CN114479580A - Graphene composite heat dissipation coating and preparation method thereof, and heat dissipation adhesive tape and preparation method thereof - Google Patents

Graphene composite heat dissipation coating and preparation method thereof, and heat dissipation adhesive tape and preparation method thereof Download PDF

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CN114479580A
CN114479580A CN202210240428.8A CN202210240428A CN114479580A CN 114479580 A CN114479580 A CN 114479580A CN 202210240428 A CN202210240428 A CN 202210240428A CN 114479580 A CN114479580 A CN 114479580A
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heat dissipation
graphene composite
parts
composite heat
graphene
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CN114479580B (en
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刘果
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Guilin Qingyan Haolong New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
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    • C09D7/61Additives non-macromolecular inorganic
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
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    • C09J133/00Adhesives based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/40Adhesives in the form of films or foils characterised by release liners
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2203/00Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/10Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/40Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • C09J2301/408Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer

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Abstract

The invention belongs to the technical field of heat dissipation tapes, and discloses a graphene composite heat dissipation coating and a preparation method thereof, and a heat dissipation tape and a preparation method thereof. According to the invention, the filling of C60 and heat conducting powder in graphene is realized through a hydrothermal reaction and a normal-temperature drying-freezing-normal-temperature drying mode, a graphene composite heat dissipation microporous structure is formed, and then the graphene composite heat dissipation coating is formed by combining with organic silicon modified acrylic resin, a dispersing agent, water and an auxiliary agent. The heat dissipation adhesive tape is composed of three layers, wherein the lowest layer is a carrier of the heat dissipation adhesive tape, the middle layer has the effects of heat conduction and insulation, and the uppermost layer is a coating formed by graphene composite heat dissipation coating and mainly has the heat dissipation effect. The heat dissipation adhesive tape disclosed by the invention is directly pasted in an electronic component, so that high-efficiency heat dissipation can be realized.

Description

Graphene composite heat dissipation coating and preparation method thereof, and heat dissipation adhesive tape and preparation method thereof
Technical Field
The invention relates to the technical field of heat dissipation tapes, in particular to a graphene composite heat dissipation coating and a preparation method thereof, and a heat dissipation tape and a preparation method thereof.
Background
With the rapid development of electronic technology, electronic components such as CPUs, LEDs and the like tend to have higher power and integration, and higher requirements are put forward on the heat dissipation performance of equipment. Poor heat dissipation not only can cause the operating temperature to rise and shorten the service life, but also can cause functional failure and more serious production accidents. Therefore, the good heat dissipation performance of the electronic components is a key support for ensuring the stable operation of the new generation of high-power electronic devices.
At present, the high-performance SOC chip brings strong computing power to the smart phone, and meanwhile, the heat dissipation problem caused by high power consumption is troubling people. The heat dissipation schemes proposed by various large mobile phone manufacturers are also various. Common heat dissipation methods for mobile phones include liquid-cooled heat dissipation, copper foil heat conduction, graphite sheet heat conduction, and the like.
Liquid cooling heat dissipation has been developed into a VC soaking plate, and the embedding mode of the VC soaking plate in the mobile phone is integrated with a metal middle frame, so that the VC soaking plate becomes an important factor in a support and heat dissipation system of the mobile phone. Novel heat sink material: graphite and graphene can achieve the effects of large-area rapid heat transfer and heat dissipation and elimination of single-point high temperature. Meanwhile, the graphite or graphene heat dissipation material is changeable in appearance, can be made into any specified shape, is convenient to use in various different products, perfectly conforms to the smart phone with limited space, but is low in yield, and relatively high in price.
Therefore, how to provide the graphene-based heat dissipation material with good heat dissipation effect and low cost has important significance for the development of electronic equipment.
Disclosure of Invention
The invention aims to provide a graphene composite heat dissipation coating and a preparation method thereof, a heat dissipation adhesive tape and a preparation method thereof, and solves the problem that the existing heat dissipation material cannot meet the high heat dissipation requirement of electronic equipment.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a graphene composite heat-dissipation coating which is prepared from the following raw materials in parts by mass:
15-30 parts of organic silicon modified acrylic resin, 5-15 parts of graphene composite heat dissipation powder, 0.5-2 parts of a dispersing agent, 15-35 parts of water and 0.01-0.05 part of an auxiliary agent;
the graphene composite heat dissipation powder is prepared from the following raw materials in parts by mass:
600.5-2 parts of C, 5-15 parts of graphene and 1-3 parts of heat conducting powder.
Preferably, in the graphene composite heat dissipation coating, the dispersant is KH560 and/or sodium polyacrylate.
Preferably, in the graphene composite heat dissipation coating, the auxiliary agent is one or more of a defoaming agent, a wetting agent and a leveling agent.
Preferably, in the graphene composite heat dissipation coating, the purity of the C60 is more than or equal to 99%; the graphene is graphene oxide, and the purity of the graphene is more than or equal to 95%; the heat conducting powder is Al2O3And SiC, wherein the particle size of the heat conducting powder is 30-50 nm.
The invention also provides a preparation method of the graphene composite heat dissipation coating, which comprises the following steps:
(1) mixing the C60, graphene and heat conducting powder, carrying out hydrothermal reaction, and then sequentially drying, freezing and drying the product to obtain graphene composite heat-dissipating powder;
(2) and mixing the organic silicon modified acrylic resin and the auxiliary agent, adding the graphene composite heat dissipation powder, water and the dispersing agent, and adjusting the viscosity to obtain the graphene composite heat dissipation coating.
Preferably, in the preparation method of the graphene composite heat dissipation coating, the temperature of the hydrothermal reaction in the step (1) is 120-180 ℃; the hydrothermal reaction time is 8-12 h; the drying time is independently 6-10 h; the freezing time is 45-50 h, and the freezing temperature is-16 to-25 ℃.
The invention also provides a heat dissipation adhesive tape, which comprises a graphene composite heat dissipation layer, a heat conduction insulating adhesive layer and a protective release layer;
the graphene composite heat dissipation layer comprises the graphene composite heat dissipation coating;
the heat-conducting insulating bonding layer is prepared from the following raw materials in parts by mass:
15-35 parts of bonding resin and 0.5-3 parts of ceramic powder;
the protective release layer is release paper, a polyethylene terephthalate release film or a polyimide release film.
Preferably, in the heat dissipation adhesive tape, the thickness of the graphene composite heat dissipation layer is 27-40 μm; the thickness of the heat-conducting insulating bonding layer is 20-28 micrometers; the thickness of the protective release layer is 20-30 μm.
Preferably, in the above heat dissipation tape, the adhesive resin is one or two of thermoplastic polyurethane elastomer rubber, ethylene-vinyl acetate copolymer, silicone modified acrylic resin and polyester resin; the ceramic powder is Al2O3And/or Si3N4,Al2O3Has a particle diameter of 1 to 3 μm, Si3N4The particle size of (A) is 8 to 12 μm.
The invention also provides a preparation method of the heat dissipation adhesive tape, which comprises the following steps:
mixing the bonding resin and the ceramic powder, stirring in vacuum, and sequentially stretching and casting to obtain a heat-conducting insulating bonding layer on the protective release layer; and spraying or printing the graphene composite heat dissipation coating on the heat conduction insulating adhesive layer, and baking to obtain the heat dissipation adhesive tape.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the filling of C60 and heat conducting powder in graphene is realized through a hydrothermal reaction and a normal temperature drying-freezing-normal temperature drying mode, so that a graphene composite heat dissipation microporous structure is formed, the structure promotes the overlapping of graphene, the ordered filling of C60 is a way for realizing an ordered conductive path, and the conductive heat dissipation performance of graphene is greatly improved.
