CN108165809A - A kind of graphite-copper based composites with network blackboard and preparation method thereof - Google Patents
A kind of graphite-copper based composites with network blackboard and preparation method thereof Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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- C22C9/00—Alloys based on copper
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Abstract
The present invention discloses a kind of preparation method of the graphite Cu-base composites with network blackboard.For the composite material mainly by two phase composition of graphite and copper, the percent by volume that wherein graphite accounts for composite material is 10 40%, and in composite inner, graphite and copper two-phase keep itself continuous respectively, form the network blackboard being interweaved.The present invention is pre-processed using continuous sheet material graphite as raw material by graphite surface；Sheet material graphite subregion configuration designs and three-dimensional；Graphite surface copper facing；Single or multiple solid graphite are nested to form porous preforming base；Copper is penetrated into the gap between graphite by vacuum pressure infiltration, finally obtains fine and close graphite Cu-base composites.The composite material graphite copper two-phase of the present invention keeps itself continuous, and composite material has good heat conductivility and mechanical property, by regulating and controlling the spatial orientation of graphite flake, can realize the efficient conduction of heat, is the electronic package material with very big application potential.
Description
Technical field
The present invention relates to electronic package materials, and in particular to a kind of graphite-copper base composite wood with network blackboard
Material and preparation method thereof.
Background technology
The power density of with the rapid development of electronic technology, electronic component gathers promotion, and heat dissipation problem is also increasingly
Prominent, therefore, modem electronic circuitry design proposes requirements at the higher level to the heat conductivility of material.Traditional first generation Invar,
The thermal conductivity of Knvar alloys, second generation W/Cu, Mo/Cu alloy and third generation silicon carbide/Al composite materials can not meet
The radiating requirements of high-power electronic device at present.
Graphite enriches, low-cost material as a kind of Domestic Resources, the thermal conductivity on its carbon atom in-plane
Up to 2000Wm-1·K-1.Its artificial synthesized graphite flake (film), thermal conductivity is up to 1200-1800Wm on lamella direction-1·K-1, volume production is successfully realized, and applied to the heat dissipation of mobile phone, tablet computer.But graphite is soft, and intensity is too low, and vertical
Thermal conductivity on graphite sheet in-plane is only 10-20Wm-1·K-1, greatly limit their application range.Copper is as biography
The Heat Conduction Material of system has good thermal conductivity and higher intensity, it is compound with the graphite of high heat conduction, can further improve
Thermal conductivity is a kind of heat sink material got a good chance of.
The research of field of radiating is used for about graphite/carbon/carbon-copper composite material at present, reinforced phase to be mostly with discrete graphite squama
Based on piece.Although the owned higher thermal conductivity of graphite flakes, scale is isolated existing in the base.Composite material because
There are thermal resistances at graphite-copper interface, and the high thermal conductivity of graphite is caused to be unable to give full play.And continuous graphite flake is used due to height
Conductive graphite is mutually continuously distributed in intrinsic silicon, and gained heat conductivity is higher.Document " Fabrication and
thermal conductivity of copper coated graphite film/aluminum composites for
Addition is reported in effective thermal management (Journal of Alloys and Compounds) "
The continuous graphite piece of 17.4-53.2% can reach the thermal conductivity on the parallel graphite plane direction (X-Y plane) of aluminum matrix composite
To 397-805Wm-1·K-1, but the thermal conductivity of this composite material in z-direction is only 10-28Wm-1·K-1.Simultaneously as
Composite material is the sandwich structure being alternately stacked by graphite flake and metallic matrix on an x-y plane, material mechanical performance
It is relatively low, cause Failure Analysis of Composite Materials easily due to graphite layers cleavage in use.
In conclusion ideal structure is, continuous, the shape of itself phase of each self-sustaining of graphite reinforced phase, metallic matrix
Into the network blackboard of two kinds of continuous phase.Specifically, the graphite reinforced phase of high heat conduction is divided in composite inner into continuous
Cloth forms continuous passage of heat, ensures the thermal conductivity in composite material all directions；Aluminum substrate is in composite inner phase simultaneously
It is mutually continuous, ensure the intensity and toughness of composite material.
Invention content
A kind of material is provided it is an object of the invention to overcome the deficiencies in the prior art with graphite and copper two-phase network
Thermal conductivity is higher on interpenetrating structure, all directions and has graphite-copper based composites of some strength and preparation method thereof.
