CN110577198A - Method for removing crushed small particles in aluminum nitride powder - Google Patents
Method for removing crushed small particles in aluminum nitride powder Download PDFInfo
- Publication number
- CN110577198A CN110577198A CN201810592462.5A CN201810592462A CN110577198A CN 110577198 A CN110577198 A CN 110577198A CN 201810592462 A CN201810592462 A CN 201810592462A CN 110577198 A CN110577198 A CN 110577198A
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- Prior art keywords
- aluminum nitride
- nitride powder
- temperature
- powder
- small particles
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Classifications
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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
- C01B21/0722—Preparation by direct nitridation of aluminium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention relates to the technical field of preparation of inorganic nonmetal powder, in particular to a method for removing broken small particles in aluminum nitride powder. The concrete measures are as follows: mixing aluminum powder and a diluent according to a certain proportion, putting the mixture into a high-temperature sintering furnace, heating the mixture to 900 ℃ in nitrogen, carrying out a nitriding reaction, then continuously heating the mixture to the high temperature, and taking certain temperature control measures to obtain the aluminum nitride powder with the D50 of 3-5 mu m. The aluminum nitride powder with the grain diameter of 3-5 mu m and compact grains is filled into the heat-conducting glue as a high-heat-conducting inorganic filler, can greatly improve the heat conductivity coefficient of the heat-conducting glue, and is very suitable for the direction of high-power devices.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic nonmetal powder, in particular to a method for removing broken small particles in aluminum nitride powder.
Background
With the rapid development of science and technology, components of circuit boards tend to be developed in the direction of smaller size, stronger function and more compact arrangement, and the heat dissipation problem becomes one of the keys. The high temperature can cause the resistivity of the material to be increased, the working efficiency of the component is reduced, and the service life is shortened. At present, the heat conducting sheet, the heat conducting glue and the like are the most common heat conducting technologies for effectively radiating heat of electronic components. The heat-conducting glue can achieve the purpose of bonding, conduct heat and simultaneously be insulating. However, with the great improvement of the integration level of electronic components, the requirement on heat dissipation is higher and higher, and the alumina commonly used in the heat-conducting adhesive can not meet the requirements on heat dissipation with high power and high integration level. The aluminum nitride is an inorganic nonmetal powder, has a plurality of excellent performances such as high thermal conductivity, low thermal expansion coefficient, high strength, wear resistance, corrosion resistance, no toxicity, excellent insulating property and the like, and is an optimal material for the inorganic filler of the heat-conducting adhesive.
the heat conductive adhesive is prepared by filling a certain amount of aluminum nitride powder into an organic polymer material, and forming effective heat conductive network chains through aluminum nitride particles to improve the heat conductivity of the heat conductive adhesive. Therefore, the key point for improving the heat conductivity coefficient is to form the effective heat conduction network chain, and the properties of the aluminum nitride powder for forming the effective heat conduction network chain include particle size, morphology, purity and the like. Generally, the grain diameter is required to be more than or equal to 3 mu m, the grains are compact, and the purity is more than 99 percent. The aluminum nitride powder has a proper amount of small crushed particles, which is beneficial to filling gaps among large particles, establishing an auxiliary heat conduction path and increasing the heat conductivity. When too many small particles are broken, the small particles can prop open the large particles, so that the density of the system is reduced; meanwhile, the small particles have higher specific surface area, so that the viscosity of the system is increased, the filling amount is low, and the heat conductivity coefficient is finally reduced. Therefore, the control of the proportion of the crushed small particles in the aluminum nitride powder is crucial to effectively improving the heat conductivity coefficient of the heat-conducting glue.
Disclosure of Invention
In order to solve the defects in the technology, the invention analyzes the aluminum powder nitriding mechanism, and adopts a certain temperature control measure, so that excessive broken small particles in the aluminum nitride powder can be effectively removed when the aluminum nitride is prepared by an aluminum powder nitriding method. The adopted specific scheme is as follows: mixing aluminum powder and a diluent according to a certain proportion, putting the mixture into a high-temperature sintering furnace, heating the mixture to 900 ℃ in nitrogen, carrying out a nitriding reaction, then continuously heating the mixture to the high temperature, and taking certain temperature control measures to obtain the aluminum nitride powder with the D50 of 3-5 mu m.
furthermore, the diluent is high-purity aluminum nitride powder with small particle size, and the weight ratio of the aluminum nitride to the aluminum powder is (0.1-0.5): 1.
Further, the heat preservation time of the low-temperature section at 900 ℃ is 0.5-4 h.
Further, the temperature control measures taken at high temperature are as follows: after the temperature is increased to 1300-1350 ℃, the temperature is slowly reduced to 1100-1200 ℃, and the temperature is kept for 1-4 h.
Further, a rapid heating rate is adopted from room temperature to 900 ℃.
