CN117483895A - Brazing preparation process of graphene/metal composite heat-spreading plate - Google Patents
Brazing preparation process of graphene/metal composite heat-spreading plate Download PDFInfo
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- CN117483895A CN117483895A CN202311400752.2A CN202311400752A CN117483895A CN 117483895 A CN117483895 A CN 117483895A CN 202311400752 A CN202311400752 A CN 202311400752A CN 117483895 A CN117483895 A CN 117483895A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 101
- 238000005219 brazing Methods 0.000 title claims abstract description 50
- 238000003892 spreading Methods 0.000 title claims abstract description 36
- 239000002905 metal composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 80
- 229910000679 solder Inorganic materials 0.000 claims abstract description 27
- 230000007480 spreading Effects 0.000 claims abstract description 14
- 238000003466 welding Methods 0.000 claims abstract description 12
- 238000007747 plating Methods 0.000 claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 132
- 229910052759 nickel Inorganic materials 0.000 claims description 66
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 37
- 239000010936 titanium Substances 0.000 claims description 37
- 229910052719 titanium Inorganic materials 0.000 claims description 37
- 239000011248 coating agent Substances 0.000 claims description 29
- 238000000576 coating method Methods 0.000 claims description 29
- 238000004544 sputter deposition Methods 0.000 claims description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 15
- 239000013077 target material Substances 0.000 claims description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000000861 blow drying Methods 0.000 claims description 7
- 239000011888 foil Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 6
- 238000007772 electroless plating Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- FJMNNXLGOUYVHO-UHFFFAOYSA-N aluminum zinc Chemical compound [Al].[Zn] FJMNNXLGOUYVHO-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 3
- 102000020897 Formins Human genes 0.000 claims description 2
- 108091022623 Formins Proteins 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 14
- 230000017525 heat dissipation Effects 0.000 abstract description 9
- 239000000945 filler Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K3/00—Tools, devices, or special appurtenances for soldering, e.g. brazing, or unsoldering, not specially adapted for particular methods
- B23K3/08—Auxiliary devices therefor
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a brazing preparation process of a graphene/metal composite heat-spreading plate, and belongs to the technical field of heat dissipation of high-power devices. The heat spreading plate comprises a graphene plate, an aluminum alloy cover plate, a groove-shaped aluminum alloy bottom plate and a Sn-based soft solder layer. The connection between the graphene plate and the aluminum alloy cover plate and the connection between the graphene plate and the groove-shaped aluminum alloy bottom plate are welded together through a brazing mode. On one hand, the high-heat-conductivity graphene plate is packaged in the middle of the aluminum alloy structure, so that the defect that the device is short-circuited due to the fact that powder is easy to fall off on the surface of the graphene plate is avoided. On the other hand, the plating film prepared on the surfaces of the graphene plate and the aluminum alloy can improve the wettability of the brazing filler metal on the surfaces of the graphene plate and the aluminum alloy, and the welding of the graphene and the aluminum alloy is realized. The invention can timely lead out the heat of the high-power device, has better heat dissipation effect and ensures the safe operation and work of equipment.
Description
Technical Field
The invention belongs to the technical field of heterogeneous material welding, and particularly relates to a brazing preparation process of a graphene/metal composite heat-spreading plate.
Background
In the technical fields of power electronic devices and aerospace, the service performance and service life of a high-power device are closely related to the working temperature of the high-power device. With the development of high-power devices to high integration and light weight, the power density in the devices is greatly improved, and the generated heat is increased. If excessive heat is accumulated and cannot be timely discharged, the temperature rise is too high, so that the safe operation of the equipment is affected.
The main heat dissipation measure of the high-power device is to lead the heat of the heating device to the cold end of the equipment through the heat conducting element, and the heat conducting element used at present is a single metal heat spreading plate or a graphite heat spreading plate, which cannot meet the heat dissipation requirement of the high-power device. It is therefore of great importance to find materials that are lightweight and thermally conductive to produce composite heat spreading plates.
