CN112760644A - Composite board, preparation method thereof and soaking plate - Google Patents

Composite board, preparation method thereof and soaking plate Download PDF

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Publication number
CN112760644A
CN112760644A CN202110017035.6A CN202110017035A CN112760644A CN 112760644 A CN112760644 A CN 112760644A CN 202110017035 A CN202110017035 A CN 202110017035A CN 112760644 A CN112760644 A CN 112760644A
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copper foil
graphene layer
composite board
copper
composite
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CN112760644B (en
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刘科海
丁志强
张志强
寇金宗
黄智�
乐湘斌
陈益
王恩哥
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Songshan Lake Materials Laboratory
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0209—Pretreatment of the material to be coated by heating
    • C23C16/0218—Pretreatment of the material to be coated by heating in a reactive atmosphere
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/367—Cooling facilitated by shape of device
    • H01L23/3672—Foil-like cooling fins or heat sinks
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3736—Metallic materials

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Abstract

The application relates to the field of materials, in particular to a composite board, a preparation method thereof and a soaking board. The composite board comprises a first copper foil, a graphene layer and a second copper foil which are sequentially stacked; wherein the number of crystal domains of the first copper foil is less than or equal to 5/square centimeter; the second copper foil is electroplated copper. The composite board is characterized in that the first copper foil with the crystal domain number smaller than or equal to 5/square centimeter has better heat conductivity, the graphene layer is arranged on the first copper foil, then the electroplated copper is arranged on the graphene layer, the thickness of the electroplated copper can be adjusted to 1 mu m to 1mm, the electroplated copper and the first copper foil can overcome the problem that the graphene layer cannot be used as a structural material, and the composite board is composed of the first copper foil with the smaller crystal domain number and the electroplated copper which are respectively positioned on the two sides of the graphene layer and has better heat conductivity coefficient and proper strength.

Description

Composite board, preparation method thereof and soaking plate
Technical Field
The application relates to the field of materials, in particular to a composite board, a preparation method thereof and a soaking board.
Background
When the chip continuously runs under high load, a large amount of heat can be generated, so that the temperature of the chip is overhigh, the phenomena of operation blockage, frame dropping, frequency reduction and the like occur, and the performance of the chip is obviously reduced. A soaking plate may be used for it to heat. The soaking plate is mainly composed of an upper cover plate, a lower cover plate, a sealed cavity, a capillary structure and a cooling medium, wherein the upper cover plate and the lower cover plate are usually made of pure copper plates and welded into a vacuum cavity with a fine structure on the inner wall. The vapor chamber is a vacuum chamber with a fine structure on the inner wall, and is usually made of copper. However, the thermal conductivity of the existing soaking plate needs to be improved.
Disclosure of Invention
The embodiment of the application aims to provide a composite plate, a preparation method thereof and a soaking plate, and aims to improve the heat conductivity coefficient of the soaking plate.
The application provides a composite board, which comprises a first copper foil, a graphene layer and a second copper foil which are sequentially stacked;
wherein the number of crystal domains of the first copper foil is less than or equal to 5/square centimeter;
the second copper foil is electroplated copper.
The composite board is characterized in that the first copper foil with the crystal domain number smaller than or equal to 5/square centimeter has better heat conductivity, the graphene layer is arranged on the first copper foil, then the electroplated copper is arranged on the graphene layer, the problem that the graphene layer cannot be used as a structural material can be solved by the electroplated copper and the first copper foil, and the composite board formed by the first copper foil with the smaller crystal domain number and the electroplated copper which are respectively positioned on the two sides of the graphene layer can have better heat conductivity coefficient.
In some embodiments of the present application, the first copper foil has a thickness of 3 to 150 μm.
In some embodiments of the present application, the first copper foil and the graphene layer have a hardness of 30-60 HV.
In some embodiments of the present application, the second copper foil has a thickness of 1 to 1000 μm;
in some embodiments of the present application, the hardness of the composite plate is 100-200 HV.
In some embodiments of the present application, the composite plate comprises a plurality of graphene layers and a plurality of second copper foils; the graphene layer and the second copper foil are arranged in a crossed mode, and the graphene layer covers the first copper foil.
The application also provides a preparation method of the composite board, which comprises the following steps:
growing a graphene layer on the first copper foil;
preparing a second copper foil on the graphene layer in an electroplating mode;
wherein the number of domains of the first copper foil is less than or equal to 5 per square centimeter.
In some embodiments of the present application, before growing the graphene layer on the first copper foil, the method further includes preparing the first copper foil, specifically including:
heating the electrolytic copper foil or rolled copper foil to 800-1075 ℃ under an inert atmosphere, and then annealing under a reducing atmosphere.
