CN109434124A - A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene - Google Patents
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene Download PDFInfo
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- CN109434124A CN109434124A CN201811381271.0A CN201811381271A CN109434124A CN 109434124 A CN109434124 A CN 109434124A CN 201811381271 A CN201811381271 A CN 201811381271A CN 109434124 A CN109434124 A CN 109434124A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
- C22C21/14—Alloys based on aluminium with copper as the next major constituent with silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3736—Metallic materials
Abstract
The invention discloses a kind of preparation methods of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, specifically includes the following steps: preparing metal mixed powder using aluminium ingot, copper ingot, silicon, niobium ingot as raw material first；It is modified that surface is carried out to graphene using neopelex, then Nickel Plating Treatment is carried out on modified graphene surface, then the graphene after nickel plating is handled with metal mixed powder mixed grinding, mixed-powder is made, finally mixed-powder obtained is placed in metal capsule, compression process 3-5min is carried out at 100-180 DEG C, then carries out vacuum degassing processing, hot-pressing processing finally is being carried out, electronic package material is made.Electronic package material good heat conductivity produced by the present invention, thermal expansion coefficient is low, and preparation is simple, and low energy consumption.
Description
Technical field:
The present invention relates to electronic package materials, are specifically related to a kind of low bulk Metal Substrate electronics modified based on graphene
The preparation method of encapsulating material.
Background technique:
With the continuous development of electronic technology, the power density of electronic component constantly increases, and the heat of generation is increasingly
More, the requirement simultaneously for material lightweight is also increasingly urgent to, and common encapsulating material is no longer satisfied Current electronic technology
Fast-developing needs.The New Materials for Electric Packing with more high heat conductance is developed, the heat that semiconductor generates is dissipated in time
Fall, guarantee the normal working temperature of power component, has become the key of electronic industry development.
Machinery support, seal protection, heat of stray electron component etc. when electronic package material main function.It is to belong to
In low-expansion high heat conductivity material, performance requirement are as follows: have higher thermal conductivity, the thermal expansion coefficient phase of thermal expansion coefficient and device
Matching.But current electronic package material heating conduction is inadequate, and mechanical property needs further to improve.
Summary of the invention:
The object of the present invention is to provide a kind of preparations of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene
Method, electronic package material heating conduction made from this method is uniform, and the coefficient of expansion is low, easy processing, and low energy consumption for preparation.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, comprising the following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 10- under the revolving speed of 580rpm
Then 15h is filtered, solid is dry, and pretreating graphite alkene is made；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and the graphene after nickel plating is made with step (1)
The metal mixed powder and ethyl alcohol obtained mixes, and is ultrasonically treated 1-6h under 500-1000W, filters, and solid is dry, is made and mixes
Powder；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3- is carried out at 100-180 DEG C
Then 5min carries out vacuum degassing processing, finally carrying out hot-pressing processing, electronic package material is made.
As a preferred embodiment of the above technical solution, in step (1), aluminium ingot, copper ingot, silicon, niobium ingot mass ratio be (10-20):
(3.25-4.55): (0.15-0.33): (0.5-1).
As a preferred embodiment of the above technical solution, in step (1), the temperature of the aerosolization is 600-800 DEG C.
As a preferred embodiment of the above technical solution, in step (2), the mass ratio of the graphene, neopelex
For 1:(0.03-0.09).
As a preferred embodiment of the above technical solution, in step (3), modified graphene, metal mixed powder mass ratio be
(0.07-0.13):1。
As a preferred embodiment of the above technical solution, in step (4), the vacuum degassed vacuum degree is 0.02-0.03Pa.
