CN109467064A - A kind of preparation method of densification pattern aluminium nitride powder - Google Patents
A kind of preparation method of densification pattern aluminium nitride powder Download PDFInfo
- Publication number
- CN109467064A CN109467064A CN201710799396.4A CN201710799396A CN109467064A CN 109467064 A CN109467064 A CN 109467064A CN 201710799396 A CN201710799396 A CN 201710799396A CN 109467064 A CN109467064 A CN 109467064A
- Authority
- CN
- China
- Prior art keywords
- aluminium nitride
- nitride powder
- preparation
- fine
- pattern
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
Abstract
The present invention relates to inorganic non-metallic Preparation Technique of Powders fields, and in particular to a kind of preparation method of densification pattern aluminium nitride powder.Specific steps are as follows: aluminium powder, diluent are uniformly mixed according to a certain percentage, is put into graphite Noah's ark with a small amount of additive and carries out nitridation reaction in vacuum sintering furnace, nitriding temperature is 800~1500 DEG C.The aluminium nitride powder nitrogenized completely is pressed, then carries out high-temperature process to optimize pattern, obtains the aluminium nitride powder of fine and close pattern.Big partial size, particle densification aluminium nitride powder, the thermal coefficient of heat-conducting glue, heat-conducting silicone grease etc. can be significantly improved as filler, in field of radiating such as high power device, circuit substrate, LED heat dissipation, heat producing devices with huge application prospect.
Description
Technical field
The invention belongs to inorganic non-metallic Preparation Technique of Powders fields, and in particular to a kind of densification pattern aluminium nitride powder
Preparation method.
Background technique
As electronic product gradually tends to micromation, densification, high performance, operating ambient temperature also tends to high temperature
Direction is developed.Data shows that electronic component temperature is every and increases 2 DEG C, and reliability just declines 10%, therefore heat dissipation problem is high collection
At one of the key factor of degree electronic device.The thermal conductivity such as common silica gel are poor, generally only 0.2W/mK or so.Height is led
Hot filler is filled into organic polymer heat-conducting glue, is a kind of economic and effective mode for improving silica gel thermal conductivity.In order to protect
The insulation performance of heat-conducting glue is demonstrate,proved, generally using metal oxide or metal nitride as heat filling.Al2O3It is most common
Heat filling, but it is limited to the thermal conductivity raising of heat-conducting glue, can no longer meet the integrated requirement of density.BN price is more expensive,
Higher cost is not suitable for industrialized production.And the theoretical conductivity of AlN is up to 320W/mK, is Al2O3Nearly 10 times, it is practical
Thermal coefficient can also be Al2O35~8 times.Furthermore AlN has excellent insulating properties, low thermal expansion coefficient, high machinery strong
The advantages that spending, is nontoxic, is the preferred material of heat-conducting glue high thermal conductivity filler.
As the AlN powder of filler, generally require partial size between 4~30 μm, pattern is spherical or compacted particulate
Pattern.Aluminium powder direct nitridation method is a kind of common method of industrially prepared aluminium nitride powder, but this method has some disadvantages just
It is low yield, powder agglomeration easy to reunite etc..This is because nitridation reaction temperature is greater than the fusing point of aluminium powder, and aluminium powder nitridation reaction is
The heat of exothermic reaction, releasing easily melts aluminum particle, so that the diffusion of nitrogen be hindered to cause reaction incomplete.Meanwhile
The nitration case formed after aluminum particle is surfaces nitrided can also prevent nitrogen from spreading to granular center.It is general that NH is added4Cl and KCl makees
For additive, the complete nitridation of aluminium powder can be effectively facilitated.But NH4The addition of Cl easily forms the patterns such as loose porous, needle-shaped, these
The powder of pattern is not easy to form effective thermally conductive network chain as heat filling, and the thermal conductivity for influencing finished product even influences heat-conducting glue
Preparation process.
Summary of the invention
The present invention is to solve above-mentioned technical problem, and the aluminum nitride powder of fine and close pattern is obtained by the way of secondary heat treatment
Body.Specific step are as follows:
(1) mixing: aluminium powder, diluent are uniformly mixed according to a certain percentage；
(2) nitridation reaction: above-mentioned mixed raw material and a small amount of additive being put into graphite Noah's ark, are placed in vacuum sintering furnace, led to
Enter nitrogen and keeps the temperature 0.5~5h progress nitridation reaction at a temperature of 800~1500 DEG C；
(3) high-temperature process: by the above-mentioned aluminium nitride powder compression moulding nitrogenized completely, then carrying out high-temperature process to optimize pattern,
Obtain the aluminium nitride powder of fine and close pattern.