The metal heat dissipation material mainly comprises copper and aluminum, but copper has high density, so that the application of the metal heat dissipation material in the technical field of heat dissipation is limited. In comparison, aluminum has small density, and meets the aim of light weight of high-power devices, but with the development of integrated devices, the heat dissipation effect is poor. Some novel carbon materials, such as graphene, have thermal conduction mainly contributed by phonons, and have thermal conductivity of 5300 W.m at most due to strong covalent bond among carbon atoms and unique two-dimensional structure -1 ·K -1 Meanwhile, the density is lower, the flexibility is good, and the heat-conducting and heat-radiating composite material has obvious advantages in the aspects of heat conduction and heat radiation. However, graphene is prone to falling dust during practical application, resulting in device shorting. Therefore, how to combine the advantages and disadvantages of aluminum and graphene, and connect the aluminum and the graphene to prepare the composite heat-spreading plate, thereby being applied to heat dissipation of high-power devices and providing technical possibility. Because the structure of the graphene and the aluminum alloy are greatly different, a plurality of problems exist in the brazing of the graphene and the aluminum alloy, and the problems are mainly reflected in the fact that the brazing filler metal is difficult to wet on a substrate. In general, the wettability of metals on graphene is poor, in addition, the chemical property of aluminum is active, a compact oxide film generated on the surface can prevent the brazing filler metal from wetting and spreading in the brazing process, and the graphene and the aluminum alloy are difficult to be connected together in a brazing mode.
Under the current situation, students at home and abroad can modify the surfaces of graphene and metal by adding active metal into brazing filler metal or by methods such as vacuum evaporation, chemical plating, magnetron sputtering and the like so as to realize connection of the graphene and the metal. Most of the prior researches adopt active brazing to weld graphene and metal, but the brazing temperature of the active brazing is higher and is generally higher than the melting point of aluminum alloy, so that the active brazing is not suitable for manufacturing the graphene/aluminum alloy composite heat-spreading plate. There is therefore still a need to develop new technologies to meet the application needs.
Disclosure of Invention
The invention provides a brazing preparation process of a graphene/metal composite diffusion plate, which solves the problem that brazing filler metal is poor in wettability and spreadability on the surfaces of graphene and aluminum alloy during brazing. The prepared heat-spreading plate can combine the advantages of high heat conduction of graphene and low density of aluminum alloy, ensures the light weight of the heat-spreading plate, and timely derives the heat generated by a high-power device, and has the heat conductivity of 650-800 W.m -1 ·K -1 And has a higher thermal conductivity than metals such as silver, copper, and aluminum.
The technical scheme of the invention is as follows:
the brazing preparation process of the graphene/metal composite heat spreading plate comprises the following steps of:
step 1, preparing a titanium coating and a nickel coating on the upper surface and the lower surface of a graphene plate 1 in sequence by adopting a magnetron sputtering method;
step 2, preparing a nickel coating on the surface of the aluminum alloy cover plate 2 and the groove-shaped aluminum alloy bottom plate 3 by adopting an electroless plating method;
step 3, filling the groove of the groove-shaped aluminum alloy bottom plate with the nickel coating with foil-shaped Sn-based soft solder 4;
step 4, placing the graphene plate plated with the titanium film and the nickel film into the groove, then fully spreading the foil-shaped Sn-based soft solder on the upper surface of the graphene plate plated with the titanium film and the nickel film, and then pressing by using the aluminum alloy cover plate plated with the nickel film to obtain a prefabricated weldment of the aluminum alloy cover plate plated with the nickel film/foil-shaped Sn-based soft solder/graphene plate plated with the titanium film and the nickel film/foil-shaped Sn-based soft solder/groove-shaped aluminum alloy bottom plate composite structure plated with the nickel film;
and 5, placing the assembled prefabricated weldment into a vacuum brazing furnace for welding to obtain the graphene/metal composite heat-spreading plate.
