CN114772563B - Preparation method of high-purity nano aluminum nitride powder - Google Patents
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 143
- 239000000843 powder Substances 0.000 title claims abstract description 122
- 238000002360 preparation method Methods 0.000 title claims abstract description 78
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 458
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 229
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 100
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 95
- 239000007788 liquid Substances 0.000 claims abstract description 94
- 238000000034 method Methods 0.000 claims abstract description 53
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000011810 insulating material Substances 0.000 claims description 11
- 239000011449 brick Substances 0.000 claims description 9
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 22
- 238000001816 cooling Methods 0.000 abstract description 21
- 238000010924 continuous production Methods 0.000 abstract description 11
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 239000012535 impurity Substances 0.000 description 10
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 8
- 238000007599 discharging Methods 0.000 description 8
- 238000005121 nitriding Methods 0.000 description 8
- 239000002243 precursor Substances 0.000 description 8
- 230000000630 rising effect Effects 0.000 description 8
- 238000003860 storage Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 239000010431 corundum Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
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- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
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- 238000000713 high-energy ball milling Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
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- 239000007789 gas Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
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- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- -1 nitrogen ions Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0722—Preparation by direct nitridation of aluminium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a preparation method of high-purity nano aluminum nitride powder, and belongs to the technical field of aluminum nitride powder preparation. The preparation method comprises the steps of reacting high-temperature aluminum liquid at 850-1600 ℃ with nitrogen bubbles to obtain an aluminum nitride film, crushing the aluminum nitride film to obtain nano aluminum nitride powder which drifts in nitrogen, cooling the nitrogen and the nano aluminum nitride powder, separating to obtain high-purity nano aluminum nitride powder and nitrogen, and reacting the separated nitrogen with nitrogen bubbles. The nano aluminum nitride powder prepared by the method has high purity (up to more than 99.5%), uniform particle size of nano powder, high sphericity, no agglomeration, continuous production, high yield, quick output and low cost.
Description
Technical Field
The invention belongs to the technical field of preparation of aluminum nitride powder, and relates to a preparation method of high-purity nanometer aluminum nitride powder.
Background
Aluminum nitride is used as a ceramic material with excellent comprehensive performance, the heat of the aluminum nitride can be compared with that of a semiconductor, a chip, an integrated circuit and the like, and the aluminum nitride is not only a strategic semiconductor material for manufacturing the chip, but also unique characteristics and advantages are favored by other numerous industries.
With the rapid development of the electronic industry, the electronic complete machine and the electronic components are rapidly developed towards miniaturization, light weight, integration, high reliability, high power output and the like, which inevitably results in high heat generation, and the heat dissipation efficiency needs to be improved, so the application of the high heat conduction material is essential to effectively solve the heat dissipation problem of the high power device.
The high heat conductive substrates which are used for practical and development application are alumina, silicon carbide, beryllium oxide, aluminum nitride and the like. Among them, aluminum nitride ceramics are used because of their extremely high thermal conductivity, non-toxicity, corrosion resistance, high temperature resistance, good thermochemical stability, etc., however aluminum nitride is a covalent compound, and has a small self-diffusion coefficient and a very high melting point, which can cause difficulty in sintering and limit the application range, especially in the aspects of heat dissipation elements of electronic complete machines and electronic components.
The existing preparation methods of aluminum nitride powder mainly comprise a direct nitriding method and a carbothermic reduction method, and further comprise a high-energy ball milling method, a self-propagating synthesis method, an in-situ self-reaction synthesis method, a plasma chemical synthesis method and the like. These methods have technical drawbacks, and are described in detail as follows:
1) Direct nitridation: the direct nitriding process is to react aluminum powder directly with nitrogen in high temperature nitrogen atmosphere to produce aluminum nitride powder at 900-1500 deg.c. Its advantages are simple process, low cost and suitable for industrial mass production. The defects are that nitride is generated on the surface of aluminum powder, so that nitrogen cannot permeate, and the conversion rate is low; the reaction speed is high, and the reaction process is difficult to control; the heat released by the reaction can cause the powder to self-sinter to form agglomeration, so that the powder particles are coarsened, and the powder particles are crushed by ball milling in the later period and doped with impurities.
