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Preparation method of ultra-fine tungsten carbide powder

A powder preparation and tungsten carbide technology, applied in the field of powder metallurgy, can solve the problems of grain growth, loss of the original performance of ultrafine grains, and restricting the high-performance application of cemented carbide materials.

Inactive Publication Date: 2016-05-04
CENT IRON & STEEL RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high-temperature sintering process used in the application of ultra-fine tungsten carbide powder, the grains grow abnormally, making it lose the original properties of ultra-fine grains, which seriously restricts the high-performance application of cemented carbide materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 10g tungsten hexacarbonyl W(CO) 6 and 0.3 g of dicobalt octacarbonyl Co 2 (CO) 8 Dissolve it in ether in a three-neck flask, stir to dissolve it completely, and distill off the ether by vacuum distillation to obtain a solid homogeneous mixture of the two. Then heat the three-neck flask to 90°C, use nitrogen as the carrier gas, and keep the flow rate at 15ml / min, and the vaporized W(CO) 6 The mixture was loaded into the pyrolysis furnace, and at the same time, methane gas preheated to 300°C with a flow rate of 5ml / min was passed into the pyrolysis furnace, and the temperature of the pyrolysis furnace was kept at 300°C for 60 minutes of reaction. Obtain 2.2 g of superfine tungsten carbide powder containing metallic cobalt, the powder particle size D50 is about 200 nm, and the metallic cobalt content is 2.1%. Example 2:

Embodiment 2

[0015] Take 10g tungsten hexacarbonyl W(CO) 6 and 0.5 g of dicobalt octacarbonyl Co 2 (CO) 8 Dissolve it in ether in a three-neck flask, stir to dissolve it completely, and distill off the ether by vacuum distillation to obtain a solid homogeneous mixture of the two. Then heat the three-necked flask to 50°C, use argon as the carrier gas, and keep the flow rate at 5ml / min, and the vaporized W(CO) 6 The mixture was loaded into the pyrolysis furnace, and at the same time, methane gas preheated to 420°C with a flow rate of 10ml / min was passed into the pyrolysis furnace, and the temperature of the pyrolysis furnace was kept at 420°C for 120 minutes of reaction. Obtain 2.4 g of superfine tungsten carbide powder containing metallic cobalt, the powder particle size D50 is about 550 nm, and the metallic cobalt content is 6.0%. Example 3:

Embodiment 3

[0016] Take 10g tungsten hexacarbonyl W(CO) 6 and 0.4 g of dicobalt octacarbonyl Co 2 (CO) 8 Dissolve it in ether in a three-neck flask, stir to dissolve it completely, and distill off the ether by vacuum distillation to obtain a solid homogeneous mixture of the two. Then heat the three-necked flask to 70°C, use argon as the carrier gas, and keep the flow rate at 10ml / min, and the vaporized W(CO) 6 The mixture was loaded into the pyrolysis furnace, and at the same time, methane gas preheated to 380°C with a flow rate of 10ml / min was passed into the pyrolysis furnace, and the temperature of the pyrolysis furnace was kept at 380°C for 90 minutes of reaction. Obtain 2.5 g of superfine tungsten carbide powder containing metallic cobalt, the powder particle size D50 is 80 nm, and the metallic cobalt content is 4.2%.

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Abstract

The invention discloses a preparation method of ultra-fine tungsten carbide powder and belongs to the technical field of powder metallurgy. The preparation method of the ultra-fine tungsten carbide powder comprises the technological steps that 100 mass parts of tungsten hexacarbonyl W(CO)6 and 3-5 mass parts of dicobalt octacarbonyl Co2(CO)8 are dissolved in diethyl ether in a three-opening bottle and stirred to be completely dissolved, and the diethyl ether is evaporated through vacuum distillation, so that a solid uniform mixture of the ungsten hexacarbonyl W(CO)6 and the dicobalt octacarbonyl Co2(CO)8 is obtained; the three-opening bottle is heated to the temperature of 50-90 DEG C, carrier gas is introduced to carry the gasified W(CO)6 mixture into a pyrolyzing furnace, methane gas preheated to the temperature of 300-450 DEG C is introduced into the pyrolyzing furnace at the same time, the temperature of the pyrolyzing furnace is kept being 300-450 DEG C, and the reaction time is 30-120 minutes; and the ultra-fine tungsten carbide powder which contains 1.0%-6.5% of cobalt by mass is finally obtained, and the granularity D50 of the powder is 50-600 nm. By the adoption of the method, the granularity of the tungsten carbide powder can be controlled; in addition, due to the fact that the tungsten carbide powder is doped with certain cobalt, abnormal growth of the tungsten carbide powder during high-temperature sintering can be restrained, and the excellent performance of the tungsten carbide powder is kept.

Description

technical field [0001] The invention belongs to the technical field of powder metallurgy, and in particular relates to a preparation method of ultrafine tungsten carbide powder. The ultrafine tungsten carbide powder containing metal cobalt is prepared through a carbonyl metal vapor deposition process. Background technique [0002] Tungsten carbide (WC) is a compound composed of tungsten and carbon. It is a black hexagonal crystal with metallic luster. It is a good conductor of electricity and heat. It has very high hardness (hardness similar to diamond) and good corrosion resistance. And compressive strength, known as modern industrial teeth, more than 98% of cemented carbide contains WC. In order to further improve the mechanical properties of WC cemented carbide, the best way is to refine its grain size. The finer the grain size of the alloy, the smaller its defects. When the grain size is less than 0.1 μm, there are almost no defects. This kind of cemented carbide not on...

Claims

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Application Information

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IPC IPC(8): B22F9/20
CPCB22F9/20
Inventor 李一张东柳学全袁凤艳李楠孟庆伟李发长
Owner CENT IRON & STEEL RES INST
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