CN113443611B - Preparation method of nitride powder - Google Patents
Preparation method of nitride powder Download PDFInfo
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- CN113443611B CN113443611B CN202110837186.6A CN202110837186A CN113443611B CN 113443611 B CN113443611 B CN 113443611B CN 202110837186 A CN202110837186 A CN 202110837186A CN 113443611 B CN113443611 B CN 113443611B
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
Abstract
The invention discloses a preparation method of nitride powder, relating to the technical field of heat-conducting inorganic powder, comprising the following steps: (1) preparing a precursor; (2) and (4) decarburization treatment. The invention utilizes the mutual contact between molecules formed by the nitrogen-containing resin and the aluminum sol or the silica sol, and the nitrogen element can directly realize the contact reaction with the aluminum element or the silicon element, thereby improving the generation rate of the aluminum nitride or the silicon nitride, shortening the reaction time and preparing the silicon nitride powder or the composite powder of the two.
Description
The technical field is as follows:
the invention relates to the technical field of heat-conducting inorganic powder, in particular to a preparation method of nitride powder.
Background art:
nitrogen has a high electronegativity and is capable of forming a series of nitrides with many elements having a lower electronegativity than nitrogen. The nitride powder is widely applied to the fields of cutting materials, high-temperature structural materials, luminescent materials, electrode materials, catalytic materials, superconducting materials, wave-absorbing materials, adsorbing materials and the like. Among them, aluminum nitride has the advantages of good chemical stability and thermal stability, high thermal conductivity (theoretical value 320W/mK), high mechanical strength, thermal expansion coefficient close to that of silicon, easy compatibility with other semiconductor materials, extremely low insulation, and the like, and has important application in the heat dissipation field of electronic components and optical devices.
At present, the synthesis methods of aluminum nitride powder mainly comprise: (1) direct nitridation method; (2) al (Al)2O3Carbothermic reduction; (3) high temperature self-propagating method; (4) aerosol method; (5) plasma synthesis method. Wherein, Al2O3The carbothermic process has achieved commercial production. However, in the nitriding process, the nitride layer generated on the surface prevents nitrogen from penetrating the interface from outside to inside, so that the reaction of nitrogen and aluminum element is difficult, the reaction time is long, and the nitriding temperature is high.
By retrieval, chinese patent application No. 201910488968.6 discloses a method for preparing high purity aluminum nitride powder, which comprises mixing alumina with carbon powders of different particle sizes, then carrying out high temperature calcination of aluminum nitride in nitrogen atmosphere, and promoting the contact of nitrogen and alumina by increasing the gaps between powders, but this improved method still cannot avoid the obstruction of nitride layer, still consumes a long time, and needs 8-15 hours.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a method for preparing nitride powder, which has low preparation temperature and less time consumption, and the obtained aluminum nitride powder has high purity.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for preparing nitride powder comprises the following steps:
(1) preparing a precursor: uniformly mixing the sol and the aqueous nitrogenous resin, placing the obtained mixed solution in an oven for heating and curing, and performing ball milling and crushing on the cured mixture to obtain mixed powder; then placing the mixed powder into a high-temperature graphite furnace, and carrying out nitriding treatment in a flowing nitrogen atmosphere;
(2) and (3) decarburization treatment: and (2) placing the nitriding product obtained in the step (1) in an air atmosphere for decarburization treatment to obtain nitride powder.
The mass ratio of the sol to the solid components contained in the aqueous nitrogen-containing resin is 1 (8-45).
The sol is one or a mixture of two of aluminum-containing sol and silicon-containing sol.
The aluminum-containing sol includes, but is not limited to, at least one of aluminum sol and aluminum hydroxide sol.
Preferably, the aluminum-containing sol is an aluminum sol.
The silica-containing sol is silica sol.
The aqueous nitrogen-containing resin comprises at least one of, but is not limited to, aqueous polyurethane, aqueous urea-formaldehyde resin and aqueous melamine resin.
Preferably, the aqueous nitrogen-containing resin is aqueous polyurethane.
Preferably, the aqueous polyurethane is an anionic aqueous polyurethane. When the surface charge of the aqueous nitrogen-containing resin is opposite to that of the sol, the interaction at the molecular level can be realized with the cationic sol.