2) Carbothermal reduction: the carbothermal reduction method is to mix Al uniformly 2 O 3 And C heating in nitrogen atmosphere, firstly Al 2 O 3 By reduction of C, the resultant Al is then reacted with N 2 AlN is generated by reaction, and the preparation method has the advantages of rich raw materials and simple process; the powder has high purity, small particle size and uniform distribution. The method has the defects of long synthesis time, higher nitriding temperature and higher production cost because excessive carbon is required to be subjected to carbon removal treatment after reaction.
3) High-energy ball milling method: the high-energy ball milling method is a method of directly nitriding aluminum nitride powder by using rotation or vibration of a ball mill under nitrogen or ammonia atmosphere to make hard balls to impact, grind and stir raw materials such as aluminum oxide or aluminum powder strongly. The advantages are that: the high-energy ball milling method has the advantages of simple equipment, short process flow, high production efficiency and the like. The defects are that: nitriding is difficult to complete, and impurities are easily introduced during ball milling, resulting in lower quality of powder.
4) The high temperature self-propagating synthesis process is one direct nitriding process and is one igniting Al powder in high pressure nitrogen and utilizing Al and N 2 The heat generated by the reaction automatically maintains the reaction until the reaction is complete, and the chemical reaction formula is as follows:
2Al(s)+N 2 (g)→2AlN(s)
the method has the advantages that the essence of the high-temperature self-propagating synthesis method is the same as that of the aluminum powder direct nitriding method, but the method does not need to carry out nitriding on the Al powder at high temperature, and only needs to ignite the Al powder at the beginning, so the energy consumption is low, the production efficiency is high, and the cost is low. The disadvantage is that to obtain completely nitrided powder, it is necessary to carry out the process under a relatively high nitrogen pressure, which directly affects the industrial production of the process.
5) The principle of the in-situ self-reaction synthesis method is basically similar to that of the direct nitridation method, and alloy formed by aluminum and other metals is used as a raw material, other metals in the alloy are melted at high temperature and react with nitrogen to generate metal nitride, and then metal Al replaces metal of the nitride to produce AlN. Its advantages are simple process, rich raw materials, low reaction temp and low content of oxygen and impurities. The disadvantage is that the metal impurities are difficult to separate, resulting in a low insulation performance.
6) Plasma chemical synthesis method: the plasma chemical synthesis method uses a direct current arc plasma generator or a high-frequency plasma generator to convey Al powder into a plasma flame zone, and immediately melts and volatilizes the powder in the flame high-temperature zone to quickly combine with nitrogen ions to form AlN powder. Its advantages are less aggregation and small particle size. The method has the defects of unstable reaction, small batch treatment, difficult realization of industrial production, high oxygen content, complex required equipment and incomplete reaction.
Still other methods of preparation exist, such as: CN113460981a discloses that an aluminum source, activated carbon and a pore-forming agent are subjected to a hydrothermal reaction to obtain a solid precursor; and calcining the solid precursor and a nitrogen source to obtain the aluminum nitride powder. Obviously, the prepared aluminum nitride powder takes the nano active carbon structure as a growing template, and the adopted hydrothermal reaction and carbothermic reduction reaction have the advantages of complex preparation process, long time, high cost, insufficient and efficient utilization of an aluminum source caused by low carbon content and the technical defect of more impurities in the aluminum nitride powder.
CN112265973a discloses that the synthesis of aluminum nitride based on aluminum gasification reaction not only requires a specially arranged reaction vessel, but also requires strict control of reaction conditions, the reaction efficiency is greatly affected by gasification conditions, and is not easy to control, the operation difficulty is high, the cost is high, continuous production is not possible, the consumption of nitrogen is high, and industrial large-scale production and use are not facilitated.
CN110015900a discloses a preparation method of composite nano aluminum nitride powder with low-temperature sintering property, firstly, a sol-gel method or a chemical coprecipitation method is needed to prepare nano aluminum hydroxide, then aluminum sheet, aluminum nitride powder, rare earth salt or rare earth oxide, ammonium salt, organic carbon source, urea, ethanol and deionized water are added, ball milling and calcination obviously increase cost and preparation time, continuous production cannot be carried out, reaction is complex, impurities are more, and carbon is not removed.
CN109019536a discloses that the reaction preparation of solid aluminum source and solid nitrogen source requires decarbonization treatment, and has the advantages of more impurities, insufficient reaction, low efficiency, high cost, incapability of continuous production, and adverse industrial mass production and use.