Further, diluent described in step (1) is AlN powder, accounts for the 0~50% of aluminium powder quality, mixing method is dry
It is mixed.
Further, the preferred NH of additive described in step (2)4Cl, additive amount are the 1~20% of Al+AlN gross mass.
Further, aluminium nitride powder briquetting pressure described in step (3) is 50~200MPa, and high-temperature process temperature is
1550~2000 DEG C, nitrogen protection is passed through in whole process always.
Further, meso-position radius is 3~15 μm after the fine and close pattern aluminium nitride ball milling of gained described in step (3), and pattern is
Compacted particulate.
Beneficial effects of the present invention: by the way of first nitrogenizing and being heat-treated afterwards, make nitridation process and topography optimization process point
It opens, is heat-treated aluminium nitride under a large pressure, it is more effective for the densification of aluminium nitride powder particle.The big partial size of gained, particle cause
Close aluminium nitride powder can be used as high thermal conductivity filler and be filled into the high-molecular organic materials such as heat-conducting glue, heat-conducting silicone grease, greatly
The thermal conductivity for improving heat-conducting glue has huge in field of radiating such as high power device, circuit substrate, LED heat dissipation, heat producing devices
Application prospect.
Detailed description of the invention
Fig. 1 is the SEM shape appearance figure of the aluminium nitride powder obtained using the preparation method of this patent.
Specific embodiment
Embodiment 1
The AlN of high-purity Al powder and 45wt% is dry-mixed uniformly, with 15% NH of Al and AlN total amount4Cl is put into togerther graphite Noah's ark
In, it is placed in vacuum sintering furnace, is passed through nitrogen in 1300 DEG C of nitridation 2h.After obtained AlN block sample broke ball milling 60MPa at
Type places into 1800 DEG C of heat treatment 1h, entire heat treatment process in vacuum sintering furnace and is passed through nitrogen protection always, after being crushed ball milling
Obtained aluminium nitride powder partial size is big, particle is fine and close, is the preferred material of heat-conducting glue filler.
Embodiment 2
The AlN of high-purity Al powder and 30wt% is dry-mixed uniformly, with 10% NH of Al and AlN total amount4Cl is put into togerther graphite Noah's ark
In, it is placed in vacuum sintering furnace, is passed through nitrogen in 1100 DEG C of nitridation 2h.After obtained AlN block sample broke ball milling 60MPa at
Type places into 1750 DEG C of heat treatment 2h, entire heat treatment process in vacuum sintering furnace and is passed through nitrogen protection always, after being crushed ball milling
Obtained aluminium nitride powder partial size is big, particle is fine and close, is the preferred material of heat-conducting glue filler.
Claims (7)
1. a kind of preparation method of densification pattern aluminium nitride powder, feature the following steps are included:
(1) mixing: aluminium powder, diluent are uniformly mixed according to a certain percentage；
(2) nitridation reaction: above-mentioned mixed raw material and a small amount of additive being put into graphite Noah's ark, are placed in vacuum sintering furnace, led to
Enter nitrogen and keeps the temperature 0.5~5h progress nitridation reaction at a temperature of 800~1500 DEG C；
(3) high-temperature process: by the above-mentioned aluminium nitride powder compression moulding nitrogenized completely, then carrying out high-temperature process to optimize pattern,
Obtain the aluminium nitride powder of fine and close pattern.
2. a kind of preparation method of fine and close pattern aluminium nitride powder according to claim 1, which is characterized in that the step
(1) diluent is AlN powder in, accounts for the 0~50% of aluminium powder quality.
3. a kind of preparation method of fine and close pattern aluminium nitride powder according to claim 1, which is characterized in that the step
(1) mixing method is dry-mixed in.
4. a kind of preparation method of fine and close pattern aluminium nitride powder according to claim 1, which is characterized in that the step
(2) the preferred NH of additive in4Cl, additive amount are the 1~20% of Al+AlN gross mass.
5. a kind of preparation method of fine and close pattern aluminium nitride powder according to claim 1, which is characterized in that the step
(3) aluminium nitride powder briquetting pressure is 50~200MPa in.
6. a kind of preparation method of fine and close pattern aluminium nitride powder according to claim 1, which is characterized in that the step
(3) high temperature treatment temperature is 1550~2000 DEG C, is carried out under nitrogen protection atmosphere always in whole process.
