CN114805887A - Insulating phase-change heat-conducting film and preparation method thereof - Google Patents

Insulating phase-change heat-conducting film and preparation method thereof Download PDF

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CN114805887A
CN114805887A CN202210293618.6A CN202210293618A CN114805887A CN 114805887 A CN114805887 A CN 114805887A CN 202210293618 A CN202210293618 A CN 202210293618A CN 114805887 A CN114805887 A CN 114805887A
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phase
conducting
change heat
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heat
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王海旭
刘创
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Shenzhen Frd Science & Technology Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • C08J7/042Coating with two or more layers, where at least one layer of a composition contains a polymer binder
    • 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
    • C09D191/00Coating compositions based on oils, fats or waxes; Coating compositions based on derivatives thereof
    • C09D191/06Waxes
    • 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2491/00Characterised by the use of oils, fats or waxes; Derivatives thereof
    • C08J2491/06Waxes
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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
    • 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
    • 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
    • C08K2003/2296Oxides; Hydroxides of metals of zinc

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  • Organic Insulating Materials (AREA)

Abstract

The invention discloses an insulating phase-change heat-conducting film and a preparation method thereof, wherein the insulating phase-change heat-conducting film comprises an insulating intermediate layer and phase-change heat-conducting layers respectively compounded on two opposite sides of the insulating intermediate layer; the phase-change heat conduction layer comprises the following raw materials in parts by weight: 1-20 parts of high polymer material, 5-25 parts of phase change material, 70-95 parts of heat conducting powder, and less than or equal to 5 parts of coupling agent and auxiliary agent. The insulating phase-change heat-conducting film is formed by compounding the insulating intermediate layer and the phase-change heat-conducting layer to form a film with a laminated structure, and has insulating property and phase-change heat-conducting property; the thickness can be controlled in a small range, the heat resistance is extremely low, the heat conducting plate can be directly contacted with a heating device in application, the heat conduction is realized by the phase change characteristic, and the heat dissipation effect is improved.

