CN107809885A - A kind of graphite film metallic composite of high-bond and preparation method thereof - Google Patents

A kind of graphite film metallic composite of high-bond and preparation method thereof Download PDF

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CN107809885A
CN107809885A CN201710938307.XA CN201710938307A CN107809885A CN 107809885 A CN107809885 A CN 107809885A CN 201710938307 A CN201710938307 A CN 201710938307A CN 107809885 A CN107809885 A CN 107809885A
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metal
graphite film
graphite
metallic composite
layer
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CN107809885B (en
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刘佩珍
戴曛晔
李鑫
杜富贵
李阳
吕新坤
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Chongqing Yuntianhua Hanen New Material Development Co Ltd
Yunnan Yuntianhua Co Ltd
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Chongqing Yuntianhua Hanen New Material Development Co Ltd
Yunnan Yuntianhua Co Ltd
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00—Constructional details common to different types of electric apparatus
    • H05K7/20—Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • 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
    • 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
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • 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
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/08—Interconnection of layers by mechanical means
    • 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
    • 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
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0088—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising a plurality of shielding layers; combining different shielding material structure
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/06—Coating on the layer surface on metal layer
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/20—Inorganic coating
    • B32B2255/205—Metallic coating
    • 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
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/212—Electromagnetic interference shielding
    • 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
    • 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
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • 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
    • B32B2311/00—Metals, their alloys or their compounds
    • B32B2311/02—Noble metals
    • B32B2311/08—Silver
    • 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
    • B32B2311/00—Metals, their alloys or their compounds
    • B32B2311/12—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
    • B32B2313/00—Elements other than metals
    • B32B2313/04—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
    • B32B2457/00—Electrical equipment

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Electromagnetism (AREA)
  • Fluid Mechanics (AREA)
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Abstract

The present invention relates to graphite film metallic composite technical field, graphite film metallic composite of a kind of high-bond and preparation method thereof is disclosed.The present invention includes graphite linings, intermediate metal and surface metal-layer, and the graphite linings are the graphite film merely through carbonization and graphitization processing.Preparation method of the present invention comprises the following steps：It is followed successively by and prepares graphite linings, fusion method and prepare intermediate metal, calendering, pickling, prepare surface metal-layer, anti-oxidation processing.The present invention is easy to prepare, and graphite film is high with metal level adhesion, has superior electrical conductivity energy and heat dispersion.

