CN107892295A - A kind of preparation method of heat conducting film and a kind of heat conducting film - Google Patents

A kind of preparation method of heat conducting film and a kind of heat conducting film Download PDF

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Publication number
CN107892295A
CN107892295A CN201710919019.XA CN201710919019A CN107892295A CN 107892295 A CN107892295 A CN 107892295A CN 201710919019 A CN201710919019 A CN 201710919019A CN 107892295 A CN107892295 A CN 107892295A
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China
Prior art keywords
conducting film
heat conducting
graphene
total amount
slurry
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CN201710919019.XA
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Chinese (zh)
Inventor
陈小刚
麻宁
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Zhuhai Carbon Carbon Composite Material Co Ltd
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Zhuhai Carbon Carbon Composite Material Co Ltd
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Priority to CN201710919019.XA priority Critical patent/CN107892295A/en
Publication of CN107892295A publication Critical patent/CN107892295A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular

Abstract

The invention discloses a kind of preparation method of heat conducting film, it comprises the following steps:S1, take out graphene slurry;S2, dispersant is added in graphene slurry, and stirred;S3, binding agent is added, and be sufficiently mixed uniformly;S4, stop stirring after adding thickener regulation viscosity, that is, graphene heat conduction slurry is made;S5, graphene heat conduction slurry is coated, drying sample is rolled;Sample after S6, rolling carries out high temperature carbonization;Sample after S7, charing carries out high temperature graphitization, that is, graphene heat conducting film is made.A kind of heat conducting film includes:Graphene slurry accounts for material total amount 95.5% 99.7%, and dispersant is 0.1% the 2.0% of material total amount, and binding agent is 0.1% the 2.0% of material total amount, and thickener is 0.1% the 0.5% of material total amount.The present invention has technique simple, is easily made, and efficiency high is made, and properties of product are stable, and cost is low, the advantages of steady quality and product good heat dissipation effect.

