CN1159263C - Method for preparing high-performance aluminium nitride powder by means of combustion synthesis process - Google Patents
Method for preparing high-performance aluminium nitride powder by means of combustion synthesis process Download PDFInfo
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- CN1159263C CN1159263C CNB011292199A CN01129219A CN1159263C CN 1159263 C CN1159263 C CN 1159263C CN B011292199 A CNB011292199 A CN B011292199A CN 01129219 A CN01129219 A CN 01129219A CN 1159263 C CN1159263 C CN 1159263C
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- powder
- raw material
- combustion
- aluminium nitride
- aluminium
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- 239000000843 powder Substances 0.000 title claims abstract description 63
- 229910017083 AlN Inorganic materials 0.000 title claims abstract description 39
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000005049 combustion synthesis Methods 0.000 title claims abstract description 15
- 230000008569 process Effects 0.000 title description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004411 aluminium Substances 0.000 claims abstract description 20
- 238000002485 combustion reaction Methods 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 12
- 230000037452 priming Effects 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 11
- 230000000996 additive effect Effects 0.000 claims description 11
- 238000006396 nitration reaction Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000002203 pretreatment Methods 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000003085 diluting agent Substances 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 238000007780 powder milling Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000002950 deficient Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000000875 high-speed ball milling Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000015598 salt intake Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
The present invention relates to a method for preparing high-performance aluminium nitride powder by combustion synthesis. Firstly, raw material aluminium powder is pretreated, a diluting agent, an addition agent and a solid nitridizing agent are added to the treated raw material aluminium powder, and ball milling is carried out to the mixture of the raw material powder on a rotary ball mill; then, the mixture is put in a combustion-synthesis reaction device, nitrogen gas is filled in the combustion-synthesis reaction device under a low vacuum, and then an igniting agent is ignited to induce the combustion of the raw material powder to synthesize aluminium nitride powder. The method has the advantages of high productive efficiency, energy saving, simple device and little investment, and the prepared aluminium nitride powder has the advantages of high purity and uniform and small crystal grain.
Description
Technical field the present invention relates to the method that a kind of burning synthesis for preparing is equipped with aluminium nitride powder, belongs to the inorganic non-metallic materials science field.
It is low that background technology AlN pottery has density, the thermal conductivity height, and electrical insulating property is good, specific modulus is big, thermal expansivity is little, and excellent comprehensive performances such as heat-shock resistance height have very wide application prospect in fields such as ic substrate, radiator element and semiconductor packages.Traditional method for preparing AlN is a lot, and wherein most typical have metallic aluminium direct nitridation method and an oxide high-temperature carbothermic method.Direct nitridation method requires high to material purity, cause the cost height, and reaction not exclusively needs the secondary nitrogenize.There is the shortcoming that the production cycle is long, energy consumption is big, efficient is low, technology is more loaded down with trivial details, cost is high in carbothermic method.We can say and also do not have a kind of method that can prepare the aluminium nitride powder of super quality and competitive price at present.Therefore the preparation of aluminium nitride powder has become the commercial key point of aluminium nitride ceramics.
Combustion synthesis method has characteristics such as save energy, efficient height, equipment are simple relatively. but disclosed combustion synthesis method prepares in the AlN powder owing to experienced very high temperature of combustion (generally be higher than 1600 ℃, even be higher than 2100 ℃) at present.Cause prepared powder sintering activity relatively poor, can not be used to prepare the Thermal Conductivity Ceramics Used that is higher than 120W/mK.Also there is some other limitation in addition.As " preparation method of aluminium nitride powder and powder constituent thing thereof " (flat 1-26494) of inventions such as Japanese palace Ben Qinsheng, need original stock is prefabricated into less, the complex procedures of briquetting, output of φ 11 * 15mm size, the product behind the briquetting is difficult to fragmentation.(the Chinese patent publication number is CN11422477A) overcome the defective of Japanese Patent to " preparation method of the synthetic aluminium nitride powder of self propagating high temperature " of inventions such as China's village Chinese is sharp substantially, but temperature of reaction is too high, and the AlN particle of generation is bigger, and sintering activity is relatively poor.Residual Cl in the while AlN finished product
-Or F
-Ion is more.Filling amount still seldom only reaches 200 * 400 * 30-40mm, can not satisfy need of industrial production.
