WO2021081820A1 - Manufacturing method for cpu heat dissipation material having heat-absorbing, heat-transferring and radiative complex mechanism - Google Patents

Manufacturing method for cpu heat dissipation material having heat-absorbing, heat-transferring and radiative complex mechanism Download PDF

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Publication number
WO2021081820A1
WO2021081820A1 PCT/CN2019/114404 CN2019114404W WO2021081820A1 WO 2021081820 A1 WO2021081820 A1 WO 2021081820A1 CN 2019114404 W CN2019114404 W CN 2019114404W WO 2021081820 A1 WO2021081820 A1 WO 2021081820A1
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parts
heat
heat dissipation
dissipation material
pressure
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PCT/CN2019/114404
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French (fr)
Chinese (zh)
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张敬敏
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追信数字科技有限公司
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Publication of WO2021081820A1 publication Critical patent/WO2021081820A1/en
Priority to ZA2021/06092A priority Critical patent/ZA202106092B/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/16—Homopolymers or copolymers or vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/02—Ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
    • C08F214/18—Monomers containing fluorine
    • C08F214/22—Vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/06—Coating with compositions not containing macromolecular substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • 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
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F1/00—Details not covered by groups G06F3/00 - G06F13/00 and G06F21/00
    • G06F1/16—Constructional details or arrangements
    • G06F1/20—Cooling means
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
    • C08F214/18—Monomers containing fluorine
    • C08F214/182—Monomers containing fluorine not covered by the groups C08F214/20 - C08F214/28
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/16—Homopolymers or copolymers of vinylidene fluoride

Definitions

  • the invention relates to the technical field of heat dissipation materials for electrical devices, in particular to a method for manufacturing a heat dissipation material for a CPU with a combined mechanism of heat absorption, heat transfer and radiation.
  • any kind of radiator on the market only uses one or two heat transfer methods, namely contact heat transfer and heat convection. At the same time, it has a more complex structure and higher material cost, which restricts high performance.
  • the heat dissipation efficiency has a limit problem. No matter how sophisticated the heat dissipation structure design is, the CPU heat sink is limited by its material and has the ultimate heat dissipation efficiency.
  • the present invention aims to provide a method for manufacturing a heat-absorbing and heat-radiation composite mechanism CPU heat-dissipating material with a water-repellent surface, large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation modes, and double radiation increase of overall heat dissipation efficiency.
  • the present invention adopts the following technical solution: a method for manufacturing a heat dissipation material for a CPU with a combined mechanism of heat absorption, heat transfer and radiation, including the following steps:
  • 2Tooling preparation prepare the bottom to be uniformly densely arranged with a hole diameter of 0.3mm-0.5mm according to a grid gap of 1mm-1.5mm, the ejection angle is 60° to the bottom surface, and the ejection angle is distributed clockwise along the tangential direction of the circumference of the air hole.
  • Cylindrical glass heating vessel with vent
  • step 2 Put the mixture A obtained in step 1 into a stainless steel autoclave, evacuated and filled with nitrogen, increase the pressure to 3.5MPa-3.8MPa, heat to 55°C-60°C, and stir at 120rpm/min-150rpm/min Stir continuously at a rate to obtain the pool to be reacted;
  • step 2 Put the reaction medium obtained in step 1 into a stainless steel autoclave, evacuate and fill with nitrogen, increase the pressure to 3.5MPa-3.8MPa, heat to 55°C-60°C, stir at 120rpm/min-150rpm/min Stir continuously at a rate to obtain a solution to be used;
  • step 2 Mechanically cut the component A obtained in step 2) in step 3 into particles with a particle size of 1mm-2mm to obtain particles A;
  • step 4 Machining the rough heat-dissipating material block obtained in step 3 into a shape with the bottom part compatible with the upper surface of the CPU and the top part compatible with the cooling fan to obtain a prefabricated composite heat-dissipating material;
  • step 5 Heat the prefabricated composite heat dissipation material obtained in step 4 to 120°C-130°C, and then rinse the surface of the heated heat dissipation material with a sufficient amount of ethanol to evaporate the attached ethanol to obtain the composite heat dissipation material to be processed;
  • 2Mix 800-900 parts of concentrated sulfuric acid, activated carbon powder and deionized water prepared in step 1) in step 1, and then put them into a glass container, and then immerse the container in the ice bath prepared in step 1 to keep the solution inside and outside the container separate.
  • the stirring rate of 30rpm/min-35rpm/min is mechanically stirred for 2.5h-3h, and then the potassium permanganate prepared in step 1) step 1 is slowly and evenly put into the container at the addition rate of 5%/min based on its total weight, and continue Stir continuously at a stirring rate of 15rpm/min-20rpm/min for 90min-100min to obtain a low-temperature reaction solution;
  • step 5 Put the product dispersion obtained in step 5) in step 5 in a spray container with a nozzle diameter of 0.2mm-0.5mm to obtain a dispersion sprayer;
  • the dried dispersion is processed to obtain the CPU heat dissipation material through the required heat absorption, heat transfer and radiation compound mechanism.
  • the heat-dissipating material consists of three parts: the base part is 55-80 parts of P(VDF-TrFE) copolymer with honeycomb multi-channel through holes in the part by weight.
  • the filler part is a blend of three components, including 15-20 parts of polymethyl methacrylate, 25-35 parts of ethylene-vinyl acetate, and 15-25 parts of graphite powder, cured inside the base part; A graphene film layer is also attached to the surface, the water contact angle of the film layer is 118°-123°, and the thermal conductivity is 4800W/m ⁇ K-5300W/m ⁇ K.
  • the present invention has the following advantages: (1) Since the graphene on the surface of the present invention has high thermal conductivity, only the film layer of the present invention can increase the heat dissipation efficiency of the original matrix heat dissipation material by 120W/m ⁇ K-150W. /m ⁇ K overall heat dissipation efficiency (calculate the overall heat dissipation structure cured with the film of the present invention). (2) After the film layer of the present invention is subjected to flash treatment, an irregular undulating structure will be formed on the surface of the film layer, which significantly increases the specific surface area of the present invention in contact with air, and further improves the heat dissipation efficiency.
  • the film of the present invention has a water contact angle of 118°-123°, has good hydrophobic properties, can keep the surface of the heat dissipation structure clean to a certain extent, and improve its service life and stability .
  • the present invention adopts a material structure which is completely different from the prior art.
  • the high temperature resistant polymer P (VDF-TrFE) copolymer with certain piezoelectric properties is used as the matrix, and it is filled with a part to improve the overall heat transfer performance.
  • the present invention uses conventional contact heat transfer and thermal convection, There are also part of the heat transfer function brought by the heat absorption when the solid is liquefied, the convection heat transfer after the solid is liquefied, and the piezoelectric material [P(VDF-TrFE) has better piezoelectric properties] (so the present invention can also be used in the heat sink Adding wires on both sides, combined with the chassis design, is used for the power supply of the decorative light-emitting diodes). Of course, the present invention only talks about the contact heat transfer performance, which is significantly lower than that of aluminum heat sinks. (5) Except for a small amount of graphite powder, the present invention has transparent organic polymers.
  • the present invention is light-transmissive and can disperse part of the heat through thermal radiation.
  • the present invention eliminates the internal stress obtained during rapid cooling of the present invention and makes the structure of the present invention more stable.
  • the opening in the substrate P is removed by liquefying part of the filler.
  • VDF-TrFE Low melting point substances (polymethyl methacrylate, EVA) and graphite powder, which are easy to fall off on the outside, and finally, in this way, the rough structure of the complex airway surface is obtained, which greatly increases the cost.
  • EVA polymethyl methacrylate
  • the present invention is a complex swirling path formed by the gas ejected at an oblique angle of 60° and naturally escapes upward in the viscous liquid. Therefore, most of the sparse holes in the present invention are through holes and densely distributed in the integral heat sink. Internally, this brings great convenience to the efficiency of air cooling.
  • the present invention can obtain non-flammable P(VDF-TrFE) fluid with extremely high viscosity after being liquefied by using an open flame to melt the bottom (you only need to heat it slightly), and then it can be self-adhesive on the surface of the CPU without setting in the middle. Additional glue, therefore, higher heat transfer efficiency, longer service life, and better reliability. Therefore, the present invention has the characteristics of hydrophobic surface, large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation methods, and double radiation enhancement of the overall heat dissipation efficiency.
