CN1724350A - Process for preparing superfine wolfram carbide powder - Google Patents
Process for preparing superfine wolfram carbide powder Download PDFInfo
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- CN1724350A CN1724350A CNA2004100450654A CN200410045065A CN1724350A CN 1724350 A CN1724350 A CN 1724350A CN A2004100450654 A CNA2004100450654 A CN A2004100450654A CN 200410045065 A CN200410045065 A CN 200410045065A CN 1724350 A CN1724350 A CN 1724350A
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Abstract
A process for preparing superfine tungsten carbide powder includes such steps as dissolving the ammonium meta-tungstate in organic solution, centrifugal spray drying to obtain porous hollow balls, and heating in protecting atmosphere or vacuum while reducing/carbonizing reaction at 1000 deg. C for 1 hr. Its advantages are 0.2 microns in average granularity and low carbonizing temp.
Description
Technical field:
The invention belongs to the preparation technology of field of metallurgy cemented carbide powder, especially the preparation method of superfine tungsten carbide powder.
Background technology:
Wimet has obtained using widely in the national economy every profession and trade, and ultra-fine cemented carbide has better comprehensive use properties, is the main developing direction of CEMENTED CARBIDE PRODUCTION, scientific research therefore.Tungsten-carbide powder prepares the main raw material(s) of hart metal product, and produce ultra-fine cemented carbide and not only need superfine tungsten carbide powder, and to powder quality have higher requirement (granularity issue evenly, crystalline form grow complete etc.).At present, the industry tungsten-carbide powder all adopts the W powder to mix with carbon black after high temperature cabonization forms, because temperature is higher in the carbonization process, the tungsten-carbide powder granularity of preparation is generally greater than 0.8 micron, and preparation during ultra-fine cemented carbide (tungsten carbide crystal grain is less than 0.3 micron) need to adopt the thinner tungsten-carbide powder of granularity.
Summary of the invention:
The object of the invention is to provide the preparation method of preparation ultrafine WC powder, the ultrafine WC powder of production high-performance ultra-fine cemented carbide demand.
Technical scheme of the present invention is: AMT (metatungstic acid amine) is dissolved in the organic solution, and strength of solution is 30%～40%; Solution carries out spraying drying in centrifugal spray dryer, obtain containing the complex compound of tungsten and the mixed powder of free matter, and powder shape is the hollow ball of porosity and looseness.This powder is heated in atmosphere or vacuum, and powder reduces/carburizing reagent, and reduction/carbonization is 1 hour in the time of 1000 ℃, and obtaining powder mean particle sizes is 0.2 micron, and grain-size is the superfine tungsten carbide powder of 60～80 nanometers; Also can be with spray-dired powder at H
2/ CH
4In reduce/carbonization.
The present invention compares with the existing method for preparing tungsten-carbide powder, and its significant advantage and positively effect are: reduce carbonization temperature greatly, shorten technological process and save energy; The carbon content of tungsten-carbide powder can be precisely controlled; Powder size is thin and the granularity issue is narrow, is the good starting material of preparation ultra-fine cemented carbide.
Embodiment:
Example one: at first be dissolved with adding 14 gram AMT in the organic solution of 25.3 grams in the 100ml deionized water, strength of solution is 35～37%; Again solution is carried out spraying drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, air outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min obtains containing the amorphous powder of tungsten complex and free matter, and powder shape is a porosity and looseness spheroidal.Then powder is carried out roasting in 350 ℃～400 ℃ protective atmospheres, tungsten complex and free matter decompose, and obtain WO
3The powder that mixes with free C atomic level, then under 1000 ℃, insulation obtained powder size in 1 hour and distributes narrowly in the vacuum, mean particle size is 0.2 micron a ultrafine WC powder.
Example two: at first be dissolved with adding 16 gram AMT in the organic solution of 25.7 grams in the 100ml deionized water, obtain the blue look solution of clear, strength of solution is 38～40%; Again solution is carried out spraying drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, air outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min obtains containing the amorphous powder of tungsten complex and free matter, and powder shape is a porosity and looseness spheroidal.Then powder is carried out calcination at 500 ℃～600 ℃, tungsten complex and free matter decompose, and obtain WO
3With the powder that free C atomic level mixes, this powder under 850～900 ℃ at H
2/ CH
4It is narrow that middle reduction/carbonization can make size-grade distribution in 40～90 minutes, and mean particle size is 0.2 micron a ultrafine WC powder.