Realization that the present invention adopts the following technical solutions：
A kind of graphite-copper based composites with network blackboard, including graphite reinforcement and Copper substrate material,
The percent by volume that middle graphite accounts for composite material is 10-40%, and graphite reinforcement is lamellar graphite, designs and adds by configuration
Work to three-dimensional three-dimensional development, is nested in matrix copper, and graphite and copper two-phase keep itself continuous respectively, form phase
The network blackboard mutually to interweave.
Further, lamellar graphite be continuous synusia graphite, thickness 0.01-6mm, graphite sheet in-plane
Upper thermal conductivity is 400-1800Wm-1·K-1, the percent by volume that graphite accounts for composite material is 10-40%, and Copper substrate material is
Copper or copper alloy, the content of copper is more than 50% in copper alloy.
The preparation method of the above-mentioned graphite-copper based composites with network blackboard, includes the following steps：
(1) surface preparation is carried out to graphite surface；
(2) configuration design is carried out to graphite sheet, is set in sheet-like plane, that is, X-Y plane of continuous graphite sheet material
Meter and processing form several local detachments, the whole subregion still connected with graphite flake layer, which are turned over to Z-direction
It rises, makes the graphite flake three-dimensional of script two-dimensional directional；
(3) copper plating treatment is carried out to the graphite flake layer of three-dimensional, obtains covering copper graphite porous preforming base or by three-dimensional
Graphite flake layer carries out nesting, obtains the superposition of several graphite flake layers, the prefabricated blank with gap；
(4) using vacuum pressure infiltration method to prefabricated blank infiltrated metal copper obtained by step (3) or copper alloy, obtain graphite-
Cu-base composites.
Further, the modes such as design and processing and utilization graduating with cutter, punching press, cutting, the lines in partial cut area can be according to feelings
Condition is different：Specific location, distribution situation such as high power radiation, " hot spot " region and the relative position of responsive to temperature type device etc.
Flexible design is carried out, i.e. the form of graphite is keeping continuous continual, can arbitrarily change.
Further, in step (1), the method for graphite surface pretreatment is preheated including graphite surface, is cleaned by ultrasonic, acid
Liquid rinses, at least one of lye rinsing technique.
Further, the graphite surface before or after further including the design of step (2) graphite configuration is modified plated film, plates film thickness
It is 0.01-2 μm to spend, and film layer type is at least one of W, Mo, Cr, Zr, B or their respective compound, further to carry
High composite materials property.
Further, the graphite three-dimensional design principle of step (2) is in the case of ensureing that graphite integrally connects, to make X-Y
The graphite flake in direction is extended to longitudinal Z-direction, and for regional area after Z-direction is dug, former graphite surface leaves hole as metal
The infiltration channel of copper or copper alloy；Flip angle, the number of " subregion of local detachment " do not limit, be it is arbitrary, can be more
It is secondary to bend to realize that hot-fluid is conducted toward specific direction.
Further, in step (3), graphite flake layer copper plating treatment is carried out using chemical plating or plating, and thickness of coating is
0.2-30μm。
Further, in step (4), vacuum pressure infiltration method, specially：System vacuum is in below 0.1MPa before infiltration
800-1000 DEG C of preheating is carried out to prefabricated blank, after keeping the temperature 5-15min, in 1000-1400 DEG C of infiltrated metal copper or copper alloy, profit
Molten metal is pressed into green body, pressure 0.1-4Mpa with high-purity argon gas, pressurize 5-30min finally cools to room temperature with the furnace, obtains
To graphite-copper based composites.
Compared with existing encapsulating material and production technology, the invention has the advantages that：
(1) graphite forms network blackboard with copper, and graphite reinforced phase forms continuous phase in composite material, makes composite wood
Material has good thermal conductivity, while Copper substrate is continuous each other, ensure that the mechanical property of composite material.
(2) the three-dimensional configuration of graphite flake is designed for specific radiating requirements, by regulating and controlling graphite flake in space
Orientation, realize heat efficient conduction in the direction indicated.
(3) graphite-copper based composites prepared by vacuum pressure infiltration, can realize the near net of complicated shape part into
Shape, production cost is low, efficient.
Description of the drawings
Fig. 1 is the preparation process flow diagram of the present invention.
Fig. 2 is the lines schematic diagram that the graphite surface configuration of embodiment 1 designs.