Preferably, the magnetron sputtering in step 1 includes the following steps:
step 1-1, placing a graphene plate, a titanium target and a nickel target which are cleaned and dried by ultrasonic waves on a sample stage and a target stage of a magnetron sputtering system, preheating a graphene substrate under a vacuum condition, and heating to 150-250 ℃;
step 1-2, introducing high-purity argon into the sample chamber, wherein the argon flow is 20 mL/min -1 ～30mL·min -1 The working pressure is 0.2 Pa-0.5 Pa;
step 1-3, sputtering a titanium coating film on the surface of the graphene plate: the sputtering power is 80W-100W, and the sputtering time is 10 min-55 min;
step 1-4, the sample table is rotated to a nickel target, and nickel coating is sputtered on the surface of the graphene plate plated with the titanium film: the sputtering power is 100W-120W, and the sputtering time is 10 min-55 min.
Further, the ultrasonic cleaning and blow-drying treatment in the step 1-1 is to immerse the target material in acetone, alcohol and deionized water in sequence for ultrasonic cleaning for 15-20 min, and blow-drying.
Further, the vacuum condition described in step 1-1 is a vacuum degree of 1.5X10 -3 Pa～5×10 -4 Pa。
Preferably, the chemical plating in the step 2 is to put the aluminum alloy into aluminum cleaning solution to be soaked for 1min to 3min, rinse with deionized water, put into aluminum zinc precipitation solution to be soaked for 30s to 60s, rinse with deionized water; soaking in 88-92 deg.c nickel plating solution for 20-30 min, washing with deionized water and drying.
Preferably, the welding in step 5 is performed by placing the assembled prefabricated weldment in a vacuum brazing furnace at 5 ℃ for min under vacuum -1 ～10℃·min -1 The temperature in the vacuum brazing furnace is raised to 240-350 ℃ at the heating rate, the heat is preserved for 20-40 min, and then the welding piece is cooled along with the furnace, and is taken out from the vacuum brazing furnace.
Further, the vacuum condition in the step 5 is that the vacuum degree is 5×10 -3 Pa。
Preferably, the Sn-based solder includes a Sn63Pb37 solder and a sn3.0ag0.5cu solder.
The thermal conductivity of the graphene/metal composite heat-spreading plate prepared by the invention is 650-800 W.m -1 ·K -1 Between them.
The invention has the following beneficial effects:
the high-heat-conductivity graphene plate is placed in the middle of the aluminum alloy structure, so that the defect that the device is short-circuited due to the fact that powder is easy to fall off on the surface of the graphene plate is avoided.
The plating film prepared on the surfaces of the graphene plate and the aluminum alloy improves the wettability and spreadability of the Sn-based soft solder on the surfaces of the graphene plate and the aluminum alloy, and realizes the brazing connection of the graphene plate and the aluminum alloy.
The graphene/metal composite heat-spreading plate combines the advantages of high heat conduction of graphene and low density of aluminum alloy, ensures light weight of the heat-spreading plate, simultaneously timely derives heat generated by a high-power device, and achieves heat conductivity of 650-800 W.m -1 ·K -1 The safe operation and work of the equipment can be effectively ensured.
Drawings
FIG. 1 is a schematic three-dimensional structure of a heat spreading plate according to the present invention.
Fig. 2 is a top view of fig. 1.
Fig. 3 is a cross-sectional view of Fig. 2 along the A-A direction.
Wherein, 1-graphene plate, 2-aluminum alloy cover plate, 3-groove-shaped aluminum alloy bottom plate and 4-Sn-based soft solder.
Detailed Description
The invention will now be described in detail with reference to the drawings and examples.
According to the brazing preparation process of the graphene/metal composite diffusion plate, as shown in fig. 1, 2 and 3, the diffusion plate comprises a graphene plate, an aluminum alloy cover plate, a groove-shaped aluminum alloy bottom plate and Sn-based soft solder, wherein the connection between the graphene plate and the aluminum alloy cover plate as well as between the graphene plate and the groove-shaped aluminum alloy bottom plate is welded together through a brazing mode by the Sn-based soft solder.
