CN102285662B - Preparation method of niobium boride powder - Google Patents
Preparation method of niobium boride powder Download PDFInfo
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- CN102285662B CN102285662B CN 201110136047 CN201110136047A CN102285662B CN 102285662 B CN102285662 B CN 102285662B CN 201110136047 CN201110136047 CN 201110136047 CN 201110136047 A CN201110136047 A CN 201110136047A CN 102285662 B CN102285662 B CN 102285662B
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Abstract
The invention provides a preparation method of niobium boride powder. The method comprises the following steps: dosing, mixing, curing, milling, briquetting, firing and milling. The method is characterized in that niobium pentoxide powder, boron carbide powder and B2O3 powder are mixed with phenolic resin, the mixture is cured at 40-100 DEG C to mill, the obtained powder is briquetted and then fired in 1350-1900 DEG C of argon or hydrogen atmosphere for 6-8 hours to prepare niobium boride blocks, and the blocks are decarbonized and milled to prepare the niobium boride powder. The method has the characteristics of simple process, high niobium boride powder purity, good sintering performance of niobium boride powder and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of niobium (Nb) boride powder, belong to the ceramic powder preparing technical field.
Background technology
The niobium (Nb) boride powder is mainly by 2Nb
2O
5Powder and carbon black or graphite powder carbothermic method make, and its reaction equation is:
2Nb
2O
5+B
4C+15C+2B
2O
3＝4Nb?B
2+16CO↑
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 powder mix inhomogeneous and carbon black or graphite powder active lower, make the Niobium Pentxoxide reduction not exclusively, become the impurity of product.In addition, the carbon black or the graphite powder active that remain in the niobium (Nb) boride 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 more high powder of temperature is more high, causes the decline of niobium (Nb) boride 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 niobium (Nb) boride powder that a kind of cost is low, sintering activity is good is provided.Its technical scheme is:
The preparation method of niobium (Nb) boride powder of the present invention is that the high-activity carbon that adopts the resol carbonization to form is that carbon source reduction niobium pentaoxide powder prepares the niobium (Nb) boride powder, may further comprise the steps:
1. feedstock production:
The first step: be niobium pentaoxide powder, 3～10 μ m boron carbide powders and 3～10 μ m B of 0.1～3 μ m with granularity
2O
3Powder is by 70～80: 14～20: 3～6 mixed obtains powder 1;
Second step: be that 5: 0.5～1 ratio mixes in mixing pan with above-mentioned powder 1 and resol with weight ratio, under 80～100 ℃ temperature, solidify, in powder-making machine, pulverize then and make the raw material powder 2 that median size is 10～20 μ m;
The 3rd step: be that 5: 1～2 ratio mixes with above-mentioned raw materials powder 2 and resol with weight ratio, under 50～100 ℃ temperature, solidify that pulverizing then and making median size is 20～50 μ m raw material powder 3 in mixing pan in powder-making machine;
The 4th step: be that 5: 2～3 ratio mixes with above-mentioned raw materials powder 3 and resol with weight ratio, under 40～80 ℃ temperature, solidify that pulverizing then and making median size is 50～100 μ m raw material powder 4 in mixing pan in powder-making machine;
2. the niobium (Nb) boride powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 0.5～3MPa., argon gas or hydrogen atmosphere are fired and were made the niobium (Nb) boride block in 6-8 hour under 1350 ℃～1900 ℃ temperature then;
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned niobium (Nb) boride block, the cooling back is pulverized and is made the niobium (Nb) boride powder.
The preparation method of described niobium (Nb) boride powder is characterized in that: niobium pentaoxide powder, boron carbide powder and B
2O
3Powder 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, the resol carbonization forms active very high porous high-activity carbon when temperature raises, make that the beginning temperature of Niobium Pentxoxide and carbon reaction is descended significantly, the micro channel of the porous high-activity carbon of acquisition can successfully be discharged the carbon monoxide of Niobium Pentxoxide and carbon reaction generation;
2, the high reactivity porous high-activity carbon that forms after the resol carbonization has wrapped up the Niobium Pentxoxide particle, the carbon of surplus is isolated different boronation Niobium crystal grain when reaction forms boronation Niobium, the overgrowth that has suppressed boronation Niobium crystal grain, can obtain the boronation Niobium powder of grain-size homogeneous, can suitably reduce the resol consumption or reduce step according to required high-activity carbon amount;
3, this technical matters is simple, stable, and production cost is low, and the powder oxygen level is low, and the powder sintering performance is good.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
1, feedstock production:
The first step: be that niobium pentaoxide powder, 3 μ m boron carbide powders and the 3 μ m B2O3 powders of 0.1 μ m evenly mix in 70: 14: 3 ratio and obtain raw material powder 1 with granularity.
Second step: be that 5: 0.5 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, under 80 ℃ temperature, solidify, in powder-making machine, pulverize then and make the raw material powder 2 that median size is 10 μ m.
The 3rd step: be that 5: 1 ratio mixes with above-mentioned raw materials powder 2 and resol with weight ratio, under 50 ℃ temperature, solidify that pulverizing then and making median size is 20 μ m raw material powder 3 in mixing pan in powder-making machine.
The 4th step: be that 5: 2 ratio mixes with above-mentioned raw materials powder 3 and resol with weight ratio, under 40 ℃ temperature, solidify that pulverizing then and making median size is 50 μ m raw material powder 4 in mixing pan in powder-making machine.
