CN1456495A - Method for preparing aluminium nitrides and nitrogen oxides by combustion synthesis - Google Patents
Method for preparing aluminium nitrides and nitrogen oxides by combustion synthesis Download PDFInfo
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Abstract
A process for preparing the nitride and hydroxide of aluminium from Al or Al-alloy powder includes such steps as proportionally adding aluminium nitride or some oxide as diluent, burning in vertical reaction furnace at 800-1900 deg.C and under 0.11-3.0 MPa for nitrogen gas pressure, cooling, and grinding under the protection of nitrogen gas.
Description
Background
Common preparation methods of aluminum nitride (AlN) include a direct nitriding method, a carbothermic method, avapor deposition method, a self-propagating combustion synthesis method, and the like. Wherein, the self-propagating combustion synthesis method has been developed rapidly in recent years, which makes full use of the characteristic that aluminum powder is directly nitrified into strong exothermic reaction, and uses Al and N after the aluminum powder is ignited in nitrogen2The heat generated by the chemical reaction between them causes the reaction to propagate automatically in the form of a combustion wave, forming AlN. The reaction is based on the formula The reaction temperature is generally between 800 and 1200 ℃; metallic aluminiumMelting at 660 ℃ and reacting with N at about 800 ℃2Carrying out reaction; AlN starts to decompose at about 2200 c, above which the reverse reaction of the above reaction is already very pronounced.
In U.S. Pat. No. 4877759, Holt et al propose a method for preparing AlN by a self-propagating high-temperature combustion synthesis method, wherein the nitrogen pressure required for the high-temperature combustion synthesis reaction is 500 to 1000atm or more. In U.S. Pat. No. 4988645, Holt et al, which utilizes metallic aluminum powder and 100MPa of nitrogen pressure for self-propagating high temperature combustion to synthesize AlN, the combustion synthesis method should be carried out at adiabatic temperature under a pressure equal to or greater than the decomposition nitrogen pressure of the final product, AlN requires a nitrogen pressure of at least 14 MPa. In U.S. Pat. No. 6482384B 1, Shyan-Lung Chung et al invented a self-propagating combustion synthesis method, in which AlN is prepared by a process comprising: loosely loading metal aluminum powder into graphite crucible, pumping 0.1 torr (1.3X 10) in reactor-5MPa) and then charged with N at a pressure of 200 torr (1.027MPa)2Gas, N is filled from the bottom of the graphite crucible2The tungsten filament is used for igniting and burning reaction, and the main component of the product is AlN and contains a small amount of Al. In the Chinese patent with application No. 00120742.3, Korean Happy et al use aluminum powder, AlN aluminum powder and NH4Mixing the raw materials in proportion, and synthesizing by self-propagating combustion, wherein the pressure of the used nitrogen is required to be 5-15 MPa. In the Chinese patent application No. 01129219.9, Chenkexin et al use aluminum powder, diluent, additive and solid nitriding agent to perform combustion synthesis reaction to prepare AlN, wherein the pressure of nitrogen is 1-4.5 MPa. The AlN preparation method has strict operation process, once ignited and combusted, the nitridation reaction is difficult to control, and the defects of high nitridation pressure, complex process, difficult complete nitridation reaction, discontinuous production, low yield, strict requirements on equipment and the like exist in different degrees.
In U.S. Pat. No. 5649278, Dunmead et al invented a method for synthesizing AlN by self-propagating combustion under low nitrogen pressure, in which AlN is synthesized by mixing aluminum powder with a diluent AlN and then self-propagating combustion under nitrogen pressure of 0.075 to 3MPa (preferably 0.09 to 0.12MPa) in a closed container. However, the method still has the defects of strict operation process, difficult control of nitridation reaction once ignited and combusted, complex process, difficult complete nitridation reaction, discontinuous production, low yield and the like.
In the Chinese patent application No. 02158760.4, Sunjunling et al invented a vertical combustion synthesis reaction furnace, which realizes continuous large-scale combustion synthesis of silicon nitride and silicon iron nitride under the low nitrogen pressure of 0.07 MPa-0.6 MPa.
Disclosure of Invention
The invention aims to: provides a method for synthesizing aluminum nitride and oxynitride by intermittent and continuous large-scale combustion in low-pressure nitrogen by using a vertical combustion synthesis reaction furnace.