Description

A kind of graphite film metallic composite of high-bond and preparation method thereof
Technical field
The present invention relates to graphite film metallic composite technical field, more particularly to a kind of graphite film gold of high-bond Belong to composite and preparation method thereof.
Background technology
With electronics, the expansion and popularization of electrical equipment application, to wanting for electronics, the performance of electrical equipment and structure Ask increasingly harsher, such as higher processing speed, smaller volume, lighter weight, higher power and preferably radiating Performance etc., it is continuous to the demand of automobile fast charging and discharging equipment especially as the continuous expansion of new-energy automobile scale in recent years Increase, heat conduction and heat dispersion to material propose higher requirement.
Traditional heat sinks have it is obvious restricted, it is especially independent in use, can not meet that current industrial and science and technology are big The demand of war.In recent years, heat-conductive composite material with its low cost, easy processing, have good electrical insulating property and mechanical property by To extensive concern, its preparation method also turns into the focus studied at present.
" a kind of native graphite/copper heat sink compound and preparation method thereof " of Chinese Patent Application No. 201510672288, Pretreatment is carried out to copper foil surface and removes pollution and the oxide layer of copper foil surface, then carries out roughening treatment and curing process, is made Copper foil surface forms the roughened layer for being evenly distributed with warty copper grain structure；Bulk electrographite monolithic is rolled over from shape again On film, artificial plumbago single slice is set to be attached on fractal film；Finally by fractal film derived above with electrographite monolithic Simultaneously it is laid on the copper foil through processing；Then through stage calendering, that is, electrographite/copper heat sink compound is obtained；Thermal diffusivity Can preferably, but complex manufacturing, operational control difficulty are big.A kind of Chinese patent CN101508596A " metal coating plumbagos Composite and preparation method thereof " is first deoiled graphite radiating material surface and roughening treatment, in sensitizing solution, activating solution Dipping, rinse, then carry out copper facing or nickel or zinc etc. in the plating solution；Metal level can be by the way of chemical plating or plating；Obtain Composite is attractive in appearance, intensity is high and heat conductivility is high, but obtained graphite film and the adhesion of metal level are not high enough.
The content of the invention
The present invention provides one kind and is easy to prepare, and graphite film is high with metal level adhesion, has superior electrical conductivity energy and radiating Graphite film metallic composite of a kind of high-bond of performance and preparation method thereof.
The technical problem of solution is：Existing composite sheet preparation method for material is complicated, and operating process is difficult to control, and is obtained Graphite film and metal level between adhesion deficiency.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of graphite film metallic composite of high-bond of the present invention, including graphite linings, intermediate metal and surface gold Belong to layer, the graphite linings are the graphite film merely through carbonization and graphitization processing.
A kind of graphite film metallic composite of high-bond of the present invention, further, the graphite linings are used with lower section Method is prepared：
Step A, it is carbonized：By Kapton under -0.1MPa, progressively it is warming up to 1100 DEG C~1400 DEG C and is carbonized Film；
Step B, graphitization：In inert gas environment, carbonized film is progressively warming up to 2600 DEG C~3000 DEG C and obtains stone Ink film.
A kind of graphite film metallic composite of high-bond of the present invention, further, the intermediate metal are copper gold Category, silver metal or its alloy, the thickness of the intermediate metal are no more than 100nm.
A kind of graphite film metallic composite of high-bond of the present invention, further, the intermediate metal is using molten The method of melting is attached to graphite layer surface, and the thickness of the intermediate metal is 20-50nm.
A kind of graphite film metallic composite of high-bond of the present invention, further, the surface metal-layer are copper gold Category or aluminum metal.
A kind of preparation method of the graphite film metallic composite of high-bond of the present invention, comprises the following steps：
Step 1: prepare graphite linings：By Kapton successively by carbonization and graphitization processing, graphite film is made；
Step 2: prepare intermediate metal：Metal powder is homogeneously disposed in graphite film surface, under -0.2~-0.3Pa, with 1 ~10 DEG C/min is warming up to 950 DEG C~1100 DEG C, keeps 1~60min, is melted；Then cooled with 0.6~0.8 DEG C/min To room temperature；
Step 3: calendering：Material made from step 2 is subjected to calendering process；
Step 4: pickling：Material made from step 3 is subjected to acid-wash activation, then dried；
Step 5: prepare surface metal-layer：Surface metal-layer is plated in metal transfer layer surface；
It is Step 6: anti-oxidation：Anti-oxidation processing is carried out to surface metal-layer.
A kind of preparation method of the graphite film metallic composite of high-bond of the present invention, further, makes in step 1 The thickness of the graphite film obtained is no more than 70 μm.
A kind of preparation method of the graphite film metallic composite of high-bond of the present invention, it is further, golden in step 2 The particle diameter for belonging to powder is 10~100nm.
A kind of preparation method of the graphite film metallic composite of high-bond of the present invention, further, table in step 5 The preparation method of face metal level is electroless plated method, galvanoplastic or vacuum plating method.