Claims (3)
1. the preparation method of superfine tungsten carbide powder, it is characterized in that: AMT (metatungstic acid amine) is dissolved in the organic solution, and strength of solution is 30%～40%; Solution carries out spraying drying in centrifugal spray dryer, obtain containing the complex compound of tungsten and the mixed powder of free matter, and powder shape is the hollow ball of porosity and looseness.This powder is heated in atmosphere or vacuum, and powder reduces/carburizing reagent, and reduction/carbonization is 1 hour in the time of 1000 ℃, and obtaining powder mean particle sizes is 0.2 micron, and grain-size is the superfine tungsten carbide powder of 60～80 nanometers; Also can be with spray-dired powder at H
2/ CH
4In reduce/carbonization.
2. according to the preparation method of right 1 described superfine tungsten carbide powder, it is characterized in that: at first be dissolved with adding 14 gram AMT in the organic solution of 25.3 grams in the 100ml deionized water, strength of solution is 35～37%; Again solution is carried out spraying drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, air outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min obtains containing the amorphous powder of tungsten complex and free matter, and powder shape is a porosity and looseness spheroidal.Then powder is carried out roasting in 350 ℃～400 ℃ protective atmospheres, tungsten complex and free matter decompose, and obtain WO
3The powder that mixes with free C atomic level, then under 1000 ℃, insulation obtained powder size in 1 hour and distributes narrowly in the vacuum, mean particle size is 0.2 micron a ultrafine WC powder.
3. according to the preparation method of right 1 described superfine tungsten carbide powder, it is characterized in that: at first be dissolved with adding 16 gram AMT in the organic solution of 25.7 grams in the 100ml deionized water, obtain the blue look solution of clear, strength of solution is 38～40%; Again solution is carried out spraying drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, air outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min obtains containing the amorphous powder of tungsten complex and free matter, and powder shape is a porosity and looseness spheroidal.Then powder is carried out calcination at 500 ℃～600 ℃, tungsten complex and free matter decompose, and obtain WO
3With the powder that free C atomic level mixes, this powder under 850900 ℃ at H
2/ CH
4It is narrow that middle reduction/carbonization can make size-grade distribution in 40～90 minutes, and mean particle size is 0.2 micron a ultrafine WC powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100450654A CN1724350A (en) | 2004-07-20 | 2004-07-20 | Process for preparing superfine wolfram carbide powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100450654A CN1724350A (en) | 2004-07-20 | 2004-07-20 | Process for preparing superfine wolfram carbide powder |
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| CN1724350A true CN1724350A (en) | 2006-01-25 |
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| CNA2004100450654A Pending CN1724350A (en) | 2004-07-20 | 2004-07-20 | Process for preparing superfine wolfram carbide powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100486740C (en) * | 2006-08-18 | 2009-05-13 | 谭天翔 | Direct reduction carbonization manufacture method for tungsten carbide or tungsten carbide-cobalt ultrafine particle powder |
| CN101264888B (en) * | 2007-03-15 | 2011-03-16 | 厦门金鹭特种合金有限公司 | Method for preparing nano-stage tungsten carbide powder |
| CN107428618A (en) * | 2015-03-31 | 2017-12-01 | 捷客斯金属株式会社 | The manufacture method of tungsten carbide |
| CN107706429A (en) * | 2017-10-22 | 2018-02-16 | 江西理工大学 | A kind of WC/WO3Core shell structure elctro-catalyst preparation method |
| CN109867286A (en) * | 2019-04-15 | 2019-06-11 | 北京科技大学 | A kind of preparation method of ultrafine tungsten carbide |
| CN112374500A (en) * | 2020-09-29 | 2021-02-19 | 燕山大学 | Preparation method of isometric crystal nano tungsten carbide powder |
-
2004
- 2004-07-20 CN CNA2004100450654A patent/CN1724350A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100486740C (en) * | 2006-08-18 | 2009-05-13 | 谭天翔 | Direct reduction carbonization manufacture method for tungsten carbide or tungsten carbide-cobalt ultrafine particle powder |
| CN101264888B (en) * | 2007-03-15 | 2011-03-16 | 厦门金鹭特种合金有限公司 | Method for preparing nano-stage tungsten carbide powder |
| CN107428618A (en) * | 2015-03-31 | 2017-12-01 | 捷客斯金属株式会社 | The manufacture method of tungsten carbide |
| CN107706429A (en) * | 2017-10-22 | 2018-02-16 | 江西理工大学 | A kind of WC/WO3Core shell structure elctro-catalyst preparation method |
| CN107706429B (en) * | 2017-10-22 | 2020-07-24 | 江西理工大学 | WC/WO3Preparation method of core-shell structure electrocatalyst |
| CN109867286A (en) * | 2019-04-15 | 2019-06-11 | 北京科技大学 | A kind of preparation method of ultrafine tungsten carbide |
| CN112374500A (en) * | 2020-09-29 | 2021-02-19 | 燕山大学 | Preparation method of isometric crystal nano tungsten carbide powder |
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