The temperature of heating and curing is 100-300 ℃.
The nitrogen flow rate of the nitriding treatment is 1-5L/min, the nitriding temperature is 1400-1600 ℃, and the nitriding time is 1-4 h.
The decarburization temperature of the decarburization treatment is 500-600 ℃, and the decarburization time is 1-4 h.
The invention has the beneficial effects that:
1. the invention utilizes the mutual contact between molecules formed by the nitrogen-containing resin and the aluminum sol or the silica sol, and the nitrogen element can directly realize the contact reaction with the aluminum element or the silicon element, thereby improving the generation rate of the aluminum nitride or the silicon nitride, shortening the reaction time and preparing the silicon nitride powder or the composite powder of the two.
2. Another reason why the present invention can achieve the shortening of the reaction time may be that gas generated by the internal reaction expands, the compactness of the nitrided layer can be destroyed, external nitrogen can rapidly react with aluminum element or silicon element, and the purity of the obtained aluminum nitride or silicon nitride is high.
3. The invention adopts the mixture of substances with opposite charges, so that the contact is tighter, the nitridation rate is improved, and the nitridation reaction time is shortened.
Description of the drawings:
FIG. 1 is the XRD analysis of the product of example 1;
FIG. 2 is the XRD analysis of the product of example 2;
FIG. 3 is the result of XRD analysis of the product of example 3;
FIG. 4 is the XRD analysis of the product of example 4;
FIG. 5 is the XRD analysis of the product of example 5;
FIG. 6 is the XRD analysis of the product of example 6;
FIG. 7 is the XRD analysis of the product of example 7;
FIG. 8 is the XRD analysis of the product of example 8;
FIG. 9 is the XRD analysis of the product of example 9;
FIG. 10 is the XRD analysis of the product of example 10;
figure 11 is the XRD analysis of the product of example 11.
The specific implementation mode is as follows:
in order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below by combining the specific drawings and the embodiments.
Aluminum sol: the purity is more than 99.95 percent, the grain diameter of colloidal particles is 100nm, and the solid content is 20 percent.
Silica sol: the purity is more than 99.95 percent, the grain diameter of colloidal particles is 20nm, and the solid content is 20 percent.
Anionic waterborne polyurethane: viscosity 50 mPas, solid content 35%.
Cationic waterborne polyurethane: viscosity 50 mPas, solid content 35%.
Aqueous urea-formaldehyde resin: viscosity 60 mPas, solid content 60%.
Aqueous melamine resin: viscosity 60 mPas, solid content 60%.
Example 1
(1) 10g of aluminum sol and 250g of anionic waterborne polyurethane are uniformly mixed to form uniform mixed liquid. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 4L/min. And (3) heating the high-temperature graphite furnace for 5.5 hours from room temperature to 1600 ℃, and preserving heat at 1600 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product aluminum nitride powder shows that the product has no diffraction peak of other phases and is a pure aluminum nitride product. The content of aluminum oxynitride is 0.6% by the test of a nitrogen-oxygen analyzer.
Example 2
(1) 10g of aluminum sol and 200g of anionic waterborne polyurethane are uniformly mixed to form a uniform mixed solution. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 200 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 4L/min. And (3) heating the high-temperature graphite furnace for 5.5 hours from room temperature to 1600 ℃, and preserving heat at 1600 ℃ for 3 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product aluminum nitride powder shows that the product has no diffraction peak of other phases and is a pure aluminum nitride product. The oxygen content in the aluminum nitride is 0.7 percent through the test of a nitrogen-oxygen analyzer.
Example 3
(1) 10g of aluminum sol and 180g of anionic waterborne polyurethane are uniformly mixed to form uniform mixed liquid. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 200 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 3L/min. And (3) heating the high-temperature graphite furnace for 5 hours from room temperature to 1500 ℃, and preserving heat at 1500 ℃ for 2 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product aluminum nitride powder shows that the product has no diffraction peak of other phases and is a pure aluminum nitride product. The aluminum nitride oxygen content was found to be 0.8%.
