CN106311581A - Manufacturing method for efficient composite heat sink for electronic product - Google Patents

Manufacturing method for efficient composite heat sink for electronic product Download PDF

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Publication number
CN106311581A
CN106311581A CN201610690050.6A CN201610690050A CN106311581A CN 106311581 A CN106311581 A CN 106311581A CN 201610690050 A CN201610690050 A CN 201610690050A CN 106311581 A CN106311581 A CN 106311581A
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graphene
weight
nitrogen
solid phase
parts
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Chinese (zh)
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不公告发明人
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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Priority to CN201610690050.6A priority Critical patent/CN106311581A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2202/00—Metallic substrate
    • B05D2202/40—Metallic substrate based on other transition elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2252/00—Sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2602/00—Organic fillers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

The invention discloses a manufacturing method for an efficient composite heat sink for an electronic product. The manufacturing method comprises the steps that graphene is peeled off through stripping liquid, in cooperation with grinding or stirring, the requirement for the grinding or stirring speed can be lowered, the graphene can be peeled off without cutting a graphite flake at a high speed, the structural integrality among carbon in the graphene can be increased easily and effectively through nitrogen doping, a used organic or inorganic solid-phase nitrogen source has the beneficial effects of being low in cost and easy to obtain, and the manufacturing cost can be reduced effectively.

