CN102225763A - Preparation method of vanadium carbide powder - Google Patents
Preparation method of vanadium carbide powder Download PDFInfo
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- CN102225763A CN102225763A CN2011101360157A CN201110136015A CN102225763A CN 102225763 A CN102225763 A CN 102225763A CN 2011101360157 A CN2011101360157 A CN 2011101360157A CN 201110136015 A CN201110136015 A CN 201110136015A CN 102225763 A CN102225763 A CN 102225763A
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Abstract
The invention provides a preparation method of vanadium carbide powder, which includes the following steps of preparing, mixing, solidifying, milling, pressing and shaping, sintering, decarburizing and milling and is characterized by mixing phenolic resin and vanadium pentoxide powder with particle size of 0.1-3 mu m to form a mud material, solidifying at the temperature of 40-100 DEG C, milling, pressing into blocks, then sintering at the temperature of 1300-1550 DEG C in an inert atmosphere or a reducing atmosphere for 6-8 hours to obtain vanadium carbide blocks, decarburizing and pulverizing to obtain the vanadium carbide powder. The preparation method provided by the invention has the characteristics of simple process, high purity of vanadium carbide powder and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of vanadium carbide powder, belong to the ceramic powder preparing technical field.
Background technology
At present, the vanadium carbide powder is mainly made by the Vanadium Pentoxide in FLAKES carbothermic method, and its reaction equation is:
V
2O
5+7C＝2VC+5CO↑
Above-mentioned reaction process belongs to the solid-solid reaction type, and reaction process is by the material diffusion control.The shortcoming of this method be Vanadium Pentoxide in FLAKES powder and carbon black or graphite powder mix inhomogeneous and carbon black or graphite powder active lower, make the Vanadium Pentoxide in FLAKES reduction not exclusively, become the impurity of product.In addition, the carbon black or the graphite powder active that remain in the vanadium carbide powder are low, need comparatively high tempss (greater than 600 ℃) just can make C generate carbon monoxide in oxidizing atmosphere during decarburization or carbonic acid gas excludes, the oxygen level in the high more powder of temperature is high more, causes the decline of vanadium carbide powder quality.
Summary of the invention
The objective of the invention is to overcome the defective that exists in the prior art, the reaction synthesis process of the vanadium carbide powder that a kind of cost is low, sintering activity is good is provided.Its technical scheme is:
The preparation method of vanadium carbide powder of the present invention is that the high-activity carbon that adopts resol to form is a carbon source reduction Vanadium Pentoxide in FLAKES powder preparing vanadium carbide powder, may further comprise the steps:
1. feedstock production:
The first step: is that 5: 0.5～1 ratio mixes in mixing pan with the Vanadium Pentoxide in FLAKES powder of 0.1～3 μ m and resol with weight ratio, under 80～100 ℃ temperature, solidify, in powder-making machine, pulverize then and make the raw material powder 1 that median size is 10～20 μ m.
Second step: is that 5: 1～2 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, solidifies under 50～100 ℃ temperature, and pulverizing in powder-making machine then and making median size is 20～50 μ m raw material powder 2.
The 3rd step: is that 5: 2～3 ratio mixes in mixing pan with above-mentioned raw materials powder 2 and resol with weight ratio, solidifies under 40～80 ℃ temperature, and pulverizing in powder-making machine then and making median size is 50～100 μ m raw material powder 3.
2. the vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 0.5～3Mpa, inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 6-8 hour under 1300 ℃～1800 ℃ temperature then.
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned vanadium carbide block, the cooling back is pulverized and is made the vanadium carbide powder.
The preparation method of described vanadium carbide powder, Vanadium Pentoxide in FLAKES powder and resol mixing proceed step by step.
