CN110564376A - Composite material for thermal management and preparation method thereof - Google Patents
Composite material for thermal management and preparation method thereof Download PDFInfo
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Abstract
the invention belongs to the technical field of graphene preparation, and particularly relates to a composite material for thermal management and a preparation method thereof. The composite material comprises two metal layers arranged at intervals, and a first heat transfer layer and a second heat transfer layer which are arranged on the two metal layers, wherein the heat transfer interfaces of the first heat transfer layer and the second heat transfer layer are vertical to each other; the composite material is a heat management material which is integrated in the horizontal direction and the vertical direction, is a high-efficiency heat management structure which is vertically positioned between a heat source and a heat sink, and has better heat conductivity and thermal expansion coefficient matching with an integrated circuit chip.
Description
Technical Field
the invention belongs to the technical field of graphene preparation, and particularly relates to a composite material for thermal management and a preparation method thereof.
Background
with the increasing integration scale of electronic circuits, the heating value of the integrated circuit in unit area during operation is correspondingly increased, which leads to the great increase of the failure probability of the packaging system. In order to improve the package reliability of integrated circuits, there is a pressing need for new thermal management materials with high thermal conductivity and matching expansion coefficients of integrated circuit chips.
graphene is the thinnest two-dimensional material discovered at present, is a carbon material formed by tightly stacking single-layer carbon atoms, has extremely high in-plane thermal conductivity coefficient, the thermal conductivity can reach 5000W/m.K, and is higher than that of a carbon nano tube and diamond, so the graphene is a thermal conductive material with the optimal performance at present, has huge application potential in the field of thermal management materials, and the preparation technology of the current graphene tends to be mature, the production cost of the current graphene is greatly reduced, and the large-scale application of the graphene in composite materials becomes possible.
chinese patent document CN108581253A discloses a method for encapsulating a sandwich-type graphene-based heat dissipation plate, which includes laser drilling, surface metallization, assembly and encapsulation, and the sandwich-type graphene-based heat dissipation plate prepared by the method can only exert the advantage of heat transfer in a horizontal plane, and the vertical heat transfer needs surface metal copper and via hole metal copper. In addition, the thermal management material graphene/metal matrix composite material has poor matching with the thermal expansion coefficient of an integrated circuit chip, and the material structure and the function are single, in the prior art, methods such as modification or addition of an auxiliary agent are adopted to modify graphene, so that the graphene can only meet the thermal management in a single dimension.
disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to overcome the defects in the prior art that the thermal management material related to graphene has poor thermal conductivity and does not meet the requirement for matching with the thermal expansion coefficient of the integrated circuit chip, and the like, so as to provide a composite material for thermal management and a preparation method thereof.
therefore, the invention provides the following technical scheme.
The invention provides a composite material for heat management, which comprises two metal layers arranged at intervals, and a first heat transfer layer and a second heat transfer layer which are arranged on the two metal layers, wherein heat transfer interfaces of the first heat transfer layer and the second heat transfer layer are vertical to each other.
The first heat transfer layer and the second heat transfer layer are stacked.
the first heat transfer layer is a graphene film, and the graphene film is arranged in parallel with the two metal layers.
The second heat transfer layer is a plurality of graphene films, and the graphene films are perpendicular to the two metal layers.
The second heat transfer layer comprises a plurality of graphene film rolls, the graphene film rolls are cylindrical, and the cross sections of the graphene film rolls are spiral.
further, the diameter of the cylindrical graphene film roll is 0.5-5mm, and the height of the cylindrical graphene film roll is 0.1-10 mm; further, the diameter and the height of the graphene film roll can be adjusted according to actual requirements.
The two metal layers comprise a first metal layer and a second metal layer;
the first metal layer has a conductivity of not less than 1 × 107m.omega; the second metal layer has a conductivity of not less than 1 × 107/m·Ω。
the first metal layer is made of high-conductivity materials such as copper, aluminum, silver-copper alloy and the like; the second metal layer is made of high-conductivity materials such as copper, aluminum, silver and the like.
The present invention also provides a method of making the above-described composite material for thermal management, comprising,
and sequentially stacking the first metal layer, the first heat transfer layer, the second heat transfer layer and the second metal layer on the heat sink substrate, and cladding to obtain the composite material.
The cladding temperature is not lower than the melting point temperature of the higher melting point of the first metal layer and the second metal layer;
the cladding time is 0.5-2 h.
