagent solution to etch away the WC grains on the surface of WC-Co cemented carbide samples, and then uses X-ray diffraction method to quantify the cobalt phase structure Test, so as to eliminate the interference of WC phase diffraction peaks, the method is simple, suitable for research and development and production analysis sample preparation

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  • Sample preparation method suitable for hard alloy cobalt phase structure X-ray diffraction method test
  • Sample preparation method suitable for hard alloy cobalt phase structure X-ray diffraction method test
  • Sample preparation method suitable for hard alloy cobalt phase structure X-ray diffraction method test

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Embodiment 1

[0030] In this embodiment, the cobalt phase structure analysis is performed on the large product cemented carbide, so the large product cemented carbide needs to be cut first. The sample preparation method suitable for the X-ray diffraction test of the cobalt phase structure of the cemented carbide provided in this embodiment includes the following steps:

[0031]S1. Cutting: Use a diamond cutting machine or wire cutting to cut the cemented carbide samples of large products to obtain cemented carbide samples. The size of the prepared samples is 20mm × 20mm × 10mm.

[0032] S2. Select the test surface: use any plane of the cemented carbide sample as the test surface;

[0033] S3. Corrosion

[0034] S31. Preparation of corrosion solution

[0035] (1) preparation of potassium ferricyanide solution: take by weighing 200g potassium ferricyanide and dissolve it in 1000mL distilled water, mix well, and load it into a 1000mL brown reagent bottle for subsequent use;

[0036] (2) Pre...

Embodiment 2

[0042] In this embodiment, the cobalt phase structure analysis is performed on the large product cemented carbide, so the large product cemented carbide needs to be cut first. The sample preparation method suitable for the X-ray diffraction test of the cobalt phase structure of the cemented carbide provided in this embodiment includes the following steps:

[0043] S1. Cutting: Use a diamond cutting machine or wire cutting to cut the cemented carbide samples of large products to obtain cemented carbide samples. The size of the prepared samples is 20mm × 20mm × 10mm.

[0044] S2. Select the test surface: use any plane of the cemented carbide sample as the test surface;

[0045] S3. Corrosion

[0046] S31. Preparation of corrosion solution

[0047] (1) preparation of potassium ferricyanide solution: take by weighing 100g potassium ferricyanide and dissolve it in 1000mL distilled water, mix, and load it into a 1000mL brown reagent bottle for subsequent use;

[0048] (2) Prepara...

Embodiment 3

[0068] In this embodiment, the surface grinding of a surface cobalt-rich alloy product is carried out, and the samples before and after grinding are subjected to X-ray diffraction qualitative scanning and X-ray fluorescence spectrum quantitative test to test the cemented carbide sample test. before and after face grinding.

[0069] Qualitative scanning of X-ray diffraction shows that the cobalt phase structure of the alloy surface before grinding contains two phases of α-Co and β-Co, and the surface of the alloy after grinding has only α-Co single phase, and the cobalt phase structure changes from two phases to single phase Mutually.

[0070] The test results of X-ray fluorescence spectroscopy are shown in Table 1.

[0071] Table 1 X-ray fluorescence spectrum test results

[0072]

[0073] It can be seen from Table 1 that the content of cobalt on the surface of the alloy product rich in cobalt is significantly reduced after grinding, which affects the accurate qualitative...

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Abstract

The invention discloses a sample preparation method suitable for X-ray diffraction method test of a hard alloy cobalt phase structure, which comprises the following steps: by taking any plane of a hard alloy sample as a test surface, placing the sample in a container filled with an etchant solution with the test surface upward; the etchant solution is an isovolumetric mixed solution of a potassium ferricyanide solution and a sodium hydroxide solution with the mass concentration of 10%-20%, the etchant solution submerges the test surface of the sample, the corrosion time is not shorter than 16 h, and after corrosion is finished, the sample is taken out, cleaned and wiped dry to be measured. According to the sample preparation method, electrolytic polishing or electrolytic extraction equipment is not used, WC grains on the surface layer of the WC-Co hard alloy sample are directly corroded and removed by adopting a chemical reagent solution, so that the interference of a WC phase diffraction peak is eliminated, and the method is simple and convenient and is suitable for research, development, production, analysis and sample preparation.

Description

technical field [0001] The invention belongs to the technical field of cemented carbide material detection, in particular to a sample preparation method suitable for the X-ray diffraction test of the cobalt phase structure of cemented carbide. Background technique [0002] Cemented carbide is an alloy material made of refractory metal compound and bonding metal through powder metallurgy process. It has high hardness, strength, wear resistance and corrosion resistance and other excellent properties. It is widely used in military industry, machinery Processing, metallurgy, oil drilling, mining tools, mold processing and other fields. Cobalt metal is a commonly used binder for cemented carbide, and there are two common crystal structures: hexagonal close-packed (hcp) α-Co and face-centered cubic (fcc) β-Co. The cobalt phase structure has an impact on the strength and toughness of cemented carbide. Since α-Co has 12 slip systems and β-Co has only 4 slip systems, it shows that α...

Claims

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Application Information

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IPC IPC(8): G01N23/20008G01N1/28G01N1/32
CPCG01N23/20008G01N1/286G01N1/32G01N2001/2873Y02E30/30
Inventor 菅豫梅王培李军项培云廖军颜娟
Owner ZIGONG CEMENTED CARBIDE CORP
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