CN107604192A - A kind of preparation method of aluminium nitride/aluminium composite material - Google Patents
A kind of preparation method of aluminium nitride/aluminium composite material Download PDFInfo
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- CN107604192A CN107604192A CN201710741697.1A CN201710741697A CN107604192A CN 107604192 A CN107604192 A CN 107604192A CN 201710741697 A CN201710741697 A CN 201710741697A CN 107604192 A CN107604192 A CN 107604192A
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- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910017083 AlN Inorganic materials 0.000 title claims abstract description 72
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 25
- 239000004411 aluminium Substances 0.000 title claims abstract description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 75
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 19
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 19
- 229920001971 elastomer Polymers 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 19
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000005269 aluminizing Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000009768 microwave sintering Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Abstract
The invention belongs to the preparation field of electronic package material, specifically discloses a kind of preparation method of aluminium nitride/aluminium composite material.Phenol-formaldehyde resin powder is dissolved in absolute ethyl alcohol；AlN powder is added in resulting solution, 40 ~ 60 DEG C stir；By SiO2Airsetting rubber powder and Al powder are sequentially added in resulting solution, and 50 ~ 70 DEG C are continued to stir, until slurry is sticky can not stir untill；Slurry is dried, is granulated sieving, then gained granular powder is compressing, obtain base substrate；By the Al of certain mass2O3Plate is placed on base substrate, the h of reaction-sintered 1 ~ 2 at 900 ~ 1000 DEG C of vacuum, obtains AlN base substrates；By AlN base substrates at 900 ~ 1100 DEG C of vacuum the h of gaseous state aluminising 0.5 ~ 1, subsequent Temperature fall cooling, produce aluminium nitride/aluminium composite material.There is the present invention technique to be simple and convenient to operate the advantages that production cost is low, and properties of product are good, and AlN/Al composites possess good mechanical strength, heat conductivility and low thermal coefficient of expansion, in electronic package material direction by with larger application prospect.
Description
Technical field
The invention belongs to the preparation field of electronic package material, and in particular to a kind of preparation of aluminium nitride/aluminium composite material
Method.
Background technology
Aluminium nitride belongs to the compound of covalent key combination, is a kind of novel inorganic nonmetallic materials of high comprehensive performance.
Aluminium nitride has good heat conductivility, and excellent electrical insulation capability, relatively low dielectric constant and dielectric loss are non-toxic, with
Silicon has a series of good characteristics such as good matched coefficients of thermal expansion.Aluminium nitride is acknowledged as highly integrated, super large of new generation
Power semiconductor substrate and the ideal material of electronic component encapsulation, receive the favor of domestic and international researcher.Aluminium nitride is led
Hot property is 8 ~ 10 times of aluminum oxide, and application potential in the electronics industry is very huge.In addition, aluminium nitride is also used as height
Level refractory material, crucible material, erosion shield, grinding-material and wear resistant parts etc..
Aluminium nitride belongs to covalent compound, and fusing point is high, and atom self-diffusion coefficient is small, and pure aluminum nitride powder is in common sintering
At a temperature of be difficult sintering densification, moreover, relatively low consistency makes aluminium nitride ceramics be difficult to have higher thermal conductivity, therefore
Seriously limit its application in electronic package material etc..In order to solve these problems, how aluminium nitride ceramics is improved
Consistency have become current study hotspot.The method for improving the consistency of aluminium nitride ceramics at present has：Hot pressed sintering,
SPS sintering, microwave sintering and infiltrated metal method etc..During using hot pressed sintering, the aluminium nitride ceramics of high-compactness can be obtained, but
It is to need expensive agglomerating plant, it is impossible to mass production, and production cost is higher.Although SPS sintering, microwave sintering can be fast
The aluminium nitride ceramics of higher-density is prepared fastly, and still, its shortcoming does not comply with industrialized production such as hot pressed sintering
Actual demand.At present, the aluminium nitride ceramics that infiltrated metal method prepares high-compactness is most potential to turn into industrialized production
Optimal selection.Infiltrated metal method is to penetrate into melting or gaseous metal in aluminium nitride precast body, aluminum-nitride-based so as to prepare
Composite ceramics, infiltrated metal are generally Al.But melting or gaseous Al and the relatively low wetability of aluminium nitride, it is difficult to prepare and cause
The higher aluminium nitride of density-aluminium ceramic matric composite, therefore limit its application in Electronic Packaging field.