(2) The heat dissipation adhesive tape disclosed by the invention is composed of a three-layer structure, the lowest layer is a carrier of the heat dissipation adhesive tape, a coating is protected before use, die cutting is facilitated, meanwhile, the heat dissipation adhesive tape is convenient to be pasted and used on an electronic component, the middle layer has the heat conduction and insulation effects, and the uppermost layer mainly has the heat dissipation effect. The heat dissipation adhesive tape disclosed by the invention is directly pasted in an electronic component, so that high-efficiency heat dissipation can be realized. The heat dissipation adhesive tape is used for modifying the conductive heat dissipation material, the high heat conduction effect of the material is realized, the insulating effect is realized by the middle layer heat conduction structure, meanwhile, the product is easy to die cut, and the product design and the application to special-shaped products are realized.
Detailed Description
The invention provides a graphene composite heat-dissipation coating which is prepared from the following raw materials in parts by mass:
15-30 parts of organic silicon modified acrylic resin, 5-15 parts of graphene composite heat dissipation powder, 0.5-2 parts of a dispersing agent, 15-35 parts of water and 0.01-0.05 part of an auxiliary agent;
the graphene composite heat dissipation powder is prepared from the following raw materials in parts by mass:
600.5-2 parts of C, 5-15 parts of graphene and 1-3 parts of heat conducting powder.
In the invention, the graphene composite heat dissipation coating is preferably prepared from the following raw materials in parts by mass: 17-28 parts of organic silicon modified acrylic resin, 6-13 parts of graphene composite heat dissipation powder, 0.8-1.6 parts of dispersing agent, 18-31 parts of water and 0.02-0.04 part of auxiliary agent;
further preferably, the feed additive is prepared from the following raw materials in parts by mass: 19-24 parts of organic silicon modified acrylic resin, 8-12 parts of graphene composite heat dissipation powder, 0.9-1.5 parts of dispersing agent, 21-30 parts of water and 0.028-0.034 parts of auxiliary agent;
more preferably, the feed additive is prepared from the following raw materials in parts by mass: 20 parts of organic silicon modified acrylic resin, 11 parts of graphene composite heat dissipation powder, 1.3 parts of a dispersing agent, 26 parts of water and 0.03 part of an auxiliary agent.
In the invention, the graphene composite heat dissipation powder is preferably prepared from the following raw materials in parts by mass: 600.7-1.9 parts of C, 7-13 parts of graphene and 1.2-2.8 parts of heat conducting powder;
further preferably, the feed additive is prepared from the following raw materials in parts by mass: c600.8-1.5 parts, graphene 9-11 parts and heat conducting powder 1.6-2.5 parts;
more preferably, the feed additive is prepared from the following raw materials in parts by mass: 601.2 parts of C, 10 parts of graphene and 1.9 parts of heat conducting powder.
In the present invention, the dispersant is preferably KH560 and/or sodium polyacrylate, and more preferably KH 560.
In the invention, the auxiliary agent is preferably one or more of a defoaming agent, a wetting agent and a leveling agent, is further preferably one or more of BYK028, TCB-1, Digao 245 and BYK378, and is more preferably BYK 378.
In the present invention, the purity of C60 is preferably 99% or more, more preferably 99.7% or more, and still more preferably 99.9% or more.
In the present invention, the graphene is preferably graphene oxide; the purity of the graphene is preferably 95% or more, more preferably 96% or more, and still more preferably 98% or more.
In the present invention, the heat conductive powder is preferably Al2O3And SiC; the particle size of the heat conducting powder is preferably 30-50 nm, more preferably 32-47 nm, and even more preferably 42 nm; al (Al)2O3And SiC preferably in a mass ratio of 2-4: 1 to 3, and more preferably 2 to 3: 1-2, more preferably 2: 1.
the invention also provides a preparation method of the graphene composite heat dissipation coating, which comprises the following steps:
(1) mixing the C60, graphene and heat conducting powder, carrying out hydrothermal reaction, and then sequentially drying the product at room temperature, freezing and drying at room temperature to obtain graphene composite heat-dissipating powder;
(2) and mixing the organic silicon modified acrylic resin and the auxiliary agent, adding the graphene composite heat dissipation powder, water and the dispersing agent, and adjusting the viscosity to obtain the graphene composite heat dissipation coating.
