CN116005029A - Graphite sheet metal matrix composite material, and preparation method, assembly die and application thereof - Google Patents
Graphite sheet metal matrix composite material, and preparation method, assembly die and application thereof Download PDFInfo
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- CN116005029A CN116005029A CN202310009022.3A CN202310009022A CN116005029A CN 116005029 A CN116005029 A CN 116005029A CN 202310009022 A CN202310009022 A CN 202310009022A CN 116005029 A CN116005029 A CN 116005029A
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- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 164
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 163
- 239000011156 metal matrix composite Substances 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 46
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 230000017525 heat dissipation Effects 0.000 claims description 11
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention discloses a graphite sheet metal matrix composite material, a preparation method, an assembly die and application thereof. The composite material is prepared by compacting a mixture of graphite flakes and metal powder to obtain a preform and sintering the preform by adopting a hot isostatic pressing method. The compaction comprises planar compaction and non-planar compaction, the compaction of the mixture is performed at least once through non-planar compaction, so that graphite flakes are distributed on vertical parallel surfaces on three intersecting lines which are not on the same plane at least, a graphite flake metal-based preform in three-dimensional arrangement is obtained, and then the graphite flake metal-based preform is sintered by a hot isostatic pressing method, and the hot isostatic pressing method can simultaneously provide three-dimensional pressure to uniformly act on the preform without damaging the three-dimensional structure of the preform, and the compactness of the preform is improved, so that the graphite flake metal-based composite material is obtained. The graphite sheets in the material are arranged in a three-dimensional structure, have high compactness, high heat conduction performance and uniform thermal expansion coefficient in all directions, and are favorable for long-acting and stable operation of electronic devices.
Description
Technical Field
The invention relates to the technical field of heat dissipation material preparation, in particular to a graphite sheet metal matrix composite material, a preparation method, an assembly die and application thereof.
Background
In recent years, graphite flake metal matrix composite materials have been applied to the field of heat dissipation of electronic chips due to their characteristics of high thermal conductivity, controllable thermal expansion coefficient, weight reduction, easiness in processing and the like. It is well known that carbon atoms in the plane of graphite flake are in sp 2 The track bond bonding has an in-plane thermal conductivity of 1000W/(mK) or more, 2 to 4 times that of pure copper. Thus, a highly oriented alignment of the graphite sheets is one of the requirements to achieve a high thermal conductivity of the composite material in the in-plane direction of the graphite sheets.
But due to the different forms of forces between the carbon atoms in and between the planes of the graphite sheets, anisotropic thermal properties occur, i.e. in-plane thermal conductivity is much greater than in-plane thermal conductivity; and the in-plane thermal expansion coefficient is-1 ppm/K, and the in-plane thermal expansion coefficient is 28ppm/K. Thus, the high orientation of the graphite flake arrangement results in a metal matrix composite having a thermal conductivity about 10 times greater in the in-plane direction of the graphite flake than in the perpendicular in-plane direction of the graphite flake; the measured value of the thermal expansion coefficient in the direction along the plane of the graphite sheet has little change compared with the metal matrix, and if the material is applied to the heat dissipation of a chip to exert a heat sink or heat dispersion effect, the arrangement direction of the graphite sheet is perpendicular to the direction in the plane of the chip to exert high heat conduction performance, and obviously, the thermal expansion coefficients in all directions parallel to the plane of the chip are inconsistent, so that thermal mismatch and thermal stress are caused, and the long-acting stable operation of an electronic device is not facilitated. It follows that this thermal performance configuration feature greatly limits the thermal matching flexibility of the graphite sheet metal matrix composite material to the chip.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a graphite sheet metal matrix composite material, a preparation method, an assembly die and application thereof, and the anisotropic thermal property of the graphite sheet metal matrix composite material is regulated and controlled by changing the spatial arrangement mode of graphite sheets, so that the prepared material can meet the heat dissipation requirement of a high-performance semiconductor device.
The invention is realized in the following way:
in a first aspect, the invention provides a method for preparing a graphite flake metal matrix composite, comprising compacting a mixture of graphite flakes and metal powder to obtain a preform, and sintering the preform by a hot isostatic pressing method to obtain the graphite flake metal matrix composite in a three-dimensional arrangement. Wherein the compacting comprises planar compacting and non-planar compacting, and the mixture of graphite flake and metal powder is compacted at least once through the non-planar compacting.
In a second aspect, the present invention provides an assembly die for a graphite sheet metal matrix composite material, for use in a method of making any of the previous embodiments, comprising a ram and a fixing assembly.
The pressing head comprises an upper pressing head and a lower pressing head, and a three-dimensional pressing head structure which can be selectively detached is arranged on the pressing surface of the upper pressing head and is used for finishing plane compaction and non-plane compaction.