CN107162599a discloses that an aluminum chloride precursor salt solution is prepared first, then dried to obtain aluminum chloride precursor salt powder, finally the aluminum chloride precursor salt powder is put into an alumina crucible, and the temperature is raised to 900-1000 ℃ under the condition of nitrogen, and the temperature is kept to obtain nano aluminum nitride powder; obviously, the reaction is the nitridation reaction of the aluminum chloride precursor salt powder and nitrogen, is insufficient and low in efficiency, is suitable for laboratory research, cannot be continuously produced, and is not beneficial to industrial mass production and use.
Disclosure of Invention
The invention aims to solve the technical problems that the existing aluminum nitride powder is low in yield, needs secondary processing at different degrees, and is complex in procedure and high in operation difficulty; the reaction is insufficient and the efficiency is low, so that the method is suitable for laboratory research, cannot be used for continuous production, and is not beneficial to industrial large-scale production and use; the purity of the finished product is low, the impurities are more, carbon needs to be removed, the consumption of nitrogen is large, and the oxygen content is more than 0.5%; high cost, long time, high energy consumption, etc.
The invention provides the following technical scheme:
the preparation method comprises the steps of reacting 850-1600 ℃ high-temperature aluminum liquid with nitrogen bubbles to obtain an aluminum nitride film, crushing the aluminum nitride film to obtain nano aluminum nitride powder which drifts in nitrogen, cooling the nitrogen and the nano aluminum nitride powder, and separating to obtain high-purity nano aluminum nitride powder and nitrogen, wherein the separated nitrogen is used for nitrogen bubble reaction.
Preferably, the reaction in the preparation process is carried out in an air-vented, nitrogen-filled reactor.
Preferably, the nitrogen gas is charged into the reactor through a nitrogen tank in the preparation method.
Preferably, the high-temperature aluminum liquid in the preparation method enters the reactor filled with nitrogen and exhausted by an aluminum liquid supply pipeline; the purity of the aluminum liquid is not less than 99.999 percent.
Preferably, nitrogen bubbles in the preparation method are formed by introducing nitrogen of high-temperature aluminum liquid, and the supply amount of the nitrogen is 100-600L/min; the purity of the nitrogen is not less than 99.99%.
Preferably, the nitrogen introduced into the high-temperature aluminum liquid in the preparation method comprises nitrogen injection through a vent pipe orifice or a high-temperature resistant air brick arranged at the bottom or at the side of the reactor.
Preferably, the reactor lining in the preparation method is a heat-resistant heat-insulating material.
Preferably, the heat-resistant and heat-insulating material of the reactor lining is graphite, corundum or other materials.
Preferably, the reaction of 850-1600 ℃ high-temperature aluminum liquid and nitrogen bubbles in the preparation method needs heating, and the preparation method of 850-1600 ℃ high-temperature aluminum liquid comprises electric furnace heating, tungsten-molybdenum heating or silicon-molybdenum rod heating.
Preferably, in the preparation method, the high-temperature aluminum liquid at 850-1600 ℃ is reacted with nitrogen bubbles, nitrogen is introduced into the high-temperature aluminum liquid, so that nitrogen bubbles are formed, the nitrogen bubbles rise in the aluminum liquid, and the surface of the nitrogen bubbles react with the high-temperature aluminum liquid in the rising process to form a layer of aluminum nitride film on the periphery of the nitrogen bubbles.
Preferably, the thickness of the aluminum nitride film in the preparation method is 0.1-0.3 μm.
Preferably, the nitrogen bubbles attached with a layer of aluminum nitride film on the surface of the preparation method rise to a liquid level of Wen Lvye, and then the nitrogen bubbles burst, so that the aluminum nitride film on the surface of the nitrogen bubbles is crushed into nano aluminum nitride powder.
Preferably, the high-purity nano aluminum nitride powder obtained by the preparation method has an average particle diameter of 0.1-0.6 mu m, an oxygen content of less than 0.5% and an aluminum nitride purity of more than 99.5%.
Preferably, in the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reactor, and the scattered aluminum nitride powder and unreacted nitrogen enter the radiator through an outlet at the top end.
Preferably, the temperature of the heat sink region in the preparation method is not higher than 300 ℃.
Preferably, the cooling mode in the preparation method is not limited to air cooling, liquid cooling and the like.
Preferably, the separation in the preparation method is performed by a gas-powder separator.
Preferably, the nitrogen separated in the preparation method is sent to a nitrogen tank through a booster pump for reuse.