The invention takes a vertical combustion synthesis reaction furnace as main equipment, takes metal aluminum powder or aluminum alloy powder as raw material, and mixes aluminum nitride or certain oxides and other diluents in proportion to prepare a batch, and in the vertical combustion synthesis reaction furnace, the amount of the batch added and the nitrogen pressure are controlled to be 0.11-3 MPa, and continuous or discontinuous combustion synthesis is carried out at 800-1900 ℃. The products after combustion synthesis are naturally cooled or forcibly cooled to form honeycomb loose structure block-shaped finished products, then crushed into particle size materials by a crusher, and then made into powder by a ball mill, a vibration mill or other grinding equipment, and in order to prevent hydration, nitrogen can be used as protective gas for sealing operation in the crushing or grinding process. The above-mentioned granular material and powder can be directly used or can be used after having been treated by making water-proofing coating, and its treatment agent can be aluminium dihydrogen phosphate, oxalic acid and silicic acid, etc.
The vertical combustion synthesis reactor of the present invention is described in chinese patent application No. 02158760.4. The structure of the device mainly comprises a material bin, a gate valve, a quantitative feeder, a distributor, a reaction container, a refractory material lining, an observation window door, a supporting structure and a temperature measuring instrument. The upper part of the main structure is provided with a material bin, a gate valve, a quantitative feeder and a distributor from top to bottom, and the main structure is a reaction container and is supported by a supporting structure. The reaction vessel is cylindrical, the periphery of the reaction vessel is provided with an observation window door, a temperature measuring instrument is arranged on one side of the reaction vessel, the inner layer and the outer layer of the reaction vessel form a sandwich structure, the outer layer is provided with a nitrogen inlet, the sandwich layer is a nitrogen air flue, the inner layer is provided with a certain number of holes, the side wall of the inner layer is made of refractory materials, and the refractory materials can be clay bricks, high-alumina bricks or other refractory materials.
In the raw materials, the metal aluminum powder refers to the metal aluminum powder with the purity generally higher than 97.0%, preferably higher than 98.5% or more preferably higher than 99.0%; the aluminum alloy powder is the alloy powder with the mass fraction of Al being more than or equal to 75%, the alloy elements can be Li and alkaline earth metal elements, Y and series metal elements and 1-3 types of other elements, and more specifically: la, Ti, Y, Cr, Ni, W, Mo, Zr, Hf, Na, Zn, K, Ca and the like.
The fineness of the raw material is 10-500 μm, preferably 10-125 μm, and most preferably 20-88 μm.
The diluent is aluminum nitride or oxide or their mixture, and the oxide is Al2O3、SiO2、ZrO2、MgO、TiO2、Y2O3、Cr2O3Alkaline earth metal elements such as CaO, and metal oxides of -series metal elements, and these oxides are actually raw materials. For example: using Al or aluminum alloy to burn and synthesize AlN, wherein the diluent is AlN; with Al and Al2O3Combustion synthesis of AlON or AlN and Al2O3Composite material with Al as diluent2O3(ii) a Al is used for combustion to synthesize a composite AlN product, and one or more oxides can be used as a diluent.
The low-pressure nitrogen is nitrogen pressure of 0.11-3 MPa, preferably 0.11-1.0 MPa, and most preferably 0.11-0.6 MPa.
The method comprises the following specific steps:
1. preparing raw materials: preparation of fine powders of the raw material particle size may be prepared using ball mills, barrel mills, pendulum mills, vibratory mills, jet mills or other milling equipment.
2. Preparing a batch: the materials need to be added with a diluent, the mixing ratio of the diluent to the raw materials is 95-20: 5-80, the preferred range is 80-40: 20-60 according to the mass of 100, and then the materials are mixed by a mixer, and the mixing time is 4-40 minutes according to the type of the mixer.
Or adding the diluent into the raw materials before grinding, and mixing and grinding in a ball mill, a cylinder mill, a vibration mill or other mills to obtain the batch.
The batch is sent into a material bin of the vertical combustion synthesis reaction furnace by lifting and conveying equipment.
3. Preheating: in order to ignite the batch materials for combustion synthesis, the temperature in the vertical combustion synthesis reaction furnace or the rotary kiln reaction vessel is preheated, and the preheating temperature can reach 800-1400 ℃ by using a common method, such as a fuel oil, coke burning or wood burning method. Meanwhile, nitrogen generally needs to be preheated before entering the reaction vessel, the preheating temperature is 25-550 ℃, and the optimal preheating temperature is 200-400 ℃.