In some embodiments of the present application, the step of growing the graphene layer on the first copper foil is performed by chemical vapor deposition.
The application also provides a soaking plate, the soaking plate is formed by connecting the composite plates.
The soaking plate provided by the embodiment of the application has the advantages of the composite plate.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
Fig. 1 shows a schematic structural view of a soaking plate provided in an embodiment of the present application.
Icon: 100-composite board; 110-a first copper foil; 120-a graphene layer; 130-second copper foil.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The soaking plate needs to meet the requirements of lightness, thinness and large size, which can lead to the weakening of the plate structure strength, and the plate structure is easy to deform under certain conditions, finally leads to the structural failure, and brings adverse effects to heat dissipation. The composite materials of copper, stainless steel or titanium alloy and the like are adopted as the upper cover plate and the lower cover plate, although the strength and the surface hardness of the plates can be increased and the plates are not easy to deform, the heat conduction performance and the welding performance of the whole soaking plate are affected due to the serious deficiency of the heat conduction performance of the stainless steel or titanium alloy materials. Some composite materials of 'Cu + Gr' or 'Cu + CNT' prepared by doping graphite sheets or CNTs in a copper cover plate material have limited improvement on the overall heat conduction and strength performance of the soaking plate due to the discontinuity of the graphite and the CNTs.
The composite sheet, the method for manufacturing the same, and the vapor chamber according to the embodiments of the present application will be described in detail below.
Fig. 1 shows a schematic structural diagram of a composite board 100 provided in an embodiment of the present application, please refer to fig. 1, where the composite board 100 includes a first copper foil 110, a graphene layer 120, and a second copper foil 130. The graphene layer 120 is covered on the first copper foil 110, and the second copper foil 130 is covered on the graphene layer 120.
In the present application, the number of domains of the first copper foil 110 is less than or equal to 5 per square centimeter. For example, the number of domains of the first copper foil 110 may be 5/cm, 4/cm, 3/cm, 2/cm, or 1/cm, etc.
The first copper foil 110 having the number of domains less than or equal to 5 per square centimeter has better thermal and electrical conductivity.
In some embodiments of the present application, the thickness of the first copper foil 110 may be 3-150 μm, for example, may be 3 μm, 5 μm, 8 μm, 18 μm, 28 μm, 36 μm, 42 μm, 70 μm, 100 μm, 150 μm, and the like. The thickness of the first copper foil 110 is 3-150 μm, which enables the first copper foil to have high strength and good thermal and electrical conductivity.
In other embodiments of the present application, the thickness of the first copper foil 110 may be other values, and may be set according to the use and usage scenario of the composite board 100.
In the present application, the first copper foil 110 having the number of crystal domains of 5 or less per square centimeter may be prepared by:
heating the electrolytic copper foil or rolled copper foil to 800-1075 ℃ under an inert atmosphere, and then annealing under a reducing atmosphere.
As an example, the inert atmosphere may be N2Ar or He, etc.; the electrolytic copper foil or rolled copper foil is heated to 800-.
For example, electrolytic copper or rolled copper (thickness 3-150 μm, number of domains > 10000/cm)2) Feeding into an annealing apparatus, introducing N2Heating with inert gas such as Ar or He;
when the temperature in the annealing equipment reaches 800-2Or a reducing gas such as CO, or the like, is startedAnnealing; the copper foil with super large crystal domains can be obtained by the high-temperature annealing method, and then the copper foil is selected, for example, the copper foil with the crystal domain number N less than or equal to 5 per square centimeter is selected, namely N is less than or equal to 5/cm2。
In other embodiments of the present application, the super-domain copper foil may be prepared without the above-mentioned high-temperature annealing method, for example, a commercially available super-domain copper foil may be obtained.
As mentioned above, the graphene layer 120 covers the first copper foil 110, and the graphene layer 120 and the first copper foil 110 can increase the heat conduction and the electric conduction performance of the composite board 100.
In an embodiment of the present application, the graphene layer 120 may be prepared by chemical vapor deposition.
For example, the first copper foil 110 is placed in a furnace, and CH is introduced4And H2The graphene layer 120 is prepared by growing single-layer or multi-layer graphene on the first copper foil 110 as a substrate.
In some embodiments of the present application, the hardness of the first copper foil 110 and the graphene layer 120 may be set to be 30 to 60HV by setting the thickness of the graphene layer 120; in other words, the hardness of the first copper foil 110 and the graphene layer 120 together is 30 to 60HV, and may be, for example, 30HV, 35HV, 40HV, 50HV, or 60 HV.
In other embodiments of the present application, the graphene layer 120 may be prepared by other preparation methods, and the preparation method thereof is not limited in the present application.