Compared with the prior art, the invention has the following beneficial effects:
in the scheme, the aluminum nitride powder synthesized by the method has high purity (more than 99.5 percent), uniform particle size of nano-scale powder, high sphericity, no agglomeration, continuous production, high yield, quick output and low cost.
According to the invention, the aluminum nitride film is obtained by reacting the high-temperature aluminum liquid with the nitrogen bubbles, so that the technical problems of insufficient reaction, high nitrogen consumption and low utilization rate in the existing gasification reaction of aluminum gas and nitrogen are avoided, and the technical problems of more reaction steps, high industrial control difficulty, high cost and incapability of continuous production in the technical scheme of calcining nitrogen after preparing the precursor by using the hydrothermal reaction are solved.
According to the invention, the nano aluminum nitride powder which drifts in the nitrogen can be obtained by crushing the aluminum nitride film, and even if the aluminum nitride powder is doped with impurities of aluminum powder, nitridation reaction can occur in the process of discharging the aluminum nitride film and the nitrogen, so that the utilization rate of aluminum liquid is very high, and continuous production can be realized.
The nitrogen and the nano aluminum nitride powder are cooled, then the high-purity nano aluminum nitride powder and the nitrogen are obtained through separation, and the separated nitrogen is used for nitrogen bubble reaction; therefore, the nitrogen can be fully utilized, the nitrogen consumption is reduced, the utilization rate is improved, the production cost is reduced, and the method is beneficial to industrial mass production and popularization and use.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of a method for preparing high purity nano aluminum nitride powder according to the present invention;
FIG. 2 is a schematic diagram of the production of alumina powder by rising nitrogen bubbles in a reactor, formation of an aluminum nitride film, and burst of the aluminum nitride film in the process for producing high purity nano aluminum nitride powder of the present invention; wherein: the reference numeral 1 is a reaction furnace, the reference numeral 2 is a height Wen Lvye, the reference numeral 3 is nitrogen bubbles without an aluminum nitride film attached, the reference numeral 4 is nitrogen bubbles with an aluminum nitride film attached, the reference numeral 5 is a burst film, the reference numeral 6 is nano aluminum nitride powder, and the reference numeral 7 is a reaction furnace outlet.
Detailed Description
The technical solutions and the technical problems to be solved in the embodiments of the present invention will be described below in conjunction with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, of the embodiments of the present patent.
As shown in fig. 1 and 2, the preparation method comprises the steps of heating aluminum particles through a heating furnace to obtain 850-1600 ℃ high-temperature aluminum liquid 2, simultaneously adding the prepared nitrogen into a nitrogen tank through a nitrogen generator for storage, filling nitrogen into a reaction furnace to discharge air, adding 850-1600 ℃ high-temperature aluminum liquid into the reaction furnace 1 through a pipeline, reacting the 850-1600 ℃ high-temperature aluminum liquid with nitrogen bubbles not attached with an aluminum nitride film in the reaction furnace 1 to obtain nitrogen bubbles 4 attached with the aluminum nitride film, cracking the nitrogen bubbles 4 attached with the aluminum nitride film to obtain a cracking film 5, crushing the cracking film 5 to obtain nano aluminum nitride powder 6 scattered in the nitrogen, cooling the nitrogen and the nano aluminum nitride powder 6 in a radiator, separating the nitrogen and the nano aluminum nitride powder through a gas-powder separator, allowing the separated nitrogen to enter the nitrogen tank through a booster pump for subsequent nitrogen reaction, and allowing the separated nitrogen to enter the separated high-purity nano aluminum nitride powder to enter the collector for collection.
In the specific reaction process, as shown in fig. 2, nitrogen bubbles 3 of the unattached aluminum nitride film in the preparation method are formed in high-temperature aluminum liquid 2 at 850-1600 ℃ through ventilation nozzles or high-temperature resistant ventilation bricks arranged at the bottom or side edges of the reactor, the purity of the aluminum liquid is not less than 99.999%, the nitrogen bubbles 3 of the unattached aluminum nitride film ascend in the aluminum liquid, and the surface of the nitrogen bubbles 3 of the unattached aluminum nitride film reacts with the high-temperature aluminum liquid 2 in the ascending process to form an aluminum nitride film with the thickness of 0.1-0.3 μm on the periphery of the nitrogen bubbles 3 of the unattached aluminum nitride film. The supply amount of nitrogen is 100-600L/min; the purity of the nitrogen is not less than 99.99%.
