CN1280183C - Method for preparing aluminium nitride powder by carbothermic reduction method - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 48
- 229910017083 AlN Inorganic materials 0.000 title claims abstract description 43
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000000725 suspension Substances 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 19
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000006229 carbon black Substances 0.000 claims description 15
- 239000000428 dust Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 235000015110 jellies Nutrition 0.000 claims description 8
- 239000008274 jelly Substances 0.000 claims description 8
- 238000005261 decarburization Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 159000000013 aluminium salts Chemical class 0.000 claims description 6
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 6
- 239000013543 active substance Substances 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract 3
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 abstract 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 238000001879 gelation Methods 0.000 abstract 1
- 150000004767 nitrides Chemical class 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 239000000499 gel Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The present invention relates to a method for preparing aluminium nitride powder by a carbon thermal reduction method, particularly to a technological method for preparing aluminium nitride powder by a carbon thermal reduction method. The present invention is characterized in that in the preparing procedure, aluminium hydroxide, fluoride and/or a boride additive are mixed; the mixture is calcined for two to four hours under the temperature of 500 DEG C to 900 DEG C, so porous activated aluminium oxide is obtained. The activated aluminium oxide which is crushed is prepared into suspension in water; aluminum salt and carbon powder are added to carry out gelation; after the mixture of the suspension, the aluminum salt and the carbon powder is dried and crushed, nitrogen gas is led in and used for reducing the mixture of the suspension, the aluminum salt and the carbon powder to obtain nitride powder. The prepared aluminium nitride powder has small particle and no hard conglobation; simultaneously, the reaction temperature is lowered.
Description
Technical field
A kind of method of preparing aluminium nitride powder by carbothermic reduction method relates to the method for preparing aluminium nitride powder by carbothermic reduction method technology.
Background technology
AlN (aluminium nitride) is an III-V family semiconductor compound, and its crystal is to be structure unit with [AlN4] tetrahedron, has the covalent linkage compound of Warzjte structure.Lattice parameter α in the time of 25 ℃
0=3.1127, c
0=4.9816, belong to hexagonal system, the powder true density is 3.255g/cm
3
It (is Al that the AlN material has the thermal conductivity height
2O
38～10 times), the high temperature electrical insulating property is good, dielectric properties are good, thermal expansivity is low by (4.4 * 10
-6℃), close with silicon single crystal, compare Al
2O
3, excellent characteristic such as BeO is low, and the strength of materials is big under heat shock resistance resistance height, the high temperature, hardness is high, nontoxic, thereby in numerous areas, be used widely.Be used for fields such as hybrid integrated circuit (HIC), microwave integrated circuit (MIC), electric power electronic module (GTRM, IGBTM), laser diode (LD), crucible, cutter material in the world.Especially its thermal expansion and semiconductor silicon material are complementary and nontoxicity, are the used support heat sink materials of comparatively ideal electronic semi-conductor encapsulation, to replace the big material of toxicity.
Present aluminium nitride synthetic method mainly contains following several: aluminium powder direct nitridation method, carbothermic method, gas-phase reaction method, cracking process, plasma method, arc melting method, self propagating high temperature synthesis method, microwave process for synthesizing etc.Every kind of aluminium nitride preparation method has the strengths and weaknesses of self, comparatively speaking, aluminium nitride powder purity height, stable performance, the powder size of carbothermic method preparation is tiny evenly, shaping and sintering character are good, is a kind of aluminum nitride powder preparation with applications well prospect.But in the process of preparing aluminium nitride powder by carbothermic reduction method, also have a lot of weak points, as temperature of reaction height, long reaction time etc.
Summary of the invention
The objective of the invention is weak point, a kind of method that effectively reduces temperature of reaction, shortening reaction times, improves the preparing aluminium nitride powder by carbothermic reduction method of aluminium nitride quality is provided at preparing aluminium nitride powder by carbothermic reduction method.
Method of the present invention is achieved through the following technical solutions.
