CN113122188A - Heat-conducting composite material, preparation method and application thereof - Google Patents
Heat-conducting composite material, preparation method and application thereof Download PDFInfo
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- CN113122188A CN113122188A CN201911419891.3A CN201911419891A CN113122188A CN 113122188 A CN113122188 A CN 113122188A CN 201911419891 A CN201911419891 A CN 201911419891A CN 113122188 A CN113122188 A CN 113122188A
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- 239000002184 metal Substances 0.000 claims abstract description 109
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C09K5/14—Solid materials, e.g. powdery or granular
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a heat-conducting composite material, a preparation method and application thereof, wherein the preparation method comprises the following steps: providing a heat-conducting filler, and enabling the heat-conducting filler to form a heat-conducting layer on the surface of the metal matrix to obtain a composite body; and under vacuum and heating conditions, applying a first pressure on the surface of the composite body to enable the heat conduction layer to form a plurality of aggregates which are arranged in the same direction, and simultaneously melting and mixing the metal matrix with the aggregates to obtain the heat conduction composite material, wherein the direction of the first pressure and the surface of the metal matrix form an included angle alpha which is more than or equal to 60 degrees and less than or equal to 90 degrees. The heat-conducting composite material disclosed by the invention has higher in-plane heat conductivity and higher mechanical strength, and has a wider application prospect in the field of heat conduction.
Description
Technical Field
The invention relates to the technical field of heat-conducting composite materials, in particular to a heat-conducting composite material, and a preparation method and application thereof.
Background
The metal material has good weldability, effective heat conductivity and excellent mechanical strength, but the heat conductivity is limited, and the problem of high heat accumulation caused by increasingly high integration cannot be met, for example, the heat conductivity of copper is only 397W/mK, and the heat conductivity of aluminum is only 220W/mK; the metal-based composite material obtained by compounding the metal material and the heat-conducting filler improves the heat conductivity to a certain extent, but the heat-conducting filler is difficult to uniformly disperse in the metal material, so that the heat-conducting property of the metal-based heat-conducting composite material is influenced.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide a heat conductive composite material, a preparation method and an application thereof; the heat-conducting composite material has high in-plane heat conductivity.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a thermally conductive composite material, comprising the steps of:
providing a heat-conducting filler, and enabling the heat-conducting filler to form a heat-conducting layer on the surface of the metal matrix to obtain a composite body;
and under vacuum and heating conditions, applying a first pressure on the surface of the composite body to enable the heat conduction layer to form a plurality of aggregates which are arranged in the same direction, and simultaneously melting and mixing the metal matrix with the aggregates to obtain the heat conduction composite material, wherein the direction of the first pressure and the surface of the metal matrix form an included angle alpha which is more than or equal to 60 degrees and less than or equal to 90 degrees.
In one embodiment, the preparation method further comprises: the composite body also comprises an adhesive layer arranged between the metal substrate and the heat conduction layer, the heat conduction layer is adhered to the metal substrate through the adhesive layer, and the thickness of the adhesive layer is 1-30 μm.
In one embodiment, the preparation method further comprises: and before the first pressure is applied to the composite body, applying a second pressure to the heat conduction layer on the surface of the heat conduction layer, wherein the direction of the second pressure forms an included angle beta with the surface of the metal substrate, and the included angle beta is more than or equal to 60 degrees and less than or equal to 90 degrees.
In one embodiment, the second pressure is 0.01MPa to 10MPa, and the pressing time of the second pressure is 1min to 10 min.
In one embodiment, the thermally conductive filler comprises at least one of scale graphite, spherical graphite, graphite fiber, alumina particles, aluminum nitride particles, silicon carbide particles, and diamond particles;
and/or the material of the metal matrix comprises at least one of aluminum, copper and silver.
In one embodiment, the thickness of the heat conduction layer is 20-200 μm;
and/or the thickness of the metal matrix is 1-500 mu m;
and/or the mass ratio of the heat conduction layer to the metal matrix is 10: 90-90: 10.
In one embodiment, the preset temperature is 500-1000 ℃;
and/or the first pressure is 10MPa to 100MPa, and the pressure maintaining time of the first pressure is 10min to 300 min.
In one embodiment, the number of the composite bodies is set to be a plurality, the composite bodies are arranged in a stacking mode along the direction perpendicular to the surface of the metal substrate, and the thickness of each composite body is 0.1 mm-300 mm.
According to another aspect of the present invention, there is provided a heat conductive composite comprising a metal skeleton and a plurality of aggregates filled in the metal skeleton, the plurality of aggregates being arranged in a same direction along a surface of the heat conductive composite, the heat conductive composite having an in-plane thermal conductivity of 200W/m-K to 1000W/m-K, and the heat conductive composite having a bending strength of 70MPa to 150 MPa.