Example 1
The size of the graphene plate is 100mm multiplied by 3.5mm, the size of the aluminum alloy cover plate is 103mm multiplied by 1mm, and the size of the groove-shaped aluminum alloy base plate is as follows: the outer frame is 113mm multiplied by 113mm, the inner frame is 100mm multiplied by 100mm, the depth of the groove is 4.5mm, the total thickness is 5.5mm, and a space for placing the aluminum alloy cover plate is reserved. The aluminum alloys are 6061 aluminum alloys, the Sn-based soft solder is Sn3.0Ag0.5Cu, and the Sn-based soft solder is foil-shaped solder.
The specific process of the embodiment comprises the following steps:
step 1, preparing a titanium coating film and a nickel coating film on the upper surface and the lower surface of a graphene plate in sequence by adopting a magnetron sputtering method, wherein the sizes of a titanium target material and a nickel target material are phi 50.8mm multiplied by 3mm, and the purities are 99.99 percent:
step 1-1, immersing the target material into acetone, alcohol and deionized water in sequence, ultrasonically cleaning for 20min, blow-drying, placing the graphene plate, the titanium target material and the nickel target material on a sample stage and a target stage of a magnetron sputtering system, and vacuumizing until the vacuum degree is 5 multiplied by 10 -4 Pa, preheating the graphene-based plate after the vacuum degree reaches the experimental requirement, and heating to 180 ℃;
step 1-2, introducing high-purity argon into the sample chamber, wherein the argon flow is 30 mL/min -1 The working pressure is 0.5Pa;
step 1-3, sputtering a titanium coating film on the surface of the graphene plate: sputtering power is 80W, and sputtering time is 45min;
step 1-4, the sample table is rotated to a nickel target, and nickel coating is sputtered on the surface of the graphene plate plated with the titanium film: the sputtering power is 100W, and the sputtering time is 45min.
Step 2, preparing a nickel coating on the surface of the aluminum alloy cover plate and the groove-shaped aluminum alloy bottom plate by adopting an electroless plating method: soaking the aluminum alloy in an aluminum cleaning solution for 3min, and washing with deionized water; soaking in aluminum zinc precipitation solution for 60s, and washing with deionized water; soaking in 90 deg.c nickel plating solution for 30min, washing with deionized water and drying.
Step 3, filling the groove of the groove-shaped aluminum alloy bottom plate with the nickel coating with foil Sn3.0Ag0.5Cu;
step 4, placing the graphene plate plated with the titanium film and the nickel film into a groove, then fully paving foil Sn3.0Ag0.5Cu on the upper surface of the graphene plate plated with the titanium film and the nickel film, and then pressing by using an aluminum alloy cover plate plated with the nickel film to obtain a prefabricated welding piece of the aluminum alloy cover plate/foil Sn3.0Ag0.5Cu/graphene plate/foil Sn3.0Ag0.5Cu/groove-shaped aluminum alloy bottom plate composite structure plated with the nickel film;
step 5, placing the assembled prefabricated weldment into a vacuum brazing furnace for welding: placing the assembled prefabricated weldment into a vacuum brazing furnace, and vacuumizing until the vacuum degree reaches 5 multiplied by 10 -3 Pa; at 7 ℃ min -1 The temperature in the vacuum brazing furnace is raised to 250 ℃ by the temperature rising rate, the heat is preserved for 25min, then the vacuum brazing furnace is cooled, and the weldment is taken out of the vacuum brazing furnace, so that the graphene/metal composite heat-spreading plate is obtained, and the heat conductivity of the graphene/metal composite heat-spreading plate is 664.76 W.m -1 ·K -1 。
Example 2
The size of the graphene plate is 200mm multiplied by 3.5mm, the size of the aluminum alloy cover plate is 203mm multiplied by 1mm, and the size of the groove-shaped aluminum alloy base plate is as follows: the outer frame is 213mm x 213mm, the inner frame is 200mm x 200mm, the depth of the groove is 4.5mm, the total thickness is 5.5mm, and a space for placing the aluminum alloy cover plate is reserved. The aluminum alloys are 6061 aluminum alloys, the Sn-based soft solder is Sn63Pb37, and the aluminum alloys are foil-shaped solder.