Description

A kind of preparation method of electronic product high efficiency composition fin
Technical field
The present invention relates to electronic product radiating field, be specifically related to the preparation side of a kind of electronic product high efficiency composition fin Method.
Background technology
For electronic product, its all parts effectively dispels the heat and obtains relatively low operating temperature and be used for the life-span Extremely important impact can be produced with the speed of service.Development and progress, particularly computer chip multinuclear along with science and technology Changing and have become as main flow, and the speed of service is constantly accelerated, power also increases, and effective heat radiation plays act to its speed of service The effect of foot weight.At present, the heat radiation main product on market is graphite-like heat conducting film, but, its heat dispersion meets far away The not radiating requirements of electronics and IT products radiating elements, becomes the heat radiation bottleneck of most electronic product.
Graphene (Graphene) be a kind of by carbon atom with sp2Hybrid orbital composition hexangle type is honeycomb lattice The monolayer flat film that (honeycomb crystal lattice) is arranged to make up, the two-dimentional material of only one of which carbon atom thickness Material.It is the hardest nano material also that Graphene is currently the thinnest, and it is almost fully transparent, only absorbs 2.3% Light；Heat conductivity is up to 5300W/m K, and higher than CNT and diamond, under room temperature, its electron mobility exceedes 15000cm2/ (V s), again ratio CNT or silicon wafer height, and resistivity about 10-6Ω cm, lower than copper or silver, for The material that resistivity is minimum in the world.Graphene has the most excellent physical and chemical performance, has been gradually available for transparent conductive film, Nano electron device (transistor, transistor circuit interconnection memory semiconductor), conductive ink, solaode, lithium battery, super The fields such as capacitor, sensor and biological medicine.
Currently, the method that prepared by Graphene mainly has: chemically grown method and physics stripping method.Low compared to efficiency, uncomfortable Together in the chemically grown method of industrialized mass production, physics stripping method mainly uses cheap graphite to be raw material, by stone Smoky quartz body applies mechanical force makes graphite layers peeling-off, breaks the Van der Waals force of graphite layers, forms monolithic graphite alkene or widow Layer graphene, this physical separation methods has more industrial prospect and applicable large-scale production.
Summary of the invention
The present invention provides the preparation method of a kind of electronic product high efficiency composition fin, and the method uses stripper to peel off stone Ink alkene, coordinates and grinds or stirring, it is possible to decrease to grinding or the requirement of mixing speed, it is not necessary to graphite flake layer ultra high shear Realize stripping to Graphene, can simply and effectively improve in Graphene the structural intergrity between carbon and carbon by N doping, and The organic or inorganic solid phase nitrogen source used has low cost and the advantage easily obtained, and can effectively reduce manufacturing cost.
To achieve these goals, the invention provides the preparation method of a kind of electronic product high efficiency composition fin, should Method comprises the steps:
(1) stripping method is used to prepare Graphene
By purity more than 99%, in particle diameter is 100 ~ 300 μm graphite flakes and the stripper injection kettle with agitator, open The motor of dynamic kettle is stirred, and makes material mix homogeneously, wherein the consisting of of stripper: ethylene glycol 90 parts by weight, poly-third Olefin(e) acid ester 40 parts by weight, silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere 1 parts by weight, Lithium chloride 1 parts by weight.Wherein, the particle diameter of silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere Below 50 microns, the particle diameter of silica core is more than 20 nanometers, and the thickness of shell is more than 10 nanometers；Polyacrylate Number-average molecular weight is more than 100000, and the weight ratio of graphite flakes and stripper is 1:3；
Heating kettle, keeping still body temperature is 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, during reaction Between 3h；By discharging opening, upper strata suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above；Will Graphene suspension in the storage tank obtained is delivered in centrifuge, and centrifuge speed is 1500 rpm/min, centrifugation time 1h, takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake, is washed with appropriate distillation by the filter cake obtained Wash, filter cake more than lyophilization 4h in freeze drying plant, i.e. obtain graphene powder；
(2) nitrogen-doped graphene
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from C6H12N4、 C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2And C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:2 to 1:10；By described mixed Compound is sintered at a temperature of 500 DEG C to 700 DEG C, and the time of sintering is 4～7 hours, obtains nitrogen-doped graphene；
(3) Graphene fin is prepared
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mix, will This slurry mix is coated at least one surface of metal base, to form composite；This composite is inserted high temperature Baking oven is dried formation fin.
Preferably, in described step (3), this high polymer binder is carboxymethyl cellulose (CMC), in slurry mix Nitrogen-doped graphene content be 65-86wt%, this metal base is native silver.
It is an advantage of the current invention that the method uses stripper to peel off Graphene, coordinate and grind or stirring, it is possible to decrease to grinding Mill or the requirement of mixing speed, it is not necessary to graphite flake layer ultra high shear can be realized the stripping to Graphene, pass through N doping Can simply and effectively improve the structural intergrity between carbon and carbon in Graphene, and the organic or inorganic solid phase nitrogen source used has Low cost and the advantage easily obtained, can effectively reduce manufacturing cost.
Detailed description of the invention
Embodiment one
By purity more than 99%, in particle diameter is 100 ~ 300 μm graphite flakes and the stripper injection kettle with agitator, open The motor of dynamic kettle is stirred, and makes material mix homogeneously, wherein the consisting of of stripper: ethylene glycol 90 parts by weight, poly-third Olefin(e) acid ester 40 parts by weight, silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere 1 parts by weight, Lithium chloride 1 parts by weight.Wherein, the particle diameter of silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere Below 50 microns, the particle diameter of silica core is more than 20 nanometers, and the thickness of shell is more than 10 nanometers；Polyacrylate Number-average molecular weight is more than 100000, and the weight ratio of graphite flakes and stripper is 1:3.
Heating kettle, keeping still body temperature is 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, instead 3h between Ying Shi；By discharging opening, upper strata suspension is expelled in storage tank after stopped reaction, stands 24h primiparity derived above Product；Graphene suspension in the storage tank that will obtain is delivered in centrifuge, and centrifuge speed is 1500 rpm/min, centrifugal Time 1h, takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake, by the filter cake that obtains with appropriate distilled water Washing, filter cake more than lyophilization 4h in freeze drying plant, i.e. obtain graphene powder.
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from C6H12N4、C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2 And C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:2；By described mixture Being sintered at a temperature of 500 DEG C, the time of sintering is 4 hours, obtains nitrogen-doped graphene.
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mixing Thing, coats this slurry mix at least one surface of metal base, to form composite；This composite is inserted High temperature oven is dried formation fin.This high polymer binder is carboxymethyl cellulose (CMC), the nitrogen in slurry mix Doped graphene content is 65wt%, and this metal base is native silver.
Embodiment two
By purity more than 99%, in particle diameter is 100 ~ 300 μm graphite flakes and the stripper injection kettle with agitator, open The motor of dynamic kettle is stirred, and makes material mix homogeneously, wherein the consisting of of stripper: ethylene glycol 90 parts by weight, poly-third Olefin(e) acid ester 40 parts by weight, silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere 1 parts by weight, Lithium chloride 1 parts by weight.Wherein, the particle diameter of silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere Below 50 microns, the particle diameter of silica core is more than 20 nanometers, and the thickness of shell is more than 10 nanometers；Polyacrylate Number-average molecular weight is more than 100000, and the weight ratio of graphite flakes and stripper is 1:3.
Heating kettle, keeping still body temperature is 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, instead 3h between Ying Shi；By discharging opening, upper strata suspension is expelled in storage tank after stopped reaction, stands 24h primiparity derived above Product；Graphene suspension in the storage tank that will obtain is delivered in centrifuge, and centrifuge speed is 1500 rpm/min, centrifugal Time 1h, takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake, by the filter cake that obtains with appropriate distilled water Washing, filter cake more than lyophilization 4h in freeze drying plant, i.e. obtain graphene powder.
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from C6H12N4、C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2 And C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:10；By described mixture Being sintered at a temperature of 700 DEG C, the time of sintering is 7 hours, obtains nitrogen-doped graphene.
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mixing Thing, coats this slurry mix at least one surface of metal base, to form composite；This composite is inserted High temperature oven is dried formation fin.This high polymer binder is carboxymethyl cellulose (CMC), the nitrogen in slurry mix Doped graphene content is 86wt%, and this metal base is native silver.