4. Nitriding and burning: the measured batch materials are continuously and uniformly put into the reaction container through the material bin, the gate valve, the constant feeder and the distributor, and the batch materials are uniformly dispersed and scattered into the reaction container in order to ensure that batch material particles are fully contacted with nitrogen. The reaction vessel is filled with nitrogen, once the batch materials pass through the introduced preheated nitrogen with measured quantity, the batch materials are subjected to nitriding combustion reaction in the process of continuously descending in the reactor, reaction products continuously fall into the lower part or the lower side of the vessel to gradually form a honeycomb loose structure, and then the honeycomb loose structure is naturally cooled or artificially and forcibly cooled to form a finished product.
5. Temperature control: the combustion temperature in the reaction vessel is controlled between 800 ℃ and 1900 ℃ by changing the amount of the added batch materials.
6. The product is as follows: the products after combustion synthesis are naturally cooled or forcibly cooled to form honeycomb loose structure block-shaped finished products, then crushed into particle size materials by a crusher, and then made into powder by a ball mill, a vibration mill or other grinding equipment. In order to prevent hydration, nitrogen can be used as protective gas for sealing operation in the crushing or grinding process. The above-mentioned granular material and powder can be directly used or can be used after having been treated by making water-proofing coating, and its treatment agent can be aluminium dihydrogen phosphate, oxalic acid and silicic acid, etc.
The invention has the advantages that: the vertical combustion synthesis reaction furnace is utilized to realize the nitridation combustion synthesis in low-pressure nitrogen, and the batch is continuously scattered through the constant feeder, so that the continuous feeding and the continuous nitridation combustion synthesis can be realized, and the large-scale continuous production of aluminum nitride and nitrogen oxide is realized.
Detailed Description
Example 1: aluminum powder and AlN powder are prepared into a batch with the granularity less than or equal to 88 mu m according to the steps 1 and 2 in a ratio of 40: 60, and the batch is conveyed into a material bin by conveying equipment. Coke and wood are piled up at the bottom of the vertical combustion synthesis reaction furnace, the wood and the coke are ignited after being piled up in the reaction vessel, and when the temperature in the reaction vessel reaches 1100 ℃, nitrogen enters the reaction vessel after being preheated by the interlayer of the reaction vessel. Meanwhile, the batch materials are uniformly scattered into the reaction container through a gate valve, a constant feeder and a distributor, the combustion synthesis reaction is carried out, the reaction temperature is controlled at 1200 ℃, the nitrogen pressure in the reaction container is controlled at-0.19 MPa, and the reactants fall under the reaction container under the action of gravity, so that the aluminum nitride product with the cellular loose block structure is finally obtained.
Example 2: al, Ca and Y are mixed with AlN powder in the ratio of 86 to 10 to 4 and 60 to 40 according to the steps 1 and 2 to prepare a batch material with the granularity of less than or equal to 88 mu m, and the batch material is conveyed into a material bin by conveying equipment. Coke and wood are piled up at the bottom of the vertical combustion synthesis reaction furnace, the wood and the coke are ignited after being piled up in the reaction vessel, and when the temperature in the reaction vessel reaches 1100 ℃, nitrogen enters the reaction vessel after being preheated by the interlayer of the reaction vessel. Meanwhile, the batch materials are uniformly scattered into the reaction container through a gate valve, a quantitative feeder and a distributor, the combustion synthesis reaction is carried out, the reaction temperature is controlled to be 1200 ℃, the nitrogen pressure in the reaction container is controlled to be 0.19MPa, the reactants fall under the reaction container under the action of gravity, and finally the composite AlN product with the cellular loose block structure is obtained.
Example 3: aluminum powder and Al2O3The powder is mixed according to the proportion of 20: 80 and the steps 1 and 2 into the mixture with the granularity less than or equal to 88 mu mAnd mixing materials, and conveying the materials into a material bin by conveying equipment. Coke and wood are piled up at the bottom of the vertical combustion synthesis reaction furnace, the wood and the coke are ignited after being piled up in the reaction vessel, and when the temperature in the reaction vessel reaches 1100 ℃, nitrogen enters the reaction vessel after being preheated by the interlayer of the reaction vessel. Meanwhile, the batch materials are uniformly scattered into the reaction container through a gate valve, a constant feeder and a distributor, the combustion synthesis reaction is carried out, the reaction temperature is controlled to be 1750 ℃, the nitrogen pressure in the reaction container is controlled to be 0.19MPa, the reactants fall under the reaction container under the action of gravity, and finally the AlON product in the cellular loose block structure is obtained.
Example 4: AlN and Al were obtained by controlling the reaction temperature at 1400 ℃ in example 32O3And (3) compounding a product.