In the invention, the temperature of the hydrothermal reaction in the step (1) is preferably 120-180 ℃, more preferably 126-171 ℃, and more preferably 154 ℃; the time for the hydrothermal reaction is preferably 8 to 12 hours, more preferably 9 to 11 hours, and even more preferably 10 hours.
In the invention, the time for drying at room temperature in the step (1) is preferably 6-10 h, more preferably 7-9 h, and even more preferably 8 h.
In the invention, the freezing time in the step (1) is preferably 45-50 h, more preferably 46-49 h, and more preferably 48 h; the freezing temperature is preferably-16 to-25 ℃, more preferably-18 to-23 ℃, and still more preferably-21 ℃.
In the invention, the organosilicon modified acrylic resin and the auxiliary agent in the step (2) are preferably mixed by stirring; the stirring speed is preferably 800-1500 r/min, more preferably 900-1400 r/min, and even more preferably 1200 r/min; the stirring time is preferably 15 to 30min, more preferably 18 to 28min, and still more preferably 21 min.
In the invention, the adding method of the graphene composite heat dissipation powder, water and the dispersing agent in the step (2) comprises the following steps: mixing graphene composite heat dissipation powder, water and a dispersing agent, and adding the mixture into a mixed solution of organic silicon modified acrylic resin and an auxiliary agent; the preferable mixing method of the graphene composite heat dissipation powder, water and the dispersing agent is ultrasonic dispersion; the time for ultrasonic dispersion is preferably 1-3 h, more preferably 1.3-2.8 h, and even more preferably 2.5 h.
In the invention, before the viscosity is adjusted in the step (2), the method also comprises the step of stirring the mixed solution of the organic silicon modified acrylic resin and the auxiliary agent and the mixed solution of the graphene composite heat dissipation powder, water and the dispersing agent; the stirring time is preferably 50-90 min, more preferably 57-82 min, and even more preferably 63 min; the stirring speed is preferably 1300-1600 r/min, more preferably 1350-1550 r/min, and even more preferably 1450 r/min.
In the invention, the viscosity in the step (2) is preferably adjusted to 800-1000 mpa.s, more preferably 830-960 mpa.s, and even more preferably 890 mpa.s.
The invention also provides a heat dissipation adhesive tape, which comprises a graphene composite heat dissipation layer, a heat conduction insulating bonding layer and a protective release layer;
the graphene composite heat dissipation layer comprises the graphene composite heat dissipation coating;
the heat-conducting insulating bonding layer is prepared from the following raw materials in parts by mass:
15-35 parts of bonding resin and 0.5-3 parts of ceramic powder;
the protective release layer is release paper, polyethylene terephthalate release film or polyimide release film.
In the invention, the thickness of the graphene composite heat dissipation layer is preferably 27-40 μm, more preferably 29-37 μm, and even more preferably 33 μm.
In the present invention, the thickness of the heat conductive insulating adhesive layer is preferably 20 to 28 μm, more preferably 22 to 26 μm, and still more preferably 25 μm.
In the present invention, the thickness of the protective release layer is preferably 20 to 30 μm, more preferably 23 to 29 μm, and still more preferably 27 μm.
In the present invention, the heat conducting insulating adhesive layer is preferably prepared from the following raw materials in parts by mass: 17-34 parts of bonding resin and 0.7-2.7 parts of ceramic powder;
further preferably, the feed additive is prepared from the following raw materials in parts by mass: 19-30 parts of bonding resin and 0.9-2.2 parts of ceramic powder;
more preferably, the feed additive is prepared from the following raw materials in parts by mass: 26 parts of bonding resin and 1.7 parts of ceramic powder.
In the present invention, the bonding resin is preferably one or two of thermoplastic polyurethane elastomer rubber (TPU), ethylene-vinyl acetate copolymer (EVA), silicone-modified acrylic resin, and polyester resin, more preferably one or two of TPU, EVA, and polyester resin, and even more preferably TPU.