A kind of method of preparing aluminium nitride powder by carbothermic reduction method is characterized in that its preparation process is:
A: aluminium hydroxide is mixed with additive fluorid and/or boride, between 500～900 ℃, calcined 2～4 hours, obtain a kind of porous activated alumina; Aluminum oxide powder is broken into the powder of 0.5～2 μ m with ball mill or airflow milling;
B: the activated alumina powder that obtains prepared in water becomes suspension, adds aluminium salt under 60～90 ℃ water bath condition, and adds tensio-active agent, and the pH value of adjusting suspension with mineral acid is 0～6, stirs 20～30 minutes, obtains steady suspension;
C: in suspension, add the superfine carbon black, the mole number that carbon black adds is 1.5～3 times of total aluminium mole number in the fine suspension, should slowly add when adding carbon black, stirs simultaneously, make the carbon black that adds form suspension with aluminum oxide, this process is carried out under 60～90 ℃ water bath condition;
D: slow dropping ammonia in suspension, adjusting the pH value is 9～14, stirs simultaneously, after 20～30 minutes, forms a kind of black jelly that mixes;
E: jelly at 70～90 ℃ temperature range inner drying, is obtained a kind of block of black after the drying;
F: block is broken into the small-particle of 2～8mm, adds entry again less than the particle of 2mm, and repeat d, e, f step, finally all obtain the small-particle of 2～8mm, broken again greater than the particle of 8mm, up to the particle that is broken into all between 2～8mm;
H: the black small-particle that fragmentation is good is put into vacuum carbon tube furnace, calcines under nitrogen atmosphere 2～6 hours, and calcining temperature is 1500～1750 ℃, and the atrament that obtains is the aluminum nitride particle that is mixed with the carbon dust that does not react completely;
I: reacted small-particle is pulverized, and the atrament that obtains is the aluminium nitride powder that is mixed with the carbon dust that does not react completely;
J: the powder that will be obtained by i obtains gray aluminium nitride powder groom's stove internal heating decarburization of 600～800 ℃.
The method of a kind of preparing aluminium nitride powder by carbothermic reduction method of the present invention is characterized in that the amount of the additive that adds is 0.5%～3.5%.
The method of a kind of preparing aluminium nitride powder by carbothermic reduction method of the present invention is characterized in that aluminium salt that suspension preparation adds is one or two or more kinds the mixture in aluminum nitrate, aluminum chloride, the Tai-Ace S 150.
The used aluminium hydroxide of method of the present invention can be the industrial aluminium hydroxide of industry, also superfine aluminium hydroxide, a crystalline size according to used aluminium hydroxide, a crystal of the prepared aluminium nitride powder that comes out is different, is about 4～5 μ m as a crystal of the prepared aluminium nitride powder that comes out of: the industrial aluminium hydroxide that (1) adopts crystal is about 3～4 μ m; A crystal of the prepared aluminium nitride powder that comes out of the industrial ultrafine aluminium hydroxide that (2) to adopt crystal be about 0.3～0.5 μ m is about 1～2 μ m.
Adopt the prepared aluminium nitride powder of method of the present invention, good dispersity, hard aggregation-free has only a spot of soft-agglomerated existence, can smash as long as grind a little.The present invention relates to a kind of aluminum nitride powder preparation, be intended to improve the quality of aluminium nitride, reduce nitriding temperature, save energy and reduce the cost, develop the method for the high-quality aluminium nitride of a kind of low cost production.
Adopting aluminium hydroxide and ultra-fine carbon dust is starting raw material, and adopt colloidal sol-gel process, all raw materials of preparing aluminium nitride powder by carbothermic reduction method are carried out anchored in place, the accelerated reaction process, introduce tensio-active agent simultaneously, stop the aluminium nitride that generates to be reunited.Aluminium hydroxide is mixed with additive, in low temperature (between 500～900 ℃) calcining down, prepare highly active alumina powder jointed, formulated suspension then, add tensio-active agent, the ultra-fine carbon black that under condition of stirring, adds some amount, after the carbon black adding finishes, through homogenizing after a while, adjust with ammoniacal liquor more than the pH value to 9 of system, obtain the jelly of black, dry and dried jelly is ground into the small-particle of 2～8mm, with small-particle sintering under the nitrogen atmosphere in vacuum carbon tube furnace, the carbon black blended granular substance that obtains aluminium nitride and do not react completely, particle is pulverized and decarburization in 600～800 ℃ the temperature range under the oxidizing atmosphere in groom's stove, obtained aluminium nitride powder.
Description of drawings
Fig. 1 is the process flow diagram of method of the present invention.