And the nitrogen bubbles 4 attached with the aluminum nitride film rise to the liquid surface of the high-temperature aluminum liquid 2, and then the nitrogen bubbles 4 attached with the aluminum nitride film burst, so that the aluminum nitride film on the surface of the nitrogen bubbles 4 attached with the aluminum nitride film is crushed into nano aluminum nitride powder 6 with the average particle size of 0.1-0.6 mu m, the oxygen content of less than 0.5% and the purity of more than 99.5%.
The lining of the reaction furnace in the preparation method is made of heat-resistant and heat-insulating materials.
The heat-resistant and heat-insulating material of the lining of the reaction furnace is graphite, corundum and other materials.
The high-temperature aluminum liquid with the temperature of 850-1600 ℃ needs to be heated when reacting with nitrogen bubbles in the preparation method, and the preparation method of the high-temperature aluminum liquid with the temperature of 850-1600 ℃ comprises electric furnace heating, tungsten-molybdenum heating or silicon-molybdenum rod heating.
In the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reaction furnace, and scattered aluminum nitride powder and unreacted nitrogen enter the radiator through the outlet 7 of the reaction furnace at the top end.
The temperature of the radiator area in the preparation method is not higher than 300 ℃.
The cooling mode in the preparation method is not limited to air cooling, liquid cooling and the like.
The separation in the preparation method is carried out by a gas-powder separator.
The nitrogen separated in the preparation method is sent into a nitrogen tank for reuse through a booster pump.
Example 1
The preparation method of the high-purity nano aluminum nitride powder specifically comprises the following steps:
s1, heating aluminum particles through an electric furnace to obtain high-temperature aluminum liquid at 1200 ℃, adding the prepared nitrogen into a nitrogen tank through a nitrogen making machine for storage, and performing nitrogen charging and air discharging operation on a reaction furnace;
s2, adding 1200 ℃ high-temperature aluminum liquid into a reaction furnace through a pipeline, wherein the purity of the aluminum liquid is not less than 99.999%, nitrogen is blown into the 1200 ℃ high-temperature aluminum liquid through a vent pipe orifice or a high-temperature resistant air brick arranged at the bottom or at the side edge of the reactor to form nitrogen bubbles, the nitrogen bubbles rise in the aluminum liquid, and the surface of the nitrogen bubbles reacts with the high-temperature aluminum liquid in the rising process to form an aluminum nitride film with the thickness of 0.1-0.3 mu m on the periphery of the nitrogen bubbles; the supply amount of nitrogen is 300L/min; the purity of the nitrogen is not less than 99.99%;
s3, the nitrogen bubbles in the S2 burst, so that an aluminum nitride film on the surface of the nitrogen bubbles is crushed into nano aluminum nitride powder with the average particle size of 0.1-0.6 mu m, the oxygen content is lower than 0.5%, and the purity is higher than 99.5%, the nitrogen and the nano aluminum nitride powder are cooled in a radiator, then are separated by a gas-powder separator to obtain high-purity nano aluminum nitride powder and nitrogen, the separated nitrogen enters a nitrogen tank through a booster pump for subsequent nitrogen bubble reaction, and the separated high-purity nano aluminum nitride powder enters a powder collector for collection.
Wherein: the heat-resistant and heat-insulating material of the reactor lining in the preparation method is a graphite material.
In the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reactor, and the scattered aluminum nitride powder and unreacted nitrogen enter the radiator through an outlet at the top end.
The temperature of the radiator area in the preparation method is not higher than 300 ℃.
The cooling mode in the preparation method can be an air cooling mode.
Example 2
The preparation method of the high-purity nano aluminum nitride powder specifically comprises the following steps:
s1, heating aluminum particles through tungsten and molybdenum to obtain high-temperature aluminum liquid at 1100 ℃, adding the prepared nitrogen into a nitrogen tank through a nitrogen making machine for storage, and performing nitrogen charging and air discharging operation on a reaction furnace;
s2, adding high-temperature aluminum liquid at 1100 ℃ into a reaction furnace through a pipeline, wherein the purity of the aluminum liquid is not less than 99.999%, nitrogen is blown into the high-temperature aluminum liquid at 1100 ℃ through a vent pipe orifice or a high-temperature resistant air brick arranged at the bottom or at the side edge of the reactor to form nitrogen bubbles, the nitrogen bubbles rise in the aluminum liquid, and the surface of the nitrogen bubbles reacts with the high-temperature aluminum liquid in the rising process to form an aluminum nitride film with the thickness of 0.1-0.3 mu m on the periphery of the nitrogen bubbles; the nitrogen supply amount is 400L/min; the purity of the nitrogen is not less than 99.99%;
s3, the nitrogen bubbles in the S2 burst, so that an aluminum nitride film on the surface of the nitrogen bubbles is crushed into nano aluminum nitride powder with the average particle diameter of 0.1-0.6 mu m, the oxygen content of less than 0.5% and the purity of more than 99.5%, the nitrogen and the nano aluminum nitride powder are cooled in a radiator, then are separated by a gas-powder separator to obtain high-purity nano aluminum nitride powder and nitrogen, the separated nitrogen enters a nitrogen tank through a booster pump for subsequent nitrogen bubble reaction, and the separated high-purity nano aluminum nitride powder enters a powder collector for collection.