  • 1Pre-preparation Prepare 1350g of concentrated sulfuric acid, 80g of activated carbon powder, 170g of potassium permanganate, 480g of vinylidene fluoride, 320g of trifluoroethylene, 270g of methyl methacrylate, 160g of vinyl acetate, 280g of ethylene, azobisisobutyronitrile Initiator 2g, graphite powder 220g, Guer gum 1.4g; prepare the bottom to be uniformly densely arranged with a grid gap of 1mm-1.5mm with a diameter of 0.3mm-0.5mm, the spray angle is 60° to the bottom surface, and the spray angle is along the stomata Cylindrical glass heating vessel with vent holes distributed clockwise in the tangential direction of the circumference;
  • component A 6Mechanically cut component A into particles with a particle size of 1mm-2mm to obtain particle A; put component B into a cylindrical glass heating vessel and heat it to completely melt to obtain molten pool B; put particle A into molten pool B After mixing thoroughly, stop heating and open the air jet hole at the bottom of the cylindrical glass heating vessel, and continue to spray nitrogen gas at a pressure of 3MPa-4MPa until the molten pool is completely cooled to obtain a block of crude heat-dissipating material;
  • the dispersion liquid is processed to obtain a CPU heat dissipation structure with the required three-dimensional structure carbon nanotube and graphene composite CPU heat dissipation material to improve the heat dissipation efficiency.
  • This embodiment has multiple heat dissipation mechanisms, large specific surface area, low noise, and has two solid-liquid conversion temperature control lines of 50°C-60°C and 80°C-90°C.
  • the overall thermal conductivity is 320W/m ⁇ K-450W/m. ⁇ K, the surface water contact angle is 118°-123°, the same below, the reliability is good, the same below.
  • 1Preparation Prepare 1400g of concentrated sulfuric acid, 60g of activated carbon powder, 160g of potassium permanganate, 500g of vinylidene fluoride, 300g of trifluoroethylene, 250g of methyl methacrylate, 150g of vinyl acetate, 250g of ethylene, and azobisisobutyronitrile.
  • Embodiment 3 The whole is consistent with embodiment 1, the difference lies in:
  • 1Pre-preparation prepare 1400g of concentrated sulfuric acid, 60g of activated carbon powder, 160g of potassium permanganate, 400g of vinylidene fluoride, 400g of trifluoroethylene, 300g of methyl methacrylate, 180g of vinyl acetate, 300g of ethylene, and azobisisobutyronitrile Initiator 2.5g, graphite powder 250g, Guer gum 2g; prepare the bottom to be uniformly densely arranged with a grid gap of 1mm-1.5mm with a diameter of 0.3mm-0.5mm, the spray angle is 60° to the bottom surface, and the spray angle is along the stomata Cylindrical glass heating vessel with vent holes distributed clockwise in the tangential direction of the circumference; 2 Mix 0.7g of azobisisobutyronitrile initiator with all methyl methacrylate, vinyl acetate, and graphite powder and stir evenly to obtain Mixture A, then put the mixture A into a stainless steel autoclave, evacuated and filled with
  • the film of the present invention has a water contact angle of 118°-123°, has good hydrophobic properties, can keep the surface of the heat dissipation structure clean to a certain extent, and improve its service life and stability .
  • the present invention adopts a material structure which is completely different from the prior art.
  • the high temperature resistant polymer P (VDF-TrFE) copolymer with certain piezoelectric properties is used as the matrix, and it is filled with a part to improve the overall heat transfer performance.
  • the present invention uses conventional contact heat transfer and thermal convection, There are also part of the heat transfer function brought by the heat absorption when the solid is liquefied, the convection heat transfer after the solid is liquefied, and the piezoelectric material [P(VDF-TrFE) has better piezoelectric properties] (so the present invention can also be used in the heat sink Adding wires on both sides, combined with the chassis design, is used for the power supply of the decorative light-emitting diodes). Of course, the present invention only talks about the contact heat transfer performance, which is significantly lower than that of aluminum heat sinks.
  • the present invention has transparent organic polymers. Therefore, the present invention is light-transmissive and can disperse part of the heat through thermal radiation.
  • the present invention eliminates the internal stress obtained during rapid cooling of the present invention and makes the structure of the present invention more stable.
  • the opening in the substrate P is removed by liquefying part of the filler.
  • VDF-TrFE Low melting point substances (polymethyl methacrylate, EVA) and graphite powder, which are easy to fall off on the outside, and finally, in this way, the rough structure of the complex airway surface is obtained, which greatly increases the cost.
  • EVA polymethyl methacrylate
  • the present invention is a complex swirling path formed by the gas ejected at an oblique angle of 60° and naturally escapes upward in the viscous liquid. Therefore, most of the sparse holes in the present invention are through holes and densely distributed in the integral heat sink. Internally, this brings great convenience to the efficiency of air cooling.
  • the present invention can obtain non-flammable P(VDF-TrFE) fluid with extremely high viscosity after being liquefied by using an open flame to melt the bottom (you only need to heat it slightly), and then it can be self-adhesive on the surface of the CPU without setting in the middle. Additional glue, therefore, higher heat transfer efficiency, longer service life, and better reliability. Therefore, the present invention has the characteristics of hydrophobic surface, large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation methods, and double radiation enhancement of the overall heat dissipation efficiency.

Abstract

Disclosed in the present invention are a CPU heat dissipation material having a heat-absorbing, heat-transferring and radiative complex mechanism and a manufacturing method therefor. The heat dissipation material is composed of three parts: a matrix part, which is 55-80 parts by weight of a P(VDF-TrFE) copolymer, inside which honeycombed multiple through holes are formed; a filler part, which is a blend comprising three components, i. e. 15-20 parts of polymethyl methacrylate, 25-35 parts of ethylene-vinyl acetate and 15-25 parts of graphite powder, cured inside the matrix part; and a graphene film layer, which is attached to an outer surface, a water contact angle of the film layer being 118° to 123°, and a thermal conductivity being 4800 W/m·K to 5300 W/m·K. The present invention has the advantages of hydrophobic surface, large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation modes, and double increase in overall heat dissipation efficiency.

Description

一种吸热传热辐射复合机制CPU散热材料的制造方法Method for manufacturing CPU heat dissipation material with composite mechanism of heat absorption, heat transfer and radiation 技术领域Technical field
本发明涉及电气装置用散热材料技术领域，尤其涉及一种吸热传热辐射复合机制CPU散热材料的制造方法。The invention relates to the technical field of heat dissipation materials for electrical devices, in particular to a method for manufacturing a heat dissipation material for a CPU with a combined mechanism of heat absorption, heat transfer and radiation.
背景技术Background technique
现在市面上任意一种散热器都仅利用了一种或两种热量传递方式，即接触式传热和热对流两种机理，同时有着较为复杂的结构和较高的材料成本，制约着高性能CPU的使用和推广。散热效率存在极限的问题，无论多精巧的散热结构设计，CPU散热器受其材料所限，有着散热的极限效率，这就导致对于性能顶尖的、功耗较大的CPU来说，要么换装价格更昂贵、可靠性更差、维护更困难的复杂散热器，要么更替为传热效率更高的高成本导热材料；最后，受限于常规散热结构的复杂性，随着使用时间的延长，其内由于空气中水、油性物质的附着，易吸附积尘，积尘过厚后会严重影响散热效率。At present, any kind of radiator on the market only uses one or two heat transfer methods, namely contact heat transfer and heat convection. At the same time, it has a more complex structure and higher material cost, which restricts high performance. The use and promotion of CPU. The heat dissipation efficiency has a limit problem. No matter how sophisticated the heat dissipation structure design is, the CPU heat sink is limited by its material and has the ultimate heat dissipation efficiency. This leads to the top performance, high power consumption CPU, or replacement Complex radiators that are more expensive, less reliable, and more difficult to maintain, can be replaced with high-cost thermally conductive materials with higher heat transfer efficiency; finally, limited by the complexity of conventional heat dissipation structures, as the use time increases, Due to the adhesion of water and oily substances in the air, it is easy to absorb dust. If the dust is too thick, it will seriously affect the heat dissipation efficiency.
技术问题technical problem
因此，市面上急需一种表面憎水、比表面积大、散热快、多种散热方式并存、整体散热效率双重增辐的吸热传热辐射复合机制CPU散热材料制造方法。Therefore, there is an urgent need in the market for a method for manufacturing a CPU heat dissipation material with a combination of heat absorption, heat transfer and radiation that has a water-repellent surface, a large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation methods, and a double increase in overall heat dissipation efficiency.