Specific embodiments
A kind of aluminum nitride powder preparation, preparation process is a: aluminium hydroxide is mixed with additive fluorid and/or boride, additive can be a solid, also can be liquid, the purpose that adds additive is to remove impurity, as sodium, calcines between 500～900 ℃ 2～4 hours, obtain a kind of porous activated alumina, the specific surface area of this aluminum oxide is at 120～300m
2Between/the g, aluminum oxide powder is broken into the powder of 0.5～2 μ m with ball mill or airflow milling; B: the activated alumina powder that obtains prepared in water becomes suspension, under 60～90 ℃ water bath condition, add aluminium salt, as aluminum nitrate, aluminum chloride, Tai-Ace S 150 etc., the aluminium salt that adds is one or more mixture wherein, and add some tensio-active agents, as polyoxyethylene glycol, the pH value of adjusting suspension with mineral acid is between 0～6, stirred 20～30 minutes, and obtained steady suspension; This process is carried out under 60～90 ℃ water bath condition; C: in suspension, add the superfine carbon black, the mole number that carbon black adds is 1.5～3 times of total aluminium mole number in the fine suspension, should slowly add when adding carbon black, stirs simultaneously, make the carbon black that adds form suspension with aluminum oxide, this process is carried out under 60～90 ℃ water bath condition; D: slow dropping ammonia in suspension, adjusting the pH value is between 9～14, stirs simultaneously, after 20～30 minutes, forms a kind of black jelly that mixes; E: at 70～90 ℃ temperature range inner drying, drying mode can be free dry, can be vacuum-drying also, obtains a kind of block of black after the drying with jelly; F: block is broken into the small-particle of 2～8mm, adds entry again less than the particle of 2mm, and repeat d, e, f step, finally all obtain the small-particle of 2～8mm, broken again greater than the particle of 8mm, up to the particle that is broken into all between 2～8mm; H: the black small-particle that fragmentation is good is put into vacuum carbon tube furnace, calcines under nitrogen atmosphere 2～6 hours, and calcining temperature is between 1500～1750 ℃, and the atrament that obtains is the aluminum nitride particle that is mixed with the carbon dust that does not react completely; I: reacted small-particle is pulverized, and the atrament that obtains is the aluminium nitride powder that is mixed with the carbon dust that does not react completely; J: the powder that will be obtained by i obtains gray aluminium nitride powder groom's stove internal heating decarburization of 600～800 ℃.
The present invention will be further described below in conjunction with example.
Embodiment 1
With the industrial aluminium hydroxide is raw material, at first 1000g aluminium hydroxide is mixed with 15 gram boric acid additives, calcined 6 hours down at 500 ℃, get the aluminum oxide after 200g calcines, put into the beaker of 1000ml, add the deionized water of 200ml, add aluminum nitrate 25g then, add surfactant soln then, adjust the pH value between 2～3 with nitric acid, add the ultra-fine carbon dust of 70g while stirring, add carbon dust after, stirred 20 minutes, slowly add ammoniacal liquor, adjust between the pH value to 12, at this moment slurry has become the spawn of an integral body, gel is dry in 90 ℃ loft drier, dried gel is broken into the small-particle of 2～8mm, and small-particle is put into vacuum carbon tube furnace, and the control nitrogen flow is at 20～25ml/s, sintering temperature is 1600 ℃, and the time is 3 hours.Material after the calcining is pulverized, and oxidizing roasting decarburization in groom's stove of 750 ℃ obtains gray aluminium nitride powder at last.
Embodiment 2
Change the aluminum oxide in the example 1 into ultrafine aluminium hydroxide, calcining temperature is 1550 ℃, also obtains same result.
Embodiment 3
With the industrial aluminium hydroxide is raw material, at first 1000g aluminium hydroxide is mixed with 15 gram boric acid additives, calcined 2 hours down at 900 ℃, get the aluminum oxide after 200g calcines, put into the beaker of 1000ml, add the deionized water of 200ml, add aluminum nitrate 25g then, add surfactant soln then, adjust the pH value between 2 with nitric acid, add the ultra-fine carbon dust of 70g while stirring, add carbon dust after, stirred 30 minutes, slowly add ammoniacal liquor, adjust between the pH value to 13, at this moment slurry has become the spawn of an integral body, gel is dry in 90 ℃ loft drier, dried gel is broken into the small-particle of 2～8mm, and small-particle is put into vacuum carbon tube furnace, and the control nitrogen flow is at 20～25ml/s, sintering temperature is 1800 ℃, and the time is 2 hours.Material after the calcining is pulverized, and oxidizing roasting decarburization in 2 hours obtains gray aluminium nitride powder at last in groom's stove of 800 ℃.
Embodiment 4
With the industrial aluminium hydroxide is raw material, at first 1000g aluminium hydroxide is mixed with 15 gram boric acid additives, calcined 4 hours down at 800 ℃, get the aluminum oxide after 200g calcines, put into the beaker of 1000ml, add the deionized water of 200ml, add aluminum nitrate 25g then, add surfactant soln then, adjust the pH value between 2 with nitric acid, add the ultra-fine carbon dust of 70g while stirring, add carbon dust after, stirred 30 minutes, slowly add ammoniacal liquor, adjust between the pH value to 13, at this moment slurry has become the spawn of an integral body, gel is dry in 80 ℃ loft drier, dried gel is broken into the small-particle of 2～8mm, and small-particle is put into vacuum carbon tube furnace, and the control nitrogen flow is at 20～25ml/s, sintering temperature is 1500 ℃, and the time is 6 hours.Material after the calcining is pulverized, and oxidizing roasting decarburization in 4 hours obtains gray aluminium nitride powder at last in groom's stove of 600 ℃, and the prepared aluminium nitride powder particle that comes out is tiny, hard aggregation-free, and temperature of reaction is lower simultaneously.