Example 4
(1) 10g of aluminum sol and 250g of anionic waterborne polyurethane are uniformly mixed to form uniform mixed solution. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing argon is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the flow speed of the argon is 4L/min. And (3) heating the high-temperature graphite furnace for 5.5 hours from room temperature to 1600 ℃, and preserving heat at 1600 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
XRD analysis of the product aluminum nitride powder shows that argon is introduced to replace nitrogen during nitriding treatment, and the product contains aluminum nitride signals, which indicates that polyurethane participates in nitriding reaction.
Example 5
(1) 10g of the aluminum sol was dehydrated in an atmosphere of 250 ℃ to obtain 2g of a solid aluminum compound. 250g of anionic waterborne polyurethane is dehydrated in an environment of 250 ℃ to obtain 87.5g of solid polyurethane compound. 2g of solid aluminum compound and 87.5g of solid polyurethane compound are subjected to ball milling and crushing to obtain uniform mixed powder, and the uniform mixed powder is placed in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 4L/min. And (3) heating the high-temperature graphite furnace for 5.5 hours from room temperature to 1600 ℃, and preserving heat at 1600 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
XRD analysis of the product aluminum nitride powder shows that the product is not completely converted into aluminum nitride and has partial aluminum oxide impurity. The oxygen content in the aluminum nitride is 8.1 percent through the test of a nitrogen-oxygen analyzer. The solid-solid mixing mode is not as good as the liquid phase mixing effect, so that the oxygen content in the aluminum nitride after the nitridation reaction is high.
Example 6
(1) 10g of aluminum sol and 250g of cationic waterborne polyurethane are uniformly mixed to form uniform mixed liquid. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the flow rate of the nitrogen is 4L/min. And (3) heating the high-temperature graphite furnace for 5.5 hours from room temperature to 1600 ℃, and preserving heat at 1600 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product at 600 ℃ in an air environment for 3 h.
XRD analysis of the product aluminum nitride powder shows that the product is not completely converted into aluminum nitride and has partial aluminum oxide impurity. The content of aluminum nitride oxide is 0.6 percent by the test of a nitrogen-oxygen analyzer. The anionic waterborne polyurethane is better than the cationic waterborne polyurethane in the preparation of the aluminum nitride.
Example 7
(1) 10g of alumina sol and 90g of aqueous urea-formaldehyde resin are uniformly mixed to form a uniform mixed solution. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 4L/min. And (3) heating the high-temperature graphite furnace for 5.5 hours from room temperature to 1600 ℃, and preserving heat at 1600 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product aluminum nitride powder shows that the product has no diffraction peak of other phases and is a pure aluminum nitride product. The content of aluminum nitride oxide is 1.2% by the test of a nitrogen-oxygen analyzer.
Example 8
(1) 10g of aluminum sol and 90g of aqueous melamine resin were uniformly mixed to form a uniform mixed solution. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 4L/min. And (3) heating the high-temperature graphite furnace for 5.5 hours from room temperature to 1600 ℃, and preserving heat at 1600 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product aluminum nitride powder shows that the product has no diffraction peak of other phases and is a pure aluminum nitride product. The content of aluminum nitride oxide is 1.4% by the test of a nitrogen-oxygen analyzer.
Example 9
(1) 10g of silica sol and 250g of anionic waterborne polyurethane are uniformly mixed to form uniform mixed liquid. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 4L/min. And (3) heating the high-temperature graphite furnace for 5 hours from room temperature to 1500 ℃, and preserving heat at 1500 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product silicon nitride powder shows that the product has no diffraction peak of other phases and is a pure silicon nitride product. The content of silicon nitride oxide is 1.6% by the test of a nitrogen-oxygen analyzer.
Example 10
(1) 10g of silica sol and 90g of aqueous urea-formaldehyde resin are uniformly mixed to form a uniform mixed solution. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the flow rate of the nitrogen is 4L/min. And (3) heating the high-temperature graphite furnace for 5 hours from room temperature to 1500 ℃, and preserving heat at 1500 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product silicon nitride powder shows that the product has no diffraction peak of other phases and is a pure silicon nitride product. The content of silicon nitride oxide is 1.7% by the test of a nitrogen-oxygen analyzer.