Example 5: al in example 42O3By TiO2Alternatively, AlN and TiO can be obtained2And (3) compounding a product.
Claims (6)
1. A method for preparing aluminum nitride and oxynitride by combustion synthesis is characterized in that:
a. the metal aluminum powder or aluminum alloy powder is used as a raw material, a diluent is added according to a proportion to prepare a batch, the batch is calculated according to 100 mass, the diluent is 95-20: 5-80, the particle size of the raw material is less than or equal to 500 mu m, the mixing time is 4-40 minutes, the purity of the metal aluminum powder is higher than 97.0%, and the diluent is aluminum nitride or oxide;
b. preheating the atmosphere in a reaction vessel of a vertical combustion synthesis reaction furnace in the vertical combustion synthesis reaction furnace to ensure that the preheating temperature reaches 800-1400 ℃, and preheating nitrogen before the nitrogen enters the reaction vessel, wherein the preheating temperature is between 25 and 550 ℃;
c. controlling the amount of the batch materials added into the vertical combustion synthesis reaction furnace, controlling the nitrogen pressure in the furnace to be 0.11-1.0 MPa, and performing combustion synthesis at 800-1900 ℃;
d. naturally cooling or forcibly cooling the combustion synthesis product, and then preparing the product into powder by a ball mill and a vibration mill.
2. The combustion synthesis process for producing aluminum nitrides and oxynitrides as claimed in claim 1, wherein: in the raw materials, the purity of the metal aluminum powder is high, and more than 98.5 percent of metal powder is preferentially selected; the granularity of the raw materials is preferably selected to be between 20 and 88 mu m; the preferential selection range of the mixing ratio of the diluent to the raw materials is 95-20: 5-80, the aluminum alloy powder refers to alloy powder with the mass fraction of Al being more than or equal to 75%, and the alloy elements can be 1-3 of Li and alkaline earth metal elements, La, Ti, Y, Cr, Ni, W, Mo, Zr, Hf, Na, Zn, K and Ca, Y and series metal elements; the oxide means: al (Al)2O3、SiO2、ZrO2、MgO、TiO2、Y2O3、Cr2O3CaO alkaline earth metal element, and series metal element oxide.
3. The method for preparing aluminum nitride and oxynitride by combustion synthesis as claimed in claim 1 or 2, wherein the optimal range of the mixing ratio of the diluent to the raw material is 0-40: 20-60.
4. The method for synthesizing silicon nitride or silicon iron nitride by low-pressure combustion as claimed in claim 1 or 2, wherein the atmosphere in the reaction vessel of the vertical combustion synthesis reactor is preheated by using fuel oil, coke or wood; the preferred temperature ranges for preheating the nitrogen prior to entry into the reaction vessel are: 200-400 ℃; the nitrogen pressure participating in the combustion reaction is preferably within the range of 0.11-1.0 MPa.
5. The combustion synthesis process for the preparation of aluminum nitrides and oxynitrides as claimed in claim 1 or 2, characterized in that: the optimum range of nitrogen pressure participating in the combustion reaction is: 0.11 to 0.6 MPa.
6. The method for preparing aluminum nitride and oxynitride by combustion synthesis as claimed in claim 1 or 2, wherein the combustion synthesis product aluminum nitride and its compound are crushed or ground and the nitrogen gas is used as a protective gas for sealing operation.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798071A (en) * | 2010-03-23 | 2010-08-11 | 西安交通大学 | Method for preparing aluminum nitride with three-dimensional sub-micron flower-like structure |
| CN102795606A (en) * | 2011-05-25 | 2012-11-28 | 华广光电股份有限公司 | Method for preparing aluminum nitride sheet |
| CN102874863A (en) * | 2012-10-24 | 2013-01-16 | 武汉大学 | Synthetic method for zinc oxide nano-particles |
| CN104609864A (en) * | 2015-02-11 | 2015-05-13 | 西安澳秦新材料有限公司 | Method for preparing bulk ceramic material from iron-silicon nitride powder |