" preparation method of high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis " (the Chinese patent publication number is CN1194959A) of inventions such as China Han Huanqing by adopting special charging method, improved single heat charge amount.Reduce Cl by reducing the ammonium salt consumption
-Residual volume improves product purity.But Al powder proportion only is 25-33% in the reaction mass, and single furnace output is still limited.
Foregoing two China patent exists simultaneously, and AlN is through the relatively poor defective of high-temperature calcination sintering activity, and their employed nitrogen pressure too high (top pressure is up to 15MPa).Requirement to equipment is comparatively harsh, and accident generation probability increases.
Summary of the invention the objective of the invention is to propose a kind of method of utilizing burning synthesis for preparing to be equipped with aluminium nitride powder, overcome the shortcoming of prior art, make the AlN powder of preparation have higher sintering activity, and it is low to prepare employed nitrogen pressure, equipment is simple, and is safe and reliable.
The burning synthesis for preparing that the present invention proposes is equipped with the method for aluminium nitride powder, comprises following each step:
1. the raw material aluminium powder is carried out pre-treatment, improve the activity of raw material aluminium powder, treatment process comprises: pickling, supersound process, high speed ball milling.Adopt the HF of dilution, HCl carries out pickling to the raw material aluminium powder, and is dry under protective atmosphere; With raw material aluminium powder supersound process; With raw material aluminium powder high speed ball milling.Three kinds of methods can be carried out separately as required, also can be in conjunction with carrying out.
2. prepare burden: add thinner, additive, solid-state nitration agent in the raw material aluminium powder after above-mentioned processing, thinner wherein is an aluminium nitride powder, and additive is NH
4F, NH
4Cl, (NH
4)
2CO
3, (NH
4)
2CO
3In any, the solid-state nitration agent is NaN
3, C
3H
6N
6, NH
4N
3, C
2H
4N
4In any, its weight percent is:
Aluminium powder: 34%-60%
The aluminium nitride thinner:: 25%-55%
Additive: 10.5-25%
Solid-state nitration agent: 0.2-2%
3. with the mixture of above-mentioned raw materials powder on rotary mill ball milling 20-30 hour, make its thorough mixing. with mixed raw material 50～70 ℃ of oven dry, be placed in the porous graphite container, put into the combustion synthesis reaction device, under rough vacuum, charge into the nitrogen pressure of 1-4.5MPa, light priming mixture, bring out the material powder burning, priming mixture is the mixture of pure titanium valve or titanium valve and carbon black, and mol ratio is 1: 1; Temperature of combustion is 1000-1500 ℃, and combustion reactions continues to be cooled to room temperature after 30 minutes, and fine grinding and stage treatment can obtain the aluminium nitride powder of excellent performance.
The method of the preparing high-performance aluminium nitride powder by means of combustion synthesis process that the present invention proposes, be difficult to control to overcome the combustion synthesis method reaction, the product purity that is obtained is low, crystal grain is thick, owing to cause the defective of sintering activity difference to be the basis through high-temperature calcination, by pre-treatment to raw material powder, improve reactive behavior, make its (1000-1500 ℃) at a lower temperature, combustion reactions still can be carried out, the suitable suitable solid-state nitration agent of successful candidate, thinner and additive, temperature of reaction and speed of reaction are reduced greatly, thereby combustion reactions is controlled effectively: add a certain amount of thinner AlN in the prescription, the effect of playing dilution on the one hand reduces temperature of reaction; On the other hand, AlN disperses molten aluminum, plays to promote the nitrogen infiltration; In prescription, add a certain amount of solid-state nitration agent, solve the microcosmic infiltration diffusion problem of nitrogen, improve degree of purity of production and nitriding rate; Add certain quantity of additive in the prescription with further reduction temperature of reaction, thereby reduce the combustion wave rate of propagation, reach the effect that reduces the product granularity.Advantages such as the present invention has that technology is simple, good reproducibility, transformation efficiency height, product uniform particles are tiny, the high and low cost of sintering activity.Its outstanding feature is:
1. by to the pre-treatment of raw material aluminium powder or add some aluminium salt, reach building-up reactions at a lower temperature (1000 ℃～1500 ℃) can carry out, institute's synthetic powder sintering activity is good.