The fixing component comprises a first fixing piece and a second fixing piece, the first fixing piece is provided with a groove, the lower pressure head is located in the groove, the second fixing piece is propped against and fixed on the surface of the groove, and the upper pressure head can be selectively contained in the groove.
Preferably, the number of the second fixing pieces is at least two, and the connection mode among the plurality of the second fixing pieces is abutting.
Preferably, the three-dimensional indenter structure comprises a surface formed by a plurality of three-dimensional polyhedral structures or a plurality of three-dimensional curved surface body structures.
In a third aspect, the present invention provides a graphite flake metal matrix composite made by the method of any of the preceding embodiments or processed through the assembly mold of the preceding embodiments.
In a fourth aspect, the present invention provides an application of the graphite flake metal matrix composite according to the foregoing embodiment in the field of heat dissipation of electronic chips.
The invention has the following beneficial effects:
the invention provides a graphite sheet metal matrix composite, a preparation method, an assembling die and an application thereof, wherein graphite sheets are arranged and distributed on vertical parallel surfaces on three intersecting lines which are not at the same plane at least by carrying out non-planar compaction on mixed powder obtained by mixing graphite sheets and metal powder, so that a graphite sheet metal matrix preform in three-dimensional arrangement is obtained, and then the graphite sheet metal matrix preform is sintered by a hot isostatic pressing method, the hot isostatic pressing method can simultaneously provide three-way pressure, the three-way pressure uniformly acts on the three-dimensional arranged graphite sheet metal matrix preform without damaging the three-dimensional structure, the compactness of the preform is improved by the hot isostatic pressing method, and the three-dimensional arranged graphite sheet metal matrix composite is further obtained. The graphite sheets in the material are arranged in a three-dimensional structure, have high compactness, high heat conduction performance and uniform thermal expansion coefficient in all directions, and are favorable for long-acting and stable operation of electronic devices.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a structural exploded view of an assembly mold of a graphite sheet metal matrix composite material provided in embodiment 1 of the present invention;
FIG. 2 is a schematic view of a non-planar upper ram according to embodiment 1 of the present invention;
FIG. 3 is a schematic plan view of a preform according to embodiment 2 of the present invention;
FIG. 4 is a physical diagram of a mixture of graphite flake and metal matrix after non-planar compaction in accordance with example 2 of the present invention;
FIG. 5 is a schematic view of the preform structure obtained in example 2 of the present invention;
FIG. 6 is a schematic view showing a structure of a preform covered with a sealed metal shell according to embodiment 2 of the present invention;
FIG. 7 is a microstructure view of a top view of a graphite flake metal matrix composite provided in comparative example 1 of the present invention;
FIGS. 8 to 9 are microstructure diagrams of side views of the graphite flake metal matrix composite provided in comparative example 1 of the present invention;
FIG. 10 is an enlarged microstructure view of a side view of the graphite flake metal matrix composite provided in comparative example 1 of the present invention;
fig. 11 is a microstructure view of the graphite flake metal matrix composite of comparative example 2 provided by the present invention in three dimensions.
Icon: assembling die of 100-graphite sheet metal matrix composite; 111-lower press head; 112-an in-plane ram; 113-a non-planar upper ram; 121-a first fixing member; 122-a second securing member; 200-preform; 300-a sealed metal housing.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The heat dissipation material needs to have high heat conductivity so as to effectively remove a large amount of heat generated during the operation of the high-performance microelectronic chip, ensure the reliable operation of the electronic device in a normal temperature range, and simultaneously, in order to avoid the heat expansion and contraction process of the heat dissipation material and the chip from generating thermal stress, the heat expansion coefficient of the heat dissipation material is required to be close to that of the chip material. The highly oriented alignment of the graphite platelets is one of the requirements for achieving a high thermal conductivity of the composite material in the in-plane direction of the graphite platelets. However, the current arrangement mode of the high-orientation graphite sheets causes that the thermal conductivity of the metal matrix composite material in the direction along the graphite sheet surface is about 10 times that of the metal matrix composite material in the direction vertical to the graphite sheet surface, the arrangement direction of the graphite sheets is vertical to the direction in the chip surface to exert high thermal conductivity, and the thermal expansion coefficients of the graphite sheets in the directions parallel to the chip surface are inconsistent, so that thermal mismatch and thermal stress are caused, and the long-acting stable operation of electronic devices is not facilitated.
In a first aspect, the invention provides a method for preparing a graphite flake metal matrix composite, comprising compacting a mixture of graphite flakes and metal powder to obtain a preform, and sintering the preform by a hot isostatic pressing method to obtain the graphite flake metal matrix composite in a three-dimensional arrangement. Wherein the compacting comprises planar compacting and non-planar compacting, and the mixture of graphite flake and metal powder is compacted at least once through the non-planar compacting.