Description

A kind of preparation method of heat conducting film and a kind of heat conducting film
Technical field
The present invention relates to a kind of preparation method of heat conducting film and a kind of heat conducting film.
Background technology
With the development of science and technology, various equipment are to radiate position or the position that need to radiate of heater members, such as CPU, LED Tool, battery, electrical equipment, radiator, engine outer wall, electric wire, rack, heat distribution pipeline, weaving, tank body, industrial equipment surface, The cooling requirements more and more higher of building, water tank, the vehicles etc..Existing leading using pi as graphite film made from raw material Although hot coefficient can reach 1500W/ (m K), its preparation process is needed by repeatedly up to 3000 DEG C of prolonged graphite Change process and also need to be made by multiple high pressure roll-in, energy consumption is big and complex process.Can be used for this problem should Graphene heat conduction slurry directly prepares heat conducting film, can reduce the cost, and can increase processing efficiency.Graphene heat conducting film can cover In that the radiating mode of heater members can be changed into face radiating from a radiating on heater members, so as to increase its area of dissipation and radiating Speed, reach the effect for the operating temperature for reducing pyrotoxin.
The content of the invention
The technical problems to be solved by the invention are overcome the deficiencies in the prior art, there is provided a kind of preparation method of heat conducting film And a kind of heat conducting film, it has, and technique is simple, is easily made, and efficiency high is made, properties of product are stable, and cost is low, steady quality And the advantages of product good heat dissipation effect.
The technical solution adopted in the present invention is:
A kind of preparation method of heat conducting film, it comprises the following steps:
S1, take out graphene slurry;
S2, dispersant is added in graphene slurry, and stirred;
S3, binding agent is added, and be sufficiently mixed uniformly;
S4, stop stirring after adding thickener regulation viscosity, that is, graphene heat conduction slurry is made;
S5, graphene heat conduction slurry is coated, drying sample is rolled;
Sample after S6, rolling carries out high temperature carbonization;
Sample after S7, charing carries out high temperature graphitization, that is, graphene heat conducting film is made.
Further, in the step S1, graphene slurry is placed into a machine mixer;In the step S2, machine The range of speeds of tool mixer is between 1500r/min-2500r/min, and mixing time scope is between 20min-40min.
Further, in the step S2, the rotating speed of machine mixer is 2000r/min, and mixing time is 30min.
Further, in the step S3, the range of speeds of machine mixer between 1500r/min-2500r/min, and Mixing time scope is between 20min-40min.
Further, the range of speeds of machine mixer is between 2000r/min in the step S1, and mixing time scope Between 30min;In the step S3, the range of speeds of machine mixer is between 2000r/min, and mixing time scope exists Between 30min;In the step S5, it is dried at 50-90 DEG C, the thickness after rolling is 20 μm.
Further, carbonization temperature scope is between 750 DEG C -850 DEG C in the step S6, and carbonization time scope is in 0.8h- Between 1.2h.
Further, carbonization temperature is 800 DEG C in the step S6, carbonization time 1h.
In a kind of preparation method of heat conducting film, the solid content of graphene slurry accounts for material total amount 95.5%- for 2%-10% 99.7%, dispersant is the 0.1%-2.0% of material total amount, and binding agent is the 0.1%-2.0% of material total amount, and thickener is that material is total The 0.1%-0.5% of amount.
A kind of heat conducting film includes:Graphene slurry accounts for material total amount 95.5%-99.7%, and dispersant is material total amount 0.1%-2.0%, binding agent are the 0.1%-2.0% of material total amount, and thickener is the 0.1%-0.5% of material total amount.
The solid content of graphene slurry is 2%-10%.
The dispersant is the copolymerization liquid solution with acidic group, and the copolymerization liquid solution with acidic group is modified poly- Urethane or polyvinylpyrrolidone;The binding agent is butadiene-styrene rubber or acrylic ester polymerization emulsion;Thickener:It is fine for carboxymethyl Plain sodium is tieed up, is either Sodium Polyacrylate or is sodium alginate.
The features of the present invention:
1st, offer is a kind of forms graphene heat conduction slurry by graphene and evenly spreading in water for different activities material composition, And the method for thus preparing graphene heat conducting film.、
2nd, prepared heat conduction slurry is directly mixed with active material, and the heat conduction of stable and uniform is formed in obtained heat conducting film Network.
3rd, the active material in heat conduction slurry is binding agent, dispersant and thickener composition.
4th, film layer made from the graphene heat conduction slurry can make film body after 800 DEG C carbonize 1h using 2400 DEG C of graphitization 1h Heat conducting film be 1000 W/ (m K).
The present invention has technique simple, is easily made, and efficiency high is made, and properties of product are stable, and cost is low, steady quality and The advantages of product good heat dissipation effect.
Embodiment