2. production efficiency height.Synthetic reaction process is rapid, generally can finish in seconds or tens of seconds, saves the process time.
3. save energy.Except that starting reaction, material is synthetic to be undertaken by the liberated heat of reaction own, does not need external heat source, thereby saves the energy, process economics.
4. equipment is simple, invests little.
5. the present invention overcomes in the conventional SHS process, because temperature of reaction is too high, speed of response is too fast, and reaction is difficult to control, causes building-up reactions to be carried out not exclusively, and transformation efficiency is low, and sintering activity is poor, synthetic product crystal grain is thick, is difficult to broken shortcoming.Add suitable solid-state nitration agent, thinner and additive,, control building-up reactions effectively, synthesize transformation efficiency and reach 100%, purity height, the aluminium nitride powder that uniform crystal particles is tiny by three's reasonable cooperation.
6. selected solid-state nitration agent of present method and additive are easy decomposition and volatile material, as NH
4N
3Fusing point be 160 ℃, and the decomposition of thereupon blasting; NaN
3Fusing point be 300 ℃, decomposing N a and N thereupon
2, the temperature of reaction of burning synthesis temperature generally all is higher than 1000 ℃, and therefore the additive that is added all can decompose moment or volatilization, reduces synthesis reaction temperature and combustion wave rate of propagation, and can not influence degree of purity of production.
7. sparking mode is flexible, can adopt Fe
3O
4+ Al, Cr
2O
3+ Al, Fe
3O
4+ Mg, MnO
2Various ignition agent such as+Mg, Ti+C, Ti cause combustion synthesis reaction.
Because speed of response is slow, temperature of combustion is low, can effectively prolong the nitrogen penetration time, thereby under low nitrogen pressure condition, still can realize complete nitrogenize.Can reduce employed nitrogen pressure significantly, reduce requirement, improve the safety coefficient of producing equipment.Because employed nitrogen pressure is lower, can make the halogenide of generation resolve into escape of gas, reduce F in the product
-, Cl
-The ionic residual quantity.
Embodiment
Embodiment one, the raw material aluminium powder is carried out pre-treatment by above-mentioned steps 1 described method, by weight Al be 52.8%, AlN is 28.5%, NH
4F is 5.7%, NH
4Cl is 11.4%, NaN
3Be 1.6%, with raw material powder ball milling 24 hours on rotary mill, make its thorough mixing, with mixed raw material 65 ℃ of oven dry, be placed in the porous graphite container, put into the combustion synthesis reaction device, under rough vacuum, charge into the nitrogen pressure of 4.5MPa, light priming mixture, bring out the material powder burning, priming mixture is the mixture of pure titanium valve or titanium valve and carbon black, and mol ratio is 1: 1; Combustion reactions continues to be cooled to room temperature after 30 minutes, and fine grinding and stage treatment can obtain nitrogen content 33.0, the aluminium nitride powder of median size 2.0 μ m.
Embodiment two, to the raw material aluminium powder set by step 1 described method carry out pre-treatment, by weight Al be 48.5%, AlN is 35.1%, NH
4F is 5.0%, NH
4Cl is 10.0%, NaN
3Be 1.3%, with above-mentioned raw materials powder ball milling 24 hours on rotary mill, make its thorough mixing, with mixed raw material 55 ℃ of oven dry, be placed in the porous graphite container, put into the combustion synthesis reaction device, under rough vacuum, charge into the nitrogen pressure of 4MPa, light priming mixture, bring out the material powder burning, priming mixture is the mixture of pure titanium valve or titanium valve and carbon black, and mol ratio is 1: 1; Combustion reactions continues to be cooled to room temperature after 30 minutes, and fine grinding and stage treatment can obtain nitrogen content 33.5, the aluminium nitride powder of median size 1.2 μ m.
