CN102225763B - Preparation method of vanadium carbide powder - Google Patents
Preparation method of vanadium carbide powder Download PDFInfo
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- CN102225763B CN102225763B CN 201110136015 CN201110136015A CN102225763B CN 102225763 B CN102225763 B CN 102225763B CN 201110136015 CN201110136015 CN 201110136015 CN 201110136015 A CN201110136015 A CN 201110136015A CN 102225763 B CN102225763 B CN 102225763B
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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, 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 composite powder mix inhomogeneous and carbon black or graphite composite powder activity lower, make the Vanadium Pentoxide in FLAKES reduction not exclusively, become the impurity of product.In addition, the carbon black or the graphite composite powder activity 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 higher powder of temperature is higher, causes the vanadium carbide powder Quality Down.
Summary of the invention
The object 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 that carbon source reduction Vanadium Pentoxide in FLAKES powder prepares vanadium carbide powder, may further comprise the steps:
1. raw material preparation:
The first step: the Vanadium Pentoxide in FLAKES powder of 0.1～3 μ m and resol are mixed in mixing pan take the ratio of weight ratio as 5: 0.5～1, under 80～100 ℃ temperature, solidify, then in powder-making machine, pulverize and make the raw material powder 1 that median size is 10～20 μ m;
Second step: above-mentioned raw materials powder 1 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 1～2, solidify under 50～100 ℃ temperature, then pulverizing in powder-making machine and making median size is 20～50 μ m raw material powder 2;
The 3rd step: above-mentioned raw materials powder 2 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 2～3, solidify under 40～80 ℃ temperature, then pulverizing in powder-making machine and making median size is 50～100 μ m raw material powder 3.
2. vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 0.5～3MPa., then inertia or reducing atmosphere are fired and were made the vanadium carbide block in 6-8 hour under 1300 ℃～1800 ℃ temperature.
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～～12 hours under 350～550 ℃ temperature of above-mentioned vanadium carbide block, pulverize after the cooling and make 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, phenolic resin carbonized forms the very much higher hole of activity high-activity carbon when temperature raises, so that the beginning temperature of Vanadium Pentoxide in FLAKES and carbon reaction is significantly descended, 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 behind the phenolic resin carbonized 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, raw material preparation:
The first step: Vanadium Pentoxide in FLAKES powder and the resol of 0.1 μ m are mixed in mixing pan take the ratio of weight ratio as 5: 0.5, under 80 ℃ temperature, solidify, then in powder-making machine, pulverize and make the raw material powder 1 that median size is 10 μ m.
Second step: above-mentioned raw materials powder 1 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 1, solidify under 50 ℃ temperature, then pulverizing in powder-making machine and making median size is 20 μ m raw material powder 2.
The 3rd step: above-mentioned raw materials powder 2 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 2, solidify under 40 ℃ temperature, then pulverizing in powder-making machine and making median size is 50 μ m raw material powder 3.
2, vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 0.5Mpa, then inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 6 hours under 1300 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6 hours under 350 ℃ temperature of above-mentioned vanadium carbide block, pulverize vanadium carbide powder processed after the cooling.
It is 99.99% pure that raw materials used purity is.
Embodiment 2
1, raw material preparation:
The first step: Vanadium Pentoxide in FLAKES powder and the resol of 1.5 μ m are mixed in mixing pan take the ratio of weight ratio as 5: 0.75, under 90 ℃ temperature, solidify, then in powder-making machine, pulverize and make the raw material powder 1 that granularity is 15 μ m.
Second step: above-mentioned raw materials powder 1 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 1.5, solidify under 75 ℃ temperature, then pulverizing in powder-making machine and making granularity is 35 μ m raw material powder 2.
The 3rd step: above-mentioned raw materials powder 2 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 2.5, solidify under 60 ℃ temperature, then pulverizing in powder-making machine and making granularity is 75 μ m raw material powder 3.
2, vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 1.5Mpa, then inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 7 hours under 1550 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 9 hours under 450 ℃ temperature of above-mentioned vanadium carbide block, pulverize after the cooling and make vanadium carbide powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 3
1, raw material preparation:
The first step: Vanadium Pentoxide in FLAKES powder and the resol of 3 μ m are mixed in mixing pan take the ratio of weight ratio as 5: 1, under 100 ℃ temperature, solidify, then in powder-making machine, pulverize and make the raw material powder 1 that granularity is 20 μ m.
Second step: above-mentioned raw materials powder 1 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 2, solidify under 100 ℃ temperature, then pulverizing in powder-making machine and making granularity is 50 μ m raw material powder 2.
The 3rd step: above-mentioned raw materials powder 2 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 3, solidify under 80 ℃ temperature, then pulverizing in powder-making machine and making granularity is 100 μ m raw material powder 3.
2, vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 3Mpa, then inertia or reducing atmosphere atmosphere are fired and were made the vanadium carbide block in 8 hours under 1800 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 12 hours under 550 ℃ temperature of above-mentioned vanadium carbide block, pulverize after the cooling and make 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 phenolic resin carbonized to form is that carbon source reduction Vanadium Pentoxide in FLAKES powder prepares vanadium carbide powder, may further comprise the steps:
1. raw material preparation:
The first step: the Vanadium Pentoxide in FLAKES powder of 0.1～3 μ m and resol are mixed in mixing pan take the ratio of weight ratio as 5: 0.5～1, under 80～100 ℃ temperature, solidify, then in powder-making machine, pulverize and make the raw material powder 1 that median size is 10～20 μ m;
Second step: above-mentioned raw materials powder 1 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 1～2, solidify under 50～100 ℃ temperature, then pulverizing in powder-making machine and making median size is 20～50 μ m raw material powder 2;
The 3rd step: above-mentioned raw materials powder 2 and resol are mixed in mixing pan take the ratio of weight ratio as 5: 2～3, solidify under 40～80 ℃ temperature, then pulverizing in powder-making machine and making median size is 50～100 μ m raw material powder 3;
2. vanadium carbide powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 3 at 0.5～3MPa, then inertia or reducing atmosphere are fired and were made the vanadium carbide block in 6-8 hour under 1300 ℃-1550 ℃ temperature;
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned vanadium carbide block, pulverize after the cooling and make 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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| CN 201110136015 CN102225763B (en) | 2011-05-25 | 2011-05-25 | Preparation method of vanadium carbide powder |
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| CN102225763B true CN102225763B (en) | 2013-02-13 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
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 | Method for preparing vanadium carbide powder |
| CN1884063A (en) * | 2006-07-06 | 2006-12-27 | 四川大学 | Process for preparing nano vanadium carbide powder |
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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 | Method for preparing vanadium carbide powder |
| CN1884063A (en) * | 2006-07-06 | 2006-12-27 | 四川大学 | Process for preparing nano vanadium carbide powder |
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