Claims (2)

1. a preparation method for electronic product high efficiency composition fin, the method comprises the steps:
(1) stripping method is used to prepare Graphene
By purity more than 99%, in particle diameter is 100 ~ 300 μm graphite flakes and the stripper injection kettle with agitator, open The motor of dynamic kettle is stirred, and makes material mix homogeneously, wherein the consisting of of stripper: ethylene glycol 90 parts by weight, poly-third Olefin(e) acid ester 40 parts by weight, silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere 1 parts by weight, Lithium chloride 1 parts by weight,
Wherein, the particle diameter of silicon dioxide/poly-(methyl methacrylate～styrene) bivalve layer complex microsphere below 50 microns, The particle diameter of silica core is more than 20 nanometers, and the thickness of shell is more than 10 nanometers；The number-average molecular weight of polyacrylate is big In 100000, the weight ratio of graphite flakes and stripper is 1:3；
Heating kettle, keeping still body temperature is 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, during reaction Between 3h；By discharging opening, upper strata suspension is expelled in storage tank after stopped reaction, stands 24h head product derived above；Will Graphene suspension in the storage tank obtained is delivered in centrifuge, and centrifuge speed is 1500 rpm/min, centrifugation time 1h, takes the supernatant, and in vacuum apparatus, vacuum is filtrated to get filter cake, is washed with appropriate distillation by the filter cake obtained Wash, filter cake more than lyophilization 4h in freeze drying plant, i.e. obtain graphene powder；
(2) nitrogen-doped graphene
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from C6H12N4、 C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2And C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:2 to 1:10；By described mixed Compound is sintered at a temperature of 500 DEG C to 700 DEG C, and the time of sintering is 4～7 hours, obtains nitrogen-doped graphene；
(3) Graphene fin is prepared
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mix, will This slurry mix is coated at least one surface of metal base, to form composite；This composite is inserted high temperature Baking oven is dried formation fin.
2. the method for claim 1, it is characterised in that in described step (3), this high polymer binder is carboxymethyl Cellulose (CMC), the nitrogen-doped graphene content in slurry mix is 65-86wt%, and this metal base is native silver.
CN201610690050.6A 2016-08-19 2016-08-19 Manufacturing method for efficient composite heat sink for electronic product Pending CN106311581A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106636726A (en) * 2017-01-12 2017-05-10 苏州思创源博电子科技有限公司 Composite copper conducting material manufacturing method
CN106676304A (en) * 2017-01-12 2017-05-17 苏州思创源博电子科技有限公司 Preparation method of graphene titanium-based composite material
CN106756175A (en) * 2017-01-26 2017-05-31 苏州思创源博电子科技有限公司 A kind of preparation method of Graphene Al-alloy
CN111548516A (en) * 2020-04-21 2020-08-18 苏州锦富技术股份有限公司 Nitrogen-doped graphene copper composite heat dissipation film and preparation method thereof

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CN103626158A (en) * 2012-08-23 2014-03-12 中国科学院宁波材料技术与工程研究所 Preparation method of nitrogen doped graphene and application of nitrogen doped graphene
CN104710912A (en) * 2015-03-31 2015-06-17 东莞市闻誉实业有限公司 Cooling fin
CN105482665A (en) * 2015-12-31 2016-04-13 普罗旺斯科技（深圳）有限公司 Graphene coating, graphene cooling fin and preparation methods of graphene coating and graphene cooling fin
CN105712326A (en) * 2014-12-01 2016-06-29 江阴碳谷科技有限公司 Method for producing graphene
CN105762123A (en) * 2016-02-03 2016-07-13 厦门大学 RGO (Reduced Graphene Oxide) polymer radiating fin
CN105776185A (en) * 2014-12-25 2016-07-20 江南石墨烯研究院 Preparation method of graphene paper with high thermal conductivity and electrical conductivity

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103626158A (en) * 2012-08-23 2014-03-12 中国科学院宁波材料技术与工程研究所 Preparation method of nitrogen doped graphene and application of nitrogen doped graphene
CN105712326A (en) * 2014-12-01 2016-06-29 江阴碳谷科技有限公司 Method for producing graphene
CN105776185A (en) * 2014-12-25 2016-07-20 江南石墨烯研究院 Preparation method of graphene paper with high thermal conductivity and electrical conductivity
CN104710912A (en) * 2015-03-31 2015-06-17 东莞市闻誉实业有限公司 Cooling fin
CN105482665A (en) * 2015-12-31 2016-04-13 普罗旺斯科技（深圳）有限公司 Graphene coating, graphene cooling fin and preparation methods of graphene coating and graphene cooling fin
CN105762123A (en) * 2016-02-03 2016-07-13 厦门大学 RGO (Reduced Graphene Oxide) polymer radiating fin

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106636726A (en) * 2017-01-12 2017-05-10 苏州思创源博电子科技有限公司 Composite copper conducting material manufacturing method
CN106676304A (en) * 2017-01-12 2017-05-17 苏州思创源博电子科技有限公司 Preparation method of graphene titanium-based composite material
CN106756175A (en) * 2017-01-26 2017-05-31 苏州思创源博电子科技有限公司 A kind of preparation method of Graphene Al-alloy
CN111548516A (en) * 2020-04-21 2020-08-18 苏州锦富技术股份有限公司 Nitrogen-doped graphene copper composite heat dissipation film and preparation method thereof
CN111548516B (en) * 2020-04-21 2022-10-21 苏州锦富技术股份有限公司 Nitrogen-doped graphene copper composite heat dissipation film and preparation method thereof

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Application publication date: 20170111