Fig. 3 is the lines schematic diagram that the graphite surface configuration of embodiment 2 designs.
Fig. 4 is the graphite preform blank schematic diagram that graphite flake stacks gradually.
Specific embodiment
The present invention is described in further details, but the present invention is not limited thereto with reference to specific embodiment.
Embodiment 1
Thickness is used as 0.2mm, thermal conductivity 1200Wm-1·K-1Continuous Sheet Graphite as reinforced phase, use acetone
It is ultrasonically treated, removes surface and oil contaminant.Using icking tool in the U-shaped lines of graphite surface quarterization, lines regional area is as shown in Figure 2.Its
Middle h, l, a, b are respectively 2mm, 3.5mm, 2mm, 3mm, and the U-shaped lines carved is dug upwards one by one, obtains the graphite of three-dimensional
Piece.
Electroless copper is carried out to graphite flake using chemical-copper-plating process：Graphite flake is is added by electroless copper sensitization stage process
Enter the 20ml/LHCl+20g/LSnCl of 500ml2Solution, agitating solution 15min remove solution, and are rinsed 3 times with distilled water；It is living
Changing stage process is：Graphite flake after sensitization adds in the 20ml/L HCI+0.5g/LPdCl of 200ml2Solution, agitating solution
15min removes solution, and is rinsed 3 times with distilled water；Graphite flake is added to 300ml, pH=12,45 DEG C of chemistry after activation
Electroless copper is carried out in plating solution, plating solution composition is：CuSO4·5H2O 15g/L, sodium potassium tartrate tetrahydrate 14g/L, EDTA19.5g/L, two
Bipyridyl 0.02g/L, potassium ferrocyanide 0.01g/L, reducing agent use 5g/L formaldehyde [w (HCHO)=36%], plating time
20min.It is rinsed 3 times with distilled water after the completion of plating, obtains the graphite preform blank of plated copper.
Graphite preform blank original sheet-like plane is put into graphite jig upward, is placed in the heating zone on infiltration stove top, stone
Black mold lower opening, connects with conduit, enters for infiltrated metal.Fine copper mold is placed in the heating in medium frequency of infiltration stove lower part
Area.Furnace body is evacuated to vacuum degree 0.1Pa；Graphite jig is preheated to 980 DEG C of heat preservation 10min, opens heating in medium frequency, it will be golden
Belong to copper and be heated to 1150 DEG C, keep the temperature 10min.To furnace body be pressed into high-purity argon gas, when in stove air pressure reach 2MPa after stop pressurising, treat
After metal copper solution is impregnated into green body completely, heat-insulation pressure keeping 10min finally cools to room temperature with the furnace, and it is compound to obtain graphite-copper base
Material.It is 468Wm to measure the thermal conductivity on the vertical graphite plane direction of graphite-copper based composites-1·K-1。
Embodiment 2
Take three pieces of equidimensions, thickness 0.1mm, thermal conductivity 1500Wm-1·K-1Continuous Sheet Graphite as enhancing
Phase is ultrasonically treated with acetone, removes surface and oil contaminant.Icking tool is in the U-shaped lines of graphite surface quarterization, lines size such as Fig. 3 institutes respectively
Show, wherein h is respectively 2.2mm, 2.1mm, 2mm, and l is respectively 6mm, 5mm, 4mm, a 3mm, b 3mm.The U-shaped line that will have been carved
Road is dug upwards one by one, obtains the graphite flake of three-dimensional.
Electroless copper is carried out to graphite flake using chemical-copper-plating process to graphite flake：Electroless copper sensitization stage process is will
Graphite flake adds in the 20ml/LHCl+20g/LSnCl of 500ml2Solution, agitating solution 15min remove solution, and are floated with distilled water
It washes 3 times；Activation stage technique is：Graphite flake after sensitization adds in the 20ml/L HCI+0.5g/LPdCl of 200ml2Solution, stirring
Solution 15min removes solution, and is rinsed 3 times with distilled water；Graphite flake is added to 300ml, pH=12,45 DEG C after activation
Electroless copper is carried out in chemical plating fluid, plating solution composition is：CuSO4·5H2O 15g/L, sodium potassium tartrate tetrahydrate 14g/L, EDTA19.5g/
L, second bipyridine 0.02g/L, potassium ferrocyanide 0.01g/L, reducing agent uses 5g/L formaldehyde [w (HCHO)=36%], during plating
Between 20min.It is rinsed 3 times with distilled water after the completion of plating, three pieces of graphite flakes is stacked gradually, obtain the graphite prefabricated blank of plated copper
Body.