According to the preparation method of the graphite flake metal matrix composite, the mixed powder obtained by mixing the graphite flakes and the metal powder is subjected to at least one non-planar compaction, so that the graphite flakes are arranged and distributed on the vertical parallel surfaces on the three intersecting lines which are at least not on the same plane, the graphite flake metal matrix preform which is arranged in three dimensions is obtained, and then the graphite flake metal matrix preform is sintered by the hot isostatic pressing method, the hot isostatic pressing method can simultaneously provide three-way pressure, the three-way pressure uniformly acts on the graphite flake metal matrix preform which is arranged in three dimensions, the three-dimensional structure of the graphite flake metal matrix preform is not damaged, the compactness of the preform is improved, and the graphite flake metal matrix composite is obtained. The graphite sheets in the material are arranged in a three-dimensional structure, have high compactness, high heat conduction performance and uniform thermal expansion coefficient in all directions, and are favorable for long-acting and stable operation of electronic devices.
In an alternative embodiment, the mixture of graphite flakes and metal powder is subjected to non-planar compaction to impart a non-planar structure to the mixture that is concave along the pressed face. The non-planar compaction of the mixture of graphite flake and metal powder can change the spatial arrangement mode of the graphite flake, thereby regulating and controlling the thermodynamic properties of the composite material prepared by the graphite flake.
Preferably, the non-planar structure comprises a surface formed by a plurality of three-dimensional polyhedral structures or a plurality of three-dimensional curved surface structures.
Preferably, in order to make the graphite sheets in the mixture have three-dimensional structures, a plurality of three-dimensional polyhedral structures or a plurality of three-dimensional curved surface structures are orderly and compactly arranged.
Preferably, the included angle between the concave surface and the pressed surface of each three-dimensional polyhedral structure is 1-89 degrees, more preferably, the three-dimensional polyhedral structure is a regular rectangular pyramid, and the side length of the bottom surface of the regular rectangular pyramid is 3-7 mm.
Preferably, each three-dimensional curved surface body structure includes any one of a spherical surface, an ellipsoidal surface, or an irregular curved surface. In the present invention, the non-planar compacting is not limited as long as it can ensure that the graphite flakes are arranged and distributed on the vertical parallel planes of the three intersecting lines which are not at least on the same plane, and the specific compacting method and the specific shape of the graphite flakes in the composite material are not limited by the present invention.
In an alternative embodiment, the compaction is a step compaction. It is understood that step compaction refers to compacting a portion of the mixture of graphite flake and metal powder at a time, repeating this step, and taking powder multiple times until compacted to a predetermined height. Since compacting all the mixtures directly may cause anisotropy between the surface layer graphite flake and the lower layer or the inner graphite flake, the thermal expansion coefficient of the graphite flake metal matrix composite is inconsistent, and the heat dissipation performance is poor. The amount of the mixture compacted by single steps can be controlled by step compaction, so that the arrangement mode of graphite flakes is controlled, and the prepared graphite flake metal matrix composite material has uniform thermal expansion coefficients in all directions, and is beneficial to long-term stable operation of electronic devices.
Specifically, in order to achieve both the uniformity of the appearance of the graphite flake metal matrix composite and the relatively uniform coefficient of thermal expansion in all directions, the first compaction and the last compaction are planar compactions, and the rest compaction is non-planar compaction.
Preferably, in order to prevent die wear caused by pressing to the die in non-planar pressing, and simultaneously control the appearance uniformity of the graphite sheet metal matrix composite material, the single pressing amount of planar pressing is 5-10 mm in thickness after pressing.
Preferably, in order to better change the morphology of graphite flakes in the graphite flake metal matrix composite, the amount of single compaction by non-planar compaction is less than or equal to 2mm in thickness after compaction.
Preferably, the relative rotation angle of the ram for each non-planar compaction is maintained constant in order to ensure uniformity of the coefficient of thermal expansion of the graphite sheet in all directions.
Preferably, the compaction pressure is 1MPa to 5MPa, and the compaction pressure can be the same or different for each compaction.
In an alternative embodiment, the metal powder includes at least one of pure copper powder and its alloy powder, pure aluminum powder and its alloy powder, pure silver powder and its alloy powder, and pure magnesium powder and its alloy powder.
Preferably, the relative bulk density of the metal powder is less than or equal to 30%, wherein the relative bulk density is a percentage of the bulk density of the powder to the theoretical density of the powder material.
In an alternative embodiment, the graphite flake has a scaly structure, the average particle size of the graphite flake is 100 μm to 1000 μm, the average thickness is 10 μm to 50 μm, and the d of the graphite flake is measured by the Gakushin method 002 The value is 0.335-0.336 nm.
Preferably, the mixing means of the mixture includes any one of manual mixing, V-type mixing and acoustic resonance mixing of the graphite flake and the metal powder.
