CN1607175A - Method for preparing vanadium carbide powder - Google Patents
Method for preparing vanadium carbide powder Download PDFInfo
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- CN1607175A CN1607175A CN 200310101104 CN200310101104A CN1607175A CN 1607175 A CN1607175 A CN 1607175A CN 200310101104 CN200310101104 CN 200310101104 CN 200310101104 A CN200310101104 A CN 200310101104A CN 1607175 A CN1607175 A CN 1607175A
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Abstract
A method for preparing powdered vanadium carbide contains following steps: V#-[2]O#-[5] is dissolved in organic acid solution heated and stirred to obtain clarified and transparent solution of 10-40 % concentration at 60-80 degree centigrade, calcinated under protective atmosphere at 850-1000 degree centigrade and carbonized for 40-90 minute to obtain ultrafine powdered vanadium carbide having 0.1 micrometer average size and 20-60 nanometer grain size. The total carbon content of prepared powdered vanadium carbide is 17.75 % , free carbon is reduced to 0.61 % to satisfy the demand in carbide alloy and special steel production. Said invention also extends the use range of VC and provides ultrafine powdered vanadium carbide for other material production industry.
Description
Technical field:
The invention belongs to the manufacturing of field of powder metallurgy metal-powder, especially the preparation method of vanadium carbide powder.
Background technology:
Vanadium carbide is as the ultra-fine cemented carbide grain inhibitor, steel additive agent, high-temperature coatings and be widely used in industry as carbon source diamond synthesis etc.Produce at present the employed method of vanadium carbide two classes are arranged: the one, adopt V
2O
5With carbon black mixing high temperature reduction carbonizatin method, the 2nd, the conventional ceramic technique of vapour phase reduction/vanadium carbide.The prepared vanadium carbide powder granularity of two kinds of methods is generally all in 2.0～3.8 micrometer ranges, and powder Free Carbon content height.And what need in the industrial application is that fine size, phase composition are formed single vanadium carbide powder, when for example preparing ultra-fine cemented carbide, the WC powder granularity is about 0.2～0.4 micron, if adopting powder size is that 2～4 microns vanadium carbides are as grain inhibitor, then can be little owing to the thick VC specific surface area of particle, surface active can be low, atomic migration speed is slow, and the effect that suppresses the grain growth of WC is difficult to give full play to, and the performance of ultra-fine cemented carbide just is difficult to a progressive raising.Therefore, when high-performance ultra-fine cemented carbide and special steel are produced, press for ultra-fine vanadium carbide powder.
Summary of the invention:
The object of the invention is to provide a kind of preparation method of vanadium carbide powder, satisfies the demand of high-performance ultra-fine cemented carbide and special steel material production with the vanadium carbide powder of producing fine size.
Technical scheme of the present invention is: at first with V
2O
5Be dissolved in the organic acid soln, heat while stirring, obtain the solution of clear in the time of 60～80 ℃, solution concentration is 10%～40%; Again solution is carried out spray-drying in centrifugal spray dryer, obtain containing the complex compound of vanadium and the mixed-powder of free matter, powder shape is porous, loose hollow ball; Then with this powder in protective atmosphere, 500～600 ℃ are carried out roasting, obtain V
2O
3With the free mixed uniformly powder of C of atomic level; Again under 850～1000 ℃, H
2Or H
2/ CH
4Middle carbonization 40～90 minutes, making powder mean particle sizes is 0.1 micron, crystallite dimension is the ultra-fine vanadium carbide powder of 20～60 nanometers.
Also can be with the direct carbonization in protective atmosphere or in the vacuum of the powder after the spray-drying.
Advantage of the present invention is compared with the existing method for preparing vanadium carbide powder with positively effect, fully shows; Reduce carbonization temperature, saved the energy; Reduced free carbon content in the powder, the vanadium carbide powder total carbon content is 17.75%, and uncombined carbon is 0.61%.Powder mean particle sizes is 0.1 micron, and grain-size is 20～60 nanometers; Further enlarged the purposes of VC, can be the other materials production provides fine ultra-fine vanadium carbide powder, has especially satisfied the demand that Wimet and special steel material are produced.
Embodiment:
Example 1:
At first in 100ml distilled water, add 3.64 gram V in the dissolving 12.4 gram organic acid solution
2O
5, heat while stirring, obtain the blue look solution of clear in the time of 60～80 ℃, solution concentration is 13～15%; Again solution is carried out spray-drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, air outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min, obtain containing the amorphous powder of vanudium complex and free organic acids, be shaped as porosity and looseness spheroidal; At last powder is carried out roasting in 500～600 ℃ protective atmosphere argon gas, vanudium complex and free organic acids decompose, and obtain V
2O
3The powder that mixes with free C atomic level; Then again under 850～1000 ℃, H
2Or H
2/ CH
4To obtain size distribution in 40～90 minutes narrow in reduction/carbonization in the atmosphere, and particle mean size is 0.1 micron ultra-fine VC powder.
Example 2:
At first in the 100ml deionized water, be dissolved with and add 4.2 gram V in the organic solution of 10.5 grams
2O
5, heat while stirring, obtain the blue look solution of clear in the time of 60～80 ℃, solution concentration is 13～15%; Again solution is carried out spray-drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min, obtain containing the amorphous powder of vanudium complex and free matter, powder shape is porosity and looseness spheroidal.Powder is carried out roasting in 500 ℃～600 ℃, vacuum, vanudium complex and free matter decompose, and obtain V
2O
3With the powder that free C atomic level mixes, under 850 ℃～1000 ℃, reduction/carbonization is 40～90 minutes in the vacuum at last, and it is narrow to make size distribution, and particle mean size is 0.1 micron ultra-fine VC powder.