Description

Insulating phase-change heat-conducting film and preparation method thereof
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to an insulating phase-change heat conduction film and a preparation method thereof.
Background
With the pursuit of the information and automation society, the electronic devices are required to be miniaturized, integrated and multifunctional, and it is desired to reduce the size and improve the computing performance of the device, and the size and power density of the device are continuously reduced and improved. Meanwhile, the coming of the 5G era brings about the introduction of high frequency, the upgrade of hardware and the doubling of the number of networking equipment and antennas, so that the heat consumption of electronic equipment is remarkably increased, and the heat productivity is rapidly increased along with the heat consumption.
If the heat energy generated by the electronic device in the using process cannot be timely dissipated from the inside, the performance of the electronic equipment is reduced due to the overhigh temperature, and the reliability, the stability and the service life of the electronic equipment are all adversely affected. For example, too high a temperature may damage the junction of the semiconductor, damage the connection interface of the circuit, increase the resistance of the conductor and cause mechanical stress damage. Therefore, thermal management materials for electronic devices have become an important issue for the development of various industries.
Disclosure of Invention
The invention aims to solve the technical problem of providing an insulating phase-change heat-conducting film and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problem is as follows: providing an insulating phase-change heat-conducting film, which comprises an insulating intermediate layer and phase-change heat-conducting layers respectively compounded on two opposite sides of the insulating intermediate layer;
the phase-change heat conduction layer comprises the following raw materials in parts by weight: 1-20 parts of high polymer material, 5-25 parts of phase change material, 70-95 parts of heat conducting powder, and less than or equal to 5 parts of coupling agent and auxiliary agent.
Preferably, the high polymer material is selected from one or more of silicone rubber, methyl silicone oil, vinyl silicone oil, polystyrene elastomer, polyethylene, polypropylene, polybutylene and copolymer thereof.
Preferably, the phase change material includes at least one of paraffin wax, liquid paraffin wax, and polyethylene wax.
Preferably, the heat conducting powder is composed of one or more of aluminum powder, aluminum nitride powder, alumina powder, zinc oxide powder, boron nitride powder and diamond powder.
Preferably, the coupling agent comprises one or more of an aluminate coupling agent, a borate coupling agent, a titanate coupling agent, a metal composite coupling agent and a silane coupling agent.
Preferably, the auxiliary agent comprises one or more of an antioxidant, a tackifier and a diluting solvent;
the antioxidant comprises one or more of hindered phenol, hindered amine and phosphite antioxidant; the tackifier comprises one or more of C9 petroleum resin, C5 petroleum resin, rosin resin and terpene resin; the diluting solvent comprises one or more of toluene, xylene, ethyl acetate and low molecular silane solvent.
Preferably, the insulating interlayer is a polyimide film layer or a polycarbonate film layer.
Preferably, the thickness of the insulating phase-change heat-conducting film is 60-150 μm.
Preferably, the insulating phase-change heat-conducting film further comprises a protective layer compounded on the phase-change heat-conducting layer.
The invention also provides a preparation method of the insulating phase-change heat-conducting film, which comprises the following steps:
s1, weighing the high polymer material, the phase-change material, the heat-conducting powder, the coupling agent and the auxiliary agent according to the parts by weight, mixing, heating at high temperature, and stirring uniformly to obtain phase-change heat-conducting slurry;
s2, respectively coating the phase-change heat-conducting slurry on two surfaces of an insulating interlayer;
and S3, drying to enable the phase-change heat-conducting slurry to form a phase-change heat-conducting layer on the insulating interlayer.
The insulating phase-change heat-conducting film is formed by compounding the insulating intermediate layer and the phase-change heat-conducting layer to form a film with a laminated structure, and has insulating property and phase-change heat-conducting property; the thickness can be controlled in a small range, the heat resistance is extremely low, the heat conducting plate can be directly contacted with a heating device in application, the heat conduction is realized by the phase change characteristic, and the heat dissipation effect is improved.
The insulating phase-change heat-conducting film can be matched with other heat management technologies, and is favorable for better solving the problem of thermal runaway caused by over-high temperature of a heating device.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
fig. 1 is a schematic cross-sectional view of an insulating phase-change thermal film according to some embodiments of the present invention.
Detailed Description
For a more clear understanding of the technical features, objects and effects of the present invention, embodiments of the present invention will now be described in detail with reference to the accompanying drawings.
As shown in fig. 1, the insulating phase-change heat conducting film of the present invention may include an insulating interlayer 10, and phase-change heat conducting layers 20 respectively compounded on two opposite sides of the insulating interlayer 10.
The insulating interlayer 10 serves as an insulating matrix of the entire film; the phase-change heat conduction layer 20 is compounded on the outer side of the insulating interlayer 10, and the phase-change heat conduction function of the film is endowed.
The thickness of the insulating phase-change heat-conducting film is 60-150 μm, and the thicknesses of the insulating intermediate layer 10 and the phase-change heat-conducting layer 20 can be correspondingly set according to the thickness range.