技术解决方案Technical solutions
本发明旨在提供一种表面憎水、比表面积大、散热快、多种散热方式并存、整体散热效率双重增辐的吸热传热辐射复合机制CPU散热材料制造方法。The present invention aims to provide a method for manufacturing a heat-absorbing and heat-radiation composite mechanism CPU heat-dissipating material with a water-repellent surface, large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation modes, and double radiation increase of overall heat dissipation efficiency.
为了实现上述目的，本发明采用以下技术方案：一种吸热传热辐射复合机制CPU散热材料的制造方法，包括以下步骤：In order to achieve the above objective, the present invention adopts the following technical solution: a method for manufacturing a heat dissipation material for a CPU with a combined mechanism of heat absorption, heat transfer and radiation, including the following steps:
1）原料准备1) Raw material preparation
①原材料准备：按重量份准备浓硫酸135份-140份、活性炭粉末6份-8份、高锰酸钾16份-17份、偏二氟乙烯40份-50份、三氟乙烯30份-40份、甲基丙烯酸甲酯25份-30份、醋酸乙烯15份-18份、乙烯25份-30份、偶氮二异丁腈引发剂0.15份-0.25份、石墨粉20份-25份、古尔胶0.1份-0.2份；① Preparation of raw materials: Prepare 135-140 parts of concentrated sulfuric acid, 6-8 parts of activated carbon powder, 16 parts of potassium permanganate, 16 parts of -17 parts of potassium permanganate, 40-50 parts of vinylidene fluoride, and 30 parts of trifluoroethylene according to parts by weight. 40 parts, methyl methacrylate 25-30 parts, vinyl acetate 15-18 parts, ethylene 25-30 parts, azobisisobutyronitrile initiator 0.15-0.25 parts, graphite powder 20-25 parts , 0.1 part -0.2 part of Guer Gum;
②工装准备：准备底部按1mm-1.5mm网格间隙均匀密排设置着孔径0.3mm-0.5mm、喷出角度与底面呈60°、喷出角度沿气孔所在圆周的切向方向顺时针分布的通气孔的圆柱形玻璃加热容器；②Tooling preparation: prepare the bottom to be uniformly densely arranged with a hole diameter of 0.3mm-0.5mm according to a grid gap of 1mm-1.5mm, the ejection angle is 60° to the bottom surface, and the ejection angle is distributed clockwise along the tangential direction of the circumference of the air hole. Cylindrical glass heating vessel with vent;
2）液体本体聚合反应2) Liquid bulk polymerization
①将阶段1）步骤①准备的偶氮二异丁腈引发剂0.05份-0.07份与全部甲基丙烯酸甲酯、醋酸乙烯、石墨粉混合并搅拌均匀，获得混合物A；① Combine 0.05 part-0.07 parts of the azobisisobutyronitrile initiator prepared in step 1) with all methyl methacrylate, vinyl acetate, and graphite powder and mix them evenly to obtain mixture A;
②将步骤①获得的混合物A投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.5MPa-3.8MPa，加热至55℃-60℃，以120rpm/min-150rpm/min的搅拌速率持续搅拌，获得待反应池；② Put the mixture A obtained in step ① into a stainless steel autoclave, evacuated and filled with nitrogen, increase the pressure to 3.5MPa-3.8MPa, heat to 55℃-60℃, and stir at 120rpm/min-150rpm/min Stir continuously at a rate to obtain the pool to be reacted;
③将阶段1）步骤①准备的乙烯持续缓慢通入步骤②获得的待反应池中，待全部通入后继续保温、保压5min-8min，然后卸压至2.4MPa-2.5MPa，炉冷至室温后完全卸压出炉，获得组份A；③Slowly pass the ethylene prepared in step 1) step ① into the waiting reaction tank obtained in step ②. After all the ethylene is passed through, continue to keep heat and keep the pressure for 5min-8min, then release the pressure to 2.4MPa-2.5MPa, and cool the furnace to After the room temperature, the pressure is completely relieved, and the component A is obtained;
3）气体悬浮聚合3) Gas suspension polymerization
①准备足量去离子水，将阶段1）步骤①准备的古尔胶、剩余的偶氮二异丁腈引发剂与去离子水搅拌均匀后获得反应介质；①Prepare a sufficient amount of deionized water, mix the Guer gum prepared in step ① of stage 1), the remaining azobisisobutyronitrile initiator and deionized water to obtain a reaction medium;
②将步骤①获得的反应介质投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.5MPa-3.8MPa，加热至55℃-60℃，以120rpm/min-150rpm/min的搅拌速率持续搅拌，获得待用溶液；② Put the reaction medium obtained in step ① into a stainless steel autoclave, evacuate and fill with nitrogen, increase the pressure to 3.5MPa-3.8MPa, heat to 55℃-60℃, stir at 120rpm/min-150rpm/min Stir continuously at a rate to obtain a solution to be used;
③将阶段1）步骤①准备的偏二氟乙烯、三氟乙烯持续缓慢均匀地通入待用溶液中，至通入完毕后继续保温、保压5min-8min，然后卸压至2.4MPa-2.5MPa，炉冷至室温后完全卸压出炉，蒸除水份，获得组份B；③Pour the vinylidene fluoride and trifluoroethylene prepared in step 1) into the solution to be used slowly and uniformly. After the feeding is completed, continue to keep the temperature and keep the pressure for 5min-8min, and then release the pressure to 2.4MPa-2.5 MPa, after the furnace is cooled to room temperature, the pressure is completely relieved from the furnace, and the water is evaporated to obtain component B;
4）散热材料成型4) Molding of heat dissipation material
①将阶段2）步骤③获得的组份A机械切割成粒径1mm-2mm的颗粒，获得颗粒A；① Mechanically cut the component A obtained in step 2) in step ③ into particles with a particle size of 1mm-2mm to obtain particles A;
②将阶段3）步骤③获得的组份B放入阶段1）步骤②准备的圆柱形玻璃加热容器中，加热至完全熔化，获得熔池B；②Put the component B obtained in stage 3) in step ③ into the cylindrical glass heating vessel prepared in stage 1) in step ②, and heat it until it is completely melted to obtain molten pool B;
③将步骤①获得的颗粒A投入步骤②的熔池B中，充分搅拌均匀后，停止加热，并开启圆柱形玻璃加热容器底部的喷气孔，以3MPa-4MPa的压力持续喷出氮气，直至熔池完全冷却，获得粗制散热材料块；③Put the particles A obtained in step ① into the molten pool B of step ②, and after fully stirring, stop heating, and open the air jet hole at the bottom of the cylindrical glass heating vessel, and continuously spray nitrogen at a pressure of 3MPa-4MPa until it melts. The pool is completely cooled to obtain a block of crude heat dissipation material;
④将步骤③获得的粗制散热材料块机械加工成底部与CPU上表面相适应，顶部与散热风扇相适应的形状，获得预制复合散热材料；④ Machining the rough heat-dissipating material block obtained in step ③ into a shape with the bottom part compatible with the upper surface of the CPU and the top part compatible with the cooling fan to obtain a prefabricated composite heat-dissipating material;
⑤将步骤④获得的预制复合散热材料加热至120℃-130℃，然后采用足量乙醇漂洗加热后的散热材料表面，蒸离附着的乙醇，获得待处理复合散热材料；⑤ Heat the prefabricated composite heat dissipation material obtained in step ④ to 120°C-130°C, and then rinse the surface of the heated heat dissipation material with a sufficient amount of ethanol to evaporate the attached ethanol to obtain the composite heat dissipation material to be processed;
5）表面改性分散液制备5) Preparation of surface modification dispersion
①装备冰水混合物组成的冰浴池；① Equipped with an ice bath composed of a mixture of ice and water;
②将阶段1）步骤①准备的浓硫酸、活性炭粉末与去离子水800份-900份混合均匀后装入玻璃容器，然后将容器浸入步骤①准备的冰浴池内，保持容器内外溶液隔离，以30rpm/min-35rpm/min的搅拌速率机械搅拌2.5h-3h，然后将阶段1）步骤①准备的高锰酸钾以自身总重量计5%/min的添加速率缓慢均匀地投入容器中，继续以15rpm/min-20rpm/min的搅拌速率持续搅拌90min-100min，获得低温反应溶液；②Mix 800-900 parts of concentrated sulfuric acid, activated carbon powder and deionized water prepared in step 1) in step ①, and then put them into a glass container, and then immerse the container in the ice bath prepared in step ① to keep the solution inside and outside the container separate. The stirring rate of 30rpm/min-35rpm/min is mechanically stirred for 2.5h-3h, and then the potassium permanganate prepared in step 1) step ① is slowly and evenly put into the container at the addition rate of 5%/min based on its total weight, and continue Stir continuously at a stirring rate of 15rpm/min-20rpm/min for 90min-100min to obtain a low-temperature reaction solution;
③将盛装低温反应溶液的玻璃容器浸入水温恒定在36℃-38℃之间的温水浴池中，保持容器内外溶液隔离，以120rpm/min-150rpm/min的搅拌速率搅拌，持续80min-90min，获得中温反应溶液；③ Immerse the glass container containing the low-temperature reaction solution in a warm water bath with a constant water temperature of 36℃-38℃, keep the solution inside and outside the container separate, and stir at a stirring rate of 120rpm/min-150rpm/min for 80min-90min to obtain Medium temperature reaction solution;