| CN106365641A (en) * | 2016-08-23 | 2017-02-01 | 安徽科创中光科技有限公司 | Method for synthesizing silicon nitride and aluminum nitride at one time |
| CN106710770A (en) * | 2017-02-24 | 2017-05-24 | 赣南师范大学 | Preparation method of samarium-iron-nitrogen magnetic material |
| CN108975949A (en) * | 2018-08-31 | 2018-12-11 | 武汉科技大学 | One kind is based on foam in place AlON-AlN porous material and preparation method thereof |
| CN110182772A (en) * | 2019-06-10 | 2019-08-30 | 宁夏秦氏新材料有限公司 | The method of kiln process synthesis aluminium nitride |
| CN110204342A (en) * | 2019-06-10 | 2019-09-06 | 宁夏秦氏新材料有限公司 | The preparation method of decanter type self- propagating aluminium nitride |
| CN110282609A (en) * | 2019-06-10 | 2019-09-27 | 宁夏秦氏新材料有限公司 | Kiln process nitride self-propagating synthesis equipment |
| CN112723406A (en) * | 2021-01-07 | 2021-04-30 | 江苏智微新材料科技有限公司 | Device and method for quickly acquiring copper oxide powder special for semiconductor |
| CN113860879A (en) * | 2021-11-24 | 2021-12-31 | 江西理工大学 | Method for preparing aluminum nitride powder by suspension reduction |
| CN114655938A (en) * | 2022-05-23 | 2022-06-24 | 苏州锦艺新材料科技股份有限公司 | Preparation method of spherical aluminum nitride granulation powder and filler powder |
| CN115038665A (en) * | 2020-02-06 | 2022-09-09 | 株式会社德山 | Method for producing aluminum nitride powder, and package |
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2003
- 2003-06-04 CN CNB031405797A patent/CN1191194C/en not_active Expired - Fee Related
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798071A (en) * | 2010-03-23 | 2010-08-11 | 西安交通大学 | Method for preparing aluminum nitride with three-dimensional sub-micron flower-like structure |
| CN102795606A (en) * | 2011-05-25 | 2012-11-28 | 华广光电股份有限公司 | Method for preparing aluminum nitride sheet |
| CN102874863A (en) * | 2012-10-24 | 2013-01-16 | 武汉大学 | Synthetic method for zinc oxide nano-particles |
| CN102874863B (en) * | 2012-10-24 | 2014-05-07 | 武汉大学 | Synthetic method for zinc oxide nano-particles |
| CN104609864A (en) * | 2015-02-11 | 2015-05-13 | 西安澳秦新材料有限公司 | Method for preparing bulk ceramic material from iron-silicon nitride powder |
| CN104609864B (en) * | 2015-02-11 | 2016-09-14 | 西安澳秦新材料有限公司 | A kind of method utilizing ferro-silicon nitride powder to prepare block body ceramic material |
| CN106365641A (en) * | 2016-08-23 | 2017-02-01 | 安徽科创中光科技有限公司 | Method for synthesizing silicon nitride and aluminum nitride at one time |
| CN106710770B (en) * | 2017-02-24 | 2019-05-17 | 赣南师范大学 | A kind of preparation method of samarium iron nitrogen magnetic material |
| CN106710770A (en) * | 2017-02-24 | 2017-05-24 | 赣南师范大学 | Preparation method of samarium-iron-nitrogen magnetic material |
| CN108975949A (en) * | 2018-08-31 | 2018-12-11 | 武汉科技大学 | One kind is based on foam in place AlON-AlN porous material and preparation method thereof |
| CN108975949B (en) * | 2018-08-31 | 2021-01-15 | 武汉科技大学 | AlON-AlN porous material based on in-situ foaming and preparation method thereof |
| CN110182772A (en) * | 2019-06-10 | 2019-08-30 | 宁夏秦氏新材料有限公司 | The method of kiln process synthesis aluminium nitride |
| CN110204342A (en) * | 2019-06-10 | 2019-09-06 | 宁夏秦氏新材料有限公司 | The preparation method of decanter type self- propagating aluminium nitride |
| CN110282609A (en) * | 2019-06-10 | 2019-09-27 | 宁夏秦氏新材料有限公司 | Kiln process nitride self-propagating synthesis equipment |
| CN115038665A (en) * | 2020-02-06 | 2022-09-09 | 株式会社德山 | Method for producing aluminum nitride powder, and package |
| CN112723406A (en) * | 2021-01-07 | 2021-04-30 | 江苏智微新材料科技有限公司 | Device and method for quickly acquiring copper oxide powder special for semiconductor |
| CN113860879A (en) * | 2021-11-24 | 2021-12-31 | 江西理工大学 | Method for preparing aluminum nitride powder by suspension reduction |
| CN114655938A (en) * | 2022-05-23 | 2022-06-24 | 苏州锦艺新材料科技股份有限公司 | Preparation method of spherical aluminum nitride granulation powder and filler powder |
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