The content of the invention
It is an object of the invention to provide a kind of preparation method of aluminium nitride/aluminium composite material, this method is by improving Al
With AlN wetability, so as to obtain high-compactness aluminium nitride/aluminium composite material, there is technique to be simple and convenient to operate, be produced into
The advantages that this is low, properties of product are good, makes AlN/Al composites possess good mechanical strength and heat conductivility, overcomes again
The defects of pure AlN is difficult to sintering densification.
To achieve the above object, the technical scheme that the present invention takes is as follows：
A kind of preparation method of aluminium nitride/aluminium composite material, step are as follows：
（1）, by phenol-formaldehyde resin powder（As adhesive）It is dissolved in absolute ethyl alcohol, the content for ensureing phenol-formaldehyde resin powder in solution is
3~5 wt%；
（2）, by the mass ratio of AlN powder and absolute ethyl alcohol be（1~1.2）: 1 meter, AlN powder is added into step（1）In resulting solution,
40 ~ 60 DEG C stir；
（3）, by SiO2Airsetting rubber powder and Al powder sequentially add step（2）In resulting solution, 50 ~ 70 DEG C are continued to stir, until slurry
Expect it is sticky can not stir untill；Wherein, SiO2The total amount of airsetting rubber powder and Al powder and the mass ratio of AlN powder are（0.04~0.08）∶
1, Al powder and SiO2The mass ratio of airsetting rubber powder is（0.6~0.9）∶1；
（4）, slurry dried, be granulated sieving, then gained granular powder is compressing, obtain base substrate；
（5）, by the Al of certain mass2O3Plate is placed on base substrate, the h of reaction-sintered 1 ~ 2 at 900 ~ 1000 DEG C of vacuum, is obtained
AlN base substrates；Wherein, Al2O3The quality of plate is can prevent base substrate from producing warpage during reaction-sintered to be defined；
（6）, by AlN base substrates at 900 ~ 1100 DEG C of vacuum the h of gaseous state aluminising 0.5 ~ 1, subsequent Temperature fall cooling, produce nitridation
Aluminium/aluminium composite material.
Preferably, the average grain diameter of the AlN powder is 5 ~ 10 μm.
Preferably, the SiO2The average grain diameter of airsetting rubber powder is 10 ~ 30 nm.
Preferably, the average grain diameter of the Al powder is 20 ~ 30 μm.
Preferably, the temperature of the drying is 70 ~ 80 DEG C.
Preferably, 60 ~ 100 mesh sieves are crossed.
Preferably, compressing Stress control is in 100 ~ 200 MPa.
The present invention provides a kind of preparation method of aluminium nitride/aluminium composite material, by improving Al and AlN wetabilitys, so as to
Aluminium nitride/aluminium composite material of high-compactness is obtained, its principle is：One layer of SiO is adsorbed in AlN particle surfaces2Airsetting rubber powder, very
Under empty 900 ~ 1000 DEG C of states, Al powder and SiO2Powder is reacted, and one layer of Al is generated in AlN particle surfaces2O3Film, Al2O3Have with Al
Good wetability, so as to during gaseous state aluminising, improve Al and AlN wetabilitys.The method has that technique is simple, operation
Conveniently, the advantages that production cost is low, properties of product are good, the AlN/Al composites of preparation possess good mechanical strength and led
Hot property, the defects of pure AlN is difficult to sintering densification is overcome again, before there is very big practicality in electronic package material field
Scape.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.It should be understood that following examples are merely to illustrate this
Invention is not for limitation the scope of the present invention.
Embodiment 1
A kind of preparation method of aluminium nitride/aluminium composite material, step are as follows：
（1）, phenol-formaldehyde resin powder is dissolved in absolute ethyl alcohol, the content for ensureing phenol-formaldehyde resin powder in solution is 3 wt%；
（2）, by the mass ratio of AlN powder (average grain diameter is 5 μm) and absolute ethyl alcohol be based on 1.2: 1, by AlN powder addition step（1）
In resulting solution, 40 DEG C stir；
（3）, by SiO2Airsetting rubber powder (average grain diameter is 10 nm) and Al powder (average grain diameter is 20 μm) sequentially add step（2）
In resulting solution, 50 DEG C are continued to stir, until slurry is sticky can not stir untill；Wherein, SiO2Airsetting rubber powder and Al powder it is total
Amount and the mass ratio of AlN powder are 0.08: 1, Al powder and SiO2The mass ratio of airsetting rubber powder is 0.6: 1；
（4）, by the drying of 70 DEG C of slurry, be granulated 100 mesh sieves, then gained granular powder is placed in mould, 200MPa is pressed into
Type, obtain base substrate；
（5）, by the Al of certain mass2O3Plate is placed on base substrate, the h of reaction-sintered 2 at 950 DEG C of vacuum, obtains AlN bases
Body；Wherein, Al2O3The quality of plate is can prevent base substrate from producing warpage during reaction-sintered to be defined；
（6）, AlN base substrates are put into aluminizing furnace, the h of gaseous state aluminising 0.5 at 1000 DEG C of vacuum, subsequent Temperature fall cooling,
Produce aluminium nitride/aluminium composite material.
