CN107791616A - A kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film - Google Patents
A kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film Download PDFInfo
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- CN107791616A CN107791616A CN201711019866.7A CN201711019866A CN107791616A CN 107791616 A CN107791616 A CN 107791616A CN 201711019866 A CN201711019866 A CN 201711019866A CN 107791616 A CN107791616 A CN 107791616A
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- copper
- graphite film
- layer laminated
- composite material
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/041—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
Abstract
The invention provides a kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film, the Electronic Packaging field of IC industry can be applied to.Composite raw material is from the netted graphite film of the anisotropic high heat conduction of performance and tough cathode powder.Copper powder is added to by the binding agent and repefral of polyvinyl butyral resin and ethanol solution preparation as in the homogeneous mixture solotion of plasticizer, and it is sufficiently stirred the uniform sizing material for good fluidity, by slurry on netted graphite film uniform drawout, through drying, cut, after degumming, it is layering, the graphite film of densification is prepared using Bidirectional-pressure sintering and metallic copper is layered the multiple-layer laminated block composite material being alternately arranged.Thermal conductivity of such a composite along graphite film in-plane can be high 1.5 2 times compared to fine copper, and density can be reduced to the 65 80% of fine copper, available for replacement traditional copper tungsten metal thermal conductive material.
Description
Technical field
The present invention relates to a kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film, there is provided is led with height
The netted graphite film material of heat is raw material, and the layer structure composite prepared with reference to specially-shaped and sintering process should
Material radiates available for miniature electronic part, belongs to integrated circuit, electronic package material field.
Technical background
The continuous progress of modern society promotes electronic equipment to develop rapidly, while premium properties is required, electronics
Equipment is intended to miniaturization, lightweight development, and this inevitably results in caloric value under its unit volume and increased, if can not dissipate in time
Heat, equipment normal operation, or even damage equipment may be influenceed.Traditional heat dissipation has been difficult to meet that radiating of today will
Ask.In the thermal conductivity of Electronic Packaging neighborhood optimization material, can effectively solve this problem.
The fundamental type of electronic package material has Plastic Package, ceramic package, Metal Packaging and metal-base composites envelope
Dress.Among these, metal-base composites has its unique advantage, can combine metal material with strengthening the advantages of mutually respective,
With excellent mechanical property and the physical property such as good heat conduction, conduction, wear-resisting, low thermal coefficient of expansion.Common Metal Substrate
Body has aluminium and aluminium alloy, copper and copper alloy etc., and reinforcement can be metal or inorganic material.
With the development of technology, it is micron-sized graphite film that can manually synthesize thickness, and thermal conductivity is reachable in its face
1500W/mK even more highs, and there is anisotropy, it is good electronic package material.But graphite film low intensity itself,
Especially interfacial bonding strength is very low, while it can not be connected with each other between metal, difficult between the bulk material interface of formation
It is urgent problem with strong bonded.
Found after document, patent retrieval to last decade, a kind of patent " high heat conduction of Application No. 201410114471.5
The preparation method of graphite film-carbon/carbon-copper composite material " first electroless copper on graphite film, one layer of copper of re-plating, obtains individual layer copper facing stone
The film material of ink film, material axial thermal conductivity, but the interface cohesion problem of unresolved graphite film and copper are improved, and failed
The block composite material that obtained shape can be processed arbitrarily.A kind of patent " high heat conduction graphite of Application No. 201511019061.3
The preparation method of film surface metal coating " is coated with one layer of copper coating to graphite film surface using PVD equipment, and graphite film is carried out
Processing, improve its performance, but coating is simply mechanically attached on graphite film, and mutual adhesion is weak, and finally obtains still
It is so film material, does not form block composite material.A kind of patent " high heat conduction graphite film of Application No. 201510052133.8
Metal block composite material and preparation method thereof " using graphite film and aluminium foil be superimposed and it is hot-forming, it is compound to have obtained block
Material, although solving the problems, such as to combine between graphite film and metallic matrix interface by the diffusion of aluminium and graphite film, stone
The problem of ink film itself interlayer low intensity, is not solved effectively, thus causes the intensity of its obtained block composite material
Not high, the composite prepared belongs to loose material, and performance is unable to reach best applications state.
The content of the invention
To improve above-mentioned material performance deficiency, the present invention provides a kind of multiple-layer laminated block composite material of copper/graphite film
Preparation method, be raw material from tough cathode powder and netted graphite film, copper powder slurry be spread to graphite using the tape casting
On film, the good mobility of slurry makes copper powder be sufficient filling with the mesh of netted graphite film, thus can be between layers of copper
Be connected with each other, form rivet arrangement, it is low to solve graphite film interlaminar strength, and copper with graphite film interface is uncombined asks
Topic, effectively improve the intensity of composite.