The heating rate of cladding is 1-20 ℃/min; the cooling rate after cladding is 1-20 ℃/min.
The cladding is carried out in vacuum or inert atmosphere;
the vacuum degree of the cladding is (1 multiplied by 10)-3-1)Pa。
The graphene film is prepared by adopting a method of combining graphene oxide vacuum filtration and chemical reduction; or the like, or, alternatively,
Prepared by adopting a chemical vapor deposition method.
the graphene film is prepared by adopting a method combining graphene oxide vacuum filtration and chemical reduction, and specifically, graphene oxide powder is dispersed in deionized water, ultrasonic dispersion is carried out to prepare 0.1-1.0g/L graphene oxide dispersion liquid, then a graphene film is prepared by adopting a vacuum filtration method, a film is formed under the pressure of 0.5-1.5bar, and the graphene film is obtained after reduction.
the size parameters of the graphene film prepared by adopting the method combining vacuum filtration and chemical reduction are as follows: the length is 10-100mm, the width is 10-100mm, and the thickness is 20-200 μm; parameters of the graphene film prepared by the chemical vapor deposition method are as follows: the length is 10-100mm, the width is 10-100mm, and the thickness is 20-200 μm;
The heat sink substrate is made of WCu, MoCu, Cu-Mo (Cu) -Cu, diamond-Cu, iron-nickel-cobalt alloy or stainless steel; the parameters of the heat sink substrate are as follows: the length is 10-100mm, the width is 10-100mm, and the thickness is 200-2000 μm;
the thickness of the first metal layer and the second metal layer is not less than 0.03 mm.
the technical scheme of the invention has the following advantages:
1. The composite material for heat management comprises two metal layers arranged at intervals, and a first heat transfer layer and a second heat transfer layer which are arranged on the two metal layers, wherein heat transfer interfaces of the first heat transfer layer and the second heat transfer layer are vertical to each other; the composite material is a heat management material which is integrated in the horizontal direction and the vertical direction, is a high-efficiency heat management structure which is vertically positioned between a heat source and a heat sink, and has better heat conductivity and thermal expansion coefficient matching with an integrated circuit chip.
2. According to the composite material for heat management, the first heat transfer layer of the composite material is the graphene film, heat transfer in the horizontal direction is achieved, the second heat transfer layer is the plurality of graphene films, the plurality of graphene films are perpendicular to the two metal layers, heat transfer in the vertical direction is achieved, the composite material is provided with graphene which in-plane vertical heat transfer and in-plane horizontal heat transfer of a planar structure are combined, and the composite material is an efficient heat management structure which is vertically located between a heat source and a heat sink.
The composite material can fully exert the high in-plane thermal conductivity of graphene and the high conductivity of metal, different metal layers can be selected according to the actual requirement of the expansion coefficient matching property of the integrated circuit chip, the height of the graphene film roll is adjusted, the thermal expansion coefficient of the composite material is adjusted, and the composite material can be suitable for the integrated circuit chips with different thermal expansion coefficient requirements.
3. according to the composite material for thermal management, the limitation of the materials of the first metal layer and the second metal layer has the characteristic of high material conductivity, and the composite material is suitable for the requirement of preparing the material by a cladding method on the low melting point of the material; the heat sink substrate material can meet the requirement of thermal expansion coefficient and thermal conductivity.
4. The invention provides a preparation method of a composite material for heat management, which melts a first metal layer and a second metal layer in a cladding mode, wherein a first heat transfer layer is in seamless connection with a heat sink substrate through the first metal layer, so that the first heat transfer layer and a second heat transfer layer are completely coated by the metal layers to realize horizontal heat transfer of the composite material, the second heat transfer layer is distributed on the first heat transfer layer in an array mode to realize vertical heat transfer of the composite material, graphene is respectively embedded into the heat sink substrate in an array spiral structure and a planar structure, the heat sink substrate, the first metal layer, the first heat transfer layer, the second heat transfer layer and the second metal layer are fused into a heat management material, multi-dimensional heat management is achieved, the composite material for heat management forms graphene with in-plane vertical heat transfer and in-plane horizontal heat transfer combination in a plane structure, and the graphene is a high-efficiency heat management structure vertically located between a heat source and a heat sink.
