CN109047754A - A kind of high thermal conductivity flake graphite/graphene/metallic composite preparation method - Google Patents
A kind of high thermal conductivity flake graphite/graphene/metallic composite preparation method Download PDFInfo
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- CN109047754A CN109047754A CN201811005948.0A CN201811005948A CN109047754A CN 109047754 A CN109047754 A CN 109047754A CN 201811005948 A CN201811005948 A CN 201811005948A CN 109047754 A CN109047754 A CN 109047754A
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- graphene
- flake graphite
- copper
- thermal conductivity
- sintering
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 43
- 239000010439 graphite Substances 0.000 title claims abstract description 42
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052802 copper Inorganic materials 0.000 claims abstract description 32
- 239000010949 copper Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 13
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000007731 hot pressing Methods 0.000 claims description 3
- 238000010348 incorporation Methods 0.000 claims description 2
- 239000012495 reaction gas Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 13
- 230000000903 blocking effect Effects 0.000 abstract 1
- 238000005229 chemical vapour deposition Methods 0.000 abstract 1
- 238000007596 consolidation process Methods 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 239000004411 aluminium Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000010432 diamond Substances 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000009716 squeeze casting Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
- B22F1/16—Metallic particles coated with a non-metal
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
Abstract
The invention belongs to electronic package material fields, are related to a kind of preparation method of high thermal conductivity flake graphite/graphene/copper composite material.The following steps are included: growing graphene in copper powders surface in situ by chemical vapour deposition technique.After mixing by graphene/copper composite powder and flake graphite later, the blocking body plate shape graphite/carbon/carbon-copper composite material of hot consolidation.The shortcomings that present invention between flake graphite by introducing graphene, forming network interconnection structure, can overcome traditional flake graphite/metallic composite anisotropic heat conductivity.While not reducing composite material plane thermal conductivity, the vertical plane thermal conductivity of composite material can be significantly promoted.
Description
Technical field
The invention belongs to electronic package material fields, are related to a kind of high thermal conductivity flake graphite/graphene/metallic composite
Preparation method.
Background technique
Metal-base composites (MMCs) is due to having both high thermal conductivity, low bulk and preferable mechanical strength, in current electricity
Sub- encapsulation field has broad application prospects.Nearly more than ten years are developed there are many Advanced Electronic Encapsulating with MMCs in succession
Come, representativeness mainly has silicon carbide/aluminium and diamond/aluminum (copper) composite material, but both materials each have it is more apparent
The shortcomings that.Silicon carbide/aluminium thermal conductivity is usually no more than 250 W/mK, is difficult to meet the cooling requirements of present high-density packages;
Although the thermal conductivity of diamond/aluminum (copper) composite material can achieve 400 ~ 700 W/mK, but due to the high rigidity of diamond,
Keep its processing abnormal difficult, limits its scale application.
Flake graphite not only has a high thermal conductivity, the characteristic of low bulk, and cheap, is easily cut processing, gradually at
For the new ideal reinforcement of MMCs used for electronic packaging.According to report as a result, the plane thermal conductivity of flake graphite/aluminium (copper) composite material
Rate can compare favourably with diamond/aluminum (copper) composite material.The Wu Gao brightness seminar of Ha Er ice polytechnical university uses squeeze casting method
Be prepared for flake graphite/aluminium composite material (Carbon 95 (2015) 545-551), flake graphite presented in aluminum substrate compared with
Ideal oriented alignment characteristic, the addition of 70 vol% flake graphites can make the plane thermal conductivity of composite material reach 714 W/mK.
The Ren Shubin seminar of University of Science & Technology, Beijing is successively by implementing overlay coating (Carbon 121 (2017) in flake graphite
25-34) surface and interface is carried out to composite material and is modified with basic asphalt mixture (Carbon 127 (2018) 412-423), can be prepared
Plane thermal conductivity reaches flake graphite/carbon/carbon-copper composite material of 466 ~ 628 W/mK.
Although flake graphite/aluminium (copper) composite material reported at this stage has excellent plane thermal conductivity, due to
The anisotropy of flake graphite intrinsic thermal conductivity and its oriented alignment in the composite, composite material obtained it is vertical
Plane thermal conductivity (60 ~ 180 W/mK) is far below plane thermal conductivity (400 ~ 800W/mK), makes it that can only be suitable for certain particular fields
The application of conjunction.Therefore how to promote the vertical plane thermal conductivity of sheet graphite/metal composite material is to expand its application range
Where critical bottleneck.