The second copper foil 130 is covered on the graphene layer 120, and in this application, the second copper foil 130 is an electrolytic copper foil, in other words, the second copper foil 130 is formed by means of electrolytic copper.
In the present embodiment, a layer of foil is plated on the graphene layer 120 to form the second copper foil 130.
In some embodiments of the present application, the thickness of the second copper foil 130 is 1-1000 μm, for example, the thickness of the second copper foil 130 may be 1 μm, 5 μm, 10 μm, 100 μm, 135 μm, 150 μm, 250 μm, 300 μm, 500 μm, and the like.
In the embodiment of the present application, the second copper foil 130 has the same crystal domain and crystal plane index as the first copper foil 110, and the crystal domain size is the same.
In the embodiment of the present application, the hardness of the second copper foil 130, the graphene layer 120 and the first copper foil 110 is 100-200 HV; for example, 100HV, 135HV, 140HV, 150HV, 160HV, 182HV, 190HV, 200HV, etc.
In some embodiments of the present disclosure, the thickness of the composite board 100 may be set as required, and a plurality of graphene layers 120 and a plurality of second copper foils 130 may be prepared, where the graphene layers 120 and the second copper foils 130 are spaced apart from each other. In other words, the composite board 100 may include a plurality of graphene layers 120, a plurality of second copper foils 130; a layer of second copper foil 130 is disposed between two adjacent graphene layers 120. Set up graphite alkene layer 120 on the first copper foil 110, set up second copper foil 130 on graphite alkene layer 120, in order to increase composite sheet 100's thickness, can continue to set up graphite alkene layer 120 on second copper foil 130, then set up second copper foil 130 on graphite alkene layer 120, set gradually until reaching preset thickness.
Accordingly, in the embodiment of the present application, the number and thickness of the graphene layer 120 and the second copper foil 130 may be set according to specific requirements.
The composite board 100 provided by the embodiment of the application has at least the following advantages:
the composite board 100 includes a first copper foil 110 having a number of domains less than or equal to 5/cm, a second copper foil 130 formed by copper electroplating, and a graphene layer 120 between the first copper foil 110 and the second copper foil 130; the graphene layer 120 has excellent tensile strength (>1GPa) and thermal conductivity (about 5000W/m · k in the transverse direction), the strength of the composite board 100 can be improved while the thickness of the composite board is reduced, the first copper foil 110 and the second copper foil 130 on both sides of the graphene layer 120 can overcome the problem that the graphene layer 120 cannot be used as a structural material alone, and the first copper foil 110 with a small number of crystal domains and the second copper foil 130 formed by electroplating can have a high thermal conductivity coefficient in combination with the graphene layer 120.
The present application further provides a method for preparing the composite board 100, which mainly comprises the following steps:
growing a graphene layer 120 on the first copper foil 110; the number of domains of the first copper foil 110 is less than or equal to 5 per square centimeter. Please refer to the above description for a specific method for growing the graphene layer 120 on the first copper foil 110, for example, the graphene layer 120 is prepared by chemical vapor deposition. The method comprises the following steps: the first copper foil 110 is placed in a furnace, CH is introduced4And H2The graphene layer 120 is prepared by growing at least one layer of graphene with the first copper foil 110 as a substrate, and illustratively, one, two or more layers of graphene may be grown to form the graphene layer 120.
Before the graphene layer 120 is grown on the first copper foil 110, preparing the first copper foil 110, wherein the first copper foil 110 with the number of crystal domains less than or equal to 5/square centimeter can be prepared by a high-temperature annealing process, for example; the method comprises the following steps: electrolytic copper or rolled copper (thickness 3-150 μm, number of crystal domains > 10000/cm)2) Feeding into an annealing apparatus, introducing N2Heating with inert gas such as Ar or He; heating to 800-1075 deg.C (such as 800 deg.C, 900 deg.C, 1000 deg.C), and introducing H2Or a reducing gas such as CO, to start annealing.
After the graphene layer 120 is prepared, a second copper foil 130 is prepared on the graphene layer 120. In the present application, the second copper foil 130 is prepared by means of electroplating.
The composite board 100 with the advantages can be obtained by the preparation method provided by the embodiment of the application, and the second copper foil 130 obtained by the preparation method has the same crystal domain number, the same crystal face index and the same crystal domain size as the first copper foil 110. The preparation method can improve the heat-conducting property of the composite board 100.
The present application also provides a vapor chamber made from the composite sheet 100. For example, the vapor chamber may be formed by welding the composite plate 100.