According to still another aspect of the present invention, there is provided a thermally conductive article comprising the above thermally conductive composite; or,
the heat-conducting product is made of the heat-conducting composite material.
In the preparation method, a first pressure is applied to the surface of the composite body, so that the heat-conducting filler is directionally spread along the direction parallel to the surface of the metal matrix, a plurality of aggregates which are basically parallel to the surface of the metal matrix are formed, and meanwhile, the metal matrix can be melted, flowed and filled between the aggregates to form a metal skeleton, so that the heat-conducting composite material is obtained.
Thus, firstly: the application of the first pressure can enable the heat-conducting filler in the heat-conducting layer to be directionally and uniformly spread on the surface of the metal matrix to form a plurality of aggregates which are arranged in the same direction along the surface of the metal matrix, so that the in-plane heat conductivity of the heat-conducting composite material is remarkably improved; secondly, the method comprises the following steps: the heat conduction filler can obviously improve the heat conductivity of the metal matrix composite material; thirdly, the method comprises the following steps: the metal has good mechanical property, and can improve the mechanical strength of the heat-conducting composite material when being used as a framework of the heat-conducting composite material; fourthly: when the metal is pressed and flows to be filled between the aggregates, the poor heat conductor air between the aggregates can be eliminated, the porosity of the heat-conducting composite material is reduced, and the density of the heat-conducting composite material is improved.
Therefore, the heat-conducting composite material obtained by the invention has the in-plane thermal conductivity of 200W/mK-1000W/mK, and the bending strength of 70 MPa-150 MPa, and has higher in-plane thermal conductivity and bending strength. Therefore, the heat-conducting composite material can meet the requirements of electronic devices on uniform heat performance, heat-conducting performance and thermal expansion performance, and has wide application prospect in the fields of high heat-conducting requirements of microelectronic equipment thermal management materials with high power density and high heat flow density and the like.
Drawings
FIG. 1 is a schematic view of a process for preparing a thermally conductive composite material according to the present invention;
FIG. 2 is a schematic view of a composite body under first and second pressures during the manufacturing process of the present invention;
FIG. 3 is a scanning electron micrograph of a thermally conductive layer obtained in example 1 of the present invention;
FIG. 4 is a scanning electron microscope image of a cross section of a thermally conductive composite material obtained in example 1 of the present invention;
fig. 5 is a scanning electron microscope image of the interface of the thermally conductive composite obtained in comparative example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The "in-plane direction" referred to herein means a surface direction of the metal base, which is also an in-plane direction of the heat conductive composite material, corresponding to a direction of an XY plane in a three-dimensional coordinate system; the "inter-plane direction" as referred to herein refers to a direction perpendicular to the surface of the metal matrix, and is also an inter-plane direction of the thermally conductive composite, corresponding to the Z direction in a three-dimensional coordinate system.
The term "homodromous arrangement" as used herein means that the arrangement of the heat conductive filler on the surface of the metal matrix is anisotropic due to its anisotropy, and the included angles between the heat conductive particles and the surface of the metal matrix are substantially the same, and the term "highly homodromous arrangement" means that the arrangement of the heat conductive particles in the heat conductive filler on the surface of the metal matrix is highly anisotropic, and the included angles between the heat conductive particles and the surface of the metal matrix are highly the same.
Because the traditional anisotropic heat conduction material such as graphite is of a laminated structure and has higher in-plane heat conductivity and lower inter-plane heat conductivity, the in-plane heat conductivity is ten orders of magnitude of the inter-plane heat conductivity, even one hundred orders of magnitude, the inter-plane heat conductivity of the heat conduction composite material can be improved by stacking or bending the graphite layers towards the inter-plane, but the overall improvement of the heat conductivity is limited, and the requirement of higher heat conductivity in actual use cannot be met. And the mechanical property of the pure heat-conducting filler is limited, so that the pure heat-conducting filler is difficult to use practically.
The filled metal matrix composite has been widely studied because the composite has a common property of the heat conductive filler and the metal material. The commonly used heat-conducting filler comprises carbon black, graphite, carbon fiber, ceramic particles, diamond and other materials, and has the advantages of low density, high heat conductivity, low expansion coefficient, excellent processability and the like. The diamond particles have high thermal conductivity, high strength and low thermal expansion coefficient. However, the heat-conducting filler is difficult to be uniformly dispersed in the metal, so that the realization of high heat conductivity and high mechanical property of the metal-based heat-conducting composite material is influenced.