As a preferred embodiment of the above technical solution, in step (4), the condition of the hot-pressing processing are as follows: first with 10-30 DEG C/
The rate of min is warming up to 100-120 DEG C, then isothermal holding 1-2h is warming up to 160-220 with the heating rate of 5-15 DEG C/min
DEG C, isothermal holding 50-70min is finally warming up to 400-500 DEG C, isothermal holding 1-2h with the heating rate of 10-20 DEG C/min,
It is continuously heating to 500-600 DEG C, when vacuumizing as 0.003-0.007Pa, compression process 1-3h under 100-120MPa.
The invention has the following advantages that
The present invention is handled by aerosolization and mixed-powder is made using aluminium ingot, copper ingot, silicon, niobium ingot as raw material, then uses stone
Black alkene is modified, and in order to improve conduction, the thermal conductivity of graphene, the present invention uses detergent alkylate to graphene surface first
Sodium sulfonate is modified, and improves the dispersibility of graphene, then carries out Nickel Plating Treatment to its surface, and by itself and metal mixed
Powder mixing and ball milling, then successively carries out precompressed, vacuum degassing, hot-pressing processing, and electronic package material even tissue obtained causes
Close property is good, and electronic package material thermal coefficient obtained is 320W/mk or more, and thermal expansion coefficient is 16.3 × 10-6/ K hereinafter,
Tensile strength is 365MPa or more.
Specific embodiment:
In order to better understand the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, comprising the following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；Wherein, aluminium
Ingot, copper ingot, silicon, niobium ingot mass ratio be 10:3.25:0.15:0.5；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 10h under the revolving speed of 580rpm,
Then it filters, solid is dry, pretreating graphite alkene is made；Wherein, the mass ratio of the graphene, neopelex
For 1:0.03；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and the graphene after nickel plating is made with step (1)
The metal mixed powder and ethyl alcohol obtained mixes, and is ultrasonically treated 1h under 500W, filters, and solid is dry, and mixed-powder is made；Its
In, modified graphene, metal mixed powder mass ratio be 0.07:1；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3-5min is carried out at 100 DEG C, so
Vacuum degassing processing is carried out afterwards, is finally carrying out hot-pressing processing, electronic package material is made；Wherein, the item of the hot-pressing processing
Part are as follows: be warming up to 100 DEG C first with the rate of 10 DEG C/min, then isothermal holding 1h is warming up to the heating rate of 5 DEG C/min
160 DEG C, isothermal holding 50min, 400 DEG C finally are warming up to the heating rate of 10 DEG C/min, isothermal holding 1h is continuously heating to
500 DEG C, when vacuumizing as 0.003Pa, compression process 1h under 100MPa.
Embodiment 2
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, comprising the following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；Wherein, aluminium
Ingot, copper ingot, silicon, niobium ingot mass ratio be 20:4.55:0.33:1；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 15h under the revolving speed of 580rpm,
Then it filters, solid is dry, pretreating graphite alkene is made；Wherein, the mass ratio of the graphene, neopelex
For 1:0.09；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and the graphene after nickel plating is made with step (1)
The metal mixed powder and ethyl alcohol obtained mixes, and is ultrasonically treated 6h under 1000W, filters, and solid is dry, and mixed-powder is made；
Wherein, modified graphene, metal mixed powder mass ratio be 0.13:1；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3-5min is carried out at 180 DEG C, so
Vacuum degassing processing is carried out afterwards, is finally carrying out hot-pressing processing, electronic package material is made；Wherein, the item of the hot-pressing processing
Part are as follows: be warming up to 120 DEG C, isothermal holding 2h first with the rate of 30 DEG C/min, then heated up with the heating rate of 15 DEG C/min
To 220 DEG C, isothermal holding 70min, 500 DEG C finally are warming up to the heating rate of 20 DEG C/min, isothermal holding 2h continues to heat up
To 600 DEG C, when vacuumizing as 0.007Pa, compression process 3h under 120MPa.