Summary of the invention
Graphene is a kind of two dimensional crystal material that the carbon atom by sp2 Covalent bonding together forms, and single-layer graphene is flat
Row reaches as high as ~ 5300 W/mK in the thermal conductivity on crystal layer direction, for the peak of existing discovery material.The present invention passes through
A small amount of graphene is introduced between flake graphite, forms network interconnection structure, traditional flake graphite/metallic composite can be overcome to lead
The shortcomings that thermal anisotropy.While not reducing composite material plane thermal conductivity, the vertical of composite material can be significantly promoted
Plane thermal conductivity.Specific implementation step are as follows:
(1) copper powder is added in PMMA solution, copper powder and drying is centrifugated out after being sufficiently stirred.By the modified copper of PMMA
Powder is placed in quartz tube furnace, and using hydrogen as reaction gas, argon gas is protection gas, adjusting gas flow, reaction temperature and reaction
Time obtains graphene/copper composite powder in Copper Powder Surface growth in situ graphene.
(2) graphene/copper composite powder is equal in ethanol solution high speed shear-mixed with a certain proportion of flake graphite
It is filtered after even and dry.The composite powder of acquisition is multiple using hot pressing or discharge plasma sintering slabbing graphite/copper
Condensation material.
2. preferably, in step (1) copper powder granularity are as follows: 20 ~ 100 μm, the concentration of PMMA solution is 0.1 ~ 1wt%.
3. preferably, mixing time is 8 ~ 12 h in step (1), centrifuge separation revolving speed is 3000 ~ 6000 rpm, time
For 5 ~ 10 min.
4. preferably, in step (1) hydrogen gas flow: 50 ~ 200 sccm, argon gas flow: 200 ~ 500
Sccm, reaction temperature: 800 DEG C ~ 1000 DEG C, the reaction time: 30 ~ 90 min.
5. preferably, the piece diameter of flake graphite is 100 ~ 1000 μm in step (2), with a thickness of 10 ~ 50 μm.
6. preferably, the revolving speed of step (2) high speed shear-mixed be 5000 ~ 10000 turns/min, incorporation time be 1 ~
3h。
7. preferably, the volume fraction of flake graphite is 40 ~ 70 vol% in step (2).
8. preferably, hot pressed sintering parameter in step (2) are as follows: sintering temperature be 800 ~ 1000 DEG C, sintering pressure be 50 ~
100 MPa, sintering time are 20 ~ 60 min.
9. preferably, discharge plasma sintering parameter in step (2) are as follows: sintering temperature is 600 ~ 800 DEG C, sintering pressure
For 40 ~ 50 MPa, sintering time is 5 ~ 10 min.
The invention has the characteristics that: (1) flake graphite/carbon/carbon-copper composite material vertical plane thermal conductivity can be substantially improved;
(2) Composition And Process is controllable, and performance is easily designed;(3) composite material is easily cut processing;(3) easy to operate, preparation cost is opposite
It is lower.
Specific embodiment:
Embodiment 1
50 μm of copper powder is added in the PMMA solution that concentration is 0.2 wt%, be centrifugated after 12 h of stirring (5000 rpm,
5 min) go out copper powder and drying.The modified copper powder of PMMA is placed in quartz tube furnace, be passed through 100 sccm hydrogen and
The argon gas of 200 sccm, reaction temperature are 950 DEG C, and the reaction time is 60 min, obtains graphene/copper composite powder.It will be compound
The flake graphite (piece diameter: 500 μm, thickness: 20 μm) of powder and 50 vol% shear (5000 rpm) in ethanol solution high speed
It is filtered after 2 h and dry.It is later 100 MPa in sintering pressure by mixed-powder, sintering temperature is hot pressing under the conditions of 1000 DEG C
60 min are sintered, block flake graphite/graphene/copper composite material is obtained.Thermal conductivity test shows the plane heat of composite material
Conductance (press perpendicular direction) is 570 W/mK, and vertical plane thermal conductivity (parallel compression aspect) is 380 W/mK.And it uses same
The plane thermal conductivity of flake graphite/carbon/carbon-copper composite material (no growth in situ graphene) of the technique preparation of sample is 580 W/mK, is hung down
Straight plane thermal conductivity is only 180 W/mK.The addition of graphene improves the vertical thermal conductivity of flake graphite/carbon/carbon-copper composite material
As many as one times.
Embodiment 2
50 μm of copper powder is added in the PMMA solution that concentration is 0.2 wt%, be centrifugated after 12 h of stirring (5000 rpm,
5 min) go out copper powder and drying.The modified copper powder of PMMA is placed in quartz tube furnace, be passed through 100 sccm hydrogen and
The argon gas of 200 sccm, reaction temperature are 950 DEG C, and the reaction time is 60 min, obtains graphene/copper composite powder.By graphite
The flake graphite (piece diameter: 500 μm, thickness: 20 μm) of alkene/copper composite powder and 50 vol% are sheared in ethanol solution high speed
It is filtered after (5000 rpm) 2 h and dry.It is later 50 MPa in sintering pressure by mixed-powder, sintering temperature is 800 DEG C of items
10 min of discharge plasma sintering under part obtains block flake graphite/graphene/copper composite material.Thermal conductivity test shows multiple
The plane thermal conductivity of condensation material is 610 W/mK, and vertical plane thermal conductivity is 420 W/mK.And prepared using same technique
The plane thermal conductivity of flake graphite/carbon/carbon-copper composite material (no growth in situ graphene) is 600 W/mK, and vertical plane thermal conductivity is only
For 200 W/mK.Flake graphite/carbon/carbon-copper composite material thermal conductivity is improved as many as one times by the addition of graphene.