A kind of preparation method of heat conducting film of the present invention, it comprises the following steps:
S1, take out graphene slurry;
S2, dispersant is added in graphene slurry, and stirred;
S3, binding agent is added, and be sufficiently mixed uniformly;
S4, stop stirring after adding thickener regulation viscosity, that is, graphene heat conduction slurry is made;
S5, graphene heat conduction slurry is coated, drying sample is rolled;
Sample after S6, rolling carries out high temperature carbonization;
Sample after S7, charing carries out high temperature graphitization, that is, graphene heat conducting film is made.
Further, in the step S1, graphene slurry is placed into a machine mixer;In the step S2, machine The range of speeds of tool mixer is between 1500r/min-2500r/min, and mixing time scope is between 20min-40min.
Further, in the step S2, the rotating speed of machine mixer is 2000r/min, and mixing time is 30min.
Further, in the step S3, the range of speeds of machine mixer between 1500r/min-2500r/min, and Mixing time scope is between 20min-40min.
Further, the range of speeds of machine mixer is between 2000r/min in the step S1, and mixing time scope Between 30min;In the step S3, the range of speeds of machine mixer is between 2000r/min, and mixing time scope exists Between 30min;In the step S5, it is dried at 50-90 DEG C, the thickness after rolling is 20 μm.
Further, carbonization temperature scope is between 750 DEG C -850 DEG C in the step S6, and carbonization time scope is in 0.8h- Between 1.2h.
Further, carbonization temperature is 800 DEG C in the step S6, carbonization time 1h.
In a kind of preparation method of heat conducting film, the solid content of graphene slurry accounts for material total amount 95.5%- for 2%-10% 99.7%, dispersant is the 0.1%-2.0% of material total amount, and binding agent is the 0.1%-2.0% of material total amount, and thickener is that material is total The 0.1%-0.5% of amount.
A kind of heat conducting film includes:Graphene slurry accounts for material total amount 95.5%-99.7%, and dispersant is material total amount 0.1%-2.0%, binding agent are the 0.1%-2.0% of material total amount, and thickener is the 0.1%-0.5% of material total amount.
The solid content of graphene slurry is 2%-10%.
The features of the present invention:
5th, offer is a kind of forms graphene heat conduction slurry by graphene and evenly spreading in water for different activities material composition, And the method for thus preparing graphene heat conducting film.、
6th, prepared heat conduction slurry is directly mixed with active material, and the heat conduction of stable and uniform is formed in obtained heat conducting film Network.
7th, the active material in heat conduction slurry is binding agent, dispersant and thickener composition.
8th, film layer made from the graphene heat conduction slurry can make film body after 800 DEG C carbonize 1h using 2400 DEG C of graphitization 1h Heat conducting film be 1000 W/ (m K).
Embodiment one:
Dispersant is added in graphene slurry, then sample is stirred using 2000r/min machine mixer 30min;
Binding agent is added, the machine mixer for reusing 2000r/min is stirred 30min to sample;
Thickener is repeatedly added using a small amount of under 2000r/min mixing speed, regulation stops stirring after arriving suitable viscosity, i.e., Graphene heat conduction slurry is made;
Graphene heat conduction slurry is coated, film layer is dried at 50 ~ 90 DEG C, and temperature is higher, and required time is shorter, applies Thickness has good effect at 20 μm after layer is dried;
Film layer obtains graphene heat conducting film after 800 DEG C carbonize 1h using 2400 DEG C of graphitization 1h.
Sample test is carried out to graphene heat conducting film.
Performance test:
Graphene heat conducting film prepared by embodiment 1 to 6 and comparative example is subjected to performance test.
Test event and method:
Resistivity:With reference to GB/T 1551-2009《Single crystal silicon resistivity assay method》;
Sheet resistance:With reference to GB/T 1552-1995《Silicon, germanium single crystal determination of resistivity DC four point probe method》;
Test result:As shown in table 2.
Thermal conductivity(W/m·K) Tensile strength (MPa) Remarks
Embodiment 1 1004 300
Embodiment 2 998 298
Embodiment 3 956 288
Embodiment 4 930 276
Embodiment 5 922 275
Embodiment 6 908 271
Compared by the graphene heat conducting film prepared by it can be seen from data in table 2 according to embodiments of the present invention 1 to 6, in graphene The capacity of heat transmission and intensity effect for increasing additivated dosage in the case that slurry addition is constant for heat conducting film are smaller.This is matched somebody with somebody Graphene heat conducting film is advantageous to the electronic component of thermal component and the radiating effect of household electrical appliance made from side.
Certainly, above is the preferred embodiment of the present invention.It should be pointed out that for those skilled in the art For, on the premise of its general principles are not departed from, some improvements and modifications can also be made, these improvements and modifications It is considered as protection scope of the present invention.
Above example the formula that may be simply used according to the different market demands, obtains difference without point of quality Performance.
The present invention has technique simple, is easily made, and efficiency high is made, and properties of product are stable, and cost is low, steady quality and The advantages of product good heat dissipation effect.