Referring to fig. 1 to 3, the method for preparing the thermal conductive composite material 200 includes the following steps:
s1: providing a heat-conducting filler, forming the heat-conducting filler into a heat-conducting layer 20 on the surface of the metal matrix 10, and obtaining a composite body 100;
s2: applying a first pressure F1 to the composite 100 on the surface of the composite 100 under vacuum and heating conditions to form a plurality of aggregates 202 arranged in the same direction on the heat conducting layer 20, and simultaneously melting the metal matrix 10 and mixing with the aggregates 202 to obtain the heat conducting composite material 200, wherein the first pressure F1 is in a direction of alpha, and the angle between the first pressure F1 and the surface of the metal matrix 10 is 60 degrees to 90 degrees.
In step S1, the material of the metal matrix 10 includes at least one of aluminum, copper, and silver, and the heat conductive filler includes at least one of flake graphite, spherical graphite, graphite fiber, alumina particles, aluminum nitride particles, silicon carbide particles, and diamond particles.
The thickness of the metal substrate 10 is 1 μm to 500 μm, and the thickness of the heat conductive layer 20 is 20 μm to 200 μm. The mass ratio of the heat conduction layer 20 to the metal matrix 10 is 10: 90-90: 10. The heat conductive layer 20 having a small mass ratio is not likely to spread uniformly and highly uniformly on the surface of the metal base 10 by the first pressure F1, and if the heat conductive layer 20 having a high mass ratio is not likely to spread uniformly on the surface of the metal base 10, it is difficult to be press-molded. Therefore, a proper mass ratio between the heat conductive layer 20 and the metal substrate 10 is very important to the heat conductive performance and the final form of the prepared heat conductive composite material 200.
Further, the composite 100 may further include an adhesive layer 30 provided between the metal base 10 and the heat conductive layer 20, and the adhesive layer 30 may have a thickness of 1 μm to 30 μm. Preferably, the adhesive layer 30 has a thickness of 1 to 20 μm.
The heat conductive layer 20 is adhered to the metal substrate 10 by the adhesive layer 30 to avoid uneven distribution of the heat conductive layer 20 on the metal substrate 10. At the same time, the adhesive layer 30 can make the heat conductive layer 20 bonded on the surface of the metal substrate 10 more tightly, which facilitates the preparation of the composite 100. The heat conductive filler has good spreading uniformity on the surface of the metal matrix 10, can obtain a thicker spreading thickness, has strong interface bonding force with the metal matrix 10, and is highly arranged in the same direction on the surface of the metal matrix 10, so that the heat conductive filler has higher in-plane thermal conductivity.
Preferably, the material of the adhesive layer 30 includes at least one of atomized glue, and solid glue.
Further, the adhesive layer 30 may be formed on the surface of the metal substrate 10 by spraying, coating, spin coating, or the like. Preferably, the spraying time of the binder on the surface of the metal substrate 10 is 5s to 100 s.
It should be noted that the adhesive layer 30 is used to spread the heat conductive filler more uniformly and firmly when the composite 100 is prepared, and the adhesive layer 30 is thermally decomposed and volatilized during the vacuum heat pressing process in step S2.
Further, the preparation method further includes, after the heat conductive filler covers the surface of the adhesive layer 30 to form the heat conductive layer 20, removing excess heat conductive filler by using a blower or the like, so that the heat conductive layer 20 covers the surface of the adhesive layer 30 more uniformly.
In one embodiment, the mass ratio of the heat conduction layer 20, the metal base 10 and the bonding layer 30 is (10-90): (9-89.9): 0.1-1).
In step S2, when a first pressure F1 is applied to the surface of the heat conductive layer 20 to the composite 100, the heat conductive fillers in the heat conductive layer 20 are uniformly spread and arranged in the same direction along the direction parallel to the surface of the metal matrix 10, and a plurality of aggregates 202 substantially parallel to the surface of the metal matrix 10 are formed.
Meanwhile, under vacuum and heating temperature, the metal matrix 10 can be melted, flowed and filled between the aggregates 202 to form the metal skeleton 201. The thermal conductivity of the heat-conducting composite material 200 in the inter-plane direction can be remarkably improved, so that the heat-conducting composite material 200 has good heat-conducting performance in all directions, the problems of poor mechanical performance and the like of the heat-conducting filler can be solved, and the mechanical strength and other performances of the heat-conducting composite material 200 are improved.
Meanwhile, when the metal flows and is filled between the aggregates 202, the poor heat conductor air between the aggregates 202 and the gas generated by the decomposition of the bonding layer 30 can be eliminated, the porosity of the heat-conducting composite material 200 is reduced, and the density of the heat-conducting composite material 200 is improved.
Preferably, alpha is greater than or equal to 75 degrees; more preferably, α ≧ 85 °; further preferably, α is 90 °.