Preferably, in order to effectively improve the thermal conductivity of the composite material, control the thermal expansion coefficient of the composite material and ensure that the composite material has certain mechanical strength, the volume fraction of the graphite flake in the mixture is controlled to be 10-50%.
In an alternative embodiment, sintering the preform using hot isostatic pressing comprises: and (3) carrying out vacuum sealing cladding on the preform, and then placing the clad preform into a hot isostatic pressing furnace for sintering. The vacuum sealing cladding is used for improving the sintering compactness of the preform and preventing the mixture compactness from being reduced due to the infiltration of high-temperature gas in the sintering process in the hot isostatic pressing furnace.
Preferably, vacuum sealing the cladding comprises welding a sealed metal shell to the preform surface under vacuum.
Preferably, the shape and size of the sealed metal housing should be the same as those of the preform to be coated, preventing damage to the internal structure of the preform when vacuum sealing coating is performed.
In some embodiments, the sealed metal housing is prepared by a drawing process.
Preferably, the welding includes any one of thermal diffusion welding or resistance welding.
Preferably, in order to prevent the structure of the preform from being damaged during the welding process, the sealing metal case may include a welding portion which is not in contact with the preform and is used only for welding.
Preferably, in order to reduce the influence of the shell material on the preform powder sintering process while having a superior heat transfer performance, the material of the sealing metal shell includes any one of a low carbon steel plate, a stainless steel plate, copper or a copper alloy plate.
In a second aspect, the present invention provides an assembly tool for preparing a graphite sheet metal matrix composite material, applicable to the preparation method of any one of the previous embodiments, and applicable to preparing a graphite sheet metal matrix composite material, including a ram and a fixing assembly.
The upper pressing head comprises a plane upper pressing head and a non-plane upper pressing head, and the plane upper pressing head and the non-plane upper pressing head are used for finishing plane compaction and non-plane compaction.
The non-planar upper pressure head is characterized in that a three-dimensional pressure head structure is arranged on the surface of the planar upper pressure head. In some embodiments, the three-dimensional indenter structure is removably disposed with the surface of the indenter on the plane; in other embodiments, the three-dimensional indenter structure is integrally formed with the surface of the indenter on the plane.
The fixing component comprises a first fixing piece and a second fixing piece, the first fixing piece is provided with a groove, the lower pressing head is located in the groove, the second fixing piece is propped against and fixed on the inner surface of the groove, and the upper pressing head can be selectively contained in the groove and used for pressing or taking out the prefabricated body.
Preferably, the groove formed on the first fixing piece can be a through groove or a non-through groove. More preferably, in order to facilitate the removal of the preform, the internal structure of the preform is prevented from being changed, and the groove formed in the first fixing member is a through groove.
Preferably, the number of the second fixing pieces is at least two, and the connection mode among the plurality of the second fixing pieces is abutting. Because the second mounting is a plurality of, and have not directly connected the relation between two adjacent second mountings, only contact butt, consequently when taking out the prefabrication body, can be with prefabrication body and assembling die complete separation, avoided the internal structure change of prefabrication body.
Preferably, the three-dimensional indenter structure comprises a surface formed by a plurality of three-dimensional polyhedral structures or a plurality of three-dimensional curved surface structures for forming a non-planar structure on the preform surface.
In an alternative embodiment, the upper ram is a cylinder, having a diameter of 30 to 60mm and a height of 35 to 45mm. It will be appreciated that the dimensions of the upper ram are merely those used in the preferred embodiment of the invention, and in other embodiments the dimensions of the upper ram may be correspondingly increased or decreased to meet different compaction requirements.
In an alternative embodiment, the upper ram is made of any one of aluminum alloy, carbon steel and stainless steel, preferably 7-series aluminum alloy. The invention is not limited to the material of the upper pressure head, and only needs to match the shape of the lower pressure head to finish the compaction process.
Preferably, the lower pressure head is a cylinder, the diameter is 30-60 mm, the height is 20-30 mm, and the lower pressure head is made of graphite.
It is understood that the upper and lower ram are cooperating compaction tools, so that the dimensions of the upper and lower ram are matched, and the dimensions of the lower ram are correspondingly changed when the dimensions of the upper ram are changed. The material of the lower pressing head is only the material of the preferred embodiment of the present invention, and the present invention is not limited to the material of the lower pressing head, as long as the shape of the lower pressing head can be matched with the shape of the upper pressing head, and the compaction process is completed.
Preferably, the first fixing piece is a circular cylinder, the outer diameter is 110-130 mm, the inner diameter is 50-70 mm, the height is 50-70 mm, and the first fixing piece is made of graphite.
Preferably, the number of the second fixing pieces is 4, the 4 second fixing pieces are sequentially abutted to form a circular cylinder, the outer diameter is 50-70 mm, the inner diameter is 40-50 mm, the height is 50-70 mm, and the second fixing pieces are made of 7-series aluminum alloy.