Claims (10)

1. a kind of preparation method of heat conducting film, it is characterised in that comprise the following steps:
S1, take out graphene slurry;
S2, dispersant is added in graphene slurry, and stirred;
S3, binding agent is added, and be sufficiently mixed uniformly;
S4, stop stirring after adding thickener regulation viscosity, that is, graphene heat conduction slurry is made;
S5, graphene heat conduction slurry is coated, drying sample is rolled;
Sample after S6, rolling carries out high temperature carbonization;
Sample after S7, charing carries out high temperature graphitization, that is, graphene heat conducting film is made.
A kind of 2. preparation method of heat conducting film according to claim 1, it is characterised in that:In the step S1, by graphite Alkene slurry is placed into a machine mixer;In the step S2, the range of speeds of machine mixer is in 1500r/min- Between 2500r/min, and mixing time scope is between 20min-40min.
A kind of 3. preparation method of heat conducting film according to claim 2, it is characterised in that:In the step S2, machinery stirs The rotating speed for mixing machine is 2000r/min, and mixing time is 30min.
A kind of 4. preparation method of heat conducting film according to claim 3, it is characterised in that:In the step S3, machinery stirs The range of speeds of machine is mixed between 1500r/min-2500r/min, and mixing time scope is between 20min-40min.
A kind of 5. preparation method of heat conducting film according to claim 4, it is characterised in that:Mechanical agitation in the step S1 The range of speeds of machine is between 2000r/min, and mixing time scope is between 30min;In the step S3, machine mixer The range of speeds between 2000r/min, and mixing time scope is between 30min;In the step S5, at 50-90 DEG C It is dried, the thickness after rolling is 20 μm.
A kind of 6. preparation method of heat conducting film according to claim 5, it is characterised in that:Carbonization temperature in the step S6 Scope is between 750 DEG C -850 DEG C, and carbonization time scope is between 0.8h-1.2h.
A kind of 7. preparation method of heat conducting film according to claim 6, it is characterised in that:Carbonization temperature in the step S6 For 800 DEG C, carbonization time 1h.
A kind of 8. preparation method of heat conducting film according to claim 1, it is characterised in that:The solid content of graphene slurry is 2%-10% accounts for material total amount 95.5%-99.7%, and dispersant is the 0.1%-2.0% of material total amount, and binding agent is material total amount 0.1%-2.0%, thickener are the 0.1%-0.5% of material total amount.
A kind of 9. heat conducting film, it is characterised in that including:Graphene slurry accounts for material total amount 95.5%-99.7%, and dispersant is material The 0.1%-2.0% of total amount, binding agent are the 0.1%-2.0% of material total amount, and thickener is the 0.1%-0.5% of material total amount.
A kind of 10. heat conducting film according to claim 9, it is characterised in that:The solid content of graphene slurry is 2%-10%;Institute It is the copolymerization liquid solution with acidic group to state dispersant, and the copolymerization liquid solution with acidic group is modified polyurethane or poly- second Alkene pyrrolidone;The binding agent is butadiene-styrene rubber or acrylic ester polymerization emulsion;Thickener:For sodium carboxymethylcellulose, or Person is Sodium Polyacrylate, or is sodium alginate.
CN201710919019.XA 2017-09-30 2017-09-30 A kind of preparation method of heat conducting film and a kind of heat conducting film Pending CN107892295A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109455702A (en) * 2018-11-06 2019-03-12 内蒙古金彩矿业有限公司 A kind of preparation method of graphene heating film
CN109517203A (en) * 2018-11-26 2019-03-26 湖南国盛石墨科技有限公司 A kind of Flexible graphene electromagnetic shielding material and preparation method thereof
CN112322258A (en) * 2020-12-08 2021-02-05 福建永安市永清石墨烯研究院有限公司 Graphene heat-conducting silica gel sheet and preparation method thereof
CN112723345A (en) * 2021-03-26 2021-04-30 云南云天墨睿科技有限公司 Composite graphene slurry with self-assembly property and preparation method thereof
CN112794314A (en) * 2021-04-07 2021-05-14 山东海科创新研究院有限公司 Preparation method of high-density graphene heat-conducting film regulated and controlled by groups and obtained product
CN111286309B (en) * 2020-03-24 2021-07-16 昆山印可达新材料科技有限公司 High-performance graphene heat dissipation film, and preparation method and application thereof
CN113480328A (en) * 2021-07-26 2021-10-08 北京中石伟业科技无锡有限公司 Large-scale graphene heat-conducting roll film and preparation method thereof

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CN109455702A (en) * 2018-11-06 2019-03-12 内蒙古金彩矿业有限公司 A kind of preparation method of graphene heating film
CN109517203A (en) * 2018-11-26 2019-03-26 湖南国盛石墨科技有限公司 A kind of Flexible graphene electromagnetic shielding material and preparation method thereof
CN111286309B (en) * 2020-03-24 2021-07-16 昆山印可达新材料科技有限公司 High-performance graphene heat dissipation film, and preparation method and application thereof
CN112322258A (en) * 2020-12-08 2021-02-05 福建永安市永清石墨烯研究院有限公司 Graphene heat-conducting silica gel sheet and preparation method thereof
CN112322258B (en) * 2020-12-08 2022-01-28 福建永安市永清石墨烯研究院有限公司 Graphene heat-conducting silica gel sheet and preparation method thereof
CN112723345A (en) * 2021-03-26 2021-04-30 云南云天墨睿科技有限公司 Composite graphene slurry with self-assembly property and preparation method thereof
CN112723345B (en) * 2021-03-26 2023-09-29 云南云天墨睿科技有限公司 Composite graphene slurry with self-assembly property and preparation method thereof
CN112794314A (en) * 2021-04-07 2021-05-14 山东海科创新研究院有限公司 Preparation method of high-density graphene heat-conducting film regulated and controlled by groups and obtained product
CN113480328A (en) * 2021-07-26 2021-10-08 北京中石伟业科技无锡有限公司 Large-scale graphene heat-conducting roll film and preparation method thereof

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Application publication date: 20180410