In the present invention, the ceramic powder is preferably Al2O3And/or Si3N4More preferably, Al2O3;Al2O3The particle size of (A) is preferably 1 to 3 μm, more preferably 1.1 to 2.9 μm, and still more preferably 2.3 μm; si3N4The particle diameter of (A) is preferably 8 to 12 μm, more preferably 8.6 to 11.3 μm, and still more preferably 10.6 μm.
The invention also provides a preparation method of the heat dissipation adhesive tape, which comprises the following steps:
mixing the bonding resin and the ceramic powder, carrying out vacuum stirring, and sequentially carrying out stretching and tape casting to obtain a heat-conducting insulating bonding layer on the protective release layer; and spraying or printing the graphene composite heat dissipation coating on the heat conduction insulating adhesive layer, and baking to obtain the heat dissipation adhesive tape.
In the present invention, the degree of vacuum stirring is preferably-0.05 to-0.09 MPa, more preferably-0.06 to-0.08 MPa, and still more preferably-0.07 MPa; the time for vacuum stirring is preferably 30-60 min, more preferably 36-54 min, and even more preferably 43 min; the speed of vacuum stirring is preferably 1200 to 2000r/min, more preferably 1400 to 1800r/min, and even more preferably 1500 r/min.
In the invention, the baking temperature is preferably 70-90 ℃, more preferably 73-87 ℃, and more preferably 79 ℃; the baking time is preferably 10 to 50min, more preferably 14 to 43min, and still more preferably 32 min.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The embodiment provides a heat dissipation adhesive tape, and a preparation method of the heat dissipation adhesive tape comprises the following steps:
(1) 1 part of C60, 5 parts of graphene oxide and 0.5 part of Al2O3Mixing the powder (the particle size is 40nm) and 0.5 part of SiC (the particle size is 40nm), carrying out hydrothermal reaction at 160 ℃ for 9h, and then sequentially drying the product at room temperature for 8h, freezing at-20 ℃ for 48h and drying at room temperature for 8h to obtain graphene composite heat dissipation powder;
(2) carrying out ultrasonic dispersion on 8 parts of graphene composite heat dissipation powder, 35 parts of water and 0.5 part of KH560 for 2 hours to obtain graphene slurry; stirring 15 parts of organic silicon modified acrylic resin, 0.01 part of TCB-1 and 0.01 part of digao 245 at a speed of 1100r/min for 20min, then adding graphene slurry, stirring at a speed of 1500r/min for 60min, and adjusting the viscosity to 900mpa.s with water to obtain the graphene composite heat dissipation coating;
(3) 35 parts of TPU and 2 parts of Si3N4Mixing (particle size is 10 μm), stirring under vacuum of-0.06 MPa at 1700r/min for 50min, sequentially stretching and casting to obtain a heat-conducting insulating adhesive layer with thickness of 25 μm on a PET release film with thickness of 25 μm; spraying the graphene composite heat dissipation coating on the heat conduction insulatorAnd (3) obtaining a graphene composite heat dissipation layer with the thickness of 30 mu m on the edge bonding layer, and baking at 80 ℃ for 20min to obtain the heat dissipation adhesive tape.