④将盛装中温反应溶液的玻璃容器浸入水温恒定在95℃-97℃之间的高温浴池中，保持容器内外溶液隔离，将重量份250份-300份的去离子水按自身总重量计5%/min的添加速率缓慢均匀地注入容器中，然后静置反应45min-50min，获得高温反应溶液；④ Immerse the glass container containing the medium-temperature reaction solution in a high-temperature bath with a constant water temperature of 95℃-97℃, keep the solution inside and outside the container isolated, and divide 250-300 parts by weight of deionized water based on 5% of its total weight. The addition rate of /min is slowly and uniformly injected into the container, and then the reaction is allowed to stand for 45min-50min to obtain a high-temperature reaction solution;
⑤在盛装高温反应溶液的玻璃容器中再次注入重量份450份-500份的去离子水，离心洗涤直至反应产物C的PH值6.5-7.5，获得产物分散液；⑤Inject again 450-500 parts by weight of deionized water into the glass container containing the high-temperature reaction solution, centrifuge and wash until the pH value of the reaction product C is 6.5-7.5, to obtain a product dispersion;
6）散热器制备6) Radiator preparation
①将阶段5）步骤⑤获得的产物分散液盛装在喷口直径0.2mm-0.5mm的喷雾容器中，获得分散液喷雾器；① Put the product dispersion obtained in step 5) in step ⑤ in a spray container with a nozzle diameter of 0.2mm-0.5mm to obtain a dispersion sprayer;
②将分散液喷雾器均匀、完整覆盖地喷润在阶段4）步骤⑤获得的待处理复合散热材料的外表面，待自然干燥后采用照强度为GN/M=30-35、照射时间1ms的闪光对干燥后的分散液进行处理，即获得经所需吸热传热辐射复合机制CPU散热材料。②Spray the dispersion sprayer uniformly and completely cover the outer surface of the composite heat dissipation material to be processed in step 4) Step ⑤, after natural drying, use a flash with an intensity of GN/M=30-35 and an irradiation time of 1ms The dried dispersion is processed to obtain the CPU heat dissipation material through the required heat absorption, heat transfer and radiation compound mechanism.
一种吸热传热辐射复合机制CPU散热材料，该散热材料由三部分组成：基体部分是按重量份计内部有蜂窝状多路通孔的P(VDF-TrFE)共聚物55份-80份，填料部分为固化在基体部分内部的包括聚甲基丙烯酸甲酯15份-20份、乙烯-醋酸乙烯25份-35份和石墨粉15份-25份三种组份的共混物；外表面还附着有石墨烯膜层，该膜层的水接触角118°-123°，热导率4800W/m·K-5300W/m·K。A CPU heat dissipation material with a heat-absorbing heat-radiation compound mechanism. The heat-dissipating material consists of three parts: the base part is 55-80 parts of P(VDF-TrFE) copolymer with honeycomb multi-channel through holes in the part by weight. , The filler part is a blend of three components, including 15-20 parts of polymethyl methacrylate, 25-35 parts of ethylene-vinyl acetate, and 15-25 parts of graphite powder, cured inside the base part; A graphene film layer is also attached to the surface, the water contact angle of the film layer is 118°-123°, and the thermal conductivity is 4800W/m·K-5300W/m·K.
有益效果Beneficial effect
本发明具有以下优点：（1）由于本发明表层的石墨烯自身导热效率就高，因此实测本发明仅膜层就能在原基体散热材料散热效率的基础上额外提升其120W/m·K-150W/m·K的整体散热效率（将固化有本发明膜层的散热结构整体计算）。（2）本发明的膜层经闪光处理后，膜层表面会形成不规则的起伏结构，明显增大本发明与空气接触的比表面积，进一步提升散热效率。（3）本发明的膜层经固化和闪光处理后，水接触角118°-123°，具有良好的憎水性能，能在一定程度上保持散热结构表面的洁净，提升其使用寿命和稳定性。（4）本发明采用了完全不同于现有技术的材料架构，由有一定压电性能的耐高温聚合物P(VDF-TrFE)共聚物作为基体，其内填充有部分提升整体传热性能的石墨粉、软化点80℃左右的部分聚甲基丙烯酸甲酯和较大量熔点在60℃左右的乙烯-醋酸乙烯（EVA），因此明显本发明除了利用了常规的接触传热和热对流外，还有固体液化时吸热、固体液化后对流传热以及压电材料[P(VDF-TrFE)具有较好的压电性能]带来的部分热转电功能（因此本发明还可以在散热块两侧添置导线，与机箱设计结合，用于装饰性发光二极管的供电），当然，本发明仅论及接触传热性能的话是明显低于铝制散热片的。（5）本发明除了少量石墨粉外，其它都有透明的有机聚合物，因此本发明是透光的，可以通过热辐射分散部分热量。（6）本发明通过最后的120℃-130℃热处理，一方面消除了本发明快冷时获得的内应力，使本发明结构更稳定，另一方面通过使部分填料液化去除了开口在基体P(VDF-TrFE)外面的低熔点物质（聚甲基丙烯酸甲酯、EVA）及易脱落物质石墨粉，最后，还通过这样的方式获得了复杂的气道表面的粗糙结构，极大地增加了本发明的比表面积。（7）本发明由于是沿60°斜角喷出的气体在粘稠液体中向上自然逸散形成的复杂回旋通路，因此本发明的所有疏孔大多数都是通孔且密布在整体散热块内，这为风冷的效率带来了极大的便利。（8）本发明可以通过采用明火融化底部获得不可燃的液化后具有极高粘度的P(VDF-TrFE)流体（只需稍稍加热即可获得），然后可以自粘在CPU表面，中间无需设置额外的胶合剂，因此，传热效率更高、使用寿命更长、可靠性更好。因此，本发明具有表面憎水、比表面积大、散热快、多种散热方式并存、整体散热效率双重增辐的特性。The present invention has the following advantages: (1) Since the graphene on the surface of the present invention has high thermal conductivity, only the film layer of the present invention can increase the heat dissipation efficiency of the original matrix heat dissipation material by 120W/m·K-150W. /m·K overall heat dissipation efficiency (calculate the overall heat dissipation structure cured with the film of the present invention). (2) After the film layer of the present invention is subjected to flash treatment, an irregular undulating structure will be formed on the surface of the film layer, which significantly increases the specific surface area of the present invention in contact with air, and further improves the heat dissipation efficiency. (3) After curing and flashing treatment, the film of the present invention has a water contact angle of 118°-123°, has good hydrophobic properties, can keep the surface of the heat dissipation structure clean to a certain extent, and improve its service life and stability . (4) The present invention adopts a material structure which is completely different from the prior art. The high temperature resistant polymer P (VDF-TrFE) copolymer with certain piezoelectric properties is used as the matrix, and it is filled with a part to improve the overall heat transfer performance. Graphite powder, part of polymethyl methacrylate with a softening point of about 80°C, and a relatively large amount of ethylene-vinyl acetate (EVA) with a melting point of about 60°C. Therefore, it is obvious that the present invention uses conventional contact heat transfer and thermal convection, There are also part of the heat transfer function brought by the heat absorption when the solid is liquefied, the convection heat transfer after the solid is liquefied, and the piezoelectric material [P(VDF-TrFE) has better piezoelectric properties] (so the present invention can also be used in the heat sink Adding wires on both sides, combined with the chassis design, is used for the power supply of the decorative light-emitting diodes). Of course, the present invention only talks about the contact heat transfer performance, which is significantly lower than that of aluminum heat sinks. (5) Except for a small amount of graphite powder, the present invention has transparent organic polymers. Therefore, the present invention is light-transmissive and can disperse part of the heat through thermal radiation. (6) Through the final heat treatment at 120°C-130°C, the present invention eliminates the internal stress obtained during rapid cooling of the present invention and makes the structure of the present invention more stable. On the other hand, the opening in the substrate P is removed by liquefying part of the filler. (VDF-TrFE) Low melting point substances (polymethyl methacrylate, EVA) and graphite powder, which are easy to fall off on the outside, and finally, in this way, the rough structure of the complex airway surface is obtained, which greatly increases the cost. Invented specific surface area. (7) The present invention is a complex swirling path formed by the gas ejected at an oblique angle of 60° and naturally escapes upward in the viscous liquid. Therefore, most of the sparse holes in the present invention are through holes and densely distributed in the integral heat sink. Internally, this brings great convenience to the efficiency of air cooling. (8) The present invention can obtain non-flammable P(VDF-TrFE) fluid with extremely high viscosity after being liquefied by using an open flame to melt the bottom (you only need to heat it slightly), and then it can be self-adhesive on the surface of the CPU without setting in the middle. Additional glue, therefore, higher heat transfer efficiency, longer service life, and better reliability. Therefore, the present invention has the characteristics of hydrophobic surface, large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation methods, and double radiation enhancement of the overall heat dissipation efficiency.