It should be understood that the first fixing member and the second fixing member are for accommodating the upper ram and the lower ram, and thus, specific dimensions thereof should be based on actual dimensions of the upper ram and the lower ram, and the above ranges are only preferred ranges provided by the present invention, and should not be construed as limiting the dimensions of the first fixing member and the second fixing member.
Further, the above materials for the first fixing member and the second fixing member are only preferred materials provided by the present invention, and should not be construed as limiting the materials for the first fixing member and the second fixing member. In other embodiments, the materials of the first fixing member and the second fixing member may be carbon steel, stainless steel, or the like.
In a third aspect, the present invention provides a graphite flake metal matrix composite made by the method of any of the preceding embodiments or processed through the assembly mold of the preceding embodiments.
In a fourth aspect, the present invention provides an application of the graphite flake metal matrix composite according to the foregoing embodiment in the field of heat dissipation of electronic chips.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
Referring to fig. 1, the present embodiment provides an assembling mold 100 for a graphite sheet metal matrix composite material, which includes a pressing head and a fixing component.
The upper ram includes a planar upper ram 112 and a non-planar upper ram 113 for performing planar compaction and non-planar compaction.
Referring to fig. 2, a non-planar ram 113 is provided with a three-dimensional ram structure on the surface of the planar ram 112. In this embodiment, the three-dimensional indenter structure is integrally formed with the surface of the indenter on the plane; in other embodiments, the three-dimensional indenter structure is removably disposed with the surface of the indenter on the plane.
In this embodiment, the upper press head has a cylindrical overall shape, a diameter of 45.4mm and a height of 40mm, and is made of 7-series aluminum alloy. The three-dimensional indenter structure comprises a surface formed by closely arranging a plurality of three-dimensional polyhedral structures, specifically, the three-dimensional polyhedral structure is a regular quadrangular pyramid, the side length of the bottom surface of the regular quadrangular pyramid is 5mm, the included angle degree between the side surface and the end surface of the indenter is 45 degrees, and the three-dimensional polyhedral structure is used for forming a non-planar structure on the surface of the preform 200.
Preferably, the lower pressing head 111 is a cylinder, the diameter is 46mm, the height is 25mm, and the lower pressing head 111 is made of graphite.
Referring to fig. 1 and fig. 3, the fixing assembly includes a first fixing member 121 and a second fixing member 122, the first fixing member 121 is provided with a groove, the lower pressing head 111 is located in the groove, and the second fixing member 122 is abutted against and fixed on the inner surface of the groove, and the upper pressing head can be selectively accommodated in the groove for compacting or taking out the preform 200.
In this embodiment, in order to facilitate the removal of the preform 200 and prevent the internal structure thereof from being changed, the groove formed in the first fixing member 121 is a through groove.
Specifically, the first fixing member 121 is a circular cylinder, the outer diameter is 120mm, the inner diameter is 60mm, the height is 60mm, and the material of the first fixing member 121 is graphite.
In this embodiment, the number of the second fixing members 122 is four, and the four second fixing members 122 are sequentially abutted to form a circular cylinder, the outer diameter is 60mm, the inner diameter is 46mm, the height is 60mm, and the material of the second fixing members 122 is 7 series aluminum alloy.
Since the number of the second fixing members 122 is plural, and there is no direct connection relationship between two adjacent second fixing members 122, only contact and abutment, the preform 200 can be completely separated from the assembly mold when the preform 200 is taken out, and the internal structure of the preform 200 is prevented from being changed.
The assembly, use and disassembly process of the assembly mold 100 of the graphite sheet metal matrix composite provided in the present embodiment:
and (3) assembling: the method comprises the steps of placing second fixing pieces 122 on the inner wall surface of a groove of a first fixing piece 121, enabling four second fixing pieces 122 to be sequentially abutted to form a cylindrical annular structure, and placing a lower pressing head 111 on the inner wall surface of the second fixing piece 122 so that the second fixing pieces 122 are fixedly abutted between the lower pressing head 111 and the first fixing piece 121.
The method comprises the following steps: when the assembly mold is configured for use, the powder to be pressed is placed in the cavity formed between the lower press head 111 and the second fixing member 122, the upper press head is placed on the inner wall surface of the second fixing member 122, and is pressed in the direction of the lower press head 111 until the powder to be pressed is completed. Wherein the upper ram may be selected to be a planar upper ram 112 and/or a non-planar upper ram 113 for compaction.
And (3) disassembly: when the powder to be pressed is finished, the upper pressing head is moved out, the first fixing piece 121 and the second fixing piece 122 are sequentially moved out, and the compacted powder is taken out from the surface of the lower pressing head 111 for later use.
Example 2
The embodiment provides a graphite sheet metal matrix composite.