Claims (3)
1. the preparation method of a vanadium carbide powder is characterized in that: at first with V
2O
5Be dissolved in the organic acid soln, heat while stirring, obtain the solution of clear in the time of 60～80 ℃, solution concentration is 10%～40%; Again solution is carried out spray-drying in centrifugal spray dryer, obtain containing the complex compound of vanadium and the mixed-powder of free matter, powder shape is porous, loose hollow ball; Then with this powder in protective atmosphere, 500～600 ℃ are carried out roasting, obtain V
2O
3With the free mixed uniformly powder of C of atomic level; Again under 850～1000 ℃, H
2Or H
2/ CH
4It is 0.1 micron that middle carbonization made powder mean particle sizes in 40～90 minutes, and crystallite dimension is the ultra-fine vanadium carbide powder of 20～60 nanometers.
2. the preparation method of 1 described vanadium carbide powder as requested is characterized in that: at first add 3.64 gram V in the dissolving 12.4 gram organic acid solution in 100ml distilled water
2O
5, heat while stirring, obtain the blue look solution of clear in the time of 60～80 ℃, solution concentration is 13～15%; Again solution is carried out spray-drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, air outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min, obtain containing the amorphous powder of vanudium complex and free organic acids, be shaped as porosity and looseness spheroidal; Then powder is carried out roasting in 500～600 ℃ protective atmosphere argon gas, vanudium complex and free organic acids decompose, and obtain V
2O
3The powder that mixes with free C atomic level; At last under 850～1000 ℃, H
2Or H
2/ CH
4To obtain size distribution in 40～90 minutes narrow in reduction/carbonization in the atmosphere, and particle mean size is 0.1 micron ultra-fine VC powder.
3. the preparation method of 1 described vanadium carbide powder as requested is characterized in that: at first be dissolved with in the 100ml deionized water and add 4.2 gram V in the organic solution of 10.5 grams
2O
5, heat while stirring, obtain the blue look solution of clear in the time of 60～80 ℃, solution concentration is 13～15%; Again solution is carried out spray-drying in centrifugal spray dryer, intake air temperature: 250 ℃～350 ℃, outlet temperature: 150 ℃, rotating speed 30000rpm, flow 30ml/min, obtain containing the amorphous powder of vanudium complex and free matter, powder shape is porosity and looseness spheroidal.Powder is carried out roasting in 500 ℃～600 ℃, vacuum, vanudium complex and free matter decompose, and obtain V
2O
3The powder that mixes with free C atomic level, at last under 850 ℃～1000 ℃, just can to make size distribution in 40～90 minutes narrow in reduction/carbonization in the vacuum, and particle mean size is 0.1 micron ultra-fine VC powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310101104 CN1269730C (en) | 2003-10-15 | 2003-10-15 | Method for preparing vanadium carbide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310101104 CN1269730C (en) | 2003-10-15 | 2003-10-15 | Method for preparing vanadium carbide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1607175A true CN1607175A (en) | 2005-04-20 |
| CN1269730C CN1269730C (en) | 2006-08-16 |
Family
ID=34756108
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310101104 Expired - Fee Related CN1269730C (en) | 2003-10-15 | 2003-10-15 | Method for preparing vanadium carbide powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225763A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of vanadium carbide powder |
| CN102225762A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of hafnium carbide powder |
| CN102285652A (en) * | 2011-05-25 | 2011-12-21 | 山东理工大学 | Preparation method of niobium carbide powder |
| CN103334042A (en) * | 2013-06-20 | 2013-10-02 | 成都工业学院 | Vanadium carbide based hard alloy |
| CN108866633A (en) * | 2018-07-25 | 2018-11-23 | 四川理工学院 | A kind of nanometer of VC whisker and preparation method thereof |
-
2003
- 2003-10-15 CN CN 200310101104 patent/CN1269730C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225763A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of vanadium carbide powder |
| CN102225762A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of hafnium carbide powder |
| CN102285652A (en) * | 2011-05-25 | 2011-12-21 | 山东理工大学 | Preparation method of niobium carbide powder |
| CN102285652B (en) * | 2011-05-25 | 2013-02-13 | 山东理工大学 | Preparation method of niobium carbide powder |
| CN102225762B (en) * | 2011-05-25 | 2013-02-13 | 山东理工大学 | Preparation method of hafnium carbide powder |
| CN102225763B (en) * | 2011-05-25 | 2013-02-13 | 山东理工大学 | Preparation method of vanadium carbide powder |
| CN103334042A (en) * | 2013-06-20 | 2013-10-02 | 成都工业学院 | Vanadium carbide based hard alloy |
| CN108866633A (en) * | 2018-07-25 | 2018-11-23 | 四川理工学院 | A kind of nanometer of VC whisker and preparation method thereof |
| CN108866633B (en) * | 2018-07-25 | 2020-04-28 | 四川理工学院 | Nano VC crystal whisker and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1269730C (en) | 2006-08-16 |
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| C14 | Grant of patent or utility model | ||
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Hunan Boyun Dongfang Powder Metallurgy Co., Ltd. Assignor: Central South University Contract fulfillment period: 2007.12.28 to 2023.10.14 contract change Contract record no.: 2008430000025 Denomination of invention: Method for preparing vanadium carbide powder Granted publication date: 20060816 License type: Exclusive license Record date: 20081114 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.12.28 TO 2023.10.14; CHANGE OF CONTRACT Name of requester: HUNAN BOYUNDONGFANG POWDER METALLURGY CO., LTD. Effective date: 20081114 |
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Granted publication date: 20060816 Termination date: 20091116 |