Example 2
The embodiment provides a heat dissipation adhesive tape, and a preparation method of the heat dissipation adhesive tape comprises the following steps:
(1) 2 parts of C60, 5 parts of graphene oxide and 1.5 parts of Al2O3Mixing (the particle size is 30nm) and 0.5 part of SiC (the particle size is 30nm), carrying out hydrothermal reaction for 12 hours at 140 ℃, and then drying the product at room temperature for 8 hours, freezing at-20 ℃ for 48 hours, and drying at room temperature for 8 hours in sequence to obtain graphene composite heat dissipation powder;
(2) ultrasonically dispersing 7 parts of graphene composite heat dissipation powder, 35 parts of water and 0.5 part of sodium polyacrylate for 2 hours to obtain graphene slurry; stirring 15 parts of organic silicon modified acrylic resin, 0.02 part of BYK028 and 0.02 part of digao 245 at 1500r/min for 30min, then adding graphene slurry, stirring at 1600r/min for 90min, and adjusting the viscosity to 1000mpa.s by using water to obtain the graphene composite heat dissipation coating;
(3) 35 parts of organic silicon modified acrylic resin and 2 parts of Si3N4Mixing (particle size is 10 μm), stirring in vacuum at 1300r/min for 30min under the condition that the vacuum degree is-0.09 MPa, and sequentially stretching and casting to obtain a heat-conducting insulating adhesive layer with the thickness of 27 μm on a PI release film with the thickness of 24 μm; and spraying the graphene composite heat dissipation coating on the heat conduction insulation adhesive layer to obtain a graphene composite heat dissipation layer with the thickness of 35 microns, and baking for 30min at 80 ℃ to obtain the heat dissipation adhesive tape.
The heat dissipating tapes of examples 1 and 2 were die-cut into the same shape, and attached to two identical aluminum block electronic components of 6 × 6 × 3cm, respectively, and heat dissipating properties were measured, and the electronic components to which the heat dissipating tapes were not attached were used as a control, and the results are shown in table 1.
Table 1 heat dissipation performance test results of heat dissipation tapes
Figure BDA0003541320150000081
Figure BDA0003541320150000091
As can be seen from table 1, after the heat dissipation tape of the present invention is adhered to an electronic component, the heat of the electronic component can be effectively reduced, and the heat dissipation of the electronic component without the heat dissipation tape is slow. The heat-dissipating adhesive tape disclosed by the invention can realize heat conduction in the transverse direction and can realize the protection of electronic products through the middle heat-conducting insulating layer in the longitudinal direction.
The graphene composite heat dissipation layers on the heat dissipation tapes of examples 1 and 2 were subjected to adhesion, water resistance, and low temperature resistance tests, and the results are shown in table 2.
Table 2 performance test results of graphene composite heat dissipation layer
Figure BDA0003541320150000092
As can be seen from table 2, the graphene composite heat dissipation coating on the heat dissipation adhesive tape of the present invention has good adhesion, is firmly adhered to the adhesive tape substrate, has excellent water resistance and low temperature resistance, has a long service life, and can be efficiently used for heat dissipation of electronic components.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The graphene composite heat dissipation coating is characterized by being prepared from the following raw materials in parts by mass:
15-30 parts of organic silicon modified acrylic resin, 5-15 parts of graphene composite heat dissipation powder, 0.5-2 parts of a dispersing agent, 15-35 parts of water and 0.01-0.05 part of an auxiliary agent;
the graphene composite heat dissipation powder is prepared from the following raw materials in parts by mass:
600.5-2 parts of C, 5-15 parts of graphene and 1-3 parts of heat conducting powder.
2. The graphene composite heat dissipation coating as claimed in claim 1, wherein the dispersant is KH560 and/or sodium polyacrylate.
3. The graphene composite heat dissipation coating as claimed in claim 1 or 2, wherein the auxiliary agent is one or more of a defoaming agent, a wetting agent and a leveling agent.
4. The graphene composite heat dissipation coating as claimed in claim 3, wherein the purity of C60 is greater than or equal to 99%; the graphene is graphene oxide, and the purity of the graphene is more than or equal to 95%; the heat conducting powder is Al2O3And SiC, wherein the particle size of the heat conducting powder is 30-50 nm.
5. The preparation method of the graphene composite heat dissipation coating as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
(1) mixing the C60, graphene and heat conducting powder, carrying out hydrothermal reaction, and then sequentially drying, freezing and drying the product to obtain graphene composite heat-dissipating powder;
(2) and mixing the organic silicon modified acrylic resin and the auxiliary agent, adding the graphene composite heat dissipation powder, water and the dispersing agent, and adjusting the viscosity to obtain the graphene composite heat dissipation coating.