Embodiment 3
50 μm of copper powder is added in the PMMA solution that concentration is 0.2 wt%, be centrifugated after 12 h of stirring (5000 rpm,
5 min) go out copper powder and drying.The modified copper powder of PMMA is placed in quartz tube furnace, be passed through 100 sccm hydrogen and
The argon gas of 200 sccm, reaction temperature are 950 DEG C, and the reaction time is 60 min, obtains graphene/copper composite powder.By graphite
The flake graphite (piece diameter: 500 μm, thickness: 20 μm) of alkene/copper composite powder and 60 vol% are sheared in ethanol solution high speed
(5000 rpm) 2 h are filtered after mixing and drying.It is later 50 MPa in sintering pressure by mixed-powder, sintering temperature is
10 min of discharge plasma sintering under the conditions of 800 DEG C obtains block flake graphite/graphene/copper composite material.Thermal conductivity test
The plane thermal conductivity (press perpendicular direction) for showing composite material is 650 W/mK, vertical plane thermal conductivity (parallel compression aspect)
For 390 W/mK.And the plane of the flake graphite/carbon/carbon-copper composite material (no growth in situ graphene) prepared using same technique
Thermal conductivity is 640 W/mK, and vertical plane thermal conductivity is only 170 W/mK.The addition of graphene is by flake graphite/carbon/carbon-copper composite material
Thermal conductivity improve as many as one times.
Claims (9)
1. a kind of preparation method of high thermal conductivity flake graphite/graphene/copper composite material, feature includes following procedure:
(1) copper powder is added in polymethyl methacrylate (PMMA) solution, copper powder is centrifugated out after being sufficiently stirred and is done
It is dry;The modified copper powder of PMMA is placed in quartz tube furnace, using hydrogen as reaction gas, argon gas is protection gas, regulating gas
Flow, reaction temperature and reaction time obtain graphene/copper composite powder in Copper Powder Surface growth in situ graphene;
(2) by graphene/copper composite powder and a certain proportion of flake graphite after ethanol solution high speed shear-mixed is uniform
It filters and dries, the composite powder of acquisition is used into hot pressing or discharge plasma sintering slabbing graphite/composite copper material
Material.
2. the method as described in claim 1, it is characterized in that in step (1) copper powder granularity are as follows: 20 ~ 100 μm, PMMA solution
Concentration be 0.1 ~ 1wt%.
3. the method as described in claim 1, it is characterized in that mixing time is 8 ~ 12 h in step (1), centrifuge separation revolving speed is
3000 ~ 6000 rpm, time are 5 ~ 10 min.
4. the method as described in claim 1, it is characterized in that in step (1) hydrogen gas flow: 50 ~ 200 sccm, argon gas
Gas flow: 200 ~ 500 sccm, reaction temperature: 800 DEG C ~ 1000 DEG C, the reaction time: 30 ~ 90 min.
5. the method as described in claim 1, it is characterized in that the piece diameter of flake graphite is 100 ~ 1000 μm in step (2), thickness
It is 10 ~ 50 μm.
6. the method as described in claim 1, it is characterized in that the revolving speed of step (2) high speed shear-mixed is 5000 ~ 10000
Turn/min, incorporation time is 1 ~ 3h.
7. the method as described in claim 1, it is characterized in that the volume fraction of flake graphite is 40 ~ 70 vol% in step (2).
8. the method as described in claim 1, it is characterized in that hot pressed sintering parameter in step (2) are as follows: sintering temperature be 800 ~
1000 DEG C, sintering pressure is 50 ~ 100 MPa, and sintering time is 20 ~ 60 min.
9. the method as described in claim 1, it is characterized in that discharge plasma sintering parameter in step (2) are as follows: sintering temperature is
600 ~ 800 DEG C, sintering pressure is 40 ~ 50 MPa, and sintering time is 5 ~ 10 min.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110241398A (en) * | 2019-06-26 | 2019-09-17 | 上海交通大学 | A kind of preparation method of graphite flake growth in situ graphene reinforced aluminum matrix composites |
CN110923662A (en) * | 2019-10-30 | 2020-03-27 | 北京碳垣新材料科技有限公司 | Preparation method of graphene-metal composite material |
CN111069605A (en) * | 2020-01-03 | 2020-04-28 | 西安交通大学 | 3D graphene/copper composite material prepared in situ on surface of copper powder by using solid carbon source and method thereof |
CN111069611A (en) * | 2019-12-23 | 2020-04-28 | 长飞光纤光缆股份有限公司 | Preparation method of graphite-graphene-metal composite material |
CN113716552A (en) * | 2021-09-08 | 2021-11-30 | 西北有色金属研究院 | Preparation method of highly-oriented high-thermal-conductivity graphene/copper composite material |
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