The preparation method provided by the invention can give full play to the high in-plane thermal conductivity of the graphene and the high conductivity of the metal layer, and the heat sink substrate can select heat sink substrate materials with different thermal expansion coefficients according to the actual requirement of the thermal expansion coefficient matching property of the integrated circuit chip, adjust the height of the graphene film roll, realize the adjustment of the overall thermal expansion coefficient of the graphene/metal-based composite material, and can be suitable for the integrated circuit chips with different thermal expansion coefficient requirements; the graphene/metal matrix composite is stably positioned between the heat source and the heat sink substrate, so that the heat dissipation efficiency is greatly improved, and the graphene/metal matrix composite has a great application value in the field of electronic packaging.
5. According to the preparation method of the composite material for heat management, provided by the invention, the metal material and graphene can be prevented from being oxidized in the cladding process by controlling the cladding atmosphere and vacuum degree, so that the bonding interface and bonding strength of the material are prevented from being influenced; the cladding temperature and time are controlled to ensure that the metal layer can be fully melted and completely bonded with other material interfaces, so that the integration of materials is realized; in the cladding process, the material failure caused by overlarge internal stress in the material preparation process can be prevented by controlling the temperature rise rate and the temperature drop rate of the temperature.
6. According to the preparation method of the composite material for heat management, the graphene film in the method is prepared by a method of combining graphene oxide vacuum filtration and chemical reduction or a chemical vapor deposition method, wherein single-layer or multi-layer graphene with uniform distribution, high quality, accurate thickness and good heat conductivity can be prepared by the vacuum filtration method; the chemical vapor deposition can prepare single-layer or multi-layer graphene with high quality, large area and good continuity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic view of a lay-up structure of a composite material for thermal management in example 1 of the present invention;
FIG. 2 is a front view of a composite material for thermal management in example 1 of the present invention;
fig. 3 is a schematic view of a composite material placed in a cladding apparatus during cladding in example 1 of the present invention;
Fig. 4 is a schematic structural diagram of a composite material after cladding in example 1 of the present invention;
FIG. 5 is a schematic structural view of a second heat transfer layer of the clad composite material after the cladding of embodiment 1 of the present invention;
Reference numerals:
1-a heat sink substrate; 2-a first metal layer; 3-a first heat transfer layer; 4-a second heat transfer layer; 5-a second metal layer; 6-molding; 7-heating means.
Detailed Description
the following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides a composite material for thermal management and a preparation method thereof, and the preparation method specifically comprises the following steps:
Preparing a graphene film: dispersing graphene oxide powder in deionized water, performing ultrasonic dispersion to prepare 1.0g/L graphene oxide dispersion liquid, preparing a graphene film with the length of 50mm, the width of 30mm and the thickness of 200 mu m by adopting a vacuum filtration method, forming the film under the pressure of 1bar, and reducing by adopting HI solution to obtain the graphene film;
Helical structure graphene: the graphene film is rolled to form a cylindrical graphene film roll with the diameter of 1mm, and the cross section of the graphene film is made to be spiral. Cutting the graphene film roll to enable the height of the graphene film roll to be 0.3mm for later use;
Preparing the composite material for thermal management by a cladding method: with the WCu10 with the length, width and thickness of 10mm multiplied by 0.5mm as the heat sink substrate 1, a copper foil (first metal layer 2) with the length, width and thickness of 10mm multiplied by 0.05mm, a graphene film (first heat transfer layer 3) with the length, width and thickness of 10mm multiplied by 0.3mm, 16 pieces of the spiral-structure graphene (second heat transfer layer 4) and a copper sheet (second metal layer 5) with the length, width and thickness of 10mm multiplied by 0.3mm are sequentially stacked on the heat sink substrate, and the stacking process is shown in the figure1 and FIG. 2, then, under a vacuum of 1.3X 10-2Heating to 1300 ℃ at the heating rate of 5 ℃/min under the condition of Pa, preserving heat for 1h, and cooling to room temperature at the heating rate of 10 ℃/min after cladding is finished to obtain the composite material for heat management, wherein the front view of the composite material is shown in figure 4; fig. 3 is a schematic view of a composite material for thermal management in a cladding apparatus; fig. 5 a and b are schematic views showing the spiral structure of the second heat transfer layer after the perspective of the second metal layer of the composite material.
