CN102249686B - Preparation method of tantalum boride powder - Google Patents
Preparation method of tantalum boride powder Download PDFInfo
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- CN102249686B CN102249686B CN 201110135960 CN201110135960A CN102249686B CN 102249686 B CN102249686 B CN 102249686B CN 201110135960 CN201110135960 CN 201110135960 CN 201110135960 A CN201110135960 A CN 201110135960A CN 102249686 B CN102249686 B CN 102249686B
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Abstract
The invention provides a preparation method of a tantalum boride powder. The preparation method comprises preparing, mixing, solidifying, milling, briquetting, firing and milling. The preparation method is characterized by comprising the following steps: mixing tantalum pentoxide powder, boron carbide powder and B2O3 powder with phenolic resin; solidifying at the temperature of 40-100 DEG C and then milling; pressing the powders into block bodies; and then firing the block bodies for 6-8 hours at the temperature of 1350 DEG C-2000 DEG C under the atmosphere of argon or hydrogen so as to prepare the tantalum boride block bodies; and then smashing the tantalum boride block bodies after decarbonization so as to prepare the tantalum boride powder. The preparation method has simple process and low cost, and the tantalum boride powder is high in purity and is good in sintering property.
Description
Technical field
The present invention relates to a kind of preparation method of tantalum boride powder, belong to the ceramic powder preparing technical field.
Background technology
Tantalum boride powder is mainly made by tantalum pentoxide powder and carbon black or graphite composite powder carbothermic method, and its reaction equation is:
2Ta
2?O
5+B
4C+15C+2B
2O
3＝4TaB
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 tantalum pentoxide powder and carbon black or graphite composite powder mix inhomogeneous and carbon black or graphite composite powder activity lower, make the tantalum pentoxide reduction not exclusively, become the impurity of product.In addition, the carbon black or the graphite composite powder activity that remain in the tantalum 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 higher powder of temperature is higher, causes the tantalum boride 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 tantalum boride powder that a kind of cost is low, sintering activity is good is provided.Its technical scheme is:
The preparation method of tantalum boride powder of the present invention is that the high-activity carbon that adopts phenolic resin carbonized to form is that carbon source reduction tantalum pentoxide powder prepares tantalum boride powder, may further comprise the steps:
1. raw material preparation:
The first step: be tantalum pentoxide 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 in 70～80: 14～20: 3～6 ratio is mixed to get powder 1;
Second step: above-mentioned powder 1 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 2 that median size is 10～20 μ m;
The 3rd step: above-mentioned raw materials powder 2 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 3;
The 4th step: above-mentioned raw materials powder 3 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 4.
2. tantalum boride powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 0.5～3MPa, then argon gas or hydrogen atmosphere are fired and were made the tantalum boride block in 6-8 hour under 1350 ℃～2000 ℃ temperature.
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned tantalum boride block, pulverize after the cooling and make tantalum boride powder.
The preparation method of described tantalum boride powder is characterized in that: tantalum pentoxide 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 the tantalum pentoxide powder is wrapped up and forms isolated micron-sized tantalum pentoxide particle, phenolic resin carbonized forms the very much higher hole of activity high-activity carbon when temperature raises, so that the beginning temperature of tantalum pentoxide and carbon reaction is significantly descended, the micro channel of the porous high-activity carbon of acquisition can successfully be discharged the carbon monoxide of tantalum pentoxide and carbon reaction generation;
2, the high reactivity porous high-activity carbon that forms behind the phenolic resin carbonized has wrapped up the tantalum pentoxide particle, when reaction forms tantalum boride, carbon is isolated different tantalum boride crystal grain, the overgrowth that has suppressed tantalum boride crystal grain, can obtain the tantalum boride 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, raw material preparation:
The first step: be tantalum pentoxide powder, 3 μ m boron carbide powders and the 3 μ m B of 0.1 μ m with granularity
2O
3Powder evenly is mixed to get raw material powder 1 in 70: 14: 3 ratio.