Note that α is 90 °, that is, the direction in which the surface of the composite body 100 applies the first pressure F1 to the composite body 100 is perpendicular to the surface of the metal base 10, and the pressing area of the first pressure F1 is not limited in the present invention, and is preferably a rolling contact.
Preferably, after the composite body 100 is prepared, the composite body 100 is placed in a hot press mold, and the hot press mold is horizontally placed. Then, the composite 100 is subjected to vacuum hot-pressing treatment, and a first pressure F1 is applied to the surface of the composite 100, so that the composite 100 is subjected to a pressure in the longitudinal direction, the heat conductive layer 20 is uniformly spread on the surface of the metal substrate 10, the heat conductive filler is arranged in the same direction on the surface of the metal substrate 10, and the included angle formed by the heat conductive filler and the surface of the metal substrate 10 is almost the same.
Preferably, the first pressure F1 is 10MPa to 100MPa, more preferably 30MPa to 600MPa, at which the heat conductive layer 20 can be spread more uniformly and arranged in the same direction.
Preferably, the dwell time under the first pressure F1 is 10min to 300min, and more preferably 10min to 30min, which is helpful for the final molding of the thermal conductive composite material 200.
Further, the first pressure F1 applied to the composite 100 may be one or a plurality of first pressures F1 applied to the composite 100 on the surface of the composite 100, preferably the first pressure F1 is applied to the composite 100 on the entire surface of the heat conductive layer 20, the first pressure F1 may be applied to the composite 100 on both the upper and lower surfaces of the composite 100, and the magnitudes and angles α of the plurality of first pressures F1 may be the same or different from each other.
Further, the heating temperature is preferably 500 to 1000 ℃, and more preferably 600 to 650 ℃. At this heating temperature, the metal matrix 10 will be in a semi-molten state or molten state and flow and fill between the aggregates 202 under the first pressure F1 to form the metal skeleton 201.
Further, before the surface of the heat conduction layer 20 applies the first pressure F1 to the composite 100, a second pressure F2 may be applied to the surface of the heat conduction layer 20, and the direction of the second pressure F2 is included by β, 60 ° β or more and 90 ° or less with respect to the surface of the metal substrate 10.
Preferably, the thermally conductive fillers in the thermally conductive layer 20 are arranged in the same direction by rolling on the surface of the thermally conductive layer 20. Thus, the heat conduction layer 20 can better adhere to the surface of the metal substrate 10, the porosity of the composite 100 in the step S2 vacuum hot pressing process can be reduced, and the density of the heat conduction composite material 200 can be increased, so that the heat conductivity of the heat conduction composite material 200 can be improved.
In addition, the heat conductive fillers in the heat conductive layer 20 are arranged in the same direction, so that the heat conductive layer 20 can be more uniformly spread in the direction parallel to the surface of the metal matrix 10 in step S2, and the in-plane thermal conductivity of the heat conductive composite material 200 is more uniform.
It is understood that in other embodiments, other pressurizing methods may be applied to the heat conductive layer 20, and the invention is not limited thereto.
Preferably, the second pressure F2 is 0.01MPa to 10MPa, and the pressing time of the second pressure F2 is 1min to 10 min.
Further, the number of the composite bodies 100 is set to be plural, and the plural composite bodies 100 are stacked and arranged along a direction perpendicular to the surface of the metal base 10, so as to prepare the thermally conductive composite material 200 having a desired thickness and high in-plane thermal conductivity. Specifically, in the preparation process, a plurality of composite bodies 100 are prepared separately, and the plurality of composite bodies 100 are stacked on each other. In the case of stacking, the metal base 10 of one composite 100 is preferably bonded to the heat conductive layer 20 of the other composite 100.
Preferably, the number of the composite 100 is 50 to 500, and more preferably, the number of the composite 100 is 100 to 300.
According to another aspect of the present invention, there is also provided a heat conductive composite material 200, wherein the heat conductive composite material 200 comprises a metal skeleton 201 and a plurality of aggregates 202 filled in the metal skeleton 201, the aggregates 202 are arranged in the same direction, the in-plane thermal conductivity of the heat conductive composite material 200 is 200W/m-K to 1000W/m-K, and the bending strength of the heat conductive composite material 200 is 70MPa to 150 MPa. Thus, the in-plane thermal conductivity of the thermal conductive composite material 200 is significantly improved, and the thermal conductive composite material has high bending strength.
In one embodiment, the thermally conductive composite 200 is made from a single composite 100 having a thickness preferably in the range of 0.04mm to 0.1 mm. The aggregates 202 are uniformly distributed in the same direction in the metal framework 201, so that the composite material has high in-plane thermal conductivity of 200W/mK-1000W/mK and high bending strength of 70 MPa-150 MPa, can be attached to a heat source and is used for soaking, and thus heat on the heat source is uniformly conducted out of the plane of the heat-conducting composite material 200.