Wherein: the heat-resistant and heat-insulating material of the reactor lining in the preparation method is corundum.
In the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reactor, and the scattered aluminum nitride powder and unreacted nitrogen enter the radiator through an outlet at the top end.
The temperature of the radiator area in the preparation method is not higher than 300 ℃.
The cooling mode in the preparation method can be a liquid cooling mode.
Example 3
The preparation method of the high-purity nano aluminum nitride powder specifically comprises the following steps:
s1, heating aluminum particles through a silicon molybdenum rod to obtain 1400 ℃ high-temperature aluminum liquid, adding the prepared nitrogen into a nitrogen tank through a nitrogen making machine for storage, and performing nitrogen charging and air discharging operation on a reaction furnace;
s2, adding 1400 ℃ high-temperature aluminum liquid into a reaction furnace through a pipeline, wherein the purity of the aluminum liquid is not less than 99.999%, nitrogen is blown into the 1400 ℃ high-temperature aluminum liquid through a vent pipe orifice or a high-temperature resistant air brick arranged at the bottom or at the side edge of the reactor to form nitrogen bubbles, the nitrogen bubbles rise in the aluminum liquid, and the surface of the nitrogen bubbles reacts with the high-temperature aluminum liquid in the rising process to form an aluminum nitride film with the thickness of 0.1-0.3 mu m on the periphery of the nitrogen bubbles; the nitrogen supply amount is 200L/min; the purity of the nitrogen is not less than 99.99%;
s3, the nitrogen bubbles in the S2 burst, so that an aluminum nitride film on the surface of the nitrogen bubbles is crushed into nano aluminum nitride powder with the average particle size of 0.1-0.6 mu m, the oxygen content is lower than 0.5%, and the purity is higher than 99.5%, the nitrogen and the nano aluminum nitride powder are cooled in a radiator, then are separated by a gas-powder separator to obtain high-purity nano aluminum nitride powder and nitrogen, the separated nitrogen enters a nitrogen tank through a booster pump for subsequent nitrogen bubble reaction, and the separated high-purity nano aluminum nitride powder enters a powder collector for collection.
Wherein: the heat-resistant and heat-insulating material of the reactor lining in the preparation method is corundum.
In the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reactor, and the scattered aluminum nitride powder and unreacted nitrogen enter the radiator through an outlet at the top end.
The temperature of the radiator area in the preparation method is not higher than 300 ℃.
The cooling mode in the preparation method can be an air cooling mode.
Example 4
The preparation method of the high-purity nano aluminum nitride powder specifically comprises the following steps:
s1, heating aluminum particles through an electric furnace to obtain high-temperature aluminum liquid at 1000 ℃, adding the prepared nitrogen into a nitrogen tank through a nitrogen making machine for storage, and performing nitrogen charging and air discharging operation on a reaction furnace;
s2, adding high-temperature aluminum liquid at 1000 ℃ into a reaction furnace through a pipeline, wherein the purity of the aluminum liquid is not less than 99.999%, nitrogen is blown into the high-temperature aluminum liquid at 1000 ℃ through a vent pipe orifice or a high-temperature resistant air brick arranged at the bottom or at the side edge of the reactor to form nitrogen bubbles, the nitrogen bubbles rise in the aluminum liquid, and the surface of the nitrogen bubbles reacts with the high-temperature aluminum liquid in the rising process to form an aluminum nitride film with the thickness of 0.1-0.3 mu m on the periphery of the nitrogen bubbles; the nitrogen gas supply amount is 500L/min; the purity of the nitrogen is not less than 99.99%;
s3, the nitrogen bubbles in the S2 burst, so that an aluminum nitride film on the surface of the nitrogen bubbles is crushed into nano aluminum nitride powder with the average particle size of 0.1-0.6 mu m, the oxygen content is lower than 0.5%, and the purity is higher than 99.5%, the nitrogen and the nano aluminum nitride powder are cooled in a radiator, then are separated by a gas-powder separator to obtain high-purity nano aluminum nitride powder and nitrogen, the separated nitrogen enters a nitrogen tank through a booster pump for subsequent nitrogen bubble reaction, and the separated high-purity nano aluminum nitride powder enters a powder collector for collection.
