CN1194959A - Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis - Google Patents
Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis Download PDFInfo
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- CN1194959A CN1194959A CN98100685A CN98100685A CN1194959A CN 1194959 A CN1194959 A CN 1194959A CN 98100685 A CN98100685 A CN 98100685A CN 98100685 A CN98100685 A CN 98100685A CN 1194959 A CN1194959 A CN 1194959A
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Abstract
A self-spreading process for high-temp synthesis of high-purity superfine AlN powder (ceramic powder) uses such raw materials (Wt.%) as Al powder (25-33), AlN powder (66-74) and NH4Cl (0.5-1.9) and includes such technological steps as proportional mixing, loading in graphite container with aluminium foil as liner, perforating with glass tube (the diameter of holes is 10-15 mm and the interval between holes is 10-20 mm), putting the container in reactor, vacuum pumping introducing nitrogen gas (5-15 MPa), and slight grinding, and features low reaction temp, full nitridation and less residual Cl ions.
Description
The invention belongs to the ceramic powder preparation field.Be particularly useful for making high pure and ultra-fine nitrogenize saw (AlN) ceramic powder.
The AlN pottery has excellent physical chemistry such as high thermal conductivity, high electric insulation, high strength, high rigidity and low thermal coefficient of expansion, more and more is subjected to the attention of material circle as important ceramic substrate and packaged material.And high pure and ultra-fine AlN powder is the basis of preparation high-performance AlN pottery.
The preparation method of AlN powder mainly contains four kinds: (1) Al
2O
3Carbothermic method; (2) Al powder direct nitridation method; (3) alkoxide process; (4) self propagating high temperature synthesis method.First three methods common shortcoming is that power consumption is serious, and the powder cost is higher.And self propagating high temperature synthesis method save energy, efficient is higher.But in the disclosed patent for preparing AlN with the self propagating high temperature synthesis method, all exist different limitation.Also wait " preparation method of nitride " (clear 64-76906) of invention to utilize liquid nitrogen to be nitrogenous source as Sea of Japan Tian Yi, the liquid nitrogen utilization ratio is low, and cost is higher, can not effectively remove the oxygen of sneaking in the reactor simultaneously, and the product oxygen level is higher.And " preparation method of aluminium nitride powder and powder constituent thing thereof " (flat 1-26494) of Japanese palace Ben Qinsheng etc. invention, be with the mixture of Al and AlN briquetting in advance, complex procedures, briquetting has only φ 11 * 15mm size simultaneously, and output is less.And the product behind the briquetting is difficult to be broken for ultrafine powder." self propagating high temperature synthesizes the preparation method of aluminium nitride powder " of inventions such as China's village Chinese is sharp (CN1142477A) overcome the shortcoming that preceding two kinds of methods exist substantially, but Al powder proportion is bigger in the reaction mass, temperature of reaction is higher, and the AlN particle of generation is bigger.The add-on of ammonium salt is too high simultaneously, reaches the 2-8% of Al and AlN mixture, makes residual Cl in the synthetic AlN finished product
-Or F
-More.In addition, owing to be subjected to the restriction of gas penetrating power, although on the wall of container of dress powder through hole is arranged, filling amount still seldom only reaches 200 * 400 * 30-40mm, can not satisfy industrial production requirement.
The objective of the invention is to propose a kind of method of utilizing the self propagating high temperature synthesis technique to prepare high pure and ultra-fine AlN powder efficiently.
According to purpose of the present invention, this preparation method's principle is the synthetic ratio juris of conventional self propagating high temperature, promptly lights starting material by the part, utilizes its exothermic heat of reaction to impel the adjacent reaction thing to participate in reaction, thereby guarantees that entire reaction carries out fully.