Embodiment three, to the raw material aluminium powder set by step 1 described method carry out pre-treatment, by weight Al be 44.0%, AlN is 42.2%, NH
4F is 4.3%, NH
4Cl is 8.6%, C
3H
6N
6Be 0.9%, with above-mentioned raw materials powder ball milling 24 hours on rotary mill, make its thorough mixing, with mixed raw material 68 ℃ of oven dry, be placed in the porous graphite container, put into the combustion synthesis reaction device, under rough vacuum, charge into the nitrogen pressure of 4MPa, light priming mixture, bring out the material powder burning, priming mixture is the mixture of pure titanium valve or titanium valve and carbon black, and mol ratio is 1: 1; Combustion reactions continues to be cooled to room temperature after 30 minutes, and fine grinding and stage treatment can obtain nitrogen content 33.0, the aluminium nitride powder of median size 1.8 μ m.
Embodiment four, 1 described method set by step, with the raw material aluminium powder after pre-treatment, by weight Al be 37.3%, AlN is 51.5%, NH
4F is 3.5%, NH
4Cl is 7.1%, NaN
3Be 0.6%, with above-mentioned raw materials powder ball milling 24 hours on rotary mill, make its thorough mixing, with mixed raw material 60 ℃ of oven dry, be placed in the porous graphite container, put into the combustion synthesis reaction device, under rough vacuum, charge into the nitrogen pressure of 3MPa, light priming mixture, bring out the material powder burning, priming mixture is the mixture of pure titanium valve or titanium valve and carbon black, and mol ratio is 1: 1; Combustion reactions continues to be cooled to room temperature after 30 minutes, and fine grinding and stage treatment can obtain nitrogen content 33.3,
Claims (1)
1, a kind of burning synthesis for preparing is equipped with the method for aluminium nitride powder, it is characterized in that this method comprises following each step:
(1) the raw material aluminium powder is carried out pre-treatment, to improve the activity of raw material aluminium powder, pretreated method is to adopt the HF of dilution, and HCl carries out pickling to the raw material aluminium powder, and is dry under protective atmosphere;
(2) batching: add thinner, additive, solid-state nitration agent in the raw material aluminium powder after above-mentioned processing, thinner wherein is an aluminium nitride powder, and additive is NH
4F, NH
4Cl, (NH
4)
2CO
3, (NH
4)
2CO
3In any, the solid-state nitration agent is NaN
3, C
3H
6N
6, NH
4N
3, C
2H
4N
4In any, its weight percent is:
Aluminium powder: 34%-60%
The aluminium nitride thinner:: 25%-55%
Additive: 10.5-25%
Solid-state nitration agent: 0.2-2%
(3) with the mixture of above-mentioned raw materials powder on rotary mill ball milling 20-30 hour, make its thorough mixing. with mixed raw material 50～70 ℃ of oven dry, be placed in the porous graphite container, put into the combustion synthesis reaction device, under rough vacuum, charge into the nitrogen pressure of 1-4.5MPa, light priming mixture, bring out the material powder burning, priming mixture is the mixture of pure titanium valve or titanium valve and carbon black, and mol ratio is 1: 1, temperature of combustion is 1000-1500 ℃, combustion reactions continues to be cooled to room temperature after 30 minutes, and fine grinding and stage treatment promptly get aluminium nitride powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011292199A CN1159263C (en) | 2001-06-15 | 2001-06-15 | Method for preparing high-performance aluminium nitride powder by means of combustion synthesis process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011292199A CN1159263C (en) | 2001-06-15 | 2001-06-15 | Method for preparing high-performance aluminium nitride powder by means of combustion synthesis process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1321621A CN1321621A (en) | 2001-11-14 |
| CN1159263C true CN1159263C (en) | 2004-07-28 |
Family
ID=4669011
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011292199A Expired - Lifetime CN1159263C (en) | 2001-06-15 | 2001-06-15 | Method for preparing high-performance aluminium nitride powder by means of combustion synthesis process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798071B (en) * | 2010-03-23 | 2011-08-31 | 西安交通大学 | Method for preparing aluminum nitride with three-dimensional sub-micron flower-like structure |
| CN103274375B (en) * | 2013-06-20 | 2015-01-07 | 西安工程大学 | Method for preparing aluminum nitride powder |
| WO2021157388A1 (en) * | 2020-02-06 | 2021-08-12 | 株式会社トクヤマ | Method for producing aluminum nitride powder, aluminum nitride powder, and package |
-
2001
- 2001-06-15 CN CNB011292199A patent/CN1159263C/en not_active Expired - Lifetime
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|---|---|
| CN1321621A (en) | 2001-11-14 |
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