example 2
The embodiment provides a composite material for thermal management and a preparation method thereof, and the preparation method specifically comprises the following steps:
Preparing a graphene film: dispersing graphene oxide powder in deionized water, performing ultrasonic dispersion to prepare 0.1g/L graphene oxide dispersion liquid, preparing a graphene film with the length of 100mm, the width of 100mm and the thickness of 200 mu m by adopting a vacuum filtration method, wherein the film forming pressure is 0.5bar, and reducing by adopting a sodium borohydride solution to obtain the graphene film;
helical structure graphene: the graphene film is rolled to form a cylindrical graphene film roll with the diameter of 5mm, and the cross section of the graphene film is made to be spiral. Cutting the graphene film roll to enable the height of the graphene film roll to be 0.5mm for later use;
preparing the composite material for thermal management by a cladding method: a copper foil (first metal layer 2) of 100mm X50 mm X0.03 mm, a graphene film (first heat transfer layer 3) of 100mm X50 mm X0.02 mm, 25 pieces of the above-mentioned spiral-structured graphene (second heat transfer layer 4), and a copper thin plate (second metal layer 5) of 50mm X0.5 mm were stacked in this order on a 50mm X0.5 mm MoCu30 heat sink substrate, and then the resultant was subjected to a vacuum of 1.3X 10-2And under the condition of Pa, heating to 1300 ℃ at the speed of 5 ℃/min, preserving heat for 0.5h, and after cladding is finished, cooling to room temperature at the speed of 10 ℃/min to obtain the composite material for heat management.
Example 3
The embodiment provides a composite material for thermal management and a preparation method thereof, and the preparation method specifically comprises the following steps:
preparing a graphene film: growing a single-layer graphene film on the surface of copper by adopting a chemical vapor deposition method to obtain a copper-graphene film with the length of 100mm, the width of 50mm and the thickness of 30 mu m;
Helical structure graphene: the rolled graphene film is formed into a cylindrical copper-graphene film roll with a diameter of 3mm, and the cross section of the copper-graphene film is made to be spiral. Cutting the copper-graphene film roll to enable the height of the copper-graphene film roll to be 0.5mm for later use;
Preparing the composite material for thermal management by a cladding method: with WCu20 of 50mm × 50mm × 0.5mm as a heat sink substrate, on the heat sink substrate were stacked in this order aluminum foil of 50mm × 50mm × 0.03mm (first metal layer 2), copper-graphene film of 50mm × 50mm × 0.03mm (first heat transfer layer 3), 64 of the above-mentioned graphene of spiral structure (second heat transfer layer 4), and aluminum sheet of 50mm × 50mm × 0.5mm (second metal layer 5), and then, the degree of vacuum was 1 × 10-1And under the condition of Pa, heating to 850 ℃ at the speed of 19 ℃/min, preserving heat for 1h, and after cladding, cooling to normal temperature at the speed of 2 ℃/min to obtain the composite material for heat management.
Example 4
The embodiment provides a composite material for thermal management and a preparation method thereof, and the preparation method specifically comprises the following steps:
Preparing a graphene film: producing a single-layer graphene film on the surface of copper by adopting a chemical vapor deposition method to obtain a copper-graphene film with the length of 100mm, the width of 100mm and the thickness of 20 mu m;
Helical structure graphene: the rolled graphene film is formed into a cylindrical copper-graphene film roll with a diameter of 2mm, and the cross section of the copper-graphene film is made to be spiral. Cutting the copper-graphene film roll to enable the height of the copper-graphene film roll to be 0.3mm for later use;
Preparing the composite material for thermal management by a cladding method: taking 20mm multiplied by 0.5mm Cu-Mo-Cu (1:1:1) as a heat sink substrate, stacking 20mm multiplied by 0.03mm silver foil (a first metal layer 2), 20mm multiplied by 0.02mm copper-graphene film (a first heat transfer layer 3), 25 spiral structure graphene (a second heat transfer layer 4) and 20mm multiplied by 0.3mm silver sheet (a second metal layer 5) on the heat sink substrate in sequence, heating to 1100 ℃ at a speed of 10 ℃/min under the condition of a vacuum degree of 1Pa, preserving heat for 1h, and cooling to room temperature at a speed of 20 ℃/min after cladding is finished, thereby obtaining the composite material for heat management.