In one embodiment, the thermally conductive composite material 200 is made from a plurality of composite bodies 100. The number of the complex 100 is preferably 50 to 500, and the thickness of the corresponding heat-conducting composite material 200 is 0.1mm to 300 mm.
Further, the number of the composite bodies 100 is preferably set to 100 to 300, and the thickness of the corresponding heat-conducting composite material 200 is 20 to 100 mm.
The traditional preparation method is difficult to prepare the heat-conducting composite material 200 with thicker thickness and high homodromous arrangement, such as more than 50 mm. Because the thickness is limited, the longitudinal section of the heat-conducting composite material is smaller after being cut along the direction vertical to the heat-conducting composite material 200, so that the pasting area of the heat-conducting composite material and a heating source is smaller, and the application of the heat-conducting composite material in heat conduction is limited.
The heat-conducting composite material 200 with a thicker thickness can be prepared by the preparation method of the invention, so that the heat-conducting composite material with a higher in-plane thermal conductivity can be conveniently applied. When the heat-conducting composite material is used, the heat-conducting composite material 200 is cut along the direction perpendicular to the heat-conducting composite material 200, and the heat-conducting composite material 200 has a large longitudinal section due to the high thickness, so that the heat-generating source can be attached to the longitudinal section, the cut heat-conducting composite material 200 has a large attachment area and high longitudinal heat conductivity, and heat conduction can be well achieved.
According to still another aspect of the present invention, there is also provided a thermally conductive article comprising the thermally conductive composite 200 described above; alternatively, the thermally conductive article is made of the thermally conductive composite material 200 described above.
Specifically, the heat conductive composite material 200 may be directly attached to a substrate of a heat dissipation source as a heat sink member for heat soaking or heat dissipation. Of course, the thermally conductive composite material 200 may be further processed into, for example, a grid-like material for use as a heat sink.
Therefore, the heat-conducting composite material 200 of the present invention has the characteristics of high in-plane thermal conductivity, high bending strength and uniform material, and can be used as a heat sink material for heat dissipation members such as computer heat dissipation modules, metal bushings, rotary sealing rings for medium load and medium speed applications, thrust washers and the like, which have high requirements for heat dissipation capability, such as electronic devices with high power density and high heat flux density, thereby ensuring stable operation of devices.
It should be noted that the application of the present invention to the above-mentioned heat conductive composite material is merely exemplary and not limited.
Hereinafter, preferred examples and comparative examples are set forth for a better understanding of the present invention. However, the following examples are merely illustrative of the present invention and are not intended to be limiting or restrictive.
Example 1:
spraying glue on an aluminum foil with the thickness of 20 micrometers at room temperature for 10 seconds, wherein the thickness of the atomized glue is 20 micrometers, pouring scale graphite powder into the glue-coated aluminum foil to form a heat conduction layer with the thickness of 40 micrometers, wherein the mass ratio of the heat conduction layer, the aluminum foil and the bonding layer is 50:49:1, then performing rolling treatment on the heat conduction layer, wherein the rolling pressure is 0.5MPa, the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 90 degrees, and the rolling time is 1 minute to obtain the scale graphite-aluminum composite. Horizontally putting the scale graphite-aluminum complex into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 650 ℃ at a heating rate of 10 ℃/min, sintering, keeping the temperature for 60min, keeping the first pressure at 60MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 60 ℃, and then cooling to room temperature along with the furnace to obtain the scale graphite-aluminum heat-conducting composite material.
Example 2:
and (2) spraying glue at room temperature on an aluminum foil with the thickness of 50 micrometers, wherein the spraying time is 5 seconds, the thickness of the atomized glue is 30 micrometers, then pouring spherical graphite powder into the glue-coated aluminum foil to form a heat conduction layer with the thickness of 20 micrometers, the mass ratio of the heat conduction layer to the aluminum foil to the bonding layer is 39.5:60:0.5, then performing rolling treatment on the heat conduction layer, the rolling pressure is 0.01MPa, the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 80 degrees, and the rolling time is 10 minutes to obtain the spherical graphite-aluminum composite. Horizontally putting the spherical graphite-aluminum complex into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 750 ℃ at a heating rate of 15 ℃/min, sintering, keeping the temperature for 10min, keeping the first pressure at 40MPa, enabling an included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 70 ℃, and then cooling to room temperature along with the furnace to obtain the spherical graphite-aluminum heat-conducting composite material.