A kind of preparation method of the graphite film metallic composite of high-bond of the present invention, further, in step 6 Anti-oxidation processing is plating anti-oxidant metal layer or coating metal oxidation resistance agent.
A kind of graphite film metallic composite of high-bond of the present invention compared with prior art, has following beneficial to effect Fruit：
A kind of graphite film metallic composite of high-bond of the present invention has excellent heat conductivility and excellent radiating Performance, do not make any organic reagent during preparation, there is preferable resistance to acids and bases and solvent resistance；In graphite film table Face is respectively provided with intermediate metal and surface metal-layer, has excellent capability of electromagnetic shielding, suitable for there is high-fire resistance In the high-end electronic of demand, electrical equipment.
The present invention is using the graphite film without calendering as base material, and graphite film surface smoothness and the degree of packing are all relatively low, surface With bigger roughness and specific surface area, loose structure is beneficial to provide more holes and anchor point, is more beneficial for metal The attachment of transition zone, the adhesion between graphite film and intermediate metal is greatly reinforced.The present invention is using heat melting method half Finished product graphite film surface sets intermediate metal, is then rolled again and subsequent treatment, easy to operate, easy to control, to construction Equipment requirement is low, greatly reduces construction cost, simplifies working procedure.
Graphite film metallic composite of a kind of high-bond of the present invention and preparation method thereof is made below in conjunction with the accompanying drawings Further illustrate.
Brief description of the drawings
Fig. 1 is a kind of structural representation of the graphite film metallic composite of high-bond of the present invention；
Fig. 2 is electron-microscope scanning figure of the graphite film base material under 100 times without calendering；
Fig. 3 is electron-microscope scanning figure of the commercially available graphite film product of 25 μ m-thicks under 300 times；
Fig. 4 is electron-microscope scanning figure of the graphite film base material under 300 times without calendering.
Reference：
1- graphite linings；2- intermediate metals；3- surface metal-layers.
Embodiment
As shown in figure 1, a kind of graphite film metallic composite of high-bond of the present invention includes graphite linings 1, metal transfer Layer 2 and surface metal-layer 3, graphite linings 1 are the graphite film merely through carbonization and graphitization processing, and the graphite film surface is shrinkage pool Structure；Intermediate metal 2 is copper metal, silver metal or its alloy, and the thickness of intermediate metal 2 is no more than 100nm；Metal transfer The thickness of layer 2 is 20-50nm；Surface metal-layer 3 is copper metal or aluminum metal.
Surface metal-layer 3 can also according to demand and physical condition, other conventional coated metals from nickel, zirconium etc..
Prepare embodiment 1
By Kapton under -0.1MPa, progressively it is warming up to 1100 DEG C~1400 DEG C and obtains carbonized film；Then lazy In property gaseous environment, carbonized film is progressively warming up to 2600 DEG C~3000 DEG C and obtains graphite film, the thickness of obtained graphite film is 70μm；Copper powder is uniformly sprayed on graphite film, the particle diameter of copper powder is 10~30nm；It is placed in high temperature furnace, under -0.2Pa, 1100 DEG C are warming up to 10 DEG C/min, 5min is kept, room temperature is progressively then cooled to 0.6 DEG C/min speed；Taking-up is gone forward side by side Row calendering process, the graphite film with copper metal transition zone is obtained, the thickness of intermediate metal is 20nm；By intermediate metal table Face carries out acid-wash activation processing, is then immersed in chemical copper plating solution, impregnates 30min at room temperature；In surface gold after drying Belong to layer surface and electroplate one layer of nickel zinc alloy layer, wherein Zn:Ni=(10-15)：(85-90), the μ g/dm of plating amount 100~10002。
Prepare embodiment 2
By Kapton under -0.1MPa, progressively it is warming up to 1100 DEG C~1400 DEG C and obtains carbonized film；Then lazy In property gaseous environment, carbonized film is progressively warming up to 2600 DEG C~3000 DEG C and obtains graphite film, the thickness of obtained graphite film is 20μm；By copper powder and silver powder with mass ratio 4:After 1 is well mixed, uniformly it is sprayed on graphite film, the average grain of copper powder and silver powder Footpath is 50nm；It is placed in high temperature furnace, under -0.3Pa, is warming up to 1050 DEG C with 8.5 DEG C/min, 5min is kept, then with 0.8 DEG C/min speed is progressively cooled to room temperature；Take out and carry out calendering process, obtain the graphite film with copper silver transition zone, metal The thickness of transition zone is 50nm；After metal transfer layer surface is carried out into acid-wash activation processing, in its electroplating surface silver metal layer；And In the surface metallization antioxidant of surface metal-layer.
Prepare embodiment 3
By Kapton under -0.1MPa, progressively it is warming up to 1100 DEG C~1400 DEG C and obtains carbonized film；Then lazy In property gaseous environment, carbonized film is progressively warming up to 2600 DEG C~3000 DEG C and obtains graphite film, the thickness of obtained graphite film is 30μm；By copper powder and silver powder with mass ratio 1:After 1 is well mixed, uniformly it is sprayed on graphite film, the average grain of copper powder and silver powder Footpath is 70nm；It is placed in high temperature furnace, under -0.2Pa, is warming up to 1000 DEG C with 5 DEG C/min, 20min is kept, then with 0.7 DEG C/min speed is progressively cooled to room temperature；Take out and carry out calendering process, obtain the graphite film with copper silver transition zone, metal The thickness of transition zone is 30nm；After metal transfer layer surface is carried out into acid-wash activation processing, plated on its surface using vacuum plating method Upper silver metal layer；And it is coated with metal oxidation resistance agent on the surface of surface metal-layer.
