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Method for preparing WC-Co nano composite powder by in situ reduction and carbonization

A nano-composite and in-situ technology, applied in the field of cemented carbide powder preparation, can solve the problems of difficult control of the process, expensive equipment, long reaction time, etc., and achieve the effects of improving efficiency, reducing energy consumption, and simple process

Inactive Publication Date: 2012-01-11
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The Nanodyne company in the United States used this method to produce WC-Co nanocomposite powder, but there were problems in the production such as expensive equipment, difficult process control, long reaction time, high consumption of high-purity gas and high cost, and was forced to stop production

Method used

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  • Method for preparing WC-Co nano composite powder by in situ reduction and carbonization
  • Method for preparing WC-Co nano composite powder by in situ reduction and carbonization
  • Method for preparing WC-Co nano composite powder by in situ reduction and carbonization

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Experimental program
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Effect test

Embodiment 1

[0041] The first step, according to the WC-15wt%Co measurement ratio, weighed 11.57g (46%) of ammonium tungstate, 7.3g (29%) of cobalt nitrate, and 6.26g (25%) of glucose, respectively dissolved in deionized water, and prepared into a clear mixed solution 75ml;

[0042] In the second step, put the mixed solution obtained in the first step in a PTFE-lined 100ml hydrothermal reaction kettle, seal it, put it in an oven, heat it to 150°C±5°C, keep it warm for 6h, and then cool it with the furnace to room temperature, and then the reactants were filtered, washed, and dried to obtain the precursor powder;

[0043] The third step is to put the precursor powder obtained in the third step into the crucible, heat it in a vacuum tube furnace, and under the condition of vacuum pressure ≤ 80Pa, heat it to 1000°C ± 5°C at a heating rate of 8°C / min, and keep it for 2h , that is, WC-Co nanocomposite powder with an average particle size of about 60nm.

[0044] Its XRD diffraction pattern is ...

Embodiment 2

[0046] In the first step, according to the WC-8wt%Co measurement ratio, weigh 11.85g (55.4%) of ammonium metatungstate, 3.2g (15%) of cobalt chloride, and 6.33g (29.6%) of glucose, and dissolve them in deionized water respectively. Prepare 75ml of clear mixed solution;

[0047] In the second step, put the mixed solution obtained in the first step into a 100ml hydrothermal reaction kettle lined with polytetrafluoroethylene, seal it, put it in an oven, heat it to 150°C±5°C, keep it warm for 10h, and then cool it down to At room temperature, the reactant is filtered, washed, and dried to obtain the precursor powder;

[0048] In the third step, put the precursor powder obtained in the second step into a crucible, heat it in a protective atmosphere furnace, and heat it to 1000°C ± 5°C at a heating rate of 8°C / min under a high-purity argon atmosphere, and keep it warm. After 3 hours, the WC-Co nanocomposite powder is obtained, with an average particle size of about 60nm.

Embodiment 3

[0050] In the first step, according to the WC-12 wt% Co measurement ratio, weigh 11.34g (49.7%) of ammonium metatungstate, 5.84g (25.6%) of cobalt nitrate, and 5.65g (24.7%) of soluble starch (AR). In deionized water, prepare 75ml of clear mixed solution;

[0051] In the second step, put the mixed solution obtained in the first step into a 100ml hydrothermal reaction kettle lined with polytetrafluoroethylene, seal it, put it in an oven, heat it to 150°C±5°C, keep it warm for 4h, and then cool it down to At room temperature, the reactant is filtered, washed, and dried to obtain the precursor powder;

[0052] In the third step, put the precursor powder obtained in the second step into the crucible, heat it in a vacuum tube furnace, and under the condition of vacuum pressure ≤ 80Pa, heat it to 1100°C ± 5°C at a heating rate of 8°C / min, and keep it for 1h , that is, WC-Co nanocomposite powder with an average particle size of about 60nm.

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Abstract

The invention discloses a method for preparing WC-Co nano composite powder by in situ reduction and carbonization, which comprises the following steps: 1, preparing a mixed solution containing W, Co and C or mixed solution containing W, Co, C and inhibitor raw materials or an emulsion; 2, carrying out hydrothermal reaction; arranging the mixed solution obtained in step 1 in a hydrothermal reaction kettle, sealing, heating to 120-200 DEG C, preserving the temperature for 2-15h, cooling to the room temperature, and then filtering, cleaning and drying the reactants to obtain presoma powder; 3, reducing and carbonizing; and 4, directly arranging the presoma powder obtained in step 2 in a vacuum furnace or protective atmosphere furnace, and heating to 800-1100 DEG C to carry out reduction and carbonization reaction with the reaction time of 0.5-6h to obtain WC-Co and WC-Co nano composite powder containing an inhibitor. The raw material used in the method is cheap, the process is simple, the product is pure, particles are fine and uniform, the defects of long cycle, nonuniform mixing and the like of a ball-milling mixed material process can be avoided, the preparation cycle is shortened, the production cost is reduced, and the method has the advantage of industrial application.

Description

technical field [0001] The invention belongs to the preparation technology of cemented carbide powder, and in particular relates to a method for preparing WC-Co nano composite powder by in-situ reduction carbonization. Background technique [0002] As a tool material for modern industrial processing, WC-Co plays an important role in industrial production. It has a wide range of applications in construction machinery, oil drilling, ships, weapons, automobiles, electronics, aerospace, etc. However, the hardness and strength of WC-Co cemented carbide metal brittle materials are a pair of contradictions. Increasing the hardness of the alloy will lead to a decrease in strength, and conversely increasing the strength of the alloy will result in a decrease in hardness. With the further development of industrial technology, more and more fields urgently need "double high" cemented carbide materials with higher strength and hardness. Therefore, how to obtain a "double-high" cemente...

Claims

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Application Information

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IPC IPC(8): B22F9/20C22C1/04C22C29/08
Inventor 林华李庆穆峰邹建
Owner SOUTHWEST UNIVERSITY
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