Example 3:
spraying glue on a copper foil with the thickness of 500 micrometers at room temperature for 100 seconds, wherein the thickness of the atomized glue is 30 micrometers, pouring silicon carbide powder into the glue-coated copper foil to form a heat conduction layer with the thickness of 100 micrometers, wherein the mass ratio of the heat conduction layer, the copper foil and the bonding layer is 10:89.9:0.1, then performing rolling treatment on the heat conduction layer, the rolling pressure is 10MPa, the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 70 degrees, and the rolling time is 10 minutes to obtain the silicon carbide-aluminum composite. Horizontally putting the silicon carbide-aluminum composite body into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 1000 ℃ at a heating rate of 10 ℃/min, sintering, keeping the temperature for 200min, keeping the first pressure at 10MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 80 degrees, and then cooling to room temperature along with the furnace to obtain the silicon carbide-copper heat-conducting composite material.
Example 4:
and (2) spraying glue at room temperature on an aluminum foil with the thickness of 20 microns, wherein the thickness of glue coating water is 10 microns, pouring aluminum nitride powder into the glue-coated aluminum foil to form a heat conduction layer with the thickness of 20 microns, wherein the mass ratio of the heat conduction layer to the aluminum foil to the bonding layer is 54:45.6:0.4, and then rolling the heat conduction layer under the rolling pressure of 5MPa for 3 minutes, wherein the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 60 degrees, so that the aluminum nitride-aluminum composite is obtained. Horizontally putting the aluminum nitride-aluminum composite body into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 660 ℃ at the heating rate of 10 ℃/min, sintering, keeping the temperature for 300min, keeping the first pressure at 100MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 90 ℃, and then cooling to room temperature along with the furnace to obtain the aluminum nitride-aluminum heat-conducting composite material.
Example 5:
spraying glue on silver foil with the thickness of 200 mu m at room temperature, wherein the glue is coated to the thickness of 30 mu m, then pouring alumina powder into the silver foil coated with the glue to form a heat conduction layer with the thickness of 40 mu m, the mass ratio of the heat conduction layer to the silver foil to the bonding layer is 20:79.7:0.3, then performing rolling treatment on the heat conduction layer, the rolling pressure is 6MPa, the direction of the rolling pressure is 90 degrees to the surface of the metal matrix, and the rolling time is 8 minutes to obtain the graphite-silver complex. Horizontally putting the aluminum oxide-silver complex into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 500 ℃ at a heating rate of 10 ℃/min, sintering, keeping the temperature for 50min, keeping the first pressure at 20MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 85 ℃, and then cooling to room temperature along with the furnace to obtain the aluminum oxide-silver heat-conducting composite material.
Example 6:
spraying glue on an aluminum foil with the thickness of 100 micrometers at room temperature for 20 seconds, wherein the thickness of the atomized glue is 5 micrometers, then pouring graphite fiber powder into the glue-coated aluminum foil to form a heat conduction layer with the thickness of 50 micrometers, wherein the mass ratio of the heat conduction layer to the aluminum foil to the bonding layer is 30.8:69:0.2, then performing rolling treatment on the heat conduction layer, the rolling pressure is 8MPa, the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 85 degrees, and the rolling time is 8 minutes, so that the graphite fiber-aluminum composite is obtained. Horizontally putting the graphite fiber-aluminum complex into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 900 ℃ at a heating rate of 10 ℃/min, sintering, keeping the temperature for 80min, keeping the first pressure at 30MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 75 ℃, and then cooling to room temperature along with the furnace to obtain the graphite fiber-aluminum heat-conducting composite material.
Example 7:
spraying glue on a copper foil with the thickness of 1 mu m at room temperature for 15 seconds, wherein the thickness of the atomized glue is 15 mu m, then pouring diamond powder into the glue-coated copper foil to form a heat conduction layer with the thickness of 200 mu m, the mass ratio of the heat conduction layer, the copper foil and the bonding layer is 80:19.8:0.2, then carrying out rolling treatment on the heat conduction layer, wherein the rolling pressure is 0.05MPa, the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 60 degrees, and the rolling time is 10 minutes, thus obtaining the diamond-copper composite. Horizontally placing the diamond-copper complex into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 600 ℃ at a heating rate of 10 ℃/min, sintering, keeping the temperature for 90min, keeping the first pressure at 100MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 65 ℃, and then cooling to room temperature along with the furnace to obtain the diamond-copper heat-conducting composite material.