The specific process of the embodiment comprises the following steps:
step 1, sequentially preparing a titanium coating and a nickel coating on the upper and lower surfaces of a graphene plate by adopting a magnetron sputtering method, wherein the sizes of a titanium target and a nickel target are phi 50.8mm multiplied by 3mm, and the purities are 99.99 percent:
step 1-1, immersing the target material into acetone, alcohol and deionized water in sequence, ultrasonically cleaning for 20min, blow-drying, placing the graphene plate, the titanium target material and the nickel target material on a sample stage and a target stage of a magnetron sputtering system, and vacuumizing until the vacuum degree is 5 multiplied by 10 -4 Pa, preheating the graphene-based plate after the vacuum degree reaches the experimental requirement, and heating to 230 ℃;
step 1-2, introducing high-purity argon into the sample chamber, wherein the argon flow is 25 mL/min -1 The working pressure is 0.5Pa;
step 1-3, sputtering a titanium coating film on the surface of the graphene plate: sputtering power is 100W, and sputtering time is 40min;
step 1-4, the sample table is rotated to a nickel target, and nickel coating is sputtered on the surface of the graphene plate plated with the titanium coating: the sputtering power is 120W, and the sputtering time is 40min.
Step 2, preparing a nickel coating on the surface of the aluminum alloy cover plate and the groove-shaped aluminum alloy bottom plate by adopting an electroless plating method: soaking the aluminum alloy in an aluminum cleaning solution for 3min, and washing with deionized water; soaking in aluminum zinc precipitation solution for 60s, and washing with deionized water; soaking in 90 deg.c nickel plating solution for 30min, washing with deionized water and drying.
Step 3, using foil Sn63Pb37 to fully cover the groove inside of the groove-shaped aluminum alloy bottom plate plated with the nickel coating;
step 4, placing the graphene plate plated with the titanium film and the nickel film into the groove, then spreading foil-shaped Sn63Pb37 on the upper surface of the graphene plate with the titanium film and the nickel film, and then pressing by using an aluminum alloy cover plate plated with the nickel film to obtain a prefabricated weldment of a composite structure of the aluminum alloy cover plate plated with the nickel film/foil-shaped Sn63Pb 37/the graphene plate plated with the titanium film and the nickel film/foil-shaped Sn63Pb 37/the groove-shaped aluminum alloy bottom plate plated with the nickel film;
step 5, placing the assembled prefabricated weldment into a vacuum brazing furnace for welding: placing the assembled prefabricated weldment into a vacuum brazing furnace, and vacuumizing until the vacuum degree reaches 5 multiplied by 10 -3 Pa; at 6 ℃ min -1 The temperature in the vacuum brazing furnace is increased to 300 ℃ at the heating rate, the temperature is kept for 30min, then the furnace is cooled, and the weldment is taken out of the vacuum brazing furnace, thus obtainingGraphene/metal composite heat-spreading plate with heat conductivity of 730 W.m -1 ·K -1 。
Example 3
The size of the graphene plate is 293mm multiplied by 148mm multiplied by 4mm, the size of the aluminum alloy cover plate is 302mm multiplied by 157mm multiplied by 1mm, and the size of the groove-shaped aluminum alloy base plate is as follows: the outer frame is 305mm multiplied by 160mm, the inner frame is 293mm multiplied by 148mm, the depth of the groove is 4mm, the total thickness is 6mm, and the space for placing the aluminum alloy cover plate is reserved. The aluminum alloys are 6061 aluminum alloys, the Sn-based soft solder is Sn63Pb37, and the aluminum alloys are foil-shaped solder.