The density of aluminium nitride/aluminium composite material made from the present embodiment is 3.12 g/cm3, thermal conductivity is 286 W/mK,
Thermal coefficient of expansion 12.0 × 10 is measured at 50 ~ 400 DEG C-6M/mK, bending strength are 230 MPa, fracture toughness 2.8
MPa·m1/2。
Embodiment 2
A kind of preparation method of aluminium nitride/aluminium composite material, step are as follows：
（1）, phenol-formaldehyde resin powder is dissolved in absolute ethyl alcohol, the content for ensureing phenol-formaldehyde resin powder in solution is 5 wt%；
（2）, by the mass ratio of AlN powder (average grain diameter is 10 μm) and absolute ethyl alcohol be based on 1: 1, by AlN powder addition step（1）
In resulting solution, 60 DEG C stir；
（3）, by SiO2Airsetting rubber powder (average grain diameter is 30 nm) and Al powder (average grain diameter is 30 μm) sequentially add step（2）
In resulting solution, 60 DEG C are continued to stir, until slurry is sticky can not stir untill；Wherein, SiO2Airsetting rubber powder and Al powder it is total
Amount and the mass ratio of AlN powder are 0.06: 1, Al powder and SiO2The mass ratio of airsetting rubber powder is 0.9: 1；
（4）, by the drying of 75 DEG C of slurry, be granulated 60 mesh sieves, then gained granular powder is placed in mould, 150MPa is compressing,
Obtain base substrate；
（5）, by the Al of certain mass2O3Plate is placed on base substrate, the h of reaction-sintered 1 at 900 DEG C of vacuum, obtains AlN bases
Body；Wherein, Al2O3The quality of plate is can prevent base substrate from producing warpage during reaction-sintered to be defined；
（6）, AlN base substrates are put into aluminizing furnace, the h of gaseous state aluminising 0.75 at 1100 DEG C of vacuum, subsequent Temperature fall cooling,
Produce aluminium nitride/aluminium composite material.
The density of aluminium nitride/aluminium composite material made from the present embodiment is 3.09 g/cm3, thermal conductivity is 265 W/mK,
Thermal coefficient of expansion 13.8 × 10 is measured at 50 ~ 400 DEG C-6M/mK, bending strength are 205 MPa, fracture toughness 3.4
MPa·m1/2。
Embodiment 3
A kind of preparation method of aluminium nitride/aluminium composite material, step are as follows：
（1）, phenol-formaldehyde resin powder is dissolved in absolute ethyl alcohol, the content for ensureing phenol-formaldehyde resin powder in solution is 4 wt%；
（2）, by the mass ratio of AlN powder (average grain diameter is 7.5 μm) and absolute ethyl alcohol be based on 1.1: 1, by AlN powder addition step
（1）In resulting solution, 50 DEG C stir；
（3）, by SiO2Airsetting rubber powder (average grain diameter is 20 nm) and Al powder (average grain diameter is 25 μm) sequentially add step（2）
In resulting solution, 60 DEG C are continued to stir, until slurry is sticky can not stir untill；Wherein, SiO2Airsetting rubber powder and Al powder it is total
Amount and the mass ratio of AlN powder are 0.04: 1, Al powder and SiO2The mass ratio of airsetting rubber powder is 0.75: 1；
（4）, by the drying of 80 DEG C of slurry, be granulated 80 mesh sieves, then gained granular powder is placed in mould, 100MPa is compressing,
Obtain base substrate；
（5）, by the Al of certain mass2O3Plate is placed on base substrate, the h of reaction-sintered 1.5 at 1000 DEG C of vacuum, obtains AlN
Base substrate；Wherein, Al2O3The quality of plate is can prevent base substrate from producing warpage during reaction-sintered to be defined；
（6）, AlN base substrates are put into aluminizing furnace, the h of gaseous state aluminising 1 at 950 DEG C of vacuum, subsequent Temperature fall cooling, produce
Aluminium nitride/aluminium composite material.