Graphite preform blank original sheet-like plane is put into graphite jig upward, is placed in the heating zone on infiltration stove top, stone
Black mold lower opening, connects with conduit, enters for infiltrated metal.Fine copper mold is placed in the heating in medium frequency of infiltration stove lower part
Area.Furnace body is evacuated to vacuum degree 0.1Pa；Graphite jig is preheated to 1000 DEG C of heat preservation 10min, opens heating in medium frequency, it will
Metallic copper is heated to 1200 DEG C, keeps the temperature 10min.To furnace body be pressed into high-purity argon gas, when in stove air pressure reach 1MPa after stop pressurising,
After metal copper solution is impregnated into green body completely, heat-insulation pressure keeping 10min finally cools to room temperature with the furnace, obtains graphite-copper base and answers
Condensation material.It is 575Wm to measure the thermal conductivity on the vertical graphite plane direction of graphite-copper based composites-1·K-1。
Embodiment 3
Thickness is 1mm, thermal conductivity 1500Wm-1·K-1Continuous Sheet Graphite as reinforced phase, at acetone ultrasound
Reason removes surface and oil contaminant.
Using icking tool in the U-shaped lines of graphite surface quarterization, lines size as shown in Fig. 2, wherein h, l, a, b be respectively 2mm,
3.5mm、2mm、3mm.The U-shaped lines carved is dug upwards one by one, obtains the graphite flake of three-dimensional.
Plating Cr in surface is carried out to graphite surface using vacuum slowly vapor deposition technology.By enough CrCl3With CrH3In mass ratio
10：1 mixing is placed in the micro- evaporation reaction chamber of vacuum, after being put into graphite flake, reaction chamber is evacuated to 10-3Pa.Heat reaction chamber
To 680 DEG C, by vacuum degree control in reative cell in the range of 5-8Pa, the micro- evaporation plating of vacuum 2 hours is carried out to graphite flake, is obtained
Cr layer thickness is the plating graphite flake of 100nm.
Electro-coppering is carried out to its surface using electroplating technology, concrete technology is as follows：Copper-bath is used to match for electroplate liquid
Side is 200g/L CuSO4·5H2O, 70g/L H2SO4.It is controlled using DC current regulator power supply voltage stabilizing, operating voltage is
1.4V.Graphite flake uses phosphorus copper plate as cathode, anode, and bath temperature is room temperature.Reaction 90 minutes, removes graphite flake, washes
And after oven drying, in leading to hydrogen reducing in tube furnace, 15 μ m thick layers of copper of coating surface, the stone with some strength are obtained
Black preform blank.
Graphite preform blank original sheet-like plane is put into graphite jig upward, is placed in the heating zone on infiltration stove top, stone
Black mold lower opening, connects with conduit, enters for infiltrated metal.Fine copper mold is placed in the heating in medium frequency of infiltration stove lower part
Area.Furnace body is evacuated to vacuum degree 0.1Pa；Graphite jig is preheated to 980 DEG C of heat preservation 10min, opens heating in medium frequency, it will be golden
Belong to copper and be heated to 1150 DEG C, keep the temperature 10min.To furnace body be pressed into high-purity argon gas, when in stove air pressure reach 2MPa after stop pressurising, treat
After metal copper solution is impregnated into green body completely, heat-insulation pressure keeping 10min finally cools to room temperature with the furnace, and it is compound to obtain graphite-copper base
Material.It is 644Wm to measure the thermal conductivity on the vertical graphite plane direction of graphite-copper based composites-1·K-1。
Claims (9)
1. a kind of graphite-copper based composites with network blackboard, which is characterized in that the composite material includes graphite
The percent by volume that reinforcement and Copper substrate material, wherein graphite account for composite material is 10-40%, and graphite reinforcement is lamellar
Graphite is designed and is processed by configuration, to three-dimensional three-dimensional development, is nested in matrix copper, graphite and copper two-phase point
It does not keep itself continuous, forms the network blackboard being interweaved.