The invention has the beneficial effects that: (1) the small broken particles in the aluminum nitride powder are effectively removed through temperature control, the filling amount of the aluminum nitride powder in the heat-conducting glue is increased, and the heat conductivity coefficient is greatly increased. (2) The highest temperature is controlled below 1350 ℃, and the preparation cost is low.
Drawings
FIG. 1 is a diagram showing the morphology of aluminum nitride powder prepared by the method of the present invention.
Detailed Description
In the case of the example 1, the following examples are given,
The aluminum powder and the diluent are uniformly mixed according to the weight ratio of 1:0.1, put into a high-temperature sintering furnace, and quickly heated to 900 ℃ in nitrogen for heat preservation for 1h to carry out nitridation reaction. Then the temperature is increased to 1315 ℃, then the temperature is slowly decreased to 1150 ℃, and the temperature is kept for 1h at 1150 ℃, thus obtaining the aluminum nitride powder with the D50 of 4.2 μm.
In the case of the example 2, the following examples are given,
The aluminum powder and the diluent are uniformly mixed according to the weight ratio of 1:0.1, put into a high-temperature sintering furnace, and quickly heated to 900 ℃ in nitrogen for heat preservation for 1.5h to carry out nitridation reaction. Then the temperature is slowly reduced to 1180 ℃ after being increased to 1330 ℃, and the temperature is kept at 1180 ℃ for 1h, thus obtaining the aluminum nitride powder with the D50 of 3.98 mu m.
Claims (6)
1. A method for removing broken small particles in aluminum nitride powder is characterized by mainly comprising the following steps: mixing aluminum powder and a diluent according to a certain proportion, putting the mixture into a high-temperature sintering furnace, heating the mixture to 900 ℃ in nitrogen, carrying out a nitriding reaction, then continuously heating the mixture to the high temperature, and taking certain temperature control measures to obtain the aluminum nitride powder with the D50 of 3-5 mu m.
2. The method of claim 1, wherein the diluent is a high purity small particle size aluminum nitride powder.
3. The method for removing the crushed small particles in the aluminum nitride powder as claimed in claim 2, wherein the weight ratio of the aluminum nitride to the aluminum powder is (0.1-0.5): 1.
4. The method for removing the crushed small particles in the aluminum nitride powder according to claim 1, wherein the heat preservation time of the low temperature section at 900 ℃ is 0.5-4 h.
5. The method for removing the crushed small particles in the aluminum nitride powder according to claim 1, wherein the temperature control measures taken at the high temperature are as follows: after the temperature is increased to 1300-1350 ℃, the temperature is slowly reduced to 1100-1200 ℃, and the temperature is kept for 1-4 h.
6. The method of claim 1, wherein the rapid ramp rate is used from room temperature to 900 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810592462.5A CN110577198A (en) | 2018-06-11 | 2018-06-11 | Method for removing crushed small particles in aluminum nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810592462.5A CN110577198A (en) | 2018-06-11 | 2018-06-11 | Method for removing crushed small particles in aluminum nitride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110577198A true CN110577198A (en) | 2019-12-17 |
Family
ID=68810316
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810592462.5A Withdrawn CN110577198A (en) | 2018-06-11 | 2018-06-11 | Method for removing crushed small particles in aluminum nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110577198A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030099590A1 (en) * | 2001-11-13 | 2003-05-29 | Ibaragi Laboratory Co., Ltd. | Process for producing aluminum nitride and aluminum nitride |
| CN105836717A (en) * | 2016-03-17 | 2016-08-10 | 宁夏艾森达新材料科技有限公司 | Preparation method of aluminum nitride electronic ceramic powder |
| CN107399973A (en) * | 2016-05-20 | 2017-11-28 | 河北高富氮化硅材料有限公司 | The technique that a kind of direct nitridation method prepares aluminium nitride powder |
| CN109095444A (en) * | 2017-11-21 | 2018-12-28 | 河北高富氮化硅材料有限公司 | A kind of broken short grained method in removal aluminium nitride powder |
-
2018
- 2018-06-11 CN CN201810592462.5A patent/CN110577198A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030099590A1 (en) * | 2001-11-13 | 2003-05-29 | Ibaragi Laboratory Co., Ltd. | Process for producing aluminum nitride and aluminum nitride |
| CN105836717A (en) * | 2016-03-17 | 2016-08-10 | 宁夏艾森达新材料科技有限公司 | Preparation method of aluminum nitride electronic ceramic powder |
| CN107399973A (en) * | 2016-05-20 | 2017-11-28 | 河北高富氮化硅材料有限公司 | The technique that a kind of direct nitridation method prepares aluminium nitride powder |
| CN109095444A (en) * | 2017-11-21 | 2018-12-28 | 河北高富氮化硅材料有限公司 | A kind of broken short grained method in removal aluminium nitride powder |
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| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20191217 |
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| WW01 | Invention patent application withdrawn after publication |