The soaking plate comprises an upper cover plate and a lower cover plate, and a cavity is formed between the upper cover plate and the lower cover plate; in this application, the composite sheet is all chooseed for use to upper cover plate and lower apron.
The embodiment of the application does not limit the specific preparation method and the shape and the size of the soaking plate, and can be set according to requirements and application scenes.
The application provides a soaking plate has the advantage of above-mentioned composite sheet 100, and heat conductivility is better when having higher intensity.
The features and properties of the present application are described in further detail below with reference to examples.
Example 1
The embodiment provides a soaking plate which is mainly prepared by the following steps:
s1, electrolyzing or rolling copper (thickness 25 μm, number of crystal domains > 10000/cm) at original polycrystalline boundary2) Feeding into an annealing apparatus, introducing N2The temperature is raised.
S2, feeding the copper foil into an annealing device, and feeding H when the temperature reaches 950 DEG C2And (6) annealing is started.
S3, preserving the heat for 4 hours at 950 ℃ to obtain a large-domain copper foil (first copper foil), wherein N is less than or equal to 5/cm2And screening the copper foil with the crystal domain number of 5 for subsequent experiments.
S4, keeping the temperature for 4 hours, and introducing CH4And H2Growing at least one graphene layer on the copper foil substrate with the ultra-large crystal domain by a CVD (chemical vapor deposition) process; the hardness of the graphene layer and the first copper foil was measured after the graphene layer was prepared.
S5, preparing a second copper foil on the graphene layer grown on the graphene layer by adopting a copper electroplating process, wherein the copper of the second copper foil is consistent with the crystal face index of the super-large domain, the domain size is consistent, the thickness of the electroplated copper is 150 microns, and the composite plate is obtained after preparing the second copper foil, and the hardness of the composite plate is 100 HV.
And S6, welding the composite plate serving as an upper cover plate material and a lower cover plate material into a vacuum cavity structure with a fine structure on the inner wall to obtain the soaking plate.
Examples 2 to 5 and comparative examples 1 to 4
Examples 2 to 5 and comparative examples 1 to 4 each provide a soaking plate, which is different from example 1 in that first copper foils having different numbers of domains were screened and fabricated into composite plates, and subsequent experiments were performed. See table 1 for details.
Test example
The composite panels of examples 1-5 and comparative examples 1-4 were tested and the results are shown in table 1.
(1) Detecting the number of crystal domains: and observing by a metallographic microscope, and randomly taking the number of the grain boundaries within the range of 10 x 10 mm.
(2) Hardness: GB-T4340.1.
(3) And (3) detecting the purity and the oxygen content of copper: GB/T5121.
(4) And (3) testing thermal conductivity: GB/T22588-.
TABLE 1
Figure BDA0002886392990000081
Figure BDA0002886392990000091
As can be seen from table 1, the composite plate provided in the examples of the present application has higher hardness and higher thermal conductivity than the composite plate provided in the comparative examples, and can be used as a soaking plate with high strength and high thermal conductivity.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A composite board is characterized by comprising a first copper foil, a graphene layer and a second copper foil which are sequentially stacked;
wherein the number of crystal domains of the first copper foil is less than or equal to 5/square centimeter;
the second copper foil is electroplated copper.
2. The composite board of claim 1, wherein the first copper foil has a thickness of 3 μ ι η to 150 μ ι η.
3. A composite board according to claim 1, wherein the first copper foil and the graphene layer have a hardness of 30HV-60 HV.
4. The composite board of claim 1, wherein the second copper foil has a thickness of 1 μ ι η to 1000 μ ι η.
5. A composite board according to claim 1, characterised in that the hardness of the composite board is 100HV-200 HV.
6. A composite board according to any of claims 1-5, wherein the composite board comprises a plurality of the graphene layers and a plurality of the second copper foils; the graphene layer and the second copper foil are arranged in a laminating and crossing mode, and the graphene layer covers the first copper foil.
7. A method of making a composite panel according to any of claims 1 to 6, comprising:
growing a graphene layer on the first copper foil;
preparing a second copper foil on the graphene layer in an electroplating mode;
wherein the number of domains of the first copper foil is less than or equal to 5 per square centimeter.
8. The method for preparing a composite board according to claim 7, wherein before growing the graphene layer on the first copper foil, the method further comprises preparing the first copper foil, and specifically comprises:
heating the electrolytic copper foil or rolled copper foil to 800-1075 ℃ under an inert atmosphere, and then annealing under a reducing atmosphere.
9. The method for preparing a composite board according to claim 7, wherein the step of growing the graphene layer on the first copper foil is carried out by growing the graphene layer by means of chemical vapor deposition.
10. A soaking plate characterized in that it is formed by joining the composite plates according to any one of claims 1 to 6.
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