Second step: above-mentioned raw materials powder 1 and resol 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 2 that median size is 10 μ m.
The 3rd step: above-mentioned raw materials powder 2 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 3.
The 4th step: above-mentioned raw materials powder 3 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 4.
2, tantalum boride powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 0.5Mpa, then argon gas or hydrogen atmosphere are fired and were made the tantalum boride block in 6 hours under 1350 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 12 hours under 350 ℃ temperature of above-mentioned tantalum boride block, pulverize after the cooling and make tantalum boride powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 2
1, raw material preparation:
The first step: be tantalum pentoxide powder, 7 μ m boron carbide powders and the 7 μ mB of 2 μ m with granularity
2O
3Powder evenly is mixed to get raw material powder 1 in 75: 17: 4.5 ratio.
Second step: above-mentioned raw materials powder 1 and resol 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 2 that granularity is 15 μ m.
The 3rd step: above-mentioned raw materials powder 2 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 3.
The 4th step: above-mentioned raw materials powder 3 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 4.
2, tantalum boride powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 1.5Mpa, then argon gas or hydrogen atmosphere are fired and were made the tantalum boride block in 7 hours under 1700 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 9 hours under 450 ℃ temperature of above-mentioned tantalum boride block, pulverize after the cooling and make tantalum boride powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 3
1, raw material preparation:
The first step: be tantalum pentoxide powder, 10 μ m boron carbide powders and the 10 μ mB of 3 μ m with granularity
2O
3Powder evenly is mixed to get raw material powder 1 in 80: 20: 6 ratio.
Second step: above-mentioned raw materials powder 1 and resol 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 2 that granularity is 20 μ m.
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 100 ℃ temperature, then pulverizing in powder-making machine and making granularity is 50 μ m raw material powder 3.
The 4th step: above-mentioned raw materials powder 3 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 4.
2, tantalum boride powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 3Mpa, then argon gas or hydrogen atmosphere are fired and were made the tantalum boride block in 8 hours under 2000 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6 hours under 550 ℃ temperature of above-mentioned tantalum boride block, pulverize after the cooling and make tantalum boride day powder.
It is 99.99% pure that raw materials used purity is.
Claims (1)
1. the preparation method of a tantalum boride powder is characterized in that: the high-activity carbon that adopts phenolic resin carbonized to form is that carbon source reduction tantalum pentoxide powder prepares tantalum boride powder, may further comprise the steps:
1. raw material preparation:
The first step: be tantalum pentoxide 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 in 70～80: 14～20: 3～6 ratio is mixed to get powder 1;
Second step: above-mentioned powder 1 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 2 that median size is 10～20 μ m;
The 3rd step: above-mentioned raw materials powder 2 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 3;
The 4th step: above-mentioned raw materials powder 3 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 4.
2. tantalum boride powder is synthetic:
With the pressure lower lock block of above-mentioned raw materials powder 4 at 0.5～3MPa., then argon gas or hydrogen atmosphere are fired and were made the tantalum boride block in 6-8 hour under 1350 ℃～2000 ℃ temperature.
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned tantalum boride block, pulverize after the cooling and make tantalum boride powder.
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| CN 201110135960 CN102249686B (en) | 2011-05-25 | 2011-05-25 | Preparation method of tantalum boride powder |
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| CN102249686B true CN102249686B (en) | 2013-02-13 |
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Non-Patent Citations (5)
| Title |
|---|
| JP昭62-158114A 1987.07.14 |
| Synthesis, densification, and mechanical properties of TaB2;Xiaohong Zhang et al;《Materials Letters》;20080629;第62卷;第4251–4253页 * |
| Xiaohong Zhang et al.Synthesis, densification, and mechanical properties of TaB2.《Materials Letters》.2008,第62卷第4251–4253页. |
| 张勇 等.超高温材料的研究进展及应用.《材料导报》.2007,第21卷(第12期),第60-64页. |
| 超高温材料的研究进展及应用;张勇 等;《材料导报》;20071231;第21卷(第12期);第60-64页 * |
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