Wherein: the heat-resistant and heat-insulating material of the reactor lining in the preparation method is corundum.
In the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reactor, and the scattered aluminum nitride powder and unreacted nitrogen enter the radiator through an outlet at the top end.
The temperature of the radiator area in the preparation method is not higher than 300 ℃.
The cooling mode in the preparation method can be a liquid cooling mode.
Example 5
The preparation method of the high-purity nano aluminum nitride powder specifically comprises the following steps:
s1, heating aluminum particles through tungsten and molybdenum to obtain 1600 ℃ high-temperature aluminum liquid, adding the prepared nitrogen into a nitrogen tank through a nitrogen making machine for storage, and performing nitrogen charging and air discharging operation on a reaction furnace;
s2, adding 1600 ℃ high-temperature aluminum liquid into a reaction furnace through a pipeline, wherein the purity of the aluminum liquid is not less than 99.999%, nitrogen is blown into the 1600 ℃ high-temperature aluminum liquid through a vent pipe orifice or a high-temperature resistant air brick arranged at the bottom or at the side edge of the reactor to form nitrogen bubbles, the nitrogen bubbles rise in the aluminum liquid, and the surface of the nitrogen bubbles reacts with the high-temperature aluminum liquid in the rising process to form an aluminum nitride film with the thickness of 0.1-0.3 mu m on the periphery of the nitrogen bubbles; the supply amount of nitrogen is 100L/min; the purity of the nitrogen is not less than 99.99%;
s3, the nitrogen bubbles in the S2 burst, so that an aluminum nitride film on the surface of the nitrogen bubbles is crushed into nano aluminum nitride powder with the average particle size of 0.1-0.6 mu m, the oxygen content is lower than 0.5%, and the purity is higher than 99.5%, the nitrogen and the nano aluminum nitride powder are cooled in a radiator, then are separated by a gas-powder separator to obtain high-purity nano aluminum nitride powder and nitrogen, the separated nitrogen enters a nitrogen tank through a booster pump for subsequent nitrogen bubble reaction, and the separated high-purity nano aluminum nitride powder enters a powder collector for collection.
Wherein: the heat-resistant and heat-insulating material of the reactor lining in the preparation method is a graphite material.
In the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reactor, and the scattered aluminum nitride powder and unreacted nitrogen enter the radiator through an outlet at the top end.
The temperature of the radiator area in the preparation method is not higher than 300 ℃.
The cooling mode in the preparation method can be an air cooling mode.
Example 6
The preparation method of the high-purity nano aluminum nitride powder specifically comprises the following steps:
s1, heating aluminum particles through a silicon-molybdenum rod to obtain 850 ℃ high-temperature aluminum liquid, adding the prepared nitrogen into a nitrogen tank through a nitrogen making machine for storage, and performing nitrogen charging and air discharging operation on a reaction furnace;
s2, adding 850 ℃ high-temperature aluminum liquid into a reaction furnace through a pipeline, wherein the purity of the aluminum liquid is not less than 99.999%, nitrogen is blown into the 850 ℃ high-temperature aluminum liquid through a ventilation pipe orifice or a high-temperature resistant ventilation brick arranged at the bottom or at the side edge of the reactor to form nitrogen bubbles, the nitrogen bubbles rise in the aluminum liquid, and the surface of the nitrogen bubbles reacts with the high-temperature aluminum liquid in the rising process to form an aluminum nitride film with the thickness of 0.1-0.3 mu m on the periphery of the nitrogen bubbles; the supply amount of nitrogen is 600L/min; the purity of the nitrogen is not less than 99.99%;
s3, the nitrogen bubbles in the S2 burst, so that an aluminum nitride film on the surface of the nitrogen bubbles is crushed into nano aluminum nitride powder with the average particle size of 0.1-0.6 mu m, the oxygen content is lower than 0.5%, and the purity is higher than 99.5%, the nitrogen and the nano aluminum nitride powder are cooled in a radiator, then are separated by a gas-powder separator to obtain high-purity nano aluminum nitride powder and nitrogen, the separated nitrogen enters a nitrogen tank through a booster pump for subsequent nitrogen bubble reaction, and the separated high-purity nano aluminum nitride powder enters a powder collector for collection.