Example 8:
spraying glue on an aluminum foil with the thickness of 5 micrometers at room temperature for 15 seconds, wherein the thickness of the atomized glue is 1 micrometer, then pouring graphite powder into the glue-coated aluminum foil to form a heat conduction layer with the thickness of 30 micrometers, wherein the mass ratio of the heat conduction layer, the aluminum foil and the bonding layer is 75.7:24:0.3, then performing rolling treatment on the heat conduction layer, wherein the rolling pressure is 0.8MPa, the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 70 degrees, and the rolling time is 8 minutes to obtain the graphite-aluminum composite. Horizontally putting the graphite-aluminum complex into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 650 ℃ at a heating rate of 10 ℃/min, sintering, keeping the temperature for 120min, keeping the first pressure at 60MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 90 degrees, and then cooling to room temperature along with the furnace to obtain the graphite-aluminum heat-conducting composite material.
Example 9:
spraying glue on a silver foil with the thickness of 800 micrometers at room temperature for 15 seconds, wherein the thickness of the atomized glue is 3 micrometers, then pouring graphite powder into the silver foil coated with the glue to form a heat conduction layer with the thickness of 40 micrometers, wherein the mass ratio of the heat conduction layer, the aluminum foil and the bonding layer is 10:89.2:0.8, then performing rolling treatment on the heat conduction layer, wherein the rolling pressure is 8MPa, the included angle alpha between the direction of the rolling pressure and the surface of the metal substrate is 85 degrees, and the rolling time is 10 minutes, so that the graphite-silver complex is obtained. Horizontally putting the graphite-silver complex into a hot-pressing die, sintering in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 800 ℃ at a heating rate of 10 ℃/min, sintering, keeping the temperature for 260min, keeping the first pressure at 50MPa, enabling the included angle alpha between the direction of the first pressure and the surface of the metal matrix to be 80 degrees, and then cooling to room temperature along with the furnace to obtain the graphite-silver heat-conducting composite material.
Example 10:
this embodiment is substantially the same as embodiment 1 except that: the number of the composites is set to 50, and the 50 composites are arranged in a stacked manner along the longitudinal direction of the composites.
Example 11:
this embodiment is substantially the same as embodiment 1 except that: the number of the composites is set to 100, and the 100 composites are arranged in a stacked manner along the longitudinal direction of the composites.
Example 12:
this embodiment is substantially the same as embodiment 1 except that: the number of the composites is set to 300, and the 300 composites are arranged in a stacked manner along the longitudinal direction of the composites.
Example 13:
this embodiment is substantially the same as embodiment 1 except that: the number of the composites is set to 500, and 500 composites are arranged in a stacked manner along the longitudinal direction of the composites.
Comparative example 1:
this embodiment is substantially the same as embodiment 1 except that:
and (3) spraying glue on the aluminum foil with the thickness of 20 microns at room temperature for 1 second, wherein the thickness of the atomized glue is 0.01 um.
Comparative example 2:
this embodiment is substantially the same as embodiment 1 except that:
the direction of the first pressure and the surface of the metal matrix form an included angle alpha of 0 degree.
Comparative example 3:
this embodiment is substantially the same as embodiment 1 except that:
the mass ratio of the heat conduction layer to the aluminum foil to the bonding layer is 98:1: 1.
Comparative example 4:
this embodiment 1 is substantially the same as the embodiment except that:
the heat conducting layer is not subjected to rolling treatment.
Comparative example 5:
uniformly dispersing metal aluminum particles and flake graphite powder to prepare a mixture, wherein the mass ratio of the metal aluminum particles to the flake graphite particles is 1:1, putting the mixture into a hot-pressing mold, sintering the mixture in a vacuum unidirectional hot-pressing sintering furnace, heating the temperature in the sintering furnace to 650 ℃ at the heating rate of 10 ℃/min for sintering, keeping the temperature for 60min, keeping the first pressure at 60MPa, and cooling the mixture to room temperature along with the furnace, so as to prepare the flake graphite-aluminum heat-conducting composite material.
The heat conductive composite materials obtained in examples 1 to 13 and comparative examples 1 to 4 were subjected to in-plane thermal conductivity measurement, in-plane thermal expansion coefficient measurement, and mechanical property measurement, and the measurement results are shown in table 1.
TABLE 1
As can be seen from table 1, the thermal conductive composite materials prepared in embodiments 1 to 13 have high in-plane thermal conductivity and high mechanical properties, and can meet the use requirements of some application scenarios summarizing electronic devices on thermal conductivity. In addition, the thermal conductive composite materials prepared in examples 1 to 13 all have better thermal expansion performance.
The heat-conducting composite material prepared in comparative example 1 has low in-plane thermal conductivity and cannot meet the heat-conducting requirement because the adhesion and uniform dispersibility of the graphite powder on the aluminum foil are affected due to the thin thickness of the atomization glue.
Comparative example 2 the heat conductive composite material obtained by applying pressure in the transverse direction of the composite body during the vacuum heat pressing treatment of the composite body had a reduced in-plane heat conductivity.