Prepare embodiment 4
By Kapton under -0.1MPa, progressively it is warming up to 1100 DEG C~1400 DEG C and obtains carbonized film；Then lazy In property gaseous environment, carbonized film is progressively warming up to 2600 DEG C~3000 DEG C and obtains graphite film, the thickness of obtained graphite film is 50μm；By copper powder and silver powder with mass ratio 1:After 4 is well mixed, uniformly it is sprayed on graphite film, the average grain of copper powder and silver powder Footpath is 100nm；It is placed in high temperature furnace, under -0.3Pa, is warming up to 980 DEG C with 1 DEG C/min, 40min is kept, then with 0.6 DEG C/min speed is progressively cooled to room temperature；Take out and carry out calendering process, obtain the graphite film with copper silver transition zone, metal The thickness of transition zone is 25nm；After metal transfer layer surface is carried out into acid-wash activation processing, in its electroplating surface silver metal layer；And In the surface metallization antioxidant of surface metal-layer.
Prepare embodiment 5
By Kapton under -0.1MPa, progressively it is warming up to 1100 DEG C~1400 DEG C and obtains carbonized film；Then lazy In property gaseous environment, carbonized film is progressively warming up to 2600 DEG C~3000 DEG C and obtains graphite film, the thickness of obtained graphite film is 60μm；Silver powder is uniformly sprayed on graphite film, the particle diameter of silver powder is 10nm；It is placed in high temperature furnace, under -0.2Pa, with 2.5 DEG C/min is warming up to 950 DEG C, keeps 60min, is then progressively cooled to room temperature with 0.8 DEG C/min speed；Take out and carry out Calendering process, the graphite film with copper silver transition zone is obtained, the thickness of intermediate metal is 40nm；Metal transfer layer surface is entered After the processing of row acid-wash activation, in its electroplating surface silver metal layer；And in the surface metallization antioxidant of surface metal-layer.
Testing example
For the graphite film base material used, the graphite film base material without calendering and commercially available stone that compared for that the present invention uses Ink film finished product, the graphite film without calendering that the commercially available graphite film product from 25 μ m-thicks is 25 μm with the thickness after calendering respectively Base material, carry out electron-microscope scanning.
Electron-microscope scanning of the graphite film base material under 100 times without calendering is as shown in Figure 2.
Electron-microscope scanning of the commercially available graphite film product of 25 μ m-thicks under 300 times is as shown in figure 3, the graphite film base without calendering Electron-microscope scanning of the material under 300 times is as shown in Figure 4.
Comparison diagram 3 and Fig. 4 understand, the present invention selects the graphite film without calendering process, the flatness on graphite film surface and The degree of packing is all relatively low, and surface is in obvious concavo-convex state；Graphite surface roughness is high, and specific surface area is big, can be with intermediate metal Multi-point-anchoring, substantially increase the bond strength of graphite film and metal level.
Comparative example 1
5 test groups and 2 control groups are set respectively, and test group is that graphite film metal made from above-mentioned preparation embodiment is answered Condensation material, control group are respectively pure copper foil and pure graphite film, are cut into the test specimens of 90*120mm specifications respectively, are carried out red Outer heat transfer test, specific test result are as shown in table 1.
The infrared heat transfer test result of 1 each material of table
As shown in Table 1, compared with pure copper foil or graphite film, graphite film metal composite that above-mentioned preparation embodiment is prepared Material has more excellent heat conductivility and heat dispersion.
Comparative example 2
5 test groups and 1 control group are set respectively, and test group is that graphite film metal made from above-mentioned preparation embodiment is answered Condensation material, control group are to bond the composite formed by adhesive layer by copper foil and graphite film, are cut into 30* respectively The test specimens of 30mm specifications, 24h in different organic solvents is immersed in, carries out the resistance to acids and bases and solvent resistance of material Test, specific test result are as shown in table 2.
The resistance to acids and bases and solvent resistance test result of 2 each material of table
As shown in Table 2, the graphite film metallic composite that above-mentioned preparation embodiment is prepared is in variety classes and property Organic solvent in soak 24h after, it is in good condition, do not occur any lamination, and only pass through adhesive layer in control group Then there is obvious lamination in cohesive copper foil/graphite film composite material, illustrates that graphite film metal produced by the present invention is answered Condensation material has excellent acid-proof alkaline and solvent resistance.
It was found from above test result, the graphite film metallic composite of high-bond proposed by the present invention a kind of has excellent Good heat conductivility and excellent heat dispersion, do not make any organic reagent during preparation, have preferably acidproof Alkalescence and solvent resistance；Intermediate metal and surface metal-layer are respectively provided with graphite film surface, there is excellent electromagnetic screen Performance is covered, suitable for having the high-end electronic of high-fire resistance demand, electrical equipment.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention The various modifications and improvement that case is made, it all should fall into the protection domain of claims of the present invention determination.