本发明的最佳实施方式The best mode of the present invention
实施例1：Example 1:
①预准备：准备浓硫酸1350g，活性炭粉末80g，高锰酸钾170g、偏二氟乙烯480g、三氟乙烯320g、甲基丙烯酸甲酯270g、醋酸乙烯160g、乙烯280g、偶氮二异丁腈引发剂2g、石墨粉220g、古尔胶1.4g；准备底部按1mm-1.5mm网格间隙均匀密排设置着孔径0.3mm-0.5mm、喷出角度与底面呈60°、喷出角度沿气孔所在圆周的切向方向顺时针分布的通气孔的圆柱形玻璃加热容器；①Pre-preparation: Prepare 1350g of concentrated sulfuric acid, 80g of activated carbon powder, 170g of potassium permanganate, 480g of vinylidene fluoride, 320g of trifluoroethylene, 270g of methyl methacrylate, 160g of vinyl acetate, 280g of ethylene, azobisisobutyronitrile Initiator 2g, graphite powder 220g, Guer gum 1.4g; prepare the bottom to be uniformly densely arranged with a grid gap of 1mm-1.5mm with a diameter of 0.3mm-0.5mm, the spray angle is 60° to the bottom surface, and the spray angle is along the stomata Cylindrical glass heating vessel with vent holes distributed clockwise in the tangential direction of the circumference;
②将偶氮二异丁腈引发剂0.6g与全部甲基丙烯酸甲酯、醋酸乙烯、石墨粉混合并搅拌均匀，获得混合物A，再将混合物A投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.6MPa，加热至55℃-60℃，以130rpm/min的搅拌速率持续搅拌，获得待反应池；② Mix 0.6 g of azobisisobutyronitrile initiator with all methyl methacrylate, vinyl acetate, and graphite powder and stir evenly to obtain mixture A, and then put mixture A into a stainless steel autoclave, and then fill it after vacuuming. Enter nitrogen, increase the pressure to 3.6MPa, heat to 55°C-60°C, and continue stirring at a stirring rate of 130rpm/min to obtain a reaction cell;
③在待反应池中持续缓慢通入乙烯，待全部通入后继续保温、保压5min-8min，然后卸压至2.4MPa-2.5MPa，炉冷至室温后完全卸压出炉，获得组份A；③Continue to slowly feed ethylene into the reaction tank, and continue to keep warm and keep the pressure for 5min-8min after it is fully introduced, and then relieve the pressure to 2.4MPa-2.5MPa. After the furnace is cooled to room temperature, the pressure is completely relieved and the furnace is released to obtain component A ；
④准备足量去离子水，将阶段1）步骤①准备的古尔胶、剩余的偶氮二异丁腈引发剂与去离子水搅拌均匀后投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.5MPa-3.8MPa，加热至55℃-60℃，以120rpm/min-150rpm/min的搅拌速率持续搅拌，获得待用溶液；④Prepare sufficient amount of deionized water, mix the Guer gum prepared in step 1), the remaining azobisisobutyronitrile initiator and deionized water, stir them evenly, put them into the stainless steel autoclave, evacuate and fill in Nitrogen, increase the pressure to 3.5MPa-3.8MPa, heat to 55°C-60°C, continue to stir at a stirring rate of 120rpm/min-150rpm/min, to obtain a ready-to-use solution;
⑤将偏二氟乙烯、三氟乙烯持续缓慢均匀地通入待用溶液中，至通入完毕后继续保温、保压5min-8min，然后卸压至2.4MPa-2.5MPa，炉冷至室温后完全卸压出炉，蒸除水份，获得组份B；⑤Pour the vinylidene fluoride and trifluoroethylene into the solution to be used slowly and uniformly. After the feeding is completed, keep the temperature and keep the pressure for 5min-8min, then release the pressure to 2.4MPa-2.5MPa, and cool the furnace to room temperature. Relieve the pressure completely and get out of the furnace, and steam to remove the water to obtain component B;
⑥将组份A机械切割成粒径1mm-2mm的颗粒，获得颗粒A；将组份B放入圆柱形玻璃加热容器中，加热至完全熔化，获得熔池B；将颗粒A投入熔池B中，充分搅拌均匀后，停止加热，并开启圆柱形玻璃加热容器底部的喷气孔，以3MPa-4MPa的压力持续喷出氮气，直至熔池完全冷却，获得粗制散热材料块；⑥Mechanically cut component A into particles with a particle size of 1mm-2mm to obtain particle A; put component B into a cylindrical glass heating vessel and heat it to completely melt to obtain molten pool B; put particle A into molten pool B After mixing thoroughly, stop heating and open the air jet hole at the bottom of the cylindrical glass heating vessel, and continue to spray nitrogen gas at a pressure of 3MPa-4MPa until the molten pool is completely cooled to obtain a block of crude heat-dissipating material;
⑦将粗制散热材料块机械加工成底部与CPU上表面相适应，顶部与散热风扇相适应的形状，再将加工好的散热块加热至120℃-130℃，然后采用足量乙醇漂洗加热后的散热材料表面，蒸离附着的乙醇，获得所需复合散热材料；⑦Machining the rough heat-dissipating material block into a shape whose bottom is compatible with the upper surface of the CPU and the top is compatible with the cooling fan, then heat the processed heat-dissipating block to 120°C-130°C, and then rinse and heat it with a sufficient amount of ethanol Evaporate the attached ethanol on the surface of the heat dissipation material to obtain the required composite heat dissipation material;
⑧将浓硫酸、活性炭粉末、多壁碳纳米管与去离子水8kg-9kg混合均匀后装入玻璃容器，将容器外表面浸入冰水混合物池内，以30rpm/min-35rpm/min的搅拌速率机械搅拌3h，再将高锰酸钾以自身总重量计8.5g/min的添加速率缓慢均匀地投入步骤②获得的低温预反应池中，投入完成后继续以15rpm/min-20rpm/min的搅拌速率持续搅拌90min-100min，获得低温反应溶液；⑧ Mix concentrated sulfuric acid, activated carbon powder, multi-walled carbon nanotubes and 8kg-9kg of deionized water into a glass container, immerse the outer surface of the container in the ice-water mixture pool, and mechanically stir at 30rpm/min-35rpm/min Stir for 3h, and then put potassium permanganate slowly and evenly into the low-temperature pre-reaction pool obtained in step ② at a rate of 8.5g/min based on its total weight, and continue to stir at a rate of 15rpm/min-20rpm/min after the input is complete Continue stirring for 90min-100min to obtain a low-temperature reaction solution;
⑨将盛装低温反应溶液的玻璃容器浸入由水温恒定在36℃-38℃之间的温水浴池中，以120rpm/min-150rpm/min的搅拌速率持续搅拌，持续80min-90min，获得中温反应溶液；再将盛装中温反应溶液的玻璃容器浸入水温恒定在95℃-97℃之间的高温浴池中，再将2.8kg的去离子水按自身总重量计140g/min的添加速率缓慢均匀地注入中温反应溶液中，静置反应45min-50min，获得高温反应溶液⑨ Immerse the glass container containing the low-temperature reaction solution in a warm water bath with a constant water temperature of 36°C-38°C, and continue stirring at a stirring rate of 120rpm/min-150rpm/min for 80min-90min to obtain a medium-temperature reaction solution; Then immerse the glass container containing the medium-temperature reaction solution in a high-temperature bath with a constant water temperature of 95℃-97℃, and then pour 2.8kg of deionized water into the medium-temperature reaction slowly and evenly at a rate of 140g/min based on its total weight. In the solution, let stand for 45min-50min to obtain a high-temperature reaction solution
⑩在高温反应溶液再次注入4.8kg的去离子水，离心洗涤直至PH值6.5-7.5，获得产物分散液；将产物分散液盛装在喷口直径0.2mm-0.5mm的喷雾容器中，获得分散液喷雾器；待用时，将分散液喷雾器均匀、完整覆盖地喷润在市售CPU散热结构的外表面，待自然干燥后采用照强度为GN/M=30-35、照射时间1ms的闪光对干燥后的分散液进行处理，获得经所需立体结构碳纳米管与石墨烯复合CPU散热材料提升散热效率的CPU散热结构。⑩Inject 4.8kg of deionized water into the high-temperature reaction solution again, centrifuge and wash until the PH value is 6.5-7.5, and obtain the product dispersion; put the product dispersion in a spray container with a nozzle diameter of 0.2mm-0.5mm to obtain a dispersion sprayer ; When ready to use, spray the dispersion sprayer evenly and completely on the outer surface of the commercially available CPU heat dissipation structure. After it is naturally dried, use a flash with an illumination intensity of GN/M=30-35 and an irradiation time of 1ms on the dried The dispersion liquid is processed to obtain a CPU heat dissipation structure with the required three-dimensional structure carbon nanotube and graphene composite CPU heat dissipation material to improve the heat dissipation efficiency.