7. a kind of preparation method of fine and close pattern aluminium nitride powder according to claim 1, which is characterized in that the step
(3) meso-position radius is 3~15 μm after the fine and close pattern aluminium nitride ball milling of gained in, and pattern is compacted particulate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710799396.4A CN109467064A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation method of densification pattern aluminium nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710799396.4A CN109467064A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation method of densification pattern aluminium nitride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109467064A true CN109467064A (en) | 2019-03-15 |
Family
ID=65657969
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710799396.4A Pending CN109467064A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation method of densification pattern aluminium nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109467064A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5728635A (en) * | 1995-08-03 | 1998-03-17 | Ngk Insulators, Ltd. | Aluminum nitride sintered bodies |
| US5908795A (en) * | 1994-06-30 | 1999-06-01 | Nkk Corporation | Boron nitride containing material |
| CN101269979A (en) * | 2007-03-23 | 2008-09-24 | 中国科学院理化技术研究所 | Method for synthesizing ultra-fine aluminum nitride powder with combustion |
| CN103588182A (en) * | 2013-10-16 | 2014-02-19 | 西安交通大学 | Method for preparing spherical aluminum nitride powder |
| CN105837224A (en) * | 2016-05-31 | 2016-08-10 | 武汉理工大学 | Method for preparing aluminum nitride ceramics by aid of ammonium fluoride which is used as additive |
-
2017
- 2017-09-07 CN CN201710799396.4A patent/CN109467064A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5908795A (en) * | 1994-06-30 | 1999-06-01 | Nkk Corporation | Boron nitride containing material |
| US5728635A (en) * | 1995-08-03 | 1998-03-17 | Ngk Insulators, Ltd. | Aluminum nitride sintered bodies |
| CN101269979A (en) * | 2007-03-23 | 2008-09-24 | 中国科学院理化技术研究所 | Method for synthesizing ultra-fine aluminum nitride powder with combustion |
| CN103588182A (en) * | 2013-10-16 | 2014-02-19 | 西安交通大学 | Method for preparing spherical aluminum nitride powder |
| CN105837224A (en) * | 2016-05-31 | 2016-08-10 | 武汉理工大学 | Method for preparing aluminum nitride ceramics by aid of ammonium fluoride which is used as additive |
Non-Patent Citations (2)
| Title |
|---|
| 王杰等: "氮化铝陶瓷粉体制备方法研究进展及展望", 《硅酸盐通报》 * |
| 郑锐等: "AlN低温烧结助剂的研究现状", 《稀有金属材料与工程》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI610884B (en) | Aluminum nitride powder | |
| JP7362151B2 (en) | High-purity, low-aluminum spherical β-silicon nitride powder, its manufacturing method and applications | |
| CN104058772A (en) | Ceramic composite material substrate and manufacturing technology thereof | |
| CN101321713A (en) | Carbon containing material | |
| CN109133927A (en) | A kind of short flow process of high performance graphite material | |
| CN103981382A (en) | Preparation method of high heat-conducting diamond/copper-based composite material | |
| CN103343266B (en) | High-thermal-conductivity graphite-high silicon aluminium-based composite material and preparation process for same | |
| CN103979507A (en) | Method for preparing spherical aluminum nitride powder under assistance of high atmospheric pressure and fluoride additive | |
| CN104909765A (en) | Method for rapidly preparing high-performance Si3N4 ceramic ball at low cost | |
| CN110104620B (en) | Method for preparing aluminum nitride nano powder by using sol-gel method | |
| CN101734923A (en) | Aluminum nitride porous ceramic and preparation method thereof | |
| CN107903069A (en) | Aluminium nitride powder and preparation method thereof | |
| CN112479630A (en) | Ceramic composite heat dissipation device and preparation method thereof | |
| CN108191434A (en) | A kind of high heat conductance, the high-voltage high-speed preparation method of high compactness silicon nitride material | |
| CN103966533B (en) | A kind of diamond heat-conducting composite and preparation method thereof | |
| JP5877684B2 (en) | Method for producing aluminum nitride sintered granules | |
| CN112028636A (en) | Preparation method of high-thermal-conductivity aluminum nitride/graphene composite ceramic device | |
| CN105884372B (en) | Organic network method synthesizes AlN ceramic powder method | |
| Wu et al. | Novel in-situ constructing approach for vertically aligned AlN skeleton and its thermal conductivity enhancement effect on epoxy | |
| CN107604192B (en) | A kind of preparation method of aluminium nitride/aluminium composite material | |
| CN108002354A (en) | A kind of preparation method of the spherical aluminium nitride powder of size tunable | |
| CN109467064A (en) | A kind of preparation method of densification pattern aluminium nitride powder | |
| CN109659281A (en) | A kind of high thermal conductivity electronic packaging composite material and preparation method thereof | |
| CN102515781A (en) | Preparation method for silicon carbide preform based on water-based adhesive | |
| US10138127B2 (en) | Method of fabricating silicon carbide powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190315 |