The thickness of the insulating phase-change heat-conducting film is controlled to be 60-150 mu m, the whole thickness is small, the insulating phase-change heat-conducting film has extremely low thermal resistance and excellent electric insulation, and the insulating phase-change heat-conducting film wets the surface when being heated through phase-change characteristics and reduces interface thermal resistance. The insulating phase change heat conduction film directly contacts the heating device in actual use, so that the heat dissipation effect is improved, and the problem of thermal runaway of the device caused under the condition of overhigh temperature is solved.
Alternatively, the insulating interlayer 10 may be a polyimide film layer or a polycarbonate film layer.
The phase-change heat conduction layer 20 comprises the following raw materials in parts by weight: 1-20 parts of high polymer material, 5-25 parts of phase change material, 70-95 parts of heat conducting powder, and less than or equal to 5 parts of coupling agent and auxiliary agent.
Wherein the high molecular material is selected from one or more of silicone rubber, methyl silicone oil, vinyl silicone oil, polystyrene elastomer, polyethylene, polypropylene, polybutylene and copolymer thereof.
The phase-change material comprises at least one of solid paraffin, liquid paraffin and polyethylene wax.
The heat conducting powder is composed of one or more of aluminum powder, aluminum nitride powder, alumina powder, zinc oxide powder, boron nitride powder and diamond powder.
The coupling agent comprises one or more of an aluminate coupling agent, a borate coupling agent, a titanate coupling agent, a metal composite coupling agent and a silane coupling agent.
The auxiliary agent comprises one or more of an antioxidant, a tackifier and a diluting solvent.
Specifically, the antioxidant comprises one or more of hindered phenol, hindered amine and phosphite antioxidant; the tackifier comprises one or more of C9 petroleum resin, C5 petroleum resin, rosin resin and terpene resin; the diluting solvent comprises one or more of toluene, xylene, ethyl acetate and low molecular weight silane solvent.
In some embodiments, the insulating phase-change thermal conductive film further includes a protective layer 30 laminated on the phase-change thermal conductive layer 20. The protective layer 30 protects the phase-change heat conduction layer 20 on the outer side thereof, and the protective layer 30 is peeled off before the insulating phase-change heat conduction film is used, so that the phase-change heat conduction characteristic of the phase-change heat conduction layer 20 is not affected during use.
The protective layer 30 may be a release film.
Referring to fig. 1, the method for preparing the insulating phase-change thermal conductive film of the present invention, in some embodiments, may include the following steps:
s1, weighing the high polymer material, the phase-change material, the heat-conducting powder, the coupling agent and the auxiliary agent according to the parts by weight, mixing, heating at high temperature, and stirring uniformly to obtain the phase-change heat-conducting slurry.
Wherein the heating temperature is 80-150 ℃; the time can be 2-8 hours, and is specifically selected according to the uniform mixing degree.
And S2, respectively coating the phase change heat conduction slurry on two sides of the insulating interlayer 10.
The insulating interlayer 10 is prepared or obtained in advance and is a polyimide film layer or a polycarbonate film layer according to actual needs. The phase-change thermal conductive paste prepared in the above step S1 is coated on both sides of the insulating interlayer 10 by a coating apparatus. The thickness of the phase-change thermal-conductive paste coated on each side of the insulating interlayer 10 is controlled according to the total thickness of the insulating phase-change thermal-conductive film of 60 μm to 150 μm.
And S3, drying to form the phase-change heat conduction layer 20 on the insulating interlayer 10 by the phase-change heat conduction slurry.
After the phase-change heat-conducting slurry is coated, the insulating interlayer with the phase-change heat-conducting slurry passes through baking equipment and is dried through a baking channel of the baking equipment, and the phase-change heat-conducting slurry forms a phase-change heat-conducting layer 20 compounded on the insulating interlayer 10.
Wherein the drying temperature can be 80-150 ℃ and the time is less than or equal to 30 min.
S4, the phase-change heat conductive layer 20 is covered with the protective layer 30 to protect it.
The present invention is further illustrated by the following specific examples.
Example 1:
10g of polyolefin and 20g of paraffin (liquid paraffin mixed with solid paraffin) were mixed and mixed uniformly by a planetary mixer, and then a mixture of 7: adding 70g of alumina powder with the particle size of 5 mu m and zinc oxide powder with the particle size of 1 mu m in a weight ratio of 3, mixing and stirring for 15min, adding an aluminate coupling agent and ethyl acetate, and stirring for 15min to obtain the phase-change heat-conducting slurry. And coating the obtained phase-change heat-conducting slurry on two surfaces of the PI film, wherein the total thickness of the phase-change heat-conducting slurry and the PI film is 100 microns, and drying to obtain the finished product of the insulation phase-change heat-conducting film.
Example 2:
3g of polyolefin and 5g of paraffin (liquid paraffin mixed with solid paraffin) were mixed and mixed uniformly by a planetary mixer, and then a mixture of 7: adding 92g of 5-micron alumina powder and 1-micron zinc oxide powder in a weight ratio of 3, mixing and stirring for 15min, adding an aluminate coupling agent and ethyl acetate, and stirring for 15min to obtain the phase-change heat-conducting slurry. And coating the obtained phase-change heat-conducting slurry on two surfaces of the PI film, wherein the total thickness of the phase-change heat-conducting slurry and the PI film is 100 microns, and drying to obtain the finished product of the insulation phase-change heat-conducting film.
Example 3:
1g of polyolefin and 13g of paraffin (liquid paraffin mixed with solid paraffin) were mixed and mixed uniformly by a planetary mixer, and then the ratio of 8: adding 85g of alumina powder with the particle size of 5 mu m and zinc oxide powder with the particle size of 1 mu m in a weight ratio of 2, mixing and stirring for 15min, adding an aluminate coupling agent and ethyl acetate, and stirring for 15min to obtain the phase-change heat-conducting slurry. And coating the obtained phase-change heat-conducting slurry on two surfaces of the PI film, wherein the total thickness of the phase-change heat-conducting slurry and the PI film is 100 microns, and drying to obtain the finished product of the insulation phase-change heat-conducting film.