According to purpose of the present invention and principle, the production method that we proposed is:
(1) batching: adopt aluminium powder, aluminum nitride powder, NH
4Cl makes raw material, and its proportioning accounts for 25-33% for (weight %) Al powder, and the AlN powder accounts for 66-74%, NH
4Cl accounts for 0.5-1.9%, and wherein aluminium powder adopts and meets GB-2085-89 standard superfine aluminium power, and median size is 13 μ m, and aluminium nitride is the composite particles work in-process less than 10 μ m, NH
4Cl is commercially available pharmaceutical chemicals;
(2) mix, feed: above-mentioned three kinds of raw materials are mixed, the reactant pine of mixing is loaded in the crystal vessel of band aluminium foil liner, the shape of container is determined by the reactor cavity shape, the container that uses among the present invention is rectangle, size is 1000 * 200 * 200mm, get ventilating pit with the double glazing pipe in reaction mass then, its hole size is φ 10-15mm, is spaced apart φ 10-20mm;
(3) high pressure nitrogenize: the above-mentioned container that installs material reinstalled charge into 5-15Mpa nitrogen after vacuumizing in the high-pressure reactor, light reactant by wire energising heating, and by the water-cooling system cooling, reaction product is ground slightly after cleaning and is submicron order high pure and ultra-fine AlN finished product.
The inventive method compared with prior art has following characteristics:
1, thinner AlN proportion is bigger in the reaction mass, makes temperature of reaction lower, and the nitrogenize of Al powder is more complete, and the fluctuation of N content is less, and the AlN particle that generates is tiny, reaches submicron order.
2, it is less to add the amount of ammonia salt additives, is the 0.5-1.9wt% of total stuff amount only, has both played the promotion nitrogenization, makes Cl among the AlN of generation again
-Residual volume less, improve product purity.
3, get through pore rather than get through the hole on wall of container in reaction mass, it is abundant to help gas-permeable, guarantees that the nitrogenize of Al powder is complete.Simultaneously,, can make the reactant of at every turn packing into more, reach the suitability for industrialized production level owing to improved the gas-permeable condition.
Embodiment
The requirement of method produced according to the present invention, we prepare the material of five kinds of different ratio of components altogether, and concrete proportioning sees Table 1, pine behind the confected materials mixing is loaded in the container, and evenly puts into reactor after the punching with Glass tubing, charges into 5-15MpaN after vacuumizing
2Gas is lighted the water-cooling system cooling of back by reactor with the wire energising.Clean out surperficial volatile matter after the product cooling, grinding a little just is high pure and ultra-fine ALN finished product, and its performance perameter sees Table 2.
Reactant ratio in table 1 embodiment of the invention (weight percent)
| The sequence number composition | ??1 | ?2 | ?3 | ?4 | ?5 |
| ?Al | ?26 | ?28 | ?30 | ?32 | ?32 |
| ?AlN | ?73.5 | ?71.2 | ?69 | ?66.8 | ?66.5 |
| ?NH 4Cl | ?0.5 | ?0.8 | ?1 | ?1.2 | ?1.5 |
AlN end properties parameter in table 2 embodiment of the invention
| The parameter sequence number | ???N | ???O | ???Fe | ?Cl - | ??C | ?d 50(μm) |
| 1 | ?33.5 | ?0.20 | ????0.06 | ?0.010 | ?0.009 | ???0.42 |
| ?2 | ?33.6 | ?0.15 | ????0.05 | ?0.010 | ?0.008 | ???0.50 |
| ?3 | ?33.4 | ?0.13 | ????0.05 | ?0.009 | ?0.008 | ???0.46 |
| ?4 | ?33.3 | ?0.17 | ????0.04 | ?0.008 | ?0.009 | ???0.52 |
| ?5 | ?33.4 | ?0.19 | ????0.05 | ?0.010 | ?0.007 | ???0.50 |
Claims (1)
1. the preparation method of a high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis comprises batching, mixing, high pressure nitrogenize, it is characterized in that:
(1) batching: adopt aluminium powder, aluminum nitride powder, NH
4Cl makes raw material, and its proportioning accounts for 25-33% for (weight %) Al powder, and the AlN powder accounts for 66-74%, NH