Embodiment 3
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, comprising the following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；Wherein, aluminium
Ingot, copper ingot, silicon, niobium ingot mass ratio be 12:3.45:0.2:0.6；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 11h under the revolving speed of 580rpm,
Then it filters, solid is dry, pretreating graphite alkene is made；Wherein, the mass ratio of the graphene, neopelex
For 1:0.04；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and the graphene after nickel plating is made with step (1)
The metal mixed powder and ethyl alcohol obtained mixes, and is ultrasonically treated 2h under 600W, filters, and solid is dry, and mixed-powder is made；Its
In, modified graphene, metal mixed powder mass ratio be 0.08:1；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3-5min is carried out at 120 DEG C, so
Vacuum degassing processing is carried out afterwards, is finally carrying out hot-pressing processing, electronic package material is made；Wherein, the item of the hot-pressing processing
Part are as follows: 100 DEG C, isothermal holding 1.2h are warming up to first with the rate of 15 DEG C/min, then with the heating rate liter of 10 DEG C/min
Temperature is finally warming up to 400 DEG C, isothermal holding 1.2h to 180 DEG C, isothermal holding 55min with the heating rate of 15 DEG C/min, continues
500 DEG C are warming up to, when vacuumizing as 0.004Pa, compression process 1.5h under 105MPa.
Embodiment 4
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, comprising the following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；Wherein, aluminium
Ingot, copper ingot, silicon, niobium ingot mass ratio be 14:3.55:0.2:0.7；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 12h under the revolving speed of 580rpm,
Then it filters, solid is dry, pretreating graphite alkene is made；Wherein, the mass ratio of the graphene, neopelex
For 1:0.05；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and the graphene after nickel plating is made with step (1)
The metal mixed powder and ethyl alcohol obtained mixes, and is ultrasonically treated 3h under 700W, filters, and solid is dry, and mixed-powder is made；Its
In, modified graphene, metal mixed powder mass ratio be 0.09:1；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3-5min is carried out at 150 DEG C, so
Vacuum degassing processing is carried out afterwards, is finally carrying out hot-pressing processing, electronic package material is made；Wherein, the item of the hot-pressing processing
Part are as follows: 110 DEG C, isothermal holding 1.4h are warming up to first with the rate of 20 DEG C/min, then with the heating rate liter of 10 DEG C/min
Temperature is finally warming up to 500 DEG C, isothermal holding 1.4h to 200 DEG C, isothermal holding 60min with the heating rate of 20 DEG C/min, continues
600 DEG C are warming up to, when vacuumizing as 0.005Pa, compression process 2h under 110MPa.
Embodiment 5
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, comprising the following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；Wherein, aluminium
Ingot, copper ingot, silicon, niobium ingot mass ratio be (10-20): 4.05:0.2:0.7；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 13h under the revolving speed of 580rpm,
Then it filters, solid is dry, pretreating graphite alkene is made；Wherein, the mass ratio of the graphene, neopelex
For 1:0.06；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and the graphene after nickel plating is made with step (1)
The metal mixed powder and ethyl alcohol obtained mixes, and is ultrasonically treated 4h under 800W, filters, and solid is dry, and mixed-powder is made；Its
In, modified graphene, metal mixed powder mass ratio be 0.09:1；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3-5min is carried out at 150 DEG C, so
Vacuum degassing processing is carried out afterwards, is finally carrying out hot-pressing processing, electronic package material is made；Wherein, the item of the hot-pressing processing
Part are as follows: 110 DEG C, isothermal holding 1.6h are warming up to first with the rate of 25 DEG C/min, then with the heating rate liter of 10 DEG C/min
Temperature is finally warming up to 450 DEG C, isothermal holding 1.6h to 200 DEG C, isothermal holding 60min with the heating rate of 20 DEG C/min, continues