The density of aluminium nitride/aluminium composite material made from the present embodiment is 3.06 g/cm3, thermal conductivity is 165 W/mK,
Thermal coefficient of expansion 9.4 × 10 is measured at 50 ~ 400 DEG C-6M/mK, bending strength are 173 MPa, fracture toughness 2.1
MPa·m1/2。
Claims (7)
- A kind of 1. preparation method of aluminium nitride/aluminium composite material, it is characterised in that：Step is as follows：（1）, phenol-formaldehyde resin powder is dissolved in absolute ethyl alcohol, the content for ensureing phenol-formaldehyde resin powder in solution is 3 ~ 5 wt%；（2）, by the mass ratio of AlN powder and absolute ethyl alcohol be（1~1.2）: 1 meter, AlN powder is added into step（1）In resulting solution, 40 ~ 60 DEG C stir；（3）, by SiO2Airsetting rubber powder and Al powder sequentially add step（2）In resulting solution, 50 ~ 70 DEG C are continued to stir, until slurry Expect it is sticky can not stir untill；Wherein, SiO2The total amount of airsetting rubber powder and Al powder and the mass ratio of AlN powder are（0.04~0.08）∶ 1, Al powder and SiO2The mass ratio of airsetting rubber powder is（0.6~0.9）∶1；（4）, slurry dried, be granulated sieving, then gained granular powder is compressing, obtain base substrate；（5）, by the Al of certain mass2O3Plate is placed on base substrate, the h of reaction-sintered 1 ~ 2 at 900 ~ 1000 DEG C of vacuum, is obtained AlN base substrates；Wherein, Al2O3The quality of plate is can prevent base substrate from producing warpage during reaction-sintered to be defined；（6）, by AlN base substrates at 900 ~ 1100 DEG C of vacuum the h of gaseous state aluminising 0.5 ~ 1, subsequent Temperature fall cooling, produce nitridation Aluminium/aluminium composite material.
- 2. preparation method as claimed in claim 1, it is characterised in that：The average grain diameter of the AlN powder is 5 ~ 10 μm.
- 3. preparation method as claimed in claim 1, it is characterised in that：The SiO2The average grain diameter of airsetting rubber powder is 10 ~ 30 nm。
- 4. preparation method as claimed in claim 1, it is characterised in that：The average grain diameter of the Al powder is 20 ~ 30 μm.
- 5. preparation method as claimed in claim 1, it is characterised in that：The temperature of the drying is 70 ~ 80 DEG C.
- 6. preparation method as claimed in claim 1, it is characterised in that：Cross 60 ~ 100 mesh sieves.
- 7. preparation method as claimed in claim 1, it is characterised in that：Compressing Stress control is in 100 ~ 200 MPa.
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Cited By (3)
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| CN109518032A (en) * | 2019-01-15 | 2019-03-26 | 中南大学 | A kind of preparation method of carbon particle enhancing metal-base composites |
| CN110964967A (en) * | 2019-12-23 | 2020-04-07 | 有研亿金新材料有限公司 | Back plate with low thermal expansion coefficient and manufacturing method thereof |
| CN113150750A (en) * | 2020-03-20 | 2021-07-23 | 姜文辉 | Dissolvable assembly for downhole tool, downhole tool and oil well drilling, production and production system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110964967B (en) * | 2019-12-23 | 2021-07-23 | 有研亿金新材料有限公司 | Back plate with low thermal expansion coefficient and manufacturing method thereof |
| CN113150750A (en) * | 2020-03-20 | 2021-07-23 | 姜文辉 | Dissolvable assembly for downhole tool, downhole tool and oil well drilling, production and production system |
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| CN107604192B (en) | 2019-07-16 |
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Effective date of registration: 20240407 Address after: 601, No. 18 Yihai Jiayuan, Jimei District, Xiamen City, Fujian Province, 361021 Patentee after: Shen Xiaofei Country or region after: China Address before: 451261 HUPO village, Zhan Jie Town, Gongyi City, Zhengzhou, Henan Patentee before: GONGYI VAN-RESEARCH YIHUI COMPOSITE MATERIAL Co.,Ltd. Country or region before: China |