The specific process of the embodiment comprises the following steps:
step 1, preparing a titanium coating film and a nickel coating film on the upper surface and the lower surface of a graphene plate in sequence by adopting a magnetron sputtering method, wherein the sizes of a titanium target material and a nickel target material are phi 50.8mm multiplied by 3mm, and the purities are 99.99 percent:
step 1-1, immersing the target material into acetone, alcohol and deionized water in sequence, ultrasonically cleaning for 20min, blow-drying, placing the graphene plate, the titanium target material and the nickel target material on a sample stage and a target stage of a magnetron sputtering system, and vacuumizing until the vacuum degree is 5 multiplied by 10 -4 Pa, preheating the graphene-based plate after the vacuum degree reaches the experimental requirement, and heating to 250 ℃;
step 1-2, introducing high-purity argon into the sample chamber, wherein the argon flow is 20 mL/min -1 The working pressure is 0.5Pa;
step 1-3, sputtering a titanium coating film on the surface of the graphene plate: sputtering power is 100W, and sputtering time is 25min;
step 1-4, the sample table is rotated to a nickel target, and nickel coating is sputtered on the surface of the graphene plate plated with the titanium film: sputtering power is 100W, and sputtering time is 25min.
Step 2, preparing a nickel coating on the surface of the aluminum alloy cover plate and the groove-shaped aluminum alloy bottom plate by adopting an electroless plating method: soaking the aluminum alloy in an aluminum cleaning solution for 2min, and washing with deionized water; soaking in aluminum zinc precipitation solution for 50s, and washing with deionized water; soaking in 88 deg.c nickel plating solution for 30min, washing with deionized water and drying.
Step 3, using foil Sn63Pb37 to spread the groove inside of the groove-shaped aluminum alloy bottom plate plated with the nickel film;
step 4, placing the graphene plate plated with the titanium film and the nickel film into the groove, then fully paving foil-shaped Sn63Pb37 on the upper surface of the graphene plate plated with the titanium film and the nickel film, and then pressing by using an aluminum alloy cover plate plated with the nickel film to obtain a prefabricated weldment of a composite structure of the aluminum alloy cover plate plated with the nickel film/foil-shaped Sn63Pb 37/the graphene plate plated with the titanium film and the nickel film/foil-shaped Sn63Pb 37/the groove-shaped aluminum alloy bottom plate plated with the nickel film;
step 5, placing the assembled prefabricated weldment into a vacuum brazing furnace for welding: placing the assembled prefabricated weldment into a vacuum brazing furnace, and vacuumizing until the vacuum degree reaches 5 multiplied by 10 -3 Pa; at 8 ℃ min -1 The temperature in the vacuum brazing furnace is increased to 300 ℃ at the heating rate, the heat is preserved for 30min, then the vacuum brazing furnace is cooled, and the weldment is taken out of the vacuum brazing furnace, so that the graphene/metal composite heat-spreading plate is obtained, and the heat conductivity of the graphene/metal composite heat-spreading plate is 775.39 W.m -1 ·K -1 。
The foregoing is only a preferred embodiment of the present invention, but the present invention is not limited thereto, and any person skilled in the art, within the scope of the present disclosure, shall cover all modifications, equivalents, improvements and the like according to the technical scheme and the inventive idea of the present invention.
