CN102285652B - Preparation method of niobium carbide powder - Google Patents
Preparation method of niobium carbide powder Download PDFInfo
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- CN102285652B CN102285652B CN 201110136013 CN201110136013A CN102285652B CN 102285652 B CN102285652 B CN 102285652B CN 201110136013 CN201110136013 CN 201110136013 CN 201110136013 A CN201110136013 A CN 201110136013A CN 102285652 B CN102285652 B CN 102285652B
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Abstract
The invention provides a preparation method of niobium carbide powder. The method comprises the following steps: dosing, mixing, curing, preparing powder, performing compression moulding, firing, decarbonizing and preparing the final powder. The method is characterized in that phenolic resin is mixed with 0.1-3 mu m of niobium pentoxide powder to form mud, the mud is cured at 40-100 DEG C, powder is prepared, the powder is briquetted, then the product is fired in the inert atmosphere or reducing atmosphere at 1300-1800 DEG C for 6-8 hours to prepare niobium carbide blocks, and the niobium carbide blocks are decarbonized to prepare the niobium carbide powder. The preparation method has the characteristics of simple process, high niobium carbide powder purity and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of niobium carbide powder, belong to the ceramic powder preparing technical field.
Background technology
At present, niobium carbide powder is mainly made by the Niobium Pentxoxide carbothermic method, and its reaction equation is:
Nb
2O
5+7C＝2NbC+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 niobium pentaoxide powder and carbon black or graphite composite powder mix inhomogeneous and carbon black or graphite composite powder activity lower, make the Niobium Pentxoxide reduction not exclusively, become the impurity of product.In addition, the carbon black or the graphite composite powder activity that remain in the niobium 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 niobium 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 niobium carbide powder that a kind of cost is low, sintering activity is good is provided.Its technical scheme is:
The preparation method of niobium carbide powder of the present invention is that the high-activity carbon that adopts resol to form is that carbon source reduction niobium pentaoxide powder prepares niobium carbide powder, may further comprise the steps:
1. raw material preparation:
The first step: the niobium pentaoxide 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. niobium 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 niobium 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 niobium carbide block, pulverize after the cooling and make niobium carbide powder.
The preparation method of described niobium carbide powder, niobium pentaoxide 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 niobium pentaoxide powder is wrapped up and forms isolated micron-sized Niobium Pentxoxide particle, phenolic resin carbonized forms the very much higher hole of activity high-activity carbon when temperature raises, so that the beginning temperature of Niobium Pentxoxide 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 Niobium Pentxoxide 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 Niobium Pentxoxide particle, has suppressed the growth of niobium carbide crystal grain when reaction forms niobium carbide, can obtain the niobium 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: niobium pentaoxide 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, niobium 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 niobium 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 niobium carbide block, pulverize niobium 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: niobium pentaoxide 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, niobium 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 niobium 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 niobium carbide block, pulverize after the cooling and make niobium carbide powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 3
1, raw material preparation:
The first step: niobium pentaoxide 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, niobium 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 niobium 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 niobium carbide block, pulverize after the cooling and make niobium carbide powder.
It is 99.99% pure that raw materials used purity is.
Claims (1)
1. the preparation method of a niobium carbide powder is characterized in that: the high-activity carbon that adopts phenolic resin carbonized to form is that carbon source reduction niobium pentaoxide powder prepares niobium carbide powder, may further comprise the steps:
1. raw material preparation:
The first step: the niobium pentaoxide 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. niobium 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 niobium 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 niobium carbide block, pulverize after the cooling and make niobium carbide powder.
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| CN 201110136013 CN102285652B (en) | 2011-05-25 | 2011-05-25 | Preparation method of niobium carbide powder |
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| CN 201110136013 CN102285652B (en) | 2011-05-25 | 2011-05-25 | Preparation method of niobium carbide powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102581288B (en) * | 2012-03-26 | 2013-07-31 | 燕山大学 | Method for preparing ultrafine niobium carbide and iron composite powder material |
| CN104261834B (en) * | 2014-09-22 | 2015-10-07 | 山东理工大学 | Niobium carbide ceramic fine bead prepares the method for high temperature high voltage resistant oil well cementing test block |
| CN106153569A (en) * | 2016-07-08 | 2016-11-23 | 株洲硬质合金集团有限公司 | The preparation of refractory metal oxygen standard sample, application and the choosing method of sample niobium powder |
| CN109401082A (en) * | 2018-10-31 | 2019-03-01 | 江苏伊顿航天材料股份有限公司 | A kind of EPDM sealing element |
| CN114538444B (en) * | 2020-11-20 | 2024-02-02 | 中国科学院大连化学物理研究所 | Niobium carbide and preparation method thereof |
| CN112777597A (en) * | 2021-03-23 | 2021-05-11 | 上海简巨医学生物工程有限公司 | Niobium carbide nano material 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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