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Method for preparing superfine tungsten carbide powder through tungsten oxide one-step carbonization

A technology of tungsten carbide powder and carbon monoxide, applied in the field of metallurgy and chemical industry, can solve the problems of shortening the process, difficult to obtain ultra-fine tungsten carbide powder, hard agglomerates, etc., and achieve the effect of short process flow

Active Publication Date: 2021-12-21
GANZHOU NONFERROUS METALLURGICAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, secondary carbonization is still required, and there are disadvantages such as long process, high energy consumption and labor costs
Patent CN108675299A adopts the mixture of 10% CH4 / 90%H2 to directly carbonize blue tungsten into tungsten carbide in one step, which shortens the process and reduces the cost; however, due to carbonization A large amount of water vapor will be produced during the reaction process, which is prone to WC grain growth or hard aggregates, and it is difficult to obtain ultra-fine tungsten carbide powder

Method used

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  • Method for preparing superfine tungsten carbide powder through tungsten oxide one-step carbonization
  • Method for preparing superfine tungsten carbide powder through tungsten oxide one-step carbonization
  • Method for preparing superfine tungsten carbide powder through tungsten oxide one-step carbonization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046](1) Weigh 182g of tungsten trioxide powder (with a particle size of 100-600nm) and 18g of carbon black (with a particle size of 20-100nm) respectively, use alcohol as the medium for wet ball milling, and perform wet ball milling at 180rpm for 10h. Dry at ℃ to obtain a homogeneously mixed powder raw material mixture.

[0047] (2) Put the powder raw material mixture in (1) in the reaction furnace, fill it with nitrogen to evacuate the air, and then pass it into CO. After the CO is stable (the gas flow rate of CO is 500mL / min), the temperature is 5°C / min. The temperature was raised to 1100°C at a rate of 1 min, and the temperature was kept for 3 hours; the feeding of CO was stopped, and nitrogen gas was used instead, and the ultrafine tungsten carbide powder was obtained by natural cooling to room temperature.

[0048] figure 2 It is the particle size distribution diagram of the obtained ultrafine tungsten carbide powder, from figure 2 It can be seen that the particle s...

Embodiment 2

[0052] (1) Weigh 176g of tungsten trioxide powder (with a particle size of 100-600nm) and 24g of carbon black (with a particle size of 20-100nm) respectively, and perform dry ball milling at a speed of 320rpm for 6 hours to obtain a uniformly mixed powder raw material mixture.

[0053] (2) Put the powder raw material mixture in (1) in the reaction furnace, fill it with nitrogen to evacuate the air, and then pass it into CO. The temperature was raised to 1100°C at a rate of 1 min, and the temperature was kept for 3 hours; the CO2 was stopped, and argon gas was used instead, and the ultrafine tungsten carbide powder was obtained by natural cooling to room temperature.

[0054] Figure 4 It is the particle size distribution diagram of the obtained ultrafine tungsten carbide powder, from Figure 4 It can be seen that the particle size of the obtained ultrafine tungsten carbide powder is ≤160nm, and the average particle size is 120±24nm.

[0055] Figure 5 Be the powder X-ray di...

Embodiment 3

[0058] (1) Weigh 188g of tungsten trioxide powder (with a particle size of 100-600nm) and 12g of carbon black (with a particle size of 20-100nm) respectively, and dry ball mill at 180rpm for 4 hours to obtain a uniformly mixed powder raw material mixture.

[0059] (2) Put the powder raw material mixture in (1) in the reaction furnace, fill it with nitrogen to evacuate the air, and then pass it into CO. After the CO is stable (the gas flow rate of CO is 800mL / min), the temperature is 5°C / min. The temperature was raised to 1000°C at a rate of 1 min, and the temperature was kept for 3 hours; the CO2 was stopped, and argon gas was used instead, and the ultrafine tungsten carbide powder was obtained by natural cooling to room temperature.

[0060] Figure 6 It is the particle size distribution diagram of the obtained ultrafine tungsten carbide powder, from Figure 6 It can be seen that the particle size of the obtained ultrafine tungsten carbide powder is ≤170nm, and the average p...

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Abstract

The invention belongs to the technical field of metallurgical chemical industry, and provides a method for preparing superfine tungsten carbide powder through tungsten oxide one-step carbonization. The solid carbon source carbon black and / or graphene can form a large number of crystal nucleuses on the surface of tungsten oxide; and in addition, the carbon black and / or the graphene can reduce the interface energy of the surface of the tungsten oxide powder, so that tungsten carbide particle powder with the particle size being smaller than or equal to 400 nm is formed after tungsten oxide is subjected to carburizing reaction. Meanwhile, the gas carbon source (carbon monoxide) is easy to control and high in migration capability, so that the defect of insufficient migration capability of solid carbon (carbon black and / or graphene) can be overcome. In addition, reaction of carbon dioxide generated in the carburizing reaction process with C and WC can be inhibited, further carbonization of W, W2C and WOx can be achieved, the content of carbon in tungsten carbide can be accurately controlled through one-step carburizing reaction, and therefore stable control over the content of carbon in tungsten carbide is achieved. The method has the advantages that the technological process is short, and the grain size of the obtained superfine tungsten carbide powder is smaller than or equal to 400 nm.

Description

technical field [0001] The invention relates to the technical field of metallurgy and chemical industry, in particular to a method for preparing superfine tungsten carbide powder by one-step carbonization of tungsten oxide. Background technique [0002] Cemented carbide has high hardness, high melting point, high strength and excellent wear resistance and corrosion resistance, and is widely used in key fields such as microelectronics, machining, mineral development, aerospace and defense industries. Tungsten carbide (WC) powder is the main raw material of tungsten carbide cemented carbide, accounting for about 90% of the direct material cost of tungsten carbide cemented carbide. [0003] At present, the main method for industrial preparation of tungsten carbide powder is to first prepare tungsten oxide into ultra-fine tungsten powder by hydrogen reduction reaction, and then carbonize with carbon black at high temperature to obtain ultra-fine tungsten carbide powder. The phas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/949B82Y40/00
CPCC01B32/949B82Y40/00C01P2004/62C01P2004/64
Inventor 郭家旺徐建兵陈冬英文小强陈后兴王明伍莺胡小洣张选旭
Owner GANZHOU NONFERROUS METALLURGICAL RES INST
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