The present invention is achieved by the following technical programs：
A kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film, it is characterised in that：With fine copper powder and
Artificial synthesized netted graphite film is raw material, is uniformly layered on copper powder on graphite film using casting molding processes, then carry out
Dry, cut, degumming, heap poststack, using Bidirectional-pressure sintering process, be molded composite, obtain the high heat conduction block of densification
Shape composite.
Further, the raw material are the tough cathode powder of 5-10 μm of particle diameter, and artificial synthesized graphite film, in netted
Structure, thickness are 25 μm, and the size of mesh and interval can designed, designeds.
Further, casting molding processes sprawl the step of copper powder and are：The polyvinyl butyral resin of configuration quality fraction 5%
With the alcohol mixeding liquid of mass fraction 95% as binding agent, pour into copper powder and stir to form slurry, copper powder and binding agent
Mass ratio is 1：1, and instill repefral and account for the 1-1.3% of total slurry as plasticizer, its mass fraction, it will starch
Material is poured into casting device, is uniformly spread out, is bonded on graphite film surface, and regulation blade height is 50-100 μm, casting belt
Operating rate is 0.4-0.8m/min.
Further, drying steps are：Molded casting films are placed in vacuum drying chamber, drying temperature is arranged to 30
DEG C, vacuum≤10-1Pa, drying time 1h.
Further, graphite film is cut into appropriate size, carries out degumming, this process is carried out in hydrogen furnace, is heated up
To 400-500 DEG C, 2h is incubated, is taken out after cooling, and carry out layered arrangement and be loaded in graphite jig.
Further, pressure sintering is carried out, sintering process is carried out in pure nitrogen gas atmosphere, and heating rate is 5 DEG C/min, extremely
950-1050 DEG C, Bidirectional-pressure pressure is 5-10MPa, heat-insulation pressure keeping 60-90min, and copper/graphite film that densification is prepared is more
Block composite material is closed layer by layer.
Advantages of the present invention
1. the graphite film that the present invention adds has heat conductivility in the face of superelevation, its network structure causes copper
It can be connected with each other between layer, solve the problems, such as that bulk material interlayer bond strength is too low, prepare with some strength
High heat conduction block composite material.
2. the present invention is uniformly spread in copper powder on netted graphite film using the tape casting, it is ensured that copper powder is filled in graphite
At film mesh, rivet arrangement is formed；The volume of graphite and copper in composite can be controlled by controlling copper layer thickness simultaneously
Than.
3. the present invention is applied widely, copper can be selected in metal material, and other heat conduction good metal and alloy also can be selected.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples are the originals for illustrating the present invention
Reason, feature and have the advantage that, contribute to it is further understood that the present invention, but the present invention is not appointed
What is limited.It will be apparent to those skilled in the art that in the case where not departing from the design of the present invention, the implementation condition of use is made necessarily
Change and adjustment, belong to protection scope of the present invention.
Embodiment 1
Polyvinyl butyral resin and alcohol mixeding liquid are configured as binding agent, copper powder is poured into and stirs to form slurry, and
Repefral is instilled as plasticizer；Casting machine is poured into after slurry agitation is uniform, regulation blade height is 40 μm,
Uniform drawout on netted graphite film, the width of mesh of graphite film is 1mm, is spaced 2mm；Molded casting films are placed in
Dried in vacuum drying chamber, then by degumming, cut, stack, be put into graphite jig and carry out pressure sintering, sintering temperature is
1000 DEG C, pressure 5MPa, the block composite material of densification is prepared；Graphite film volume fraction is in composite
50vol%, it is 5.52g/cm to measure composite density using drainage3, composite thermal conductivity is measured using the laser method of shining
Rate is 590W/mK.
Embodiment 2
Polyvinyl butyral resin and alcohol mixeding liquid are configured as binding agent, copper powder is poured into and stirs to form slurry, and
Repefral is instilled as plasticizer；Casting machine is poured into after slurry agitation is uniform, regulation blade height is 80 μm,
Uniform drawout on netted graphite film, the width of mesh of graphite film is 1mm, is spaced 2mm；Molded casting films are placed in
Dried in vacuum drying chamber, then by degumming, cut, stack, be put into graphite jig and carry out pressure sintering, sintering temperature is
1000 DEG C, pressure 5MPa；Graphite film volume fraction is 35vol% in composite, and composite is measured using drainage
Density is 6.53g/cm3, it is 497W/mK to measure heat conductivity using the laser method of shining.