Claims (3)
1. the method for a preparing aluminium nitride powder by carbothermic reduction method is characterized in that its preparation process is:
A: aluminium hydroxide is mixed with additive fluorid and/or boride, between 500～900 ℃, calcined 2～4 hours, obtain a kind of porous activated alumina; Aluminum oxide powder is broken into the powder of 0.5～2 μ m with ball mill or airflow milling;
B: the activated alumina powder that obtains prepared in water becomes suspension, adds aluminium salt under 60～90 ℃ water bath condition, and adds tensio-active agent, and the pH value of adjusting suspension with mineral acid is 0～6, stirs 20～30 minutes, obtains steady suspension;
C: in suspension, add the superfine carbon black, the mole number that carbon black adds is 1.5～3 times of total aluminium mole number in the fine suspension, should slowly add when adding carbon black, stirs simultaneously, make the carbon black that adds form suspension with aluminum oxide, this process is carried out under 60～90 ℃ water bath condition;
D: slow dropping ammonia in suspension, adjusting the pH value is 9～14, stirs simultaneously, after 20～30 minutes, forms a kind of black jelly that mixes;
E: jelly at 70～90 ℃ temperature range inner drying, is obtained a kind of block of black after the drying;
F: block is broken into the small-particle of 2～8mm, adds entry again less than the particle of 2mm, and repeat d, e, f step, finally all obtain the small-particle of 2～8mm, broken again greater than the particle of 8mm, up to the particle that is broken into all between 2～8mm;
H: the black small-particle that fragmentation is good is put into vacuum carbon tube furnace, calcines under nitrogen atmosphere 2～6 hours, and calcining temperature is 1500～1750 ℃, and the atrament that obtains is the aluminum nitride particle that is mixed with the carbon dust that does not react completely;
I: reacted small-particle is pulverized, and the atrament that obtains is the aluminium nitride powder that is mixed with the carbon dust that does not react completely;
J: the powder that will be obtained by i obtains gray aluminium nitride powder groom's stove internal heating decarburization of 600～800 ℃.
2, the method for a kind of preparing aluminium nitride powder by carbothermic reduction method according to claim 1 is characterized in that the amount of the additive that adds is 0.5%～3.5%.
3, the method for a kind of preparing aluminium nitride powder by carbothermic reduction method according to claim 1 is characterized in that aluminium salt that suspension preparation adds is one or two or more kinds the mixture in aluminum nitrate, aluminum chloride, the Tai-Ace S 150.
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| CN1326318C (en) * | 2005-06-23 | 2007-07-11 | 南京航空航天大学 | Control method of double-salient-pole electric machine without position sensor |
| CN102502534B (en) * | 2011-11-18 | 2013-09-04 | 西安理工大学 | Preparation method of mesoporous AlN or GaN microparticle |
| US9403680B2 (en) * | 2013-02-04 | 2016-08-02 | Tokuyama Corporation | Method for producing sintered aluminum nitride granules |
| CN104988335B (en) * | 2015-06-17 | 2018-02-09 | 昆明理工大学 | A kind of method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition |
| CN105884372B (en) * | 2016-04-12 | 2018-11-13 | 武汉理工大学 | Organic network method synthesizes AlN ceramic powder method |
| CN107162600A (en) * | 2017-07-14 | 2017-09-15 | 河北利福光电技术有限公司 | It is a kind of for high-purity aluminium nitride powder material of ceramic substrate and preparation method thereof |
| CN110627509B (en) * | 2019-10-11 | 2022-03-15 | 航天特种材料及工艺技术研究所 | Preparation method of aluminum nitride powder |
| TWI769913B (en) | 2021-08-24 | 2022-07-01 | 財團法人工業技術研究院 | Ceramic composite and method of preparing the same |
| CN113830807B (en) * | 2021-10-14 | 2023-04-07 | 暨南大学 | Preparation method of intrinsic black alumina powder |
| CN114380279A (en) * | 2021-10-29 | 2022-04-22 | 江苏悟晴电子新材料有限公司 | Preparation method of high-performance aluminum nitride material |
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