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A preparation method of a high-hardness value nano-hardness standard substance for calibrating a nano-indenter

A nano-indenter and nano-hardness technology, which is applied in the direction of instruments, scientific instruments, strength characteristics, etc., can solve the problems of inability to coat the bonding phase, inability to have a uniform hardness value, difficulty in controlling the particle size and agglomeration of WC particles, etc.

Active Publication Date: 2019-11-05
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The preparation process of WC often adopts the direct carbonization of W powder and carbon or the improvement of this process, but the reaction speed of this method is slow, it is difficult to obtain WC with theoretical carbon content, and the particle size and agglomeration degree of the obtained WC are difficult. control
In addition, cemented carbide is a two-phase structure material composed of metal carbide particles and a binder phase. In the traditional process, the combination of WC particles and the binder phase is achieved by mechanical mixing and sintering, but it is difficult to control the particles in the binder phase. The uniform dispersion in the medium cannot make the binder phase achieve good coating, and the hardness value cannot be highly uniform at the microscopic level of the nanometer scale.
After a large number of tests and comparisons, it was found that the current WC cemented carbide materials cannot meet the performance requirements for nano-hard standard substances

Method used

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  • A preparation method of a high-hardness value nano-hardness standard substance for calibrating a nano-indenter
  • A preparation method of a high-hardness value nano-hardness standard substance for calibrating a nano-indenter
  • A preparation method of a high-hardness value nano-hardness standard substance for calibrating a nano-indenter

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The first step of high temperature liquid phase reaction: 25kg WO 3 , 500L CH 3 OH, 500LC 2 h 5 Add OH and 16kg Mg into a high-pressure stainless steel reaction kettle with a capacity of 2000L, stir evenly and then seal it (the rotation speed of the stirring blade is 100r / min), set the temperature rise program, the initial temperature is 25°C, it takes 50min to rise to 300°C, and the temperature is constant After 12 hours, after the reaction was completed, it was naturally cooled to room temperature, centrifuged and washed to obtain nano WC particles. Put the obtained particles into 1mol / L diluted HCl solution and soak for 2 hours to dissolve the reducing agent contained in the sample, wash and filter with pure water; then soak in hot concentrated NaOH solution (6mol / L) for 2 hours hours, the MgWO produced by the dissolution reaction 4 With the W salt that may be generated, the filtered product is finally washed with distilled water, soaked in ethanol for 12 hours, ...

Embodiment 2

[0036] The first step of high temperature liquid phase reaction: 45kg WO 3 , 500L CH 3 OH, 1000LC 2 h 5 Add OH and 30kg Mg into a high-pressure stainless steel reactor with a capacity of 2000L, stir evenly and seal it (the rotation speed of the stirring blade is 300rpm), set the temperature rise program, the initial temperature is 25°C, take 50min to rise to 320°C, and keep the temperature for 24h. After the reaction was finished, it was naturally cooled to room temperature, centrifuged and washed to obtain nano WC particles. Put the obtained particles into 1mol / L diluted HCl solution and soak for 2.5 hours to dissolve the reducing agent contained in the sample, wash and filter with pure water; then soak in hot concentrated NaOH solution (6mol / L) for 2 hours hours, the MgWO produced by the dissolution reaction 4 With the W salt that may be generated, the filtered product is finally washed with distilled water, soaked in ethanol for 12 hours, and filtered to obtain a sample...

Embodiment 3

[0042] The first step of high temperature liquid phase reaction: 45kg WO 3 , 500L CH 3 OH, 1000LC 2 h 5 Add OH and 30kg Mg into a high-pressure stainless steel reactor with a capacity of 2000L, stir evenly and seal it (the rotation speed of the stirring blade is 300rpm), set the temperature rise program, the initial temperature is 25°C, take 50min to rise to 320°C, and keep the temperature for 24h. After the reaction was finished, it was naturally cooled to room temperature, centrifuged and washed to obtain nano WC particles. Put the obtained particles into 1mol / L diluted HCl solution and soak for 3 hours to dissolve the reducing agent contained in the sample, wash and filter with pure water; then soak in hot concentrated NaOH solution (6mol / L) for 2 hours , the MgWO produced by the dissolution reaction 4 With the W salt that may be generated, the filtered product is finally washed with distilled water, soaked in ethanol for 12 hours, and 33.45kg of the sample is obtained ...

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Abstract

The invention provides a preparation method of a high-hardness nano-hardness standard substance for calibrating a nano indentation instrument.The preparation method particularly includes: mixing a tungsten source, a carbon source and a reductant for high-temperature liquid-phase reaction to obtain WC nanoparticles; performing in-situ coating of a rare earth oxide grain growth inhibitor through high-temperature liquid-phase reaction; subjecting the WC nanoparticles and spherical nano Co powder to wet ball milling to obtain WC-Co powder; subjecting the WC-Co powder to impurity removing, forming, pressing, degumming, calcining, cutting and polishing to obtain hard alloy standard sample blocks.For micro-nano technology metering standardization, the hard alloy standard substance can meet needs of the nano indentation instruction on instrument calibration and tracing chain building within a high-hardness interval.In addition, the nano tungsten-based hard alloy standard substance can fill a gap of rigid nano-hardness standard substances at home and abroad and meet needs for related detection technology studying, product arbitration and international comparison.

Description

technical field [0001] The present invention relates to the technical field of measurement and test standard quantity transfer, more specifically, the present invention relates to a preparation method of WC-Co alloy used as a nano-hardness standard material with high hardness value. Background technique [0002] Since the advent of nanomaterials, it has penetrated into almost every discipline and every field of engineering technology. Due to the unique properties of nanoparticles, such as quantum size effect, volume effect, surface effect, and quantum tunneling effect, the functionality and applicability of nanomaterials have attracted widespread attention. As we all know, the wear resistance of materials is closely related to the hardness of materials, which is a comprehensive reflection of the mechanical properties of materials. The wear resistance of nanomaterials is better, the performance of abrasive wear resistance and sliding wear has been significantly improved, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22C1/05G01N3/62
CPCC22C1/051G01N3/62
Inventor 王奇王震沈根利
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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