600 DEG C are warming up to, when vacuumizing as 0.005Pa, compression process 2.5h under 110MPa.
Embodiment 6
A kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, comprising the following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；Wherein, aluminium
Ingot, copper ingot, silicon, niobium ingot mass ratio be 18:4.25:0.3:0.9；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 14h under the revolving speed of 580rpm,
Then it filters, solid is dry, pretreating graphite alkene is made；Wherein, the mass ratio of the graphene, neopelex
For 1:0.08；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and the graphene after nickel plating is made with step (1)
The metal mixed powder and ethyl alcohol obtained mixes, and is ultrasonically treated 5h under 900W, filters, and solid is dry, and mixed-powder is made；Its
In, modified graphene, metal mixed powder mass ratio be 0.12:1；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3-5min is carried out at 160 DEG C, so
Vacuum degassing processing is carried out afterwards, is finally carrying out hot-pressing processing, electronic package material is made；Wherein, the item of the hot-pressing processing
Part are as follows: 110 DEG C, isothermal holding 1.8h are warming up to first with the rate of 25 DEG C/min, then with the heating rate liter of 13 DEG C/min
Temperature is finally warming up to 500 DEG C, isothermal holding 1.8h to 210 DEG C, isothermal holding 65min with the heating rate of 20 DEG C/min, continues
500 DEG C are warming up to, when vacuumizing as 0.006Pa, compression process 2.5h under 120MPa.
Claims (7)
1. a kind of preparation method of the low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene, which is characterized in that including
Following steps:
(1) aluminium ingot, copper ingot, silicon, niobium ingot are uniformly mixed, carry out aerosolization and handles obtained metal mixed powder；
(2) graphene, neopelex, deionized water are uniformly mixed, ball milling 10-15h under the revolving speed of 580rpm, so
After filter, solid is dry, pretreating graphite alkene is made；
(3) by pretreating graphite alkene plating nickel on surface obtained above processing, and by after nickel plating graphene and step (1) it is obtained
Metal mixed powder and ethyl alcohol mix, and are ultrasonically treated 1-6h under 500-1000W, filter, and solid is dry, and mixed powder is made
End；
(4) mixed-powder obtained above is placed in metal capsule, compression process 3-5min is carried out at 100-180 DEG C, so
Vacuum degassing processing is carried out afterwards, is finally carrying out hot-pressing processing, electronic package material is made.
2. a kind of preparation side of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene as described in claim 1
Method, it is characterised in that: in step (1), aluminium ingot, copper ingot, silicon, niobium ingot mass ratio be (10-20): (3.25-4.55): (0.15-
0.33): (0.5-1).
3. a kind of preparation side of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene as described in claim 1
Method, it is characterised in that: in step (1), the temperature of the aerosolization processing is 600-800 DEG C.
4. a kind of preparation side of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene as described in claim 1
Method, it is characterised in that: in step (2), the graphene, neopelex mass ratio be 1:(0.03-0.09).
5. a kind of preparation side of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene as described in claim 1
Method, it is characterised in that: in step (3), modified graphene, metal mixed powder mass ratio be (0.07-0.13): 1.
6. a kind of preparation side of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene as described in claim 1
Method, it is characterised in that: in step (4), the vacuum degassed vacuum degree is 0.02-0.03Pa.
7. a kind of preparation side of low bulk METAL-MATRIX MATERIAL FOR ELECTRONIC PACKAGING modified based on graphene as described in claim 1
Method, which is characterized in that in step (4), the condition of the hot-pressing processing are as follows: be warming up to first with the rate of 10-30 DEG C/min
100-120 DEG C, isothermal holding 1-2h, it then is warming up to 160-220 DEG C with the heating rate of 5-15 DEG C/min, isothermal holding 50-
70min, is finally warming up to 400-500 DEG C with the heating rate of 10-20 DEG C/min, and isothermal holding 1-2h is continuously heating to 500-
600 DEG C, when vacuumizing as 0.003-0.007Pa, compression process 1-3h under 100-120MPa.
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| CN112139512A (en) * | 2020-08-25 | 2020-12-29 | 湖南大学 | Preparation method of copper-based composite material precursor powder |
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