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Production method of ultrafine tungsten carbide powder with good dispersity, perfect crystals and high purity

A high-purity, tungsten carbide technology, applied in the direction of tungsten/molybdenum carbides, carbides, etc., can solve the problems of a large number of agglomerates, uneven particle size, incomplete crystallization, etc., to reduce the chance of introducing impurities and low activity. , Crystal complete effect

Inactive Publication Date: 2019-08-16
蓬莱市超硬复合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method of ultrafine tungsten carbide powder commonly used in the market at present will lead to the existence of a large number of agglomerates, incomplete crystallization, poor dispersion, uneven particle size, and high impurity content. The crystal nuclei with abnormal grain growth in the medium cannot be reduced. At the same time, the activity of tungsten carbide powder is increased through pretreatment, which leads to the abnormal growth of grains during the sintering process.
However, other preparation methods have the disadvantages of high cost, complicated process, and difficulty in scale-up.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: A preparation method of ultrafine tungsten carbide powder with good dispersion, complete crystallization and high purity, including the following steps

[0018] Step (1) Using ammonium paratungstate as a raw material, calcining to generate a tungsten oxide precursor. During calcination, the feed rate is 50kg / h, the calcination temperature is 500°C, and the conversion rate of ammonium paratungstate is at least 98.5% when calcining the tungsten oxide precursor. ; The calcination process of ammonium paratungstate more effectively removes some difficult impurities;

[0019] Step (2) The tungsten oxide precursor obtained in step (1) is reduced by hydrogen through an automatic boat four-tube furnace to obtain tungsten powder; the process parameters of hydrogen reduction are: five belt temperatures of 620℃, 680℃, 740 ℃, 800℃, 860℃, hydrogen flow rate is 34m 3 / h, the boat pushing time is 15 minutes / boat, and the loading capacity is 0.7 kg / boat; the automatic boat pushing...

Embodiment 2

[0022] Embodiment 2: A preparation method of ultrafine tungsten carbide powder with good dispersion, complete crystallization and high purity, including the following steps:

[0023] Step (1) Use ammonium paratungstate as a raw material to generate a tungsten oxide precursor through calcination. During calcination, the feed rate is 150kg / h, the calcination temperature is 600°C, and the conversion rate of ammonium paratungstate is at least 98.5% when calcining the tungsten oxide precursor. ; The calcination process of ammonium paratungstate more effectively removes some difficult impurities;

[0024] Step (2) The tungsten oxide precursor obtained in step (1) is reduced by hydrogen through an automatic boat four-tube furnace to obtain tungsten powder; the process parameters of hydrogen reduction are: five belt temperatures of 630℃, 690℃, 750 ℃, 810℃, 870℃, hydrogen flow rate is 38m 3 / h, the pushing time is 18 minutes / boat, and the loading capacity is 0.8 kg / boat;

[0025] Step (3) Th...

Embodiment 3

[0027] Embodiment 3: A preparation method of ultrafine tungsten carbide powder with good dispersion, complete crystallization and high purity, including the following steps:

[0028] Step (1) Use ammonium paratungstate as a raw material to generate a tungsten oxide precursor through calcination. During calcination, the feed rate is 200kg / h and the calcination temperature is 700°C; the conversion rate of ammonium paratungstate is at least 98.5% when calcining the tungsten oxide precursor. ; The calcination process of ammonium paratungstate more effectively removes some difficult impurities;

[0029] Step (2) The tungsten oxide precursor obtained in step (1) is reduced by hydrogen through an automatic boat four-tube furnace to obtain tungsten powder; the process parameters of hydrogen reduction are: five belt temperatures of 640℃, 700℃, 760 ℃, 820℃, 880℃, hydrogen flow rate is 40m 3 / h, the pushing time is 20 minutes / boat, and the loading capacity is 0.9 kg / boat; step (3) the tungste...

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Abstract

The invention discloses a production method of ultrafine tungsten carbide powder with good dispersity, perfect crystals and high purity. The production method of the ultrafine tungsten carbide powderwith the good dispersity, the perfect crystals and the high purity comprises the steps of (1) using ammonium paratungstate as a raw material, and conducting calcination to generate a tungsten oxide precursor; (2) conducting hydrogen reduction on the tungsten oxide precursor obtained in the step (1) through an automatic pusher four-tube furnace to obtain tungsten powder; and (3) conducting carbon addition on the tungsten powder produced in the step (2), using carbon black as a C source, adopting a planetary ball mill for dry-milling, placing a material subjected to ball milling in a tube atmosphere furnace, and conducting carbonation in a hydrogen atmosphere to produce the ultrafine tungsten carbide powder. According to the production method of the ultrafine tungsten carbide powder with thegood dispersity, the perfect crystals and the high purity, the ammonium paratungstate is used as the raw material, by adjusting and controlling a calcination technology, the ultrafine tungsten oxideprecursor is obtained, furthermore, in the reduction process, synchronous crystallization of tungsten crystals is controlled, a fast and complete carbonation process is achieved, meanwhile, impurity elements are monitored, a gas deoxygenation technology is used, the key impurity content and the oxygen content are controlled, and finally, the ultrafine tungsten carbide powder with the good dispersity, the perfect crystals and the high purity is obtained.

Description

Technical field [0001] The invention belongs to the technical field of material preparation, and mainly relates to a preparation method of ultrafine tungsten carbide powder with good dispersion, complete crystallization and high purity. Background technique [0002] At present, due to the excellent mechanical properties of ultrafine cemented carbide, it is widely used in metal processing, electronics industry, medicine and other fields, such as micro-drills, milling cutters, integral hole processing tools, precision molds for printed circuit boards , Difficult to process materials, tools, etc. [0003] The preparation method of ultrafine tungsten carbide powder commonly used in the market will cause a large number of agglomerates, incomplete crystallization, poor dispersion, uneven particle size, and high impurity content. Although a large amount of agglomerates are eliminated by treatment, it will cause a sintering process. The abnormally grown crystal nuclei of the medium grains...

Claims

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Application Information

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IPC IPC(8): C01B32/949
CPCC01B32/949C01P2004/62
Inventor 孙浩斌张华姚海滨司守佶李昌业刘欣付道龙李晓艳常江王焕涛
Owner 蓬莱市超硬复合材料有限公司
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