CN102225762B - Preparation method of hafnium carbide powder - Google Patents
Preparation method of hafnium carbide powder Download PDFInfo
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- CN102225762B CN102225762B CN 201110135995 CN201110135995A CN102225762B CN 102225762 B CN102225762 B CN 102225762B CN 201110135995 CN201110135995 CN 201110135995 CN 201110135995 A CN201110135995 A CN 201110135995A CN 102225762 B CN102225762 B CN 102225762B
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Abstract
The invention provides a preparation method of hafnium carbide powder, which comprises the following steps of material preparation, mixing, curing, pulverization, compression molding, sintering, decarburization and pulverization, and is characterized in that: phenolic resin is mixed with hafnium dioxide powder with a particle size of 0.1-3 microns to form sludge; the sludge is cured at 40 DEG C-100 DEGC, and is pulverized and compressed to become a block; the block is sintered at 1300 DEG C-1800 DEG C in inert gas or reducing gas atmosphere for 6-8 hours to prepare a hafnium carbide block; and the hafnium carbide powder is obtained by decarburization and pulverization. The invention has the characteristics of simple process, high purity of the hafnium carbide powder, and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of hafnium carbide powder, belong to the ceramic powder preparing technical field.
Background technology
At present, hafnium carbide powder is mainly made by the hafnium oxide carbothermic method, and its reaction equation is:
HfO
2+3C＝HfC+2CO↑
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 hafnium oxide powder and carbon black or graphite composite powder mix inhomogeneous and carbon black or graphite composite powder activity lower, make the hafnium oxide reduction not exclusively, become the impurity of product.In addition, the carbon black or the graphite composite powder activity that remain in the hafnium 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 hafnium 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 hafnium carbide powder that a kind of cost is low, sintering activity is good is provided.Its technical scheme is:
The preparation method of hafnium carbide powder of the present invention is that the high-activity carbon that adopts resol to form is that carbon source reduction hafnium oxide powder prepares hafnium carbide powder, may further comprise the steps:
1. raw material preparation:
The first step: the hafnium oxide 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. hafnium 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 hafnium carbide block in 6-8 hour under 1300 ℃～2000 ℃ temperature.
3. carbonization treatment
With the oxidizing atmosphere insulation decarburization in 6～12 hours under 350～550 ℃ temperature of above-mentioned hafnium carbide block, pulverize after the cooling and make hafnium carbide powder.
The preparation method of described hafnium carbide powder, hafnium oxide 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 hafnium oxide powder is wrapped up and forms isolated micron-sized hafnium oxide particle, phenolic resin carbonized forms the very much higher hole of activity high-activity carbon when temperature raises, so that the beginning temperature of hafnium oxide 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 hafnium oxide 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 hafnium oxide particle, has suppressed the growth of hafnium carbide crystal grain when reaction forms hafnium carbide, can obtain the hafnium 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: hafnium oxide 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, hafnium 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 hafnium 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 hafnium carbide block, pulverize hafnium 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: hafnium oxide 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, hafnium 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 hafnium carbide block in 7 hours under 1650 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 9 hours under 450 ℃ temperature of above-mentioned hafnium carbide block, pulverize after the cooling and make hafnium carbide powder.
It is 99.99% pure that raw materials used purity is.
Embodiment 3
1, raw material preparation:
The first step: hafnium oxide 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, hafnium 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 hafnium carbide block in 8 hours under 2000 ℃ ℃ temperature.
3, carbonization treatment
With the oxidizing atmosphere insulation decarburization in 12 hours under 550 ℃ temperature of above-mentioned hafnium carbide block, pulverize after the cooling and make hafnium carbide powder.
It is 99.99% pure that raw materials used purity is.
Claims (1)
1. the preparation method of a hafnium carbide powder is characterized in that: the high-activity carbon that adopts phenolic resin carbonized to form is that carbon source reduction hafnium oxide powder prepares hafnium carbide powder, may further comprise the steps:
1. raw material preparation:
The first step: the hafnium oxide 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. hafnium 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 hafnium 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 hafnium carbide block, pulverize after the cooling and make hafnium carbide powder.
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| CN 201110135995 CN102225762B (en) | 2011-05-25 | 2011-05-25 | Preparation method of hafnium carbide powder |
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| CN 201110135995 CN102225762B (en) | 2011-05-25 | 2011-05-25 | Preparation method of hafnium carbide powder |
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| CN102225762A CN102225762A (en) | 2011-10-26 |
| CN102225762B true CN102225762B (en) | 2013-02-13 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730685B (en) * | 2012-07-03 | 2014-04-02 | 西北工业大学 | Method for preparing one-dimensional hafnium carbide nanometer material |
| CN103253669B (en) * | 2013-05-17 | 2015-07-08 | 航天材料及工艺研究所 | Method for preparing HfC powder at low temperature by carbothermic method |
| CN103435307B (en) * | 2013-09-02 | 2015-05-06 | 山东理工大学 | Method for preparing low-density oil well cement briquettes by using hafnium carbide microbeads |
| CN105780123B (en) * | 2016-02-04 | 2018-02-09 | 武汉科技大学 | A kind of hafnium carbide nano whisker and preparation method thereof |
| CN107601508B (en) * | 2017-09-12 | 2020-02-14 | 江苏理工学院 | Hafnium 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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