The present invention compared with prior art has the following advantages:
1, the present invention adopts resol that the Vanadium Pentoxide in FLAKES powder is wrapped up and forms isolated micron-sized Vanadium Pentoxide in FLAKES particle, the resol carbonization forms active very high porous high-activity carbon when temperature raises, make that the beginning temperature of Vanadium Pentoxide in FLAKES and carbon reaction is descended significantly, the micro channel of the porous high-activity carbon that obtains can successfully be discharged the carbon monoxide of Vanadium Pentoxide in FLAKES and carbon reaction generation, simultaneously, can suitably reduce the resol consumption or reduce step according to required high-activity carbon amount;
2, the high reactivity porous high-activity carbon that forms after the resol carbonization has wrapped up the Vanadium Pentoxide in FLAKES particle, has suppressed the growth of vanadium carbide crystal grain when reaction forms vanadium carbide, can obtain the vanadium carbide powder of grain-size homogeneous.
3, this technical matters is simple, stable, and production cost is low, and the powder application performance is good.
Embodiment
Embodiment 1
1, feedstock production:
The first step: is that 5: 0.5 ratio mixes in mixing pan with the Vanadium Pentoxide in FLAKES powder of 0.1 μ m and resol with weight ratio, solidifies under 80 ℃ temperature, pulverizes in powder-making machine then and makes the raw material powder 1 that median size is 10 μ m.
Second step: is that 5: 1 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, solidifies under 50 ℃ temperature, and pulverizing in powder-making machine then and making median size is 20 μ m raw material powder 2.
The 3rd step: is that 5: 2 ratio mixes in mixing pan with above-mentioned raw materials powder 2 and resol with weight ratio, solidifies under 40 ℃ temperature, and pulverizing in powder-making machine then and making median size is 50 μ m raw material powder 3.
2, the vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 0.5Mpa, inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 6 hours under 1300 ℃ ℃ temperature then.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6 hours under 350 ℃ temperature of above-mentioned vanadium carbide block, system vanadium carbide powder is pulverized in the cooling back.
It is 99.99% pure that raw materials used purity is.
Embodiment 2
1, feedstock production:
The first step: is that 5: 0.75 ratio mixes in mixing pan with the Vanadium Pentoxide in FLAKES powder of 1.5 μ m and resol with weight ratio, solidifies under 90 ℃ temperature, pulverizes in powder-making machine then and makes the raw material powder 1 that granularity is 15 μ m.
Second step: is that 5: 1.5 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, solidifies under 75 ℃ temperature, and pulverizing in powder-making machine then and making granularity is 35 μ m raw material powder 2.
The 3rd step: is that 5: 2.5 ratio mixes in mixing pan with above-mentioned raw materials powder 2 and resol with weight ratio, solidifies under 60 ℃ temperature, and pulverizing in powder-making machine then and making granularity is 75 μ m raw material powder 3.
2, the vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 1.5Mpa, inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 7 hours under 1550 ℃ ℃ temperature then.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 9 hours under 450 ℃ temperature of above-mentioned vanadium carbide block, the cooling back is pulverized and is made the vanadium carbide powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 3
1, feedstock production:
The first step: is that 5: 1 ratio mixes in mixing pan with the Vanadium Pentoxide in FLAKES powder of 3 μ m and resol with weight ratio, solidifies under 100 ℃ temperature, pulverizes in powder-making machine then and makes the raw material powder 1 that granularity is 20 μ m.
Second step: is that 5: 2 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, solidifies under 100 ℃ temperature, and pulverizing in powder-making machine then and making granularity is 50 μ m raw material powder 2.
The 3rd step: is that 5: 3 ratio mixes in mixing pan with above-mentioned raw materials powder 2 and resol with weight ratio, solidifies under 80 ℃ temperature, and pulverizing in powder-making machine then and making granularity is 100 μ m raw material powder 3.
2, the vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 3Mpa, inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 8 hours under 1800 ℃ ℃ temperature then.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 12 hours under 550 ℃ temperature of above-mentioned vanadium carbide block, the cooling back is pulverized and is made the vanadium carbide powder.
It is 99.99% pure that raw materials used purity is.
Claims (1)
1. the preparation method of a vanadium carbide powder is characterized in that: the high-activity carbon that adopts the resol carbonization to form is a carbon source reduction Vanadium Pentoxide in FLAKES powder preparing vanadium carbide powder, may further comprise the steps:
1. feedstock production:
The first step: is that 5: 0.5～1 ratio mixes in mixing pan with the Vanadium Pentoxide in FLAKES powder of 0.1～3 μ m and resol with weight ratio, under 80～100 ℃ temperature, solidify, in powder-making machine, pulverize then and make the raw material powder 1 that median size is 10～20 μ m.
Second step: is that 5: 1～2 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, solidifies under 50～100 ℃ temperature, and pulverizing in powder-making machine then and making median size is 20～50 μ m raw material powder 2.
The 3rd step: is that 5: 2～3 ratio mixes in mixing pan with above-mentioned raw materials powder 2 and resol with weight ratio, solidifies under 40～80 ℃ temperature, and pulverizing in powder-making machine then and making median size is 50～100 μ m raw material powder 3.
2. the vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 0.5～3Mpa, inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 6-8 hour under 1300 ℃-1550 ℃ temperature then.
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned vanadium carbide block, the cooling back is pulverized and is made the vanadium carbide powder.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110136015 CN102225763B (en) | 2011-05-25 | 2011-05-25 | Preparation method of vanadium carbide powder |
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| CN 201110136015 CN102225763B (en) | 2011-05-25 | 2011-05-25 | Preparation method of vanadium carbide powder |
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| CN102225763A true CN102225763A (en) | 2011-10-26 |
| CN102225763B CN102225763B (en) | 2013-02-13 |
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| CN 201110136015 Expired - Fee Related CN102225763B (en) | 2011-05-25 | 2011-05-25 | Preparation method of vanadium carbide powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449435A (en) * | 2013-08-27 | 2013-12-18 | 哈尔滨工业大学 | Method for producing micro-nanoscale carbide ceramics by carbon coating |
| CN114686970A (en) * | 2022-04-13 | 2022-07-01 | 合肥世纪金光半导体有限公司 | Dopant and preparation method thereof and crystal-form-controllable semi-insulating silicon carbide crystal growth method |
| CN117247014A (en) * | 2023-09-08 | 2023-12-19 | 株洲鸿达实业有限公司 | Vanadium carbide powder and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176313A (en) * | 1996-09-06 | 1998-03-18 | 汪兆泉 | Production process of vanadium carbide |
| CN1607175A (en) * | 2003-10-15 | 2005-04-20 | 中南大学 | Preparation method of vanadium carbide powder |
| CN1884063A (en) * | 2006-07-06 | 2006-12-27 | 四川大学 | Process for preparing nano vanadium carbide powder |
-
2011
- 2011-05-25 CN CN 201110136015 patent/CN102225763B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176313A (en) * | 1996-09-06 | 1998-03-18 | 汪兆泉 | Production process of vanadium carbide |
| CN1607175A (en) * | 2003-10-15 | 2005-04-20 | 中南大学 | Preparation method of vanadium carbide powder |
| CN1884063A (en) * | 2006-07-06 | 2006-12-27 | 四川大学 | Process for preparing nano vanadium carbide powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449435A (en) * | 2013-08-27 | 2013-12-18 | 哈尔滨工业大学 | Method for producing micro-nanoscale carbide ceramics by carbon coating |
| CN114686970A (en) * | 2022-04-13 | 2022-07-01 | 合肥世纪金光半导体有限公司 | Dopant and preparation method thereof and crystal-form-controllable semi-insulating silicon carbide crystal growth method |
| CN114686970B (en) * | 2022-04-13 | 2024-01-09 | 合肥世纪金光半导体有限公司 | Dopant, preparation method thereof and crystal form controllable semi-insulating silicon carbide crystal growth method |
| CN117247014A (en) * | 2023-09-08 | 2023-12-19 | 株洲鸿达实业有限公司 | Vanadium carbide powder and preparation method thereof |
| CN117247014B (en) * | 2023-09-08 | 2024-08-13 | 株洲鸿达实业有限公司 | Vanadium carbide powder and preparation method thereof |
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| CN102225763B (en) | 2013-02-13 |
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