Wherein the graphite flake has a scaly structure, the average grain diameter is 400 mu m, the average thickness is 10 mu m, the crystallinity of the graphite flake is measured by using a Gakushin method, and d 002 The value is 0.3355-0.3360 nm, the length-thickness ratio is 40, and the true density is 2.26g/cm 3 。
The metal powder is flake copper powder, the average grain diameter is 15 μm, the average thickness is 100nm, the length-thickness ratio is 150, and the true density is 8.9g/cm 3 Bulk density of 0.9g/cm 3 The relative bulk density was 10%.
The preparation method of the graphite flake metal matrix composite comprises the following steps:
s1, preparing a mixture of graphite flakes and metal powder
71.1g copper powder and 11.9g graphite flake are weighed, put into a plastic bottle with the volume of 500ml, covered and sealed, the volume ratio of the graphite flake in the mixture reaches 40%, and the mixture is mixed manually for 10 minutes.
S2, preparing a preform
The assembly mold 100 of the graphite sheet metal matrix composite of example 1 was used for the preparation, and specifically the following steps were adopted:
the assembly mold 100 of the graphite flake metal matrix composite is assembled as in the assembly process of example 1, and then the mixture of graphite flakes and metal powder is charged into the mold for stepwise compaction, wherein the first compaction and the last compaction are planar compactions and the remaining compaction are non-planar compactions. As shown in fig. 4, the powder surface after non-planar compaction is given a non-planar indenter structure and the orientation of the graphite flakes in the mixture is changed.
The weight of the mixture of graphite flake and metal powder was 10g each time of planar compaction, and the weight of the mixture of graphite flake and metal powder was 6g each time of non-planar compaction.
After each compaction, the upper ram is separated from the powder layer, the mixture of graphite flakes and metal powder is added again, and then the planar ram or the non-planar ram is selected according to the compaction requirement to compact the powder again until a preform of a preset height is obtained, as shown in fig. 5.
In this example, the pressure is 2MPa for each compaction, the number of non-planar compactions is 10, and the preset height of the preform is 14mm.
In this embodiment, in order to ensure that the non-planar structure of the powder surface is not destroyed, the relative rotation angle of the ram for each non-planar compaction remains unchanged.
S3, sintering by hot isostatic pressing
The preform was removed for use as in the mold removal method of example 1.
Preparation of a sealed metal housing 300: and drawing the two same copper sheets by adopting a drawing process to prepare two cap-shaped structures with the drawing depth of 7mm and the inner diameter of 46 mm. Wherein, the thickness of copper sheet is 1mm, and the diameter is 100mm.
The preform 200 is put into one of the cap-shaped metal shells obtained by drawing, and the other cap-shaped metal shell is covered on the surface of the preform 200, so that the two cap-shaped metal shells can completely cover the preform 200, as shown in fig. 6. Maintaining the vacuum degree at 10 -1 And (3) performing thermal diffusion welding below Pa to seal and weld the two cap-shaped metal shells, and completing vacuum sealing cladding of the preform 200.
And placing the vacuum-sealed and coated preform 200 and the sealed metal shell 300 on the surface of the preform in a hot isostatic pressing furnace for densification and sintering. Technological parameters: the temperature is raised to 700 ℃ from room temperature at 5 ℃ per minute, and the mixture is cooled after heat preservation for 45 minutes; in the heat preservation stage at 700 ℃, the isostatic pressure is kept at 100MPa, and the pressure is released to the atmospheric pressure after cooling. Cutting the sealed metal shell 300 on the surface, and taking out the sintered preform 200 to obtain the prepared graphite sheet metal matrix composite material.
Comparative example 1
The comparative example provides a graphite flake metal matrix composite, which is similar to example 2 in terms of raw materials and preparation methods, except that hot isostatic pressing sintering is not adopted, but instead, a graphite flake metal matrix composite preform is pretreated by adopting cold hydrostatic equipment, and then the preform is freely sintered in a vacuum environment to obtain the graphite flake metal matrix composite. Microstructure characterization is carried out on the graphite flake metal matrix composite, and the results shown in figures 7-10 are obtained.
As can be seen from fig. 7, the graphite sheets are arranged along concentric square sides and distributed in concentric square arrays, consistent with model predictions. In fig. 8, the graphite sheets are arranged in parallel from left to right and then are arranged along a folding line, the acute angle of the folding line is about 80 degrees, and the theoretical model value is 70 degrees. In fig. 9, the graphite sheets are arranged along a folding line from left to right, the angle at which the folding line turns is about 99 degrees, and the theoretical model value is 89 degrees. However, as can be seen from fig. 10, there are a large number of voids in the microstructure of the copper matrix, and although the graphite flake arrangement structure substantially retains the three-dimensional shape and is substantially close to the preform model prediction, the microstructure has a large number of voids and the material properties are poor.