4Cl accounts for 0.5-1.9%;
(2) mix, feed: above-mentioned three kinds of raw materials are mixed, the reactant pine of mixing is packed into be with in the crystal vessel of aluminium foil liner, get ventilating pit with the double glazing pipe in reaction mass then, its hole size is φ 10-15mm, is spaced apart φ 10-20mm;
(3) high pressure nitrogenize: the above-mentioned container that installs material reinstalled charges into 5-15Mpa nitrogen after vacuumizing in the high-pressure reactor, light reactant by wire energising heating, reaction product after cleaning slightly mill be submicron order high pure and ultra-fine AlN finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98100685A CN1065845C (en) | 1998-03-09 | 1998-03-09 | Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98100685A CN1065845C (en) | 1998-03-09 | 1998-03-09 | Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1194959A true CN1194959A (en) | 1998-10-07 |
| CN1065845C CN1065845C (en) | 2001-05-16 |
Family
ID=5216178
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98100685A Expired - Fee Related CN1065845C (en) | 1998-03-09 | 1998-03-09 | Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis |
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| CN (1) | CN1065845C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100372804C (en) * | 2006-07-28 | 2008-03-05 | 北京科技大学 | Method of self propagating reaction sinterad Si3N4BN complex phase processable ceramic |
| CN100379679C (en) * | 2003-05-09 | 2008-04-09 | 株式会社茨木研究所 | Process for producing aluminium nitrid and aluminium nitrid |
| CN101269979B (en) * | 2007-03-23 | 2011-01-12 | 中国科学院理化技术研究所 | Method for synthesizing superfine aluminium nitride powder by combustion |
| CN112390653A (en) * | 2020-11-16 | 2021-02-23 | 中国工程物理研究院材料研究所 | Method for preparing ceramic powder based on freezing casting molding |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100464904C (en) * | 2007-06-01 | 2009-03-04 | 北京科技大学 | Method for preparing Al/AlN electronic package material |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6476906A (en) * | 1987-09-18 | 1989-03-23 | Nat Res Inst Metals | Production of nitride |
| JPH01264914A (en) * | 1988-04-14 | 1989-10-23 | Univ Osaka | Production of aluminum nitride powder and powder composition |
| CN1057063C (en) * | 1995-08-04 | 2000-10-04 | 中国科学院上海硅酸盐研究所 | Process for producing aluminum nitride powders by self diffusion process at high temperature |
| RU2091300C1 (en) * | 1996-03-27 | 1997-09-27 | Институт структурной макрокинетики РАН | Method of producing aluminium nitride |
-
1998
- 1998-03-09 CN CN98100685A patent/CN1065845C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100379679C (en) * | 2003-05-09 | 2008-04-09 | 株式会社茨木研究所 | Process for producing aluminium nitrid and aluminium nitrid |
| CN100372804C (en) * | 2006-07-28 | 2008-03-05 | 北京科技大学 | Method of self propagating reaction sinterad Si3N4BN complex phase processable ceramic |
| CN101269979B (en) * | 2007-03-23 | 2011-01-12 | 中国科学院理化技术研究所 | Method for synthesizing superfine aluminium nitride powder by combustion |
| CN112390653A (en) * | 2020-11-16 | 2021-02-23 | 中国工程物理研究院材料研究所 | Method for preparing ceramic powder based on freezing casting molding |
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|---|---|
| CN1065845C (en) | 2001-05-16 |
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Owner name: ANTAI SCIENCE AND TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: GENERAL RESEARCH INST. OF IRON AND STEEL, MINISTRY OF METALLURGICAL INDUSTRY Effective date: 20070914 |
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Assignee: Beijing Gang Yan Diamond Products Company Assignor: Antai Science and Technology Co., Ltd. Contract fulfillment period: 2007.12.15 to 2013.12.15 contract change Contract record no.: 2008990001251 Denomination of invention: Process for preparing high-purity superfine aluminium nitride powder by self-spreading high-temp synthesis Granted publication date: 20010315 License type: Exclusive license Record date: 20081121 |
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