Claims (9)
1. The brazing preparation process of the graphene/metal composite heat spreading plate is characterized in that the heat spreading plate consists of a graphene plate (1), an aluminum alloy cover plate (2), a groove-shaped aluminum alloy bottom plate (3) and Sn-based soft solder (4), and specifically comprises the following steps of:
step 1, preparing a titanium coating and a nickel coating on the upper surface and the lower surface of a graphene plate (1) in sequence by adopting a magnetron sputtering method;
step 2, preparing nickel plating films on the surfaces of the aluminum alloy cover plate (2) and the groove-shaped aluminum alloy bottom plate (3) by adopting an electroless plating method;
step 3, using foil Sn-based soft solder (4) to spread the groove inside of the groove-shaped aluminum alloy bottom plate with the nickel coating;
step 4, placing the graphene plate plated with the titanium film and the nickel film into the groove, then fully spreading the foil-shaped Sn-based soft solder on the upper surface of the graphene plate plated with the titanium film and the nickel film, and then pressing by using the aluminum alloy cover plate plated with the nickel film to obtain a prefabricated weldment of the aluminum alloy cover plate plated with the nickel film/foil-shaped Sn-based soft solder/graphene plate plated with the titanium film and the nickel film/foil-shaped Sn-based soft solder/groove-shaped aluminum alloy bottom plate composite structure plated with the nickel film;
and 5, placing the assembled prefabricated weldment into a vacuum brazing furnace for welding to obtain the graphene/metal composite heat-spreading plate.
2. The process for preparing the graphene/metal composite diffusion plate according to claim 1, wherein the magnetron sputtering in the step 1 comprises the following steps:
step 1-1, placing a graphene plate, a titanium target and a nickel target which are cleaned and dried by ultrasonic waves on a sample stage and a target stage of a magnetron sputtering system, preheating a graphene substrate under a vacuum condition, and heating to 150-250 ℃;
step 1-2, introducing high-purity argon into the sample chamber, wherein the argon flow is 20 mL/min -1 ～30mL·min -1 The working pressure is 0.2 Pa-0.5 Pa;
step 1-3, sputtering a titanium coating film on the surface of the graphene plate: the sputtering power is 80W-100W, and the sputtering time is 10 min-55 min;
step 1-4, the sample table is rotated to a nickel target, and nickel coating is sputtered on the surface of the graphene plate plated with the titanium film: the sputtering power is 100W-120W, and the sputtering time is 10 min-55 min.
3. The process for preparing the brazing of the graphene/metal composite heat-spreading plate according to claim 2, wherein the ultrasonic cleaning and blow-drying treatment in the step 1-1 is to sequentially immerse the target material in acetone, alcohol and deionized water for ultrasonic cleaning for 15-20 min, and blow-drying.
4. The process for preparing the graphene/metal composite diffusion plate according to claim 2, wherein the vacuum condition in the step 1-1 is a vacuum degree of 1.5X10 -3 Pa～5×10 -4 Pa。
5. The process for preparing the brazing of the graphene/metal composite heat-spreading plate according to claim 1, wherein the electroless plating in the step 2 is to soak an aluminum alloy in an aluminum cleaning solution for 1-3 min, rinse the aluminum alloy with deionized water, soak the aluminum alloy in an aluminum zinc precipitation solution for 30-60 s, and rinse the aluminum alloy with deionized water; soaking in 88-92 deg.c nickel plating solution for 20-30 min, washing with deionized water and drying.
6. The process for preparing the graphene/metal composite heat-spreading plate according to claim 1, wherein the welding in the step 5 is to put the assembled prefabricated weldment into a vacuum brazing furnace at 5 ℃ for min under vacuum condition -1 ～10℃·min -1 The temperature in the vacuum brazing furnace is raised to 240-350 ℃ at the heating rate, the heat is preserved for 20-40 min, and then the welding piece is cooled along with the furnace, and is taken out from the vacuum brazing furnace.
7. The process for preparing a graphene/metal composite heat-spreading plate according to claim 6, wherein the vacuum condition in step 5 is a vacuum degree of 5×10 -3 Pa。
8. The brazing preparation process of the graphene/metal composite diffusion plate according to claim 1, wherein the Sn-based solder comprises Sn63Pb37 solder and sn3.0ag0.5cu solder.
9. The brazing preparation process of the graphene/metal composite heat spreading plate according to claim 1, wherein the thermal conductivity of the graphene/metal composite heat spreading plate is 650-800 W.m -1 ·K -1 Between them.
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