2, boronation Niobium powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 0.5Mpa, argon gas atmosphere is fired and was made boronation Niobium block in 6 hours under 1350 ℃ ℃ temperature then.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 12 hours under 350 ℃ temperature of above-mentioned boronation Niobium block, the cooling back is pulverized and is made boronation Niobium powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 2
1, feedstock production:
The first step: be niobium pentaoxide powder, 7 μ m boron carbide powders and the 7 μ mB of 2 μ m with granularity
2O
3Powder obtains raw material powder 1 in 75: 17: 4.5 even mixing of ratio.
Second step: be that 5: 0.75 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, under 90 ℃ temperature, solidify, in powder-making machine, pulverize then and make the raw material powder 2 that granularity is 15 μ m.
The 3rd step: be that 5: 1.5 ratio mixes with above-mentioned raw materials powder 2 and resol with weight ratio, under 75 ℃ temperature, solidify that pulverizing then and making granularity is 35 μ m raw material powder 3 in mixing pan in powder-making machine.
The 4th step: be that 5: 2.5 ratio mixes with above-mentioned raw materials powder 3 and resol with weight ratio, under 60 ℃ temperature, solidify that pulverizing then and making granularity is 75 μ m raw material powder 4 in mixing pan in powder-making machine.
2, boronation Niobium powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 1.5Mpa, hydrogen atmosphere is fired and was made boronation Niobium block in 7 hours under 1700 ℃ ℃ temperature then.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 9 hours under 450 ℃ temperature of above-mentioned boronation Niobium block, the cooling back is pulverized and is made boronation Niobium powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 3
1, feedstock production:
The first step: be niobium pentaoxide powder, 10 μ m boron carbide powders and the 10 μ mB of 3 μ m with granularity
2O
3Powder obtains raw material powder 1 in 80: 20: 6 even mixing of ratio.
Second step: be that 5: 1 ratio mixes in mixing pan with above-mentioned raw materials powder 1 and resol with weight ratio, under 100 ℃ temperature, solidify, in powder-making machine, pulverize then and make the raw material powder 2 that granularity is 20 μ m.
The 3rd step: be that 5: 2 ratio mixes with above-mentioned raw materials powder 2 and resol with weight ratio, under 100 ℃ temperature, solidify that pulverizing then and making granularity is 50 μ m raw material powder 3 in mixing pan in powder-making machine.
The 4th step: be that 5: 3 ratio mixes with above-mentioned raw materials powder 3 and resol with weight ratio, under 80 ℃ temperature, solidify that pulverizing then and making granularity is 100 μ m raw material powder 4 in mixing pan in powder-making machine.
2, boronation Niobium powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 3Mpa, hydrogen atmosphere is fired and was made boronation Niobium block in 8 hours under 1900 ℃ ℃ temperature then.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6 hours under 550 ℃ temperature of above-mentioned boronation Niobium block, the cooling back is pulverized and is made boronation Niobium powder.
It is 99.99% pure that raw materials used purity is.
Claims (1)
1. the preparation method of a niobium (Nb) boride powder is characterized in that: the high-activity carbon that adopts the resol carbonization to form is that carbon source reduction niobium pentaoxide powder prepares the niobium (Nb) boride powder, may further comprise the steps:
1. feedstock production:
The first step: be niobium pentaoxide powder, 3～10 μ m boron carbide powders and 3～10 μ m B of 0.1～3 μ m with granularity
2O
3Powder is by 70～80: 14～20: 3～6 mixed obtains powder 1;
Second step: be that 5: 0.5～1 ratio mixes in mixing pan with above-mentioned powder 1 and resol with weight ratio, under 80～100 ℃ temperature, solidify, in powder-making machine, pulverize then and make the raw material powder 2 that median size is 10～20 μ m;
The 3rd step: be that 5: 1～2 ratio mixes with above-mentioned raw materials powder 2 and resol with weight ratio, under 50～100 ℃ temperature, solidify that pulverizing then and making median size is 20～50 μ m raw material powder 3 in mixing pan in powder-making machine;
The 4th step: be that 5: 2～3 ratio mixes with above-mentioned raw materials powder 3 and resol with weight ratio, under 40～80 ℃ temperature, solidify that pulverizing then and making median size is 50～100 μ m raw material powder 4 in mixing pan in powder-making machine;
2. the niobium (Nb) boride powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 0.5～3MPa., argon gas or hydrogen atmosphere are fired and were made the niobium (Nb) boride block in 6-8 hour under 1350 ℃～1900 ℃ temperature then;
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned niobium (Nb) boride block, the cooling back is pulverized and is made the niobium (Nb) boride powder.
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|---|---|---|---|
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| CN102285662B true CN102285662B (en) | 2013-07-17 |
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| CN104326763B (en) * | 2014-09-23 | 2016-02-03 | 山东理工大学 | Niobium (Nb) boride ceramic fine bead prepares the method for high temperature high voltage resistant oil well cementing test block |
| CN114409277B (en) * | 2021-12-30 | 2023-10-20 | 东海县亚连玻璃有限公司 | Low-radiation LOW-E hollow glass |
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| JP4140324B2 (en) * | 2002-09-10 | 2008-08-27 | 住友金属鉱山株式会社 | Metal boride powder and method for producing the same |
| CN101372339A (en) * | 2008-10-24 | 2009-02-25 | 北京工业大学 | Preparation of high purity high dense polycrystal CeB6 block cathode material |
| CN101973559B (en) * | 2010-10-11 | 2011-12-28 | 吉林大学 | Method for preparing boride of manganese at high temperature and high pressure |
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