The insulation phase-change heat-conducting film obtained in the above examples 1 to 3 was subjected to thermal resistance test, electrical breakdown test, and withstand voltage test, respectively, and the results are shown in table 1 below.
TABLE 1
Figure BDA0003562427530000061
As can be seen from the data in table 1, the insulating phase-change thermal conductive films prepared in embodiments 1 to 3 of the present invention have low thermal resistance, no overflow risk, and good breakdown resistance, and satisfy the heat dissipation requirements of miniaturized, multifunctional, and other electronic devices.
It can be understood that, in the insulating phase-change heat-conducting film of the present invention, the content of the polymer material, the phase-change material, the heat-conducting powder and other raw materials is selected in addition to those in examples 1 to 3, and the effects of low thermal resistance and good breakdown resistance under an extremely thin condition can be achieved within the mass portion range of the present invention.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. An insulating phase-change heat-conducting film is characterized by comprising an insulating intermediate layer and phase-change heat-conducting layers respectively compounded on two opposite sides of the insulating intermediate layer;
the phase change heat conduction layer comprises the following raw materials in parts by weight: 1-20 parts of high polymer material, 5-25 parts of phase change material, 70-95 parts of heat conducting powder, and less than or equal to 5 parts of coupling agent and auxiliary agent.
2. The insulating phase-change thermal film according to claim 1, wherein the polymer material is selected from one or more of silicone rubber, methyl silicone oil, vinyl silicone oil, polystyrene elastomer, polyethylene, polypropylene, polybutylene and copolymer thereof.
3. The insulating phase-change heat conducting film according to claim 1, wherein the phase-change material comprises at least one of paraffin wax, liquid paraffin wax and polyethylene wax.
4. The insulating phase-change heat-conducting film according to claim 1, wherein the heat-conducting powder is composed of one or more of aluminum powder, aluminum nitride powder, aluminum oxide powder, zinc oxide powder, boron nitride powder and diamond powder.
5. The insulation phase-change thermal conductive film according to claim 1, wherein the coupling agent comprises one or more of an aluminate coupling agent, a borate coupling agent, a titanate coupling agent, a metal composite coupling agent, and a silane coupling agent.
6. The insulating phase-change heat-conducting film according to claim 1, wherein the auxiliary agent comprises one or more of an antioxidant, an adhesion promoter and a diluting solvent;
the antioxidant comprises one or more of hindered phenol, hindered amine and phosphite antioxidant; the tackifier comprises one or more of C9 petroleum resin, C5 petroleum resin, rosin resin and terpene resin; the diluting solvent comprises one or more of toluene, xylene, ethyl acetate and low molecular silane solvent.
7. The insulating phase-change heat-conducting film according to claim 1, wherein the insulating intermediate layer is a polyimide film layer or a polycarbonate film layer.
8. The insulated phase-change heat-conducting film according to any one of claims 1 to 7, wherein the thickness of the insulated phase-change heat-conducting film is 60 μm to 150 μm.
9. The insulated phase-change heat-conducting film according to any one of claims 1 to 7, further comprising a protective layer compounded on the phase-change heat-conducting layer.
10. The preparation method of the insulating phase-change heat-conducting film according to any one of claims 1 to 9, comprising the following steps:
s1, weighing the high polymer material, the phase-change material, the heat-conducting powder, the coupling agent and the auxiliary agent according to the parts by weight, mixing, heating at high temperature, and stirring uniformly to obtain phase-change heat-conducting slurry;
s2, respectively coating the phase-change heat-conducting slurry on two surfaces of an insulating interlayer;
and S3, drying to enable the phase-change heat-conducting slurry to form a phase-change heat-conducting layer on the insulating interlayer.
CN202210293618.6A 2022-03-24 2022-03-24 Insulating phase-change heat-conducting film and preparation method thereof Pending CN114805887A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101225293A (en) * 2008-02-01 2008-07-23 南京凯汇工业科技有限公司 Phase-change heat conductive material and preparation method thereof
JP2013086433A (en) * 2011-10-20 2013-05-13 Shin-Etsu Chemical Co Ltd Thermally conductive silicone composite sheet
CN108003812A (en) * 2017-12-14 2018-05-08 中国科学院深圳先进技术研究院 A kind of response type heat conductive insulating two-sided tape and preparation method thereof
CN110698994A (en) * 2019-09-12 2020-01-17 广州视源电子科技股份有限公司 Heat-conducting insulating adhesive tape and preparation method thereof
CN112175538A (en) * 2020-10-14 2021-01-05 深圳市飞荣达科技股份有限公司 Film and preparation method thereof
CN113493657A (en) * 2020-03-20 2021-10-12 深圳先进电子材料国际创新研究院 Composite phase-change material film and preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101225293A (en) * 2008-02-01 2008-07-23 南京凯汇工业科技有限公司 Phase-change heat conductive material and preparation method thereof
JP2013086433A (en) * 2011-10-20 2013-05-13 Shin-Etsu Chemical Co Ltd Thermally conductive silicone composite sheet
CN108003812A (en) * 2017-12-14 2018-05-08 中国科学院深圳先进技术研究院 A kind of response type heat conductive insulating two-sided tape and preparation method thereof
CN110698994A (en) * 2019-09-12 2020-01-17 广州视源电子科技股份有限公司 Heat-conducting insulating adhesive tape and preparation method thereof
CN113493657A (en) * 2020-03-20 2021-10-12 深圳先进电子材料国际创新研究院 Composite phase-change material film and preparation method and application thereof
CN112175538A (en) * 2020-10-14 2021-01-05 深圳市飞荣达科技股份有限公司 Film and preparation method thereof

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Application publication date: 20220729