Comparative example 2
This comparative example provides a graphite flake metal-based composite, which is similar to example 2 in that it is produced by pressing a mixture of flake aluminum powder and graphite flakes, the flake aluminum powder having an average particle diameter of 40 μm, an average thickness of 500nm, a length to thickness ratio of 80, and a true density of 2.7g/cm 3 Bulk density of 0.5g/cm 3 The relative bulk density was 19%.
The graphite flake was in accordance with example 2. The difference is that the graphite flake aluminum-based composite material is prepared by adopting the method of the embodiment 1, then directly adopting hot-pressing sintering, and observing microstructure after densification sintering. The difference between the obtained graphite flake arrangement structure and the prefabricated body is remarkable, as shown in fig. 11, the graphite flakes are arranged along concentric square sides and distributed in concentric square arrays in the top view, the graphite flakes are arranged along fold lines in the side view, the fold line angle is about 150 degrees, and the predicted value of the theoretical model is 90 degrees. The graphite sheets are arranged along the vertical pressure direction in a unidirectional pressure state in a hot-press sintering mode, the included angle of the graphite sheets arranged along the bending position is greatly changed, the difference between the graphite sheets and a theoretical prediction model is large, and the process controllability is poor.
Test example 1
According to known data, the high orientation direction thermal conductivity of the high orientation graphite flake aluminum-based composite (graphite flake volume fraction 40%) is 430W/mK, and the thermal expansion coefficient is 23×10 -6 K; the thermal conductivity in the vertical high orientation direction is 60W/mK, and the thermal expansion coefficient is-19 multiplied by 10 -6 /K。
High orientation graphite flake copper-based composite material (graphite flake volume fraction 40%) with high orientation direction thermal conductivity of 630W/mK and thermal expansion coefficient of 14×10 -6 K; the thermal conductivity in the vertical high orientation direction is 90W/mK, and the thermal expansion coefficient is 3 multiplied by 10 -6 and/K. And then according to a transformation rule, carrying out theoretical prediction on thermal properties (thermal expansion coefficient and thermal conductivity) of the graphite flake metal matrix composite materials prepared in the example 2 and the comparative examples 1-2, wherein the prediction formula is as follows:
T θ ＝T 0° cos 2 θ+T 90° sin 2 θ
ε θ ＝ε 0° cos 2 θ+ε 90° sin 2 θ
wherein T is θ Representing the thermal conductivity of the high-orientation graphite flake metal matrix composite along the direction with an included angle theta with the high-orientation direction, T 0° Exhibits high orientation direction thermal conductivity, T 90° Indicating the vertical high orientation direction thermal conductivity.
ε θ Representing the thermal expansion coefficient epsilon of the high-orientation graphite flake metal-based composite material along the direction with the included angle theta with the high-orientation direction 0° Indicating the coefficient of thermal expansion in the high orientation direction, ε 90° Indicating the coefficient of thermal expansion in the vertical high orientation direction.
The results shown in table 1 are obtained by a predictive formula according to the test performance of the high-orientation graphite flake metal composite.
Table 1 thermal prediction of graphite flake metal matrix composites
Remarks: x, y, z denote the test direction.
The graphite flake metal matrix composite provided by the invention has at least the following advantages:
by carrying out at least one non-planar compaction on the mixed powder obtained by mixing the graphite flakes and the metal powder, the graphite flakes are arranged and distributed on vertical parallel surfaces on three intersecting lines which are not at the same plane at least, so that the graphite flake metal-based preform 200 which is three-dimensionally arranged is obtained, and then the graphite flake metal-based preform 200 is sintered by a hot isostatic pressing method, and the hot isostatic pressing method can simultaneously provide three-dimensional pressure which uniformly acts on the graphite flake metal-based preform 200 which is three-dimensionally arranged without damaging the three-dimensional structure of the graphite flake metal-based preform 200, and the compactness of the preform 200 is improved, so that the graphite flake metal-based composite material is obtained. The graphite sheets in the material are arranged in a three-dimensional structure, have high compactness, high heat conduction performance and uniform thermal expansion coefficient in all directions, and are favorable for long-acting and stable operation of electronic devices.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the graphite flake metal matrix composite is characterized by comprising the steps of compacting a mixture of graphite flakes and metal powder to obtain a preform, and sintering the preform by adopting a hot isostatic pressing method to obtain the graphite flake metal matrix composite in three-dimensional arrangement;
the compacting includes planar compacting and non-planar compacting, and the mixture of graphite flakes and metal powder is compacted at least once through the non-planar compacting.