本实施例具有多重散热机理，比表面积大、噪音小，且有50℃-60℃，80℃-90℃两道固液转换温控防线，整体热导率320W/m·K-450W/m·K，表面水接触角118°-123°下同，可靠性好，下同。This embodiment has multiple heat dissipation mechanisms, large specific surface area, low noise, and has two solid-liquid conversion temperature control lines of 50℃-60℃ and 80℃-90℃. The overall thermal conductivity is 320W/m·K-450W/m. ·K, the surface water contact angle is 118°-123°, the same below, the reliability is good, the same below.
实施例2：Example 2:
整体与实施例1一致，差异之处在于：The whole is consistent with Example 1, the difference lies in:
①准备：准备浓硫酸1400g，活性炭粉末60g，高锰酸钾160g、偏二氟乙烯500g、三氟乙烯300g、甲基丙烯酸甲酯250g、醋酸乙烯150g、乙烯250g、偶氮二异丁腈引发剂1.5g、石墨粉200g、古尔胶1g；准备底部按1mm-1.5mm网格间隙均匀密排设置着孔径0.3mm-0.5mm、喷出角度与底面呈60°、喷出角度沿气孔所在圆周的切向方向顺时针分布的通气孔的圆柱形玻璃加热容器；②将偶氮二异丁腈引发剂0.5g与全部甲基丙烯酸甲酯、醋酸乙烯、石墨粉混合并搅拌均匀，获得混合物A，再将混合物A投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.5MPa，加热至55℃-60℃，以120rpm/min的搅拌速率持续搅拌，获得待反应池；①Preparation: Prepare 1400g of concentrated sulfuric acid, 60g of activated carbon powder, 160g of potassium permanganate, 500g of vinylidene fluoride, 300g of trifluoroethylene, 250g of methyl methacrylate, 150g of vinyl acetate, 250g of ethylene, and azobisisobutyronitrile. 1.5g of graphite powder, 200g of graphite powder, 1g of Guer gum; prepare the bottom to be uniformly and densely arranged according to the grid gap of 1mm-1.5mm. The aperture is 0.3mm-0.5mm, the spray angle is 60° to the bottom surface, and the spray angle is along the stomata. Cylindrical glass heating vessel with vent holes distributed clockwise in the tangential direction of the circumference; ②0.5g of azobisisobutyronitrile initiator is mixed with all methyl methacrylate, vinyl acetate, and graphite powder and stirred evenly to obtain a mixture A. Put the mixture A into a stainless steel autoclave, vacuumize and fill with nitrogen, increase the pressure to 3.5MPa, heat to 55°C-60°C, and continue to stir at a stirring rate of 120rpm/min to obtain a reaction pool;
实施例3：整体与实施例1一致，差异之处在于：Embodiment 3: The whole is consistent with embodiment 1, the difference lies in:
①预准备：准备浓硫酸1400g，活性炭粉末60g，高锰酸钾160g、偏二氟乙烯400g、三氟乙烯400g、甲基丙烯酸甲酯300g、醋酸乙烯180g、乙烯300g、偶氮二异丁腈引发剂2.5g、石墨粉250g、古尔胶2g；准备底部按1mm-1.5mm网格间隙均匀密排设置着孔径0.3mm-0.5mm、喷出角度与底面呈60°、喷出角度沿气孔所在圆周的切向方向顺时针分布的通气孔的圆柱形玻璃加热容器；②将偶氮二异丁腈引发剂0.7g与全部甲基丙烯酸甲酯、醋酸乙烯、石墨粉混合并搅拌均匀，获得混合物A，再将混合物A投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.8MPa，加热至55℃-60℃，以150rpm/min的搅拌速率持续搅拌，获得待反应池；①Pre-preparation: prepare 1400g of concentrated sulfuric acid, 60g of activated carbon powder, 160g of potassium permanganate, 400g of vinylidene fluoride, 400g of trifluoroethylene, 300g of methyl methacrylate, 180g of vinyl acetate, 300g of ethylene, and azobisisobutyronitrile Initiator 2.5g, graphite powder 250g, Guer gum 2g; prepare the bottom to be uniformly densely arranged with a grid gap of 1mm-1.5mm with a diameter of 0.3mm-0.5mm, the spray angle is 60° to the bottom surface, and the spray angle is along the stomata Cylindrical glass heating vessel with vent holes distributed clockwise in the tangential direction of the circumference; ② Mix 0.7g of azobisisobutyronitrile initiator with all methyl methacrylate, vinyl acetate, and graphite powder and stir evenly to obtain Mixture A, then put the mixture A into a stainless steel autoclave, evacuated and filled with nitrogen, increased the pressure to 3.8MPa, heated to 55℃-60℃, and continued stirring at a stirring rate of 150rpm/min to obtain the reaction pool ；
工业实用性Industrial applicability
（1）由于本发明表层的石墨烯自身导热效率就高，因此实测本发明仅膜层就能在原基体散热材料散热效率的基础上额外提升其120W/m·K-150W/m·K的整体散热效率（将固化有本发明膜层的散热结构整体计算）。(1) Since the graphene on the surface of the present invention has a high thermal conductivity efficiency, it is measured that only the film layer of the present invention can increase the overall heat dissipation efficiency of 120W/m·K-150W/m·K on the basis of the heat dissipation efficiency of the original matrix heat dissipation material. Heat dissipation efficiency (calculate the overall heat dissipation structure cured with the film layer of the present invention).
（2）本发明的膜层经闪光处理后，膜层表面会形成不规则的起伏结构，明显增大本发明与空气接触的比表面积，进一步提升散热效率。(2) After the film layer of the present invention is subjected to flash treatment, an irregular undulating structure will be formed on the surface of the film layer, which significantly increases the specific surface area of the present invention in contact with air, and further improves the heat dissipation efficiency.