In comparative example 3, the metal skeleton cannot be formed during the hot pressing due to the small content of the aluminum foil, and the graphite material is brittle, so that the heat conductive composite material cannot be molded during the vacuum hot pressing.
Comparative example 4 was directly subjected to vacuum thermocompression without subjecting the heat conductive layer to rolling treatment, and the in-plane thermal conductivity was low.
Comparative example 5 the conventional dispersion method was used to uniformly disperse the aluminum metal and the crystalline flake graphite powder, and the in-plane thermal conductivity of the thermally conductive composite material obtained by the same hot pressing treatment was low.
Further, SEM scanning was performed on the heat conductive layer in the heat conductive composite material prepared in example 1, and the result is shown in fig. 3, in which graphite particles in the heat conductive layer are well dispersed and are relatively dense, and the porosity is relatively low; a cross-sectional SEM scan is performed on the heat conductive composite material prepared in example 1, and as a result, as shown in fig. 4, the aggregates 202 in the heat conductive composite material are arranged in the same direction, and the metal aluminum is filled between the adjacent aggregates 202 and connected with each other to form a metal skeleton 201, which has a stable structure; the result of performing SEM scanning on the interface of the heat conductive composite material obtained in example 1 is shown in fig. 5, where the interface between the metal skeleton 201 and the aggregate 202 is clear, almost no pores are present, and the compactness is high, which indicates that the vacuum hot pressing process substantially excludes the gas in the heat conductive composite material.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the heat-conducting composite material is characterized by comprising the following steps of:
providing a heat-conducting filler, and enabling the heat-conducting filler to form a heat-conducting layer on the surface of the metal matrix to obtain a composite body;
and under vacuum and heating conditions, applying a first pressure on the surface of the composite body to enable the heat conduction layer to form a plurality of aggregates which are arranged in the same direction, and simultaneously melting and mixing the metal matrix with the aggregates to obtain the heat conduction composite material, wherein the direction of the first pressure and the surface of the metal matrix form an included angle alpha which is more than or equal to 60 degrees and less than or equal to 90 degrees.
2. The method of claim 1, wherein the composite further comprises an adhesive layer disposed between the metal substrate and the heat conductive layer, the heat conductive layer is adhered to the metal substrate through the adhesive layer, and the adhesive layer has a thickness of 1 μm to 30 μm.
3. The method of making a thermally conductive composite material as claimed in claim 1, further comprising: and before the first pressure is applied to the composite body, applying a second pressure to the heat conduction layer on the surface of the heat conduction layer, wherein the direction of the second pressure forms an included angle beta with the surface of the metal substrate, and the included angle beta is more than or equal to 60 degrees and less than or equal to 90 degrees.
4. The method for preparing the heat-conducting composite material as claimed in claim 3, wherein the second pressure is 0.01MPa to 10MPa, and the pressing time of the second pressure is 1min to 10 min.
5. The method of claim 1, wherein the thermally conductive filler comprises at least one of scale graphite, spherical graphite, graphite fiber, alumina particles, aluminum nitride particles, silicon carbide particles, and diamond particles;
and/or the material of the metal matrix comprises at least one of aluminum, copper and silver.
6. The method for preparing a heat conductive composite material according to claim 1, wherein the thickness of the heat conductive layer is 20 to 200 μm;
and/or the thickness of the metal matrix is 1-500 mu m;
and/or the mass ratio of the heat conduction layer to the metal matrix is 10: 90-90: 10.
7. The method for preparing the heat-conducting composite material as claimed in claim 1, wherein the heating temperature is 500-1000 ℃;
and/or the first pressure is 10MPa to 100MPa, and the pressure maintaining time of the first pressure is 10min to 300 min.
8. The method for preparing the heat-conducting composite material as claimed in any one of claims 1 to 7, wherein the number of the composite bodies is set to be plural, the plural composite bodies are stacked and arranged along a direction perpendicular to the surface of the metal substrate, and the thickness of the composite bodies is 0.1mm to 300 mm.
9. The heat-conducting composite material is characterized by comprising a metal framework and a plurality of aggregates filled in the metal framework, wherein the aggregates are arranged in the same direction along the surface of the heat-conducting composite material, the in-plane heat conductivity of the heat-conducting composite material is 200W/m.K-1000W/m.K, and the bending strength of the heat-conducting composite material is 70 MPa-150 MPa.
10. A thermally conductive article, comprising the thermally conductive composite of claim 9;
alternatively, the thermally conductive article is made of the thermally conductive composite material of claim 9.
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| CN115195218B (en) * | 2022-06-27 | 2024-05-28 | 中国科学院宁波材料技术与工程研究所 | Heat-conducting composite material and preparation method and application thereof |
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