2. the preparation method of the graphite-copper based composites described in claim 1 with network blackboard, feature exist
In including the following steps：
(1) surface preparation is carried out to graphite surface；
(2) to graphite sheet carry out configuration design, sheet-like plane, that is, X-Y plane of continuous graphite sheet material be designed with
Processing forms several local detachments, the whole subregion still connected with graphite flake layer, which to Z-direction is dug, is made
The graphite flake three-dimensional of script two-dimensional directional；
(3) copper plating treatment is carried out to the graphite flake layer of three-dimensional, obtains covering copper graphite porous preforming base or the graphite by three-dimensional
Lamella carries out nesting, obtains the superposition of several graphite flake layers, the prefabricated blank with gap；
(4) composite material is obtained to prefabricated blank infiltration Copper substrate obtained by step (3) using vacuum pressure infiltration method.
3. the preparation method of the graphite-copper based composites according to claim 2 with network blackboard, feature
It is, in step (1), graphite is continuous synusia graphite, thickness 0.01-6mm, thermal conductivity on graphite sheet in-plane
For 400-1800Wm-1·K-1, the percent by volume that graphite accounts for composite material is 10-40%.
4. the preparation method of the graphite-copper based composites according to claim 2 with network blackboard, feature
It is, in step (1), the method for graphite surface pretreatment is preheated including graphite surface, is cleaned by ultrasonic, acid solution rinsing, lye
At least one of rinsing technique.
5. the preparation method of the graphite-copper based composites according to claim 2 with network blackboard, feature
It is, the graphite surface before or after further including the design of step (2) graphite configuration is modified plated film, and coating film thickness is 0.01-2 μ
M, film layer type are at least one of W, Mo, Cr, Zr, B or their respective compound.
6. the preparation method of the graphite-copper based composites according to claim 2 with network blackboard, feature
It is, in step (2), the principle of graphite configuration design is to make the graphite flake in X-Y directions in the case of ensureing that graphite integrally connects
Extended to longitudinal Z-direction, regional area after Z-direction is dug, former graphite surface leave hole as Copper substrate i.e. metallic copper or
The infiltration channel of copper alloy, " subregion of local detachment " flip angle and number are arbitrary.
7. the preparation method of the graphite-copper based composites according to claim 2 with network blackboard, feature
It is, in step (3), graphite flake layer copper plating treatment is carried out using chemical plating or plating, and thickness of coating is 0.2-30 μm.
8. the preparation method of the graphite-copper based composites according to claim 2 with network blackboard, feature
It is, in step (4), Copper substrate is copper or copper alloy, and the content of copper is more than 50% in copper alloy；The tool of vacuum pressure infiltration
Body technology is：System vacuum carries out prefabricated blank in below 0.1MPa 800-1000 DEG C of preheating before infiltration, keeps the temperature 5-15min
Afterwards, then molten metal is pressed into green body using high-purity argon gas, pressure is in 1000-1400 DEG C of infiltrated metal copper or copper alloy
0.1-4Mpa, pressurize 5-30min, finally cools to room temperature with the furnace, obtains graphite-copper based composites.
9. application of the graphite-copper based composites described in claim 1 in Electronic Packaging.
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| CN108790368A (en) * | 2018-08-30 | 2018-11-13 | 兰州交通大学 | A kind of preparation method of bullet train IGBT encapsulation graphene/metallic composite |
| CN111747372A (en) * | 2019-03-26 | 2020-10-09 | 北京清正泰科技术有限公司 | Metal cover graphite island without edge protrusions and preparation method thereof |
| CN111761061A (en) * | 2020-07-14 | 2020-10-13 | 广东科学技术职业学院 | 3D printing three-dimensional network structure graphite/metal composite material and atmospheric pressure casting infiltration preparation method thereof |
| CN114425647A (en) * | 2020-10-29 | 2022-05-03 | 哈尔滨工业大学（威海） | Method for connecting graphite film and copper |
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| CN111761061B (en) * | 2020-07-14 | 2022-07-19 | 广东科学技术职业学院 | 3D printing three-dimensional network structure graphite/metal composite material and atmospheric pressure casting infiltration preparation method thereof |
| CN114425647A (en) * | 2020-10-29 | 2022-05-03 | 哈尔滨工业大学（威海） | Method for connecting graphite film and copper |
| CN114425647B (en) * | 2020-10-29 | 2023-08-18 | 哈尔滨工业大学（威海） | Method for connecting graphite film and copper |
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