CN109880545A - The preparation method of thermostable heat-conductive one-faced tapes - Google Patents

The preparation method of thermostable heat-conductive one-faced tapes Download PDF

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Publication number
CN109880545A
CN109880545A CN201910103918.1A CN201910103918A CN109880545A CN 109880545 A CN109880545 A CN 109880545A CN 201910103918 A CN201910103918 A CN 201910103918A CN 109880545 A CN109880545 A CN 109880545A
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heat
conductive
metal foil
foil layer
parts
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金闯
张庆杰
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Jiangsu Stick New Materials Polytron Technologies Inc
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Jiangsu Stick New Materials Polytron Technologies Inc
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Priority to CN201910103918.1A priority Critical patent/CN109880545A/en
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Abstract

The invention discloses a kind of preparation methods of thermostable heat-conductive one-faced tapes, the following steps are included: S1. is by hydroxy-terminated polysiloxane, epoxy resin, MQ resin, tetraethoxysilane, 4,4 '-two (propyloxy phenyl base) diphenylamines, benzotriazole and organic solvent are added in reaction kettle, the metatitanic acid tert-butyl ester and organic tin catalyst are added after being warming up to, silicone pressure sensitive glue is made after reaction;S2. graphene powder, nm-class boron nitride, 3- mercaptopropyltriethoxysilane, ethyoxyl acetylenic glycols and organic solvent are added to the dispersion of stirred tank high speed, then silicone pressure sensitive glue is added in stirred tank, stirred and high-heat-conductivity glue stick is made;S3. insulating coating is set in the coated on one side of metal foil layer, is coated with high-heat-conductivity glue stick, drying, solidification in the another side of metal foil layer;S4. a release film layer is covered on high-heat-conductivity glue adhesion coating surface;Adhesive tape good heat conductivity produced by the present invention, it is practical with thermally conductive and bonding function.

Description

The preparation method of thermostable heat-conductive one-faced tapes
Technical field
The present invention relates to adhesive tape area more particularly to a kind of preparation methods of thermostable heat-conductive one-faced tapes.
Background technique
With the fast development of electronics industry, electronic product tends to be light, and volume is smaller and smaller, thus the collection of electronic component Cheng Du is with regard to higher and higher, so to the requirement for leading heat dissipation performance of electronic component with regard to higher and higher.Heat-conducting glue band is led because having Heat and the function that is bonded as one and be widely used, and it is with flexibility, compressibility, docile property and adaptive temperature range The characteristics such as big and in occupation of biggish Heat Conduction Material market.
At present prepare heat-conducting glue band method be that heat filling is added in colloid, achieve the purpose that it is thermally conductive, but at present Heat-conducting glue band thermal coefficient it is generally smaller, and colloid is easy to produce heat ageing under long term high temperature working environment, occurs The problems such as cracking falls off.Therefore, a kind of good heat conductivity how is developed, and there is good heat resistance, can be avoided The thermostable heat-conductive one-faced tapes that situation is fallen off after heated for a long time, become the direction of those skilled in the art's effort.
Summary of the invention
It is an object of that present invention to provide a kind of preparation method of thermostable heat-conductive one-faced tapes, the glue that this method is prepared Band glue-line heat aging property is strong, and adhesive tape is enable to work at a higher temperature for a long time, and its adhesive property weakens without obvious, Effectively prevent the case where falling off after adhesive tape is heated for a long time.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of preparation side of thermostable heat-conductive one-faced tapes Method, the thermostable heat-conductive one-faced tapes include metal foil layer 2, and the one side of this metal foil layer 2 is coated with an insulating coating 1, gold The another side for belonging to layers of foil 2 is provided with a high-heat-conductivity glue adhesion coating 3, a release film layer 4 be covered on the high-heat-conductivity glue adhesion coating 3 opposite to each other in The one side of metal foil layer 2;
The preparation methