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Process for preparing nanometer WC (wolfram carbide) powder through vacuum aerogel carbonization process

An airgel carbon and process technology, applied in the direction of carbide, nanotechnology, tungsten/molybdenum carbide, etc., can solve the problems that it is difficult to ensure that the particle size of WC powder is less than 100nm, and the detailed quantitative research is not enough, so as to achieve easy continuous The effects of automated control, narrow particle size distribution range, and simple equipment

Inactive Publication Date: 2013-04-24
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when using PF in the above two patents, how many (quantitative) activated carbon elements can be provided by PF under different temperatures and different vacuum degrees, and under what atmosphere conditions and at what temperature the organic phenolic resin is softened and decomposed. , pyrolysis, carbonization, graphitization, and the characteristics and distribution of product carbon particles are not enough.
Therefore it is inevitable that the nano-WC powder contains too much free carbon or W 2 C heterophase, especially the latter patent, without using a high-speed shearing machine, it is difficult to ensure that the particle size of WC powder is less than 100nm (actually 150~280nm) due to the large number of "bridging" aggregates. See patent figure 1

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of 1Kg nanometer WC powder should follow the steps below:

[0037] (1) High speed shear

[0038] will nano(d 50 ≤30nm) grade tungsten powder, 938.8g (nano tungsten powder: absolute ethanol = 1:8 (mass ratio)) to make a mixed solution. Put the mixed liquid into the feed liquid bin of the high-speed shearing machine. According to 60min / kg to determine the shear time is 60min. After shearing, the material is discharged, after precipitation for 4 hours, the upper part of absolute ethanol is removed, and the precipitated tungsten powder slurry is directly transferred to the next process for standby.

[0039] (2) Preparation of phenolic-alcohol solution (A solution)

[0040] Weigh 30g of alcohol-soluble phenolic resin powder, press (phenolic resin (PF): absolute ethanol = 1:5 (mass ratio)). Under the condition of 30~50℃ water bath, keep stirring until dissolved. Make the A solution 150g of 20% (mass) concentration for subsequent use.

[0041] (3) Preparatio...

Embodiment 2

[0050] Preparation of 10Kg nano WC powder should follow the steps below:

[0051] (1) High speed shear

[0052] will nano(d 50 ≤30nm) grade tungsten powder, 9388g (nano tungsten powder: absolute ethanol = 1:8 (mass ratio)) to make a mixed solution. Put the mixed liquid into the feed liquid bin of the high-speed shearing machine. According to 50min / kg to determine the shear time is 500min. After shearing, the material is discharged, after precipitation for 4 hours, the upper part of absolute ethanol is removed, and the precipitated tungsten powder slurry is directly transferred to the next process for standby.

[0053] (2) Preparation of phenolic-alcohol solution (A solution)

[0054] Weigh 300g of alcohol-soluble phenolic resin powder, press (phenolic resin (PF): absolute ethanol = 1:5 (mass ratio)). Under the condition of 30~50℃ water bath, keep stirring until dissolved. Make the A solution 1500g of 20% (mass) concentration for subsequent use.

[0055] (3) Preparation ...

Embodiment 3

[0064] Preparation of 4.5Kg nano WC powder should follow the steps below:

[0065] (1) High speed shear

[0066] will nano(d 50 ≤30nm) grade tungsten powder, 4224.6g is made into a mixed solution according to (nano tungsten powder: absolute ethanol = 1:8 (mass ratio)). Put the mixed liquid into the feed liquid bin of the high-speed shearing machine. According to 45min / kg to determine the shear time is 205min. After shearing, the material is discharged, after precipitation for 4 hours, the upper part of absolute ethanol is removed, and the precipitated tungsten powder slurry is directly transferred to the next process for standby.

[0067] (2) Preparation of phenolic-alcohol solution (A solution)

[0068] Weigh 135g of alcohol-soluble phenolic resin powder, press (phenolic resin (PF): absolute ethanol = 1:5 (mass ratio)). Under the condition of 30~50℃ water bath, keep stirring until dissolved. Make the A solution 675g of 20% (mass) concentration for subsequent use.

[00...

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Abstract

The invention relates to a process for preparing nanometer WC (wolfram carbide) powder through a vacuum aerogel carbonization process, which comprises the following steps of: after nanometer wolfram powder with an average grain size d50 being less than or equal to 30 nm is cut at a high speed through SAXS (small-angle X-ray scattering), agitating and drying with anhydrous alcohol solution of phenolic resin under the ultrasonic dispersion to prepare nanometer-coated wolfram powder with a phenolic resin jacket; carbonizing for 45-60 minutes at a low temperature of 980-1050 DEG C and under the vacuum condition of 1-10 Pa; and preparing the nanometer WC powder with an average grain size d50 being equal to 60.5 nm and a maximum grain size dmax being less than or equal to 100 nm (The BET (Brunaure, Emmet and Teller) specific surface area is more than or equal to 6.4 m<2> / g). In the nanometer WC powder, the content of combined carbon is 6.00-6.10 percent (mass fraction), and the content of free carbon is 0.01-0.50 percent (mass fraction). The process has the beneficial effects that the process achieves the level of completely practical and mass production and has wide promotion significance and practical value. As the process is brief and short and has less investment, the process is also suitable for the investment and the production of middle-sized and small-sized enterprises.

Description

technical field [0001] The invention belongs to the technical field of preparation of tungsten carbide powder for cemented carbide, and in particular provides an industrialized production technology for preparing nanometer WC powder by using a vacuum aerosol carbonization process. Background technique [0002] WC powder is the main raw material of cemented carbide. Cemented carbide has been widely used in almost all sectors of the national economy because of its excellent properties such as high hardness, high red hardness, extremely high compressive strength, high wear resistance and corrosion resistance. my country is a big producer of cemented carbide and has more than 60 years of production experience. my country's tungsten ore resources are very rich, the annual output of cemented carbide has exceeded 7600 tons, and the annual demand for WC powder is about 6000 tons. The progress of material science in recent years has revealed that when the particle size of WC powder...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/34B82Y40/00C01B32/949
Inventor 吴成义郭雷辰辛延君郭志猛季业李艳军马毅龙杨薇薇
Owner UNIV OF SCI & TECH BEIJING
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