6. The preparation method of the graphene composite heat dissipation coating according to claim 5, wherein the temperature of hydrothermal reaction in the step (1) is 120-180 ℃; the hydrothermal reaction time is 8-12 h; the drying time is independently 6-10 h; the freezing time is 45-50 h, and the freezing temperature is-16 to-25 ℃.
7. The heat dissipation adhesive tape is characterized by comprising a graphene composite heat dissipation layer, a heat conduction insulating bonding layer and a protective release layer;
wherein the graphene composite heat dissipation layer comprises the graphene composite heat dissipation coating as recited in any one of claims 1 to 4;
the heat-conducting insulating bonding layer is prepared from the following raw materials in parts by mass:
15-35 parts of bonding resin and 0.5-3 parts of ceramic powder;
the protective release layer is release paper, a polyethylene terephthalate release film or a polyimide release film.
8. The heat dissipation tape of claim 7, wherein the thickness of the graphene composite heat dissipation layer is 27-40 μm; the thickness of the heat-conducting insulating bonding layer is 20-28 micrometers; the thickness of the protective release layer is 20-30 μm.
9. The heat dissipating tape of claim 7 or 8, wherein the bonding resin is one or two of thermoplastic polyurethane elastomer rubber, ethylene-vinyl acetate copolymer, silicone-modified acrylic resin, and polyester resin; the ceramic powder is Al2O3And/or Si3N4,Al2O3Has a particle diameter of 1 to 3 μm, Si3N4The particle size of (A) is 8 to 12 μm.
10. The method for preparing a heat dissipating tape according to any one of claims 7 to 9, comprising the steps of:
mixing the bonding resin and the ceramic powder, stirring in vacuum, and sequentially stretching and casting to obtain a heat-conducting insulating bonding layer on the protective release layer; and spraying or printing the graphene composite heat dissipation coating on the heat conduction insulating adhesive layer, and baking to obtain the heat dissipation adhesive tape.
CN202210240428.8A 2022-03-10 2022-03-10 Graphene composite heat dissipation coating and preparation method thereof, and heat dissipation adhesive tape and preparation method thereof Active CN114479580B (en)

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Citations (5)

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Publication number Priority date Publication date Assignee Title
CN104694033A (en) * 2013-12-04 2015-06-10 凯尔凯德新材料科技泰州有限公司 Heat conducting adhesive tape with heat dissipating and heat storing functions, and making method thereof
CN107903751A (en) * 2017-11-30 2018-04-13 深圳天元羲王材料科技有限公司 A kind of graphene heat radiation coating and preparation method thereof
CN109233590A (en) * 2018-07-12 2019-01-18 厦门奈福电子有限公司 Watersoluble plumbago alkene heat radiation coating and preparation method thereof, spraying method
CN109777316A (en) * 2019-01-28 2019-05-21 东莞市澳中电子材料有限公司 A kind of high thermal conductivity graphite glue band and preparation method thereof
CN113881295A (en) * 2021-09-03 2022-01-04 北京旭碳新材料科技有限公司 Water-based graphene heat dissipation coating and preparation and spraying methods thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104694033A (en) * 2013-12-04 2015-06-10 凯尔凯德新材料科技泰州有限公司 Heat conducting adhesive tape with heat dissipating and heat storing functions, and making method thereof
CN107903751A (en) * 2017-11-30 2018-04-13 深圳天元羲王材料科技有限公司 A kind of graphene heat radiation coating and preparation method thereof
CN109233590A (en) * 2018-07-12 2019-01-18 厦门奈福电子有限公司 Watersoluble plumbago alkene heat radiation coating and preparation method thereof, spraying method
CN109777316A (en) * 2019-01-28 2019-05-21 东莞市澳中电子材料有限公司 A kind of high thermal conductivity graphite glue band and preparation method thereof
CN113881295A (en) * 2021-09-03 2022-01-04 北京旭碳新材料科技有限公司 Water-based graphene heat dissipation coating and preparation and spraying methods thereof

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