Example 11
(1) 10g of silica sol and 90g of aqueous melamine resin are uniformly mixed to form a uniform mixed solution. And (3) placing the mixed solution in an oven for heating and curing, wherein the curing temperature is 250 ℃. And ball-milling and crushing the solidified mixture to obtain uniform mixed powder, and placing the uniform mixed powder in a high-temperature graphite furnace. Flowing nitrogen is introduced into the high-temperature graphite furnace to exhaust the air in the furnace, and the nitrogen flow rate is 4L/min. And (3) heating the high-temperature graphite furnace for 5 hours from room temperature to 1500 ℃, and preserving heat at 1500 ℃ for 4 hours.
(2) And (3) decarburizing the nitrified product in an air environment at 600 ℃, wherein the decarburizing time is 2 h.
The XRD analysis of the product silicon nitride powder shows that the product has no diffraction peak of other phases and is a pure silicon nitride product. The content of silicon nitride oxide is 1.9% by the test of a nitrogen-oxygen analyzer.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The preparation method of the nitride powder is characterized by comprising the following steps:
(1) preparing a precursor: uniformly mixing the sol and the aqueous nitrogenous resin, placing the obtained mixed solution in an oven for heating and curing, and performing ball milling and crushing on the cured mixture to obtain mixed powder; then placing the mixed powder into a high-temperature graphite furnace, and carrying out nitriding treatment in a flowing nitrogen atmosphere;
(2) and (3) decarburization treatment: placing the nitriding product obtained in the step (1) in an air atmosphere for decarburization treatment to obtain nitride powder;
the sol is one or a mixture of two of aluminum-containing sol and silicon-containing sol;
the water-based nitrogen-containing resin comprises at least one of water-based polyurethane, water-based urea-formaldehyde resin and water-based melamine resin.
2. The method for preparing a nitride powder according to claim 1, wherein: the mass ratio of the sol to the solid components contained in the aqueous nitrogen-containing resin is 1 (8-45).
3. The method for preparing a nitride powder according to claim 1, wherein: the aluminum-containing sol includes, but is not limited to, at least one of aluminum sol and aluminum hydroxide sol.
4. The method for preparing a nitride powder according to claim 1, wherein: the silica-containing sol is silica sol.
5. The method for preparing a nitride powder according to claim 1, wherein: the waterborne polyurethane is anionic waterborne polyurethane.
6. The method for preparing a nitride powder according to claim 1, wherein: the temperature of heating and curing is 100-300 ℃.
7. The method for preparing a nitride powder according to claim 1, wherein: the nitrogen flow rate of the nitriding treatment is 1-5L/min, the nitriding temperature is 1400-1600 ℃, and the nitriding time is 1-4 h.
8. The method for preparing a nitride powder according to claim 1, wherein: the decarburization temperature of the decarburization treatment is 500-600 ℃, and the decarburization time is 1-4 h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63139008A (en) * | 1986-11-28 | 1988-06-10 | Kawasaki Steel Corp | Production of powdery aluminum nitride |
| CN109437918A (en) * | 2018-12-07 | 2019-03-08 | 中国电子科技集团公司第四十三研究所 | A kind of aluminium nitride powder and its preparation method and application |
| CN110104620A (en) * | 2019-05-24 | 2019-08-09 | 安徽壹石通材料科技股份有限公司 | A method of aluminum nitride nanometer powder is prepared using sol-gel method |
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| CN103539088B (en) * | 2013-11-05 | 2015-10-07 | 河北工业大学 | A kind of synthetic method of aluminum nitride nanometer particle |
| TWI548591B (en) * | 2015-03-06 | 2016-09-11 | Nat Inst Chung Shan Science & Technology | An atmosphere - controlled method for the preparation of aluminum nitride powder by carbothermal reduction |
| TWI579231B (en) * | 2016-05-20 | 2017-04-21 | 國家中山科學研究院 | A method for preparing spherical aln granules |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63139008A (en) * | 1986-11-28 | 1988-06-10 | Kawasaki Steel Corp | Production of powdery aluminum nitride |
| CN109437918A (en) * | 2018-12-07 | 2019-03-08 | 中国电子科技集团公司第四十三研究所 | A kind of aluminium nitride powder and its preparation method and application |
| CN110104620A (en) * | 2019-05-24 | 2019-08-09 | 安徽壹石通材料科技股份有限公司 | A method of aluminum nitride nanometer powder is prepared using sol-gel method |
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