（3）本发明的膜层经固化和闪光处理后，水接触角118°-123°，具有良好的憎水性能，能在一定程度上保持散热结构表面的洁净，提升其使用寿命和稳定性。（4）本发明采用了完全不同于现有技术的材料架构，由有一定压电性能的耐高温聚合物P(VDF-TrFE)共聚物作为基体，其内填充有部分提升整体传热性能的石墨粉、软化点80℃左右的部分聚甲基丙烯酸甲酯和较大量熔点在60℃左右的乙烯-醋酸乙烯（EVA），因此明显本发明除了利用了常规的接触传热和热对流外，还有固体液化时吸热、固体液化后对流传热以及压电材料[P(VDF-TrFE)具有较好的压电性能]带来的部分热转电功能（因此本发明还可以在散热块两侧添置导线，与机箱设计结合，用于装饰性发光二极管的供电），当然，本发明仅论及接触传热性能的话是明显低于铝制散热片的。(3) After curing and flashing treatment, the film of the present invention has a water contact angle of 118°-123°, has good hydrophobic properties, can keep the surface of the heat dissipation structure clean to a certain extent, and improve its service life and stability . (4) The present invention adopts a material structure which is completely different from the prior art. The high temperature resistant polymer P (VDF-TrFE) copolymer with certain piezoelectric properties is used as the matrix, and it is filled with a part to improve the overall heat transfer performance. Graphite powder, part of polymethyl methacrylate with a softening point of about 80°C, and a relatively large amount of ethylene-vinyl acetate (EVA) with a melting point of about 60°C. Therefore, it is obvious that the present invention uses conventional contact heat transfer and thermal convection, There are also part of the heat transfer function brought by the heat absorption when the solid is liquefied, the convection heat transfer after the solid is liquefied, and the piezoelectric material [P(VDF-TrFE) has better piezoelectric properties] (so the present invention can also be used in the heat sink Adding wires on both sides, combined with the chassis design, is used for the power supply of the decorative light-emitting diodes). Of course, the present invention only talks about the contact heat transfer performance, which is significantly lower than that of aluminum heat sinks.
（5）本发明除了少量石墨粉外，其它都有透明的有机聚合物，因此本发明是透光的，可以通过热辐射分散部分热量。(5) Except for a small amount of graphite powder, the present invention has transparent organic polymers. Therefore, the present invention is light-transmissive and can disperse part of the heat through thermal radiation.
（6）本发明通过最后的120℃-130℃热处理，一方面消除了本发明快冷时获得的内应力，使本发明结构更稳定，另一方面通过使部分填料液化去除了开口在基体P(VDF-TrFE)外面的低熔点物质（聚甲基丙烯酸甲酯、EVA）及易脱落物质石墨粉，最后，还通过这样的方式获得了复杂的气道表面的粗糙结构，极大地增加了本发明的比表面积。(6) Through the final heat treatment at 120°C-130°C, the present invention eliminates the internal stress obtained during rapid cooling of the present invention and makes the structure of the present invention more stable. On the other hand, the opening in the substrate P is removed by liquefying part of the filler. (VDF-TrFE) Low melting point substances (polymethyl methacrylate, EVA) and graphite powder, which are easy to fall off on the outside, and finally, in this way, the rough structure of the complex airway surface is obtained, which greatly increases the cost. Invented specific surface area.
（7）本发明由于是沿60°斜角喷出的气体在粘稠液体中向上自然逸散形成的复杂回旋通路，因此本发明的所有疏孔大多数都是通孔且密布在整体散热块内，这为风冷的效率带来了极大的便利。(7) The present invention is a complex swirling path formed by the gas ejected at an oblique angle of 60° and naturally escapes upward in the viscous liquid. Therefore, most of the sparse holes in the present invention are through holes and densely distributed in the integral heat sink. Internally, this brings great convenience to the efficiency of air cooling.
（8）本发明可以通过采用明火融化底部获得不可燃的液化后具有极高粘度的P(VDF-TrFE)流体（只需稍稍加热即可获得），然后可以自粘在CPU表面，中间无需设置额外的胶合剂，因此，传热效率更高、使用寿命更长、可靠性更好。因此，本发明具有表面憎水、比表面积大、散热快、多种散热方式并存、整体散热效率双重增辐的特性。(8) The present invention can obtain non-flammable P(VDF-TrFE) fluid with extremely high viscosity after being liquefied by using an open flame to melt the bottom (you only need to heat it slightly), and then it can be self-adhesive on the surface of the CPU without setting in the middle. Additional glue, therefore, higher heat transfer efficiency, longer service life, and better reliability. Therefore, the present invention has the characteristics of hydrophobic surface, large specific surface area, fast heat dissipation, coexistence of multiple heat dissipation methods, and double radiation enhancement of the overall heat dissipation efficiency.
序列表自由内容Sequence Listing Free Content
对所公开的实施例的上述说明，仅为了使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。The foregoing description of the disclosed embodiments is only to enable those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown in this document, but should conform to the widest scope consistent with the principles and novel features disclosed in this document.

Claims (2)

  1. 一种吸热传热辐射复合机制CPU散热材料的制造方法，其特征在于包括以下步骤：A method for manufacturing a heat dissipation material for a CPU with a combined mechanism of heat absorption, heat transfer and radiation, which is characterized in that it comprises the following steps:
    1）原料准备1) Raw material preparation
    ①原材料准备：按重量份准备浓硫酸135份-140份、活性炭粉末6份-8份、高锰酸钾16份-17份、偏二氟乙烯40份-50份、三氟乙烯30份-40份、甲基丙烯酸甲酯25份-30份、醋酸乙烯15份-18份、乙烯25份-30份、偶氮二异丁腈引发剂0.15份-0.25份、石墨粉20份-25份、古尔胶0.1份-0.2份；① Preparation of raw materials: Prepare 135-140 parts of concentrated sulfuric acid, 6-8 parts of activated carbon powder, 16 parts of potassium permanganate, 16 parts of -17 parts of potassium permanganate, 40-50 parts of vinylidene fluoride, and 30 parts of trifluoroethylene according to parts by weight. 40 parts, methyl methacrylate 25-30 parts, vinyl acetate 15-18 parts, ethylene 25-30 parts, azobisisobutyronitrile initiator 0.15-0.25 parts, graphite powder 20-25 parts , 0.1 part -0.2 part of Guer Gum;
    ②工装准备：准备底部按1mm-1.5mm网格间隙均匀密排设置着孔径0.3mm-0.5mm、喷出角度与底面呈60°、喷出角度沿气孔所在圆周的切向方向顺时针分布的通气孔的圆柱形玻璃加热容器；②Tooling preparation: prepare the bottom to be uniformly densely arranged with a hole diameter of 0.3mm-0.5mm according to a grid gap of 1mm-1.5mm, the ejection angle is 60° to the bottom surface, and the ejection angle is distributed clockwise along the tangential direction of the circumference of the air hole. Cylindrical glass heating vessel with vent;
    2）液体本体聚合反应2) Liquid bulk polymerization
    ①将阶段1）步骤①准备的偶氮二异丁腈引发剂0.05份-0.07份与全部甲基丙烯酸甲酯、醋酸乙烯、石墨粉混合并搅拌均匀，获得混合物A；① Combine 0.05 part-0.07 parts of the azobisisobutyronitrile initiator prepared in step 1) with all methyl methacrylate, vinyl acetate, and graphite powder and mix them evenly to obtain mixture A;
    ②将步骤①获得的混合物A投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.5MPa-3.8MPa，加热至55℃-60℃，以120rpm/min-150rpm/min的搅拌速率持续搅拌，获得待反应池；② Put the mixture A obtained in step ① into a stainless steel autoclave, evacuated and filled with nitrogen, increase the pressure to 3.5MPa-3.8MPa, heat to 55℃-60℃, and stir at 120rpm/min-150rpm/min Stir continuously at a rate to obtain the pool to be reacted;
    ③将阶段1）步骤①准备的乙烯持续缓慢通入步骤②获得的待反应池中，待全部通入后继续保温、保压5min-8min，然后卸压至2.4MPa-2.5MPa，炉冷至室温后完全卸压出炉，获得组份A；③Slowly pass the ethylene prepared in step 1) step ① into the waiting reaction tank obtained in step ②. After all the ethylene is passed through, continue to keep heat and keep the pressure for 5min-8min, then release the pressure to 2.4MPa-2.5MPa, and cool the furnace to After the room temperature, the pressure is completely relieved, and the component A is obtained;