Claims (10)

  1. A kind of 1. graphite film metallic composite of high-bond, it is characterised in that：Including graphite linings (1), intermediate metal (2) With surface metal-layer (3), the graphite linings (1) are the graphite film merely through carbonization and graphitization processing.
  2. A kind of 2. graphite film metallic composite of high-bond according to claim 1, it is characterised in that：The graphite Layer (1) is prepared using following methods：
    Step A, it is carbonized：By Kapton under -0.1MPa, progressively it is warming up to 1100 DEG C~1400 DEG C and obtains carbonized film；
    Step B, graphitization：In inert gas environment, carbonized film is progressively warming up to 2600 DEG C~3000 DEG C and obtains graphite film.
  3. A kind of 3. graphite film metallic composite of high-bond according to claim 2, it is characterised in that：The metal Transition zone (2) is copper metal, silver metal or its alloy, and the thickness of the intermediate metal (2) is no more than 100nm.
  4. A kind of 4. graphite film metallic composite of high-bond according to claim 3, it is characterised in that：The metal Transition zone (2) is attached to graphite linings (1) surface using fusion method, and the thickness of the intermediate metal (2) is 20-50nm.
  5. A kind of 5. graphite film metallic composite of high-bond according to claim 4, it is characterised in that：The surface Metal level (3) is copper metal or aluminum metal.
  6. A kind of 6. preparation method of the graphite film metallic composite of high-bond described in claim 5, it is characterised in that：Bag Include following steps：
    Step 1: prepare graphite linings：By Kapton successively by carbonization and graphitization processing, graphite film is made；
    Step 2: prepare intermediate metal：Metal powder is homogeneously disposed in graphite film surface, under -0.2~-0.3Pa, with 1~10 DEG C/min is warming up to 950 DEG C~1100 DEG C, 1~60min is kept, is melted；Then room is cooled to 0.6~0.8 DEG C/min Temperature；
    Step 3: calendering：Material made from step 2 is subjected to calendering process；
    Step 4: pickling：Material made from step 3 is subjected to acid-wash activation, then dried；
    Step 5: prepare surface metal-layer：In intermediate metal (2) surface plating surface metal-layer (3)；
    It is Step 6: anti-oxidation：Anti-oxidation processing is carried out to surface metal-layer (3).
  7. A kind of 7. preparation method of the graphite film metallic composite for the high-bond stated according to claim 6, it is characterised in that： The thickness of obtained graphite film is no more than 70 μm in step 1.
  8. 8. a kind of preparation method of the graphite film metallic composite of high-bond according to claim 6, its feature exist In：The particle diameter of metal powder is 10~100nm in step 2.
  9. 9. a kind of preparation method of the graphite film metallic composite of high-bond according to claim 6, its feature exist In：The preparation method of surface metal-layer (3) is electroless plated method, galvanoplastic or vacuum plating method in step 5.
  10. 10. a kind of preparation method of the graphite film metallic composite of high-bond according to claim 6, its feature exist In：Anti-oxidation processing in step 6 is plating anti-oxidant metal layer or coating metal oxidation resistance agent.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110232989A (en) * 2019-05-30 2019-09-13 王奉瑾 A kind of preparation method of graphene conductive structural body
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