2. The method of claim 1, wherein the non-planar compaction of the mixture of graphite flakes and metal powder is performed to impart a non-planar structure to the mixture that is concave along the pressed surface;
preferably, the non-planar structure comprises a surface formed by a plurality of three-dimensional polyhedral structures or a plurality of three-dimensional curved surface structures;
preferably, the included angle between the concave surface and the pressed surface of each three-dimensional polyhedral structure is 1-89 degrees, more preferably, the three-dimensional polyhedral structure is a regular rectangular pyramid, and the side length of the bottom surface of the regular rectangular pyramid is 3-7 mm;
preferably, each of the three-dimensional curved surface body structures includes any one of a spherical surface, an ellipsoidal surface, or an irregular curved surface.
3. The method of claim 2, wherein the compaction is a stepwise compaction, the first compaction and the last compaction being a planar compaction, the remaining compaction being a non-planar compaction;
preferably, the single compacting amount of the planar compaction is 5 mm-10 mm in thickness after compaction;
preferably, the single compacting amount of non-planar compaction is that the thickness after compaction is less than or equal to 2mm;
preferably, the relative rotation angle of the ram for each non-planar compaction remains unchanged;
preferably, the compacting pressure is 1MPa to 5MPa.
4. The method of manufacturing according to claim 1, wherein the metal powder comprises at least one of pure copper powder and its alloy powder, pure aluminum powder and its alloy powder, pure silver powder and its alloy powder, and pure magnesium powder and its alloy powder;
preferably, the metal powder is flake, the average grain diameter is 10-100 μm, the average thickness is 0.1-20 μm, the length-thickness ratio is 10-500, and the relative bulk density is less than or equal to 30%.
5. The method according to claim 1, wherein the graphite flakes have a scaly structure, the average particle diameter of the graphite flakes is 100 μm to 1000 μm, the average thickness is 10 μm to 50 μm, and d 002 The value is 0.335-0.336 nm, and the length-thickness ratio is 35-45;
preferably, the mixing means of the mixture includes any one of manual mixing, V-type mixing and acoustic resonance mixing of graphite flakes and metal powder;
preferably, the volume fraction of graphite flakes in the mixture is 10% to 50%.
6. The method of manufacturing according to claim 1, wherein sintering the preform using hot isostatic pressing comprises: vacuum sealing and coating the preform, and then placing the coated preform into a hot isostatic pressing furnace for sintering;
preferably, the vacuum sealing cladding comprises welding a sealing metal shell on the surface of the preform under a vacuum environment;
preferably, the material of the sealing metal shell comprises any one of a low-carbon steel plate, a stainless steel plate, copper or a copper alloy plate;
preferably, the welding includes any one of thermal diffusion welding or resistance welding.
7. An assembling die of a graphite sheet metal matrix composite material, which is applied to the preparation method of any one of claims 1 to 6 and comprises a pressing head and a fixing component;
the pressing head comprises an upper pressing head and a lower pressing head, and a selectively detachable three-dimensional pressing head structure is arranged on a pressing surface of the upper pressing head and is used for finishing the planar compaction and the non-planar compaction;
the fixing assembly comprises a first fixing piece and a second fixing piece, a groove is formed in the first fixing piece, the lower pressure head is located in the groove, the second fixing piece is abutted against and fixed on the surface of the groove, and the upper pressure head can be selectively contained in the groove;
preferably, the number of the second fixing pieces is at least two, and the connection modes among the plurality of the second fixing pieces are butt joint;
preferably, the three-dimensional indenter structure comprises a surface formed by a plurality of three-dimensional polyhedral structures or a plurality of three-dimensional curved surface body structures.
8. The assembly die according to claim 7, wherein the upper pressing head is a cylinder, the diameter is 30-60 mm, the height is 35-45 mm, and the upper pressing head is made of 7-series aluminum alloy or 304 stainless steel;
preferably, the lower pressure head is a cylinder, the diameter is 30-60 mm, the height is 20-30 mm, and the lower pressure head is made of graphite;
preferably, the first fixing piece is a circular cylinder, the outer diameter is 110-130 mm, the inner diameter is 50-70 mm, and the height is 50-70 mm, and the first fixing piece is made of graphite;
preferably, the number of the second fixing pieces is 4, the 4 second fixing pieces are sequentially abutted to form a circular cylinder, the outer diameter is 50-70 mm, the inner diameter is 40-50 mm, the height is 50-70 mm, and the second fixing pieces are made of 7-series aluminum alloy.
9. A graphite sheet metal matrix composite material produced by the production method according to any one of claims 1 to 6 or processed by the assembly mold according to claim 7 or 8.
10. Use of the graphite flake metal matrix composite of claim 9 in the field of heat dissipation of electronic chips.
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| AU2086600A (en) * | 1998-12-16 | 2000-07-03 | Da Hai He | Low resistivity materials with improved wear performance for electrical current transfer and methods for preparing same |
| WO2001044436A1 (en) * | 1999-12-17 | 2001-06-21 | Henkel Kommanditgesellschaft Auf Aktien | Method for compacting multi-phase detergent and cleansing-agent shaped bodies |
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