Claims (7)
- A kind of 1. preparation method of the multiple-layer laminated block composite material of copper/graphite film, it is characterised in that：Using flow casting molding Tough cathode slurry material is spread on artificial synthesized netted graphite film by method, copper powder is sufficient filling with netted graphite film Mesh at, there is provided connection function, then through drying, cut, degumming, and be layering, the method for utilizing Bidirectional-pressure sintering Prepare the graphite film and the multiple-layer laminated block composite material of copper of densification.
- 2. the preparation method of the multiple-layer laminated block composite material of copper/graphite film as described in the appended claim 1, it is characterised in that： The tough cathode powder of selection, 5-10 μm of particle diameter, 25 μm artificial synthesized of high heat conduction graphite film thickness, in network structure, mesh Size and mesh between interval can voluntarily adjust as desired.
- 3. the preparation method of the multiple-layer laminated block composite material of copper/graphite film as described in the appended claim 1, it is characterised in that copper The configuration of slurry material, by polyvinyl butyral resin and alcohol mixed solution in mass ratio 1：19 weigh, and are well mixed, as bonding Agent；Then copper powder is added, the mass ratio of copper powder and binding agent is 1：1, stir as uniform sizing material；Finally, phthalic acid is added Diformazan ester solution accounts for the 1-1.3% of total slurry as plasticizer, plasticizer mass fraction, is sufficiently stirred to form uniform slurry again Material.
- 4. the preparation method of the multiple-layer laminated block composite material of copper/graphite film as described in the appended claim 1, it is characterised in that logical Cross the tape casting copper slurry is spread on graphite film, mainly comprise the following steps：Uniform copper slurry is poured into casting device, adjusts knife For piece to proper height, it is 0.4-0.8m/min to make casting belt operating rate, ensures slurry uniform drawout on graphite film；It is logical The volume ratio of graphite and copper in composite can be controlled by crossing the thickness of control metal copper layer.
- 5. the preparation method of the multiple-layer laminated block composite material of copper/graphite film as described in the appended claim 1, it is characterised in that： Copper slurry is sprawled after graphite film using the tape casting, is placed on 1h in vacuum drying chamber, it is 30 DEG C to set temperature, vacuum ≤10-1Pa；It is cut into further according to actual conditions suitably sized；Then degumming is carried out, is warming up to 400-500 in a hydrogen atmosphere DEG C, the oxidation of copper is prevented, is incubated 2h.
- 6. the preparation method of the multiple-layer laminated block composite material of copper/graphite film as described in the appended claim 1, it is characterised in that： Material after degumming is placed in progress Bidirectional-pressure sintering in graphite jig, sintering temperature is 950-1050 DEG C, and moulding pressure is 5-10MPa, heat-insulation pressure keeping 60-90min.
- 7. the preparation method of the multiple-layer laminated block composite material of copper/graphite film as described in the appended claim 1, it is characterised in that： In the composite, layers of copper and graphite linings layering folded array are in layered composite structure, and its thermal conductivity is in anisotropy, along graphite The thermal conductivity in thin film planar direction is reduced to 5.62g/cm up to 590W/mK, the density of composite3。
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| CN201711019866.7A CN107791616B (en) | 2017-10-26 | 2017-10-26 | A kind of preparation method of the multiple-layer laminated block composite material of copper/graphite film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109175356A (en) * | 2018-10-16 | 2019-01-11 | 中国科学院兰州化学物理研究所 | A kind of graphite-copper laminar composite and preparation method thereof |
| CN110340368A (en) * | 2019-08-02 | 2019-10-18 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of high performance graphite film Cu-base composites |
| CN110449590A (en) * | 2018-05-08 | 2019-11-15 | 长飞光纤光缆股份有限公司 | A kind of preparation method and product of graphene-Cu-base composites |
| CN111114041A (en) * | 2020-01-07 | 2020-05-08 | 中国电子科技集团公司第十六研究所 | Composite material with high-thermal-conductivity graphite-copper interpenetrating structure and preparation method thereof |
| CN112108654A (en) * | 2020-09-23 | 2020-12-22 | 长飞光纤光缆股份有限公司 | Preparation method of high-thermal-conductivity composite material and graphite-aluminum metal composite material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110449590A (en) * | 2018-05-08 | 2019-11-15 | 长飞光纤光缆股份有限公司 | A kind of preparation method and product of graphene-Cu-base composites |
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| CN111114041A (en) * | 2020-01-07 | 2020-05-08 | 中国电子科技集团公司第十六研究所 | Composite material with high-thermal-conductivity graphite-copper interpenetrating structure and preparation method thereof |
| CN112108654A (en) * | 2020-09-23 | 2020-12-22 | 长飞光纤光缆股份有限公司 | Preparation method of high-thermal-conductivity composite material and graphite-aluminum metal composite material |
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