    3）气体悬浮聚合3) Gas suspension polymerization
    ①准备足量去离子水，将阶段1）步骤①准备的古尔胶、剩余的偶氮二异丁腈引发剂与去离子水搅拌均匀后获得反应介质；①Prepare a sufficient amount of deionized water, mix the Guer gum prepared in step ① of stage 1), the remaining azobisisobutyronitrile initiator and deionized water to obtain a reaction medium;
    ②将步骤①获得的反应介质投入到不锈钢高压反应釜中，抽真空后填入氮气，升压至3.5MPa-3.8MPa，加热至55℃-60℃，以120rpm/min-150rpm/min的搅拌速率持续搅拌，获得待用溶液；② Put the reaction medium obtained in step ① into a stainless steel autoclave, evacuate and fill with nitrogen, increase the pressure to 3.5MPa-3.8MPa, heat to 55℃-60℃, stir at 120rpm/min-150rpm/min Stir continuously at a rate to obtain a solution to be used;
    ③将阶段1）步骤①准备的偏二氟乙烯、三氟乙烯持续缓慢均匀地通入待用溶液中，至通入完毕后继续保温、保压5min-8min，然后卸压至2.4MPa-2.5MPa，炉冷至室温后完全卸压出炉，蒸除水份，获得组份B；③Pour the vinylidene fluoride and trifluoroethylene prepared in step 1) into the solution to be used slowly and uniformly. After the feeding is completed, continue to keep the temperature and keep the pressure for 5min-8min, and then release the pressure to 2.4MPa-2.5 MPa, after the furnace is cooled to room temperature, the pressure is completely relieved from the furnace, and the water is evaporated to obtain component B;
    4）散热材料成型4) Molding of heat dissipation material
    ①将阶段2）步骤③获得的组份A机械切割成粒径1mm-2mm的颗粒，获得颗粒A；① Mechanically cut the component A obtained in step 2) in step ③ into particles with a particle size of 1mm-2mm to obtain particles A;
    ②将阶段3）步骤③获得的组份B放入阶段1）步骤②准备的圆柱形玻璃加热容器中，加热至完全熔化，获得熔池B；②Put the component B obtained in stage 3) in step ③ into the cylindrical glass heating vessel prepared in stage 1) in step ②, and heat it until it is completely melted to obtain molten pool B;
    ③将步骤①获得的颗粒A投入步骤②的熔池B中，充分搅拌均匀后，停止加热，并开启圆柱形玻璃加热容器底部的喷气孔，以3MPa-4MPa的压力持续喷出氮气，直至熔池完全冷却，获得粗制散热材料块；③Put the particles A obtained in step ① into the molten pool B of step ②, and after fully stirring, stop heating, and open the air jet hole at the bottom of the cylindrical glass heating vessel, and continuously spray nitrogen at a pressure of 3MPa-4MPa until it melts. The pool is completely cooled to obtain a block of crude heat dissipation material;
    ④将步骤③获得的粗制散热材料块机械加工成底部与CPU上表面相适应，顶部与散热风扇相适应的形状，获得预制复合散热材料；④ Machining the rough heat-dissipating material block obtained in step ③ into a shape with the bottom part compatible with the upper surface of the CPU and the top part compatible with the cooling fan to obtain a prefabricated composite heat-dissipating material;
    ⑤将步骤④获得的预制复合散热材料加热至120℃-130℃，然后采用足量乙醇漂洗加热后的散热材料表面，蒸离附着的乙醇，获得待处理复合散热材料；⑤ Heat the prefabricated composite heat dissipation material obtained in step ④ to 120°C-130°C, and then rinse the surface of the heated heat dissipation material with a sufficient amount of ethanol to evaporate the attached ethanol to obtain the composite heat dissipation material to be processed;
    5）表面改性分散液制备5) Preparation of surface modification dispersion
    ①装备冰水混合物组成的冰浴池；① Equipped with an ice bath composed of a mixture of ice and water;
    ②将阶段1）步骤①准备的浓硫酸、活性炭粉末与去离子水800份-900份混合均匀后装入玻璃容器，然后将容器浸入步骤①准备的冰浴池内，保持容器内外溶液隔离，以30rpm/min-35rpm/min的搅拌速率机械搅拌2.5h-3h，然后将阶段1）步骤①准备的高锰酸钾以自身总重量计5%/min的添加速率缓慢均匀地投入容器中，继续以15rpm/min-20rpm/min的搅拌速率持续搅拌90min-100min，获得低温反应溶液；②Mix 800-900 parts of concentrated sulfuric acid, activated carbon powder and deionized water prepared in step 1) in step ①, and then put them into a glass container, and then immerse the container in the ice bath prepared in step ① to keep the solution inside and outside the container separate. The stirring rate of 30rpm/min-35rpm/min is mechanically stirred for 2.5h-3h, and then the potassium permanganate prepared in step 1) step ① is slowly and evenly put into the container at the addition rate of 5%/min based on its total weight, and continue Stir continuously at a stirring rate of 15rpm/min-20rpm/min for 90min-100min to obtain a low-temperature reaction solution;
    ③将盛装低温反应溶液的玻璃容器浸入水温恒定在36℃-38℃之间的温水浴池中，保持容器内外溶液隔离，以120rpm/min-150rpm/min的搅拌速率搅拌，持续80min-90min，获得中温反应溶液；③ Immerse the glass container containing the low-temperature reaction solution in a warm water bath with a constant water temperature of 36℃-38℃, keep the solution inside and outside the container separate, and stir at a stirring rate of 120rpm/min-150rpm/min for 80min-90min to obtain Medium temperature reaction solution;
    ④将盛装中温反应溶液的玻璃容器浸入水温恒定在95℃-97℃之间的高温浴池中，保持容器内外溶液隔离，将重量份250份-300份的去离子水按自身总重量计5%/min的添加速率缓慢均匀地注入容器中，然后静置反应45min-50min，获得高温反应溶液；⑤在盛装高温反应溶液的玻璃容器中再次注入重量份450份-500份的去离子水，离心洗涤直至反应产物C的PH值6.5-7.5，获得产物分散液；④ Immerse the glass container containing the medium-temperature reaction solution in a high-temperature bath with a constant water temperature of 95℃-97℃, keep the solution inside and outside the container isolated, and divide 250-300 parts by weight of deionized water based on 5% of its total weight. Slowly and uniformly inject into the container at an addition rate of 1/min, and then let stand for 45min-50min to obtain a high-temperature reaction solution; ⑤Inject 450-500 parts by weight of deionized water again into the glass container containing the high-temperature reaction solution, and centrifuge Wash until the PH value of the reaction product C is 6.5-7.5 to obtain a product dispersion;
    6）散热器制备6) Radiator preparation
    ①将阶段5）步骤⑤获得的产物分散液盛装在喷口直径0.2mm-0.5mm的喷雾容器中，获得分散液喷雾器；① Put the product dispersion obtained in step 5) in step ⑤ in a spray container with a nozzle diameter of 0.2mm-0.5mm to obtain a dispersion sprayer;
    ②将分散液喷雾器均匀、完整覆盖地喷润在阶段4）步骤⑤获得的待处理复合散热材料的外表面，待自然干燥后采用照强度为GN/M=30-35、照射时间1ms的闪光对干燥后的分散液进行处理，即获得经所需吸热传热辐射复合机制CPU散热材料。②Spray the dispersion sprayer uniformly and completely cover the outer surface of the composite heat dissipation material to be processed in step 4) Step ⑤, after natural drying, use a flash with an intensity of GN/M=30-35 and an irradiation time of 1ms The dried dispersion is processed to obtain the CPU heat dissipation material through the required heat absorption, heat transfer and radiation compound mechanism.
  2. 一种吸热传热辐射复合机制CPU散热材料，其特征在于：该散热材料由三部分组成：基体部分是按重量份计内部有蜂窝状多路通孔的P(VDF-TrFE)共聚物55份-80份，填料部分为固化在基体部分内部的包括聚甲基丙烯酸甲酯15份-20份、乙烯-醋酸乙烯25份-35份和石墨粉15份-25份三种组份的共混物；外表面还附着有石墨烯膜层，该膜层的水接触角118°-123°，热导率4800W/m·K-5300W/m·K。A heat-absorbing heat-radiation composite mechanism CPU heat dissipation material, which is characterized in that: the heat dissipation material consists of three parts: the base part is P(VDF-TrFE) copolymer 55 with honeycomb multi-channel through holes in the part by weight. Parts-80 parts, the filler part is a total of three components, including 15-20 parts of polymethyl methacrylate, 25-35 parts of ethylene-vinyl acetate, and 15-25 parts of graphite powder, which are cured inside the matrix part. Mixture: Graphene film is also attached to the outer surface, the water contact angle of the film is 118°-123°, and the thermal conductivity is 4800W/m·K-5300W/m·K.
     To
PCT/CN2019/114404 2019-10-29 2019-10-30 Manufacturing method for cpu heat dissipation material having heat-absorbing, heat-transferring and radiative complex mechanism WO2021081820A1 (en)

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