Wherein: the heat-resistant and heat-insulating material of the reactor lining in the preparation method is corundum.
In the preparation method, positive pressure is kept above the liquid level of the aluminum liquid in the reactor, and the scattered aluminum nitride powder and unreacted nitrogen enter the radiator through an outlet at the top end.
The temperature of the radiator area in the preparation method is not higher than 300 ℃.
The cooling mode in the preparation method can be a liquid cooling mode.
In the scheme, the aluminum nitride powder synthesized by the method has high purity (more than 99.5 percent), uniform particle size of nano-scale powder, high sphericity, no agglomeration, continuous production, high yield, quick output and low cost.
According to the invention, the aluminum nitride film is obtained by reacting the high-temperature aluminum liquid with the nitrogen bubbles, so that the technical problems of insufficient reaction, high nitrogen consumption and low utilization rate in the existing gasification reaction of aluminum gas and nitrogen are avoided, and the technical problems of more reaction steps, high industrial control difficulty, high cost and incapability of continuous production in the technical scheme of calcining nitrogen after preparing the precursor by using the hydrothermal reaction are solved.
According to the invention, the nano aluminum nitride powder which drifts in the nitrogen can be obtained by crushing the aluminum nitride film, and even if the aluminum nitride powder is doped with impurities of aluminum powder, nitridation reaction can occur in the process of discharging the aluminum nitride film and the nitrogen, so that the utilization rate of aluminum liquid is very high, and continuous production can be realized.
The nitrogen and the nano aluminum nitride powder are cooled, then the high-purity nano aluminum nitride powder and the nitrogen are obtained through separation, and the separated nitrogen is used for nitrogen bubble reaction; therefore, the nitrogen can be fully utilized, the nitrogen consumption is reduced, the utilization rate is improved, the production cost is reduced, and the method is beneficial to industrial mass production and popularization and use.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (5)
1. The preparation method is characterized in that an aluminum nitride film is obtained by reacting 850-1600 ℃ high-temperature aluminum liquid with nitrogen bubbles, the aluminum nitride film is crushed to obtain nano aluminum nitride powder which drifts in nitrogen, the nitrogen and the nano aluminum nitride powder are cooled, then the high-purity nano aluminum nitride powder and the nitrogen are separated, and the separated nitrogen is used for nitrogen bubble reaction;
the nitrogen bubbles are formed by introducing nitrogen of high-temperature aluminum liquid, the nitrogen introduced into the high-temperature aluminum liquid comprises nitrogen injection through a vent pipe orifice or a high-temperature resistant air brick arranged at the bottom or at the side of the reactor, and the supply amount of the nitrogen is 100-600L/min; the purity of the nitrogen is not less than 99.99%;
the thickness of the aluminum nitride film is 0.1-0.3 mu m;
the grain size of the high-purity nanometer aluminum nitride powder is 0.1-0.6 mu m, the oxygen content is lower than 0.5%, and the purity of the aluminum nitride is more than 99.5%.
2. The method for preparing high purity nano aluminum nitride powder according to claim 1, wherein the reaction in the preparation method is performed in a reactor filled with nitrogen gas while evacuating air.
3. The method for preparing high-purity nano aluminum nitride powder according to claim 2, wherein the high-temperature aluminum liquid in the preparation method enters an evacuated air-filled nitrogen-filled reactor through an aluminum liquid supply pipeline; the purity of the aluminum liquid is not less than 99.999 percent.
4. The method for preparing high purity nano aluminum nitride powder according to claim 2, wherein the reactor lining in the preparation method is a heat-resistant and heat-insulating material.
5. The method for preparing high-purity nano aluminum nitride powder according to claim 1, wherein the reaction between 850-1600 ℃ high-temperature aluminum liquid and nitrogen bubbles in the preparation method requires heating, and the preparation method of 850-1600 ℃ high-temperature aluminum liquid comprises electric furnace heating, tungsten-molybdenum heating or silicon-molybdenum rod heating.
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