Example 5
The embodiment provides a composite material for thermal management and a preparation method thereof, and the preparation method specifically comprises the following steps:
Preparing a graphene film: producing a single-layer graphene film on the surface of copper by adopting a chemical vapor deposition method to obtain a copper-graphene film with the length of 100mm, the width of 80mm and the thickness of 20 mu m;
Helical structure graphene: the graphene film is rolled to form a cylindrical graphene film roll with the diameter of 2mm, and the cross section of the graphene film is made to be spiral. Cutting the graphene film roll to enable the height of the graphene film roll to be 0.3mm for later use;
Preparing the composite material for thermal management by a cladding method: with 20mm × 20mm × 0.5mm MoCu15 as a heat sink substrate, a 20mm × 20mm × 0.03mm silver foil (first metal layer 2), a 20mm × 20mm × 0.5mm copper-graphene thin film (first heat transfer layer 3), 36 of the above-described spiral-structured graphene (second heat transfer layer 4), and a 20mm × 20mm × 0.3mm copper thin plate (second metal layer 5) were stacked in this order on the heat sink substrate, and then, the heat sink substrate was evacuated at a vacuum degree of 1 × 10mm × 0.3mm-3And under the condition of Pa, heating to 1200 ℃ at the speed of 5 ℃/min, preserving heat for 1h, and after cladding is finished, cooling to room temperature at the speed of 10 ℃/min to obtain the composite material for heat management.
test examples
The test example provides performance tests and test results of the composite materials prepared in examples 1-5, the test method is as follows, and the test results are shown in table 1;
TABLE 1 results of performance testing of composites prepared in examples 1-5
M1, M2, M3, M4, and M5 in table 1 represent the composites for thermal management prepared in examples 1 to 5, respectively.
As can be seen from table 1, the composite material for thermal management prepared by the present invention can adjust the thermal expansion coefficient of the composite material by adjusting parameters such as the type of the metal layer, the height of the graphene film roll, and the like, and is suitable for integrated circuit chips with different thermal expansion coefficient requirements; the composite material for thermal management provided by the invention has higher thermal conductivity.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (13)
1. The composite material for heat management is characterized by comprising two metal layers arranged at intervals and a first heat transfer layer and a second heat transfer layer which are arranged on the two metal layers, wherein heat transfer interfaces of the first heat transfer layer and the second heat transfer layer are vertical to each other.
2. The composite for thermal management of claim 1, wherein said first heat transfer layer and said second heat transfer layer are disposed in a stack.
3. the composite for thermal management of claim 1 or 2, wherein the first heat transfer layer is a graphene film, and the graphene film is disposed parallel to the two metal layers.
4. The composite for heat management according to any of claims 1 to 3, wherein the second heat transfer layer is a plurality of graphene thin films, and the plurality of graphene thin films are arranged perpendicular to the two metal layers.
5. the composite for thermal management of claim 4, wherein said second heat transfer layer comprises a plurality of graphene film rolls, said graphene film rolls being cylindrical and having a cross-section that is helical.
6. The composite for heat management according to claim 5, wherein the cylindrical graphene film roll has a diameter of 0.5-5mm and a height of 0.1-10 mm.
7. The composite for thermal management according to any of claims 1-6, wherein said two metal layers comprise a first metal layer and a second metal layer;
The first metal layer has a conductivity of not less than 1 × 107/m·Ω；
The second metal layer has a conductivity of not less than 1 × 107/m·Ω。
8. The composite for thermal management according to claim 7, wherein said first metal layer is copper, aluminum, silver copper alloy;
The second metal layer is made of copper, aluminum and silver.
9. A method of making a composite material for thermal management according to any one of claims 1 to 8, comprising,
and sequentially stacking the first metal layer, the first heat transfer layer, the second heat transfer layer and the second metal layer on the heat sink substrate, and cladding to obtain the composite material.
10. The method of claim 9, wherein the cladding temperature is not lower than the melting point temperature of the higher melting point of the first metal layer and the second metal layer;
The cladding time is 0.5-2 h.
11. The method of claim 9 or 10, wherein the cladding heating rate is 1-20 ℃/min; the cooling rate after cladding is 1-20 ℃/min.
12. The method of any one of claims 9-11, wherein the cladding is performed under vacuum or an inert atmosphere;
The vacuum degree of the cladding is (1 multiplied by 10)-3-1)Pa。
13. the preparation method according to any one of claims 9 to 12, wherein the graphene film is prepared by combining vacuum filtration and chemical reduction of graphene oxide; or the like, or, alternatively,
prepared by adopting a chemical vapor deposition method.
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