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110744875A (en) * 2019-10-25 2020-02-04 北京中石伟业科技无锡有限公司 High-thermal-conductivity composite graphite radiating fin and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864067A (en) * 2014-03-26 2014-06-18 苏州格优碳素新材料有限公司 Preparation method of high thermal conductivity graphite membrane-copper composite material
CN104057653A (en) * 2014-06-13 2014-09-24 江苏悦达新材料科技有限公司 Graphite membrane/metal composite cooling fin and preparation method thereof
CN104972708A (en) * 2014-04-10 2015-10-14 苏州驭奇材料科技有限公司 Wave-absorbing and heat-dissipating double-function composite apparatus and manufacturing method thereof
CN106531706A (en) * 2016-08-17 2017-03-22 常州国成新材料科技有限公司 Artificial graphite film heat conduction and heat dissipation material with composite structure and preparation method of artificial graphite film heat conduction and heat dissipation material with composite structure
CN106847767A (en) * 2017-02-22 2017-06-13 东莞市鸿亿导热材料有限公司 A kind of graphite Copper Foil heat sink compound

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864067A (en) * 2014-03-26 2014-06-18 苏州格优碳素新材料有限公司 Preparation method of high thermal conductivity graphite membrane-copper composite material
CN104972708A (en) * 2014-04-10 2015-10-14 苏州驭奇材料科技有限公司 Wave-absorbing and heat-dissipating double-function composite apparatus and manufacturing method thereof
CN104057653A (en) * 2014-06-13 2014-09-24 江苏悦达新材料科技有限公司 Graphite membrane/metal composite cooling fin and preparation method thereof
CN106531706A (en) * 2016-08-17 2017-03-22 常州国成新材料科技有限公司 Artificial graphite film heat conduction and heat dissipation material with composite structure and preparation method of artificial graphite film heat conduction and heat dissipation material with composite structure
CN106847767A (en) * 2017-02-22 2017-06-13 东莞市鸿亿导热材料有限公司 A kind of graphite Copper Foil heat sink compound

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110232989A (en) * 2019-05-30 2019-09-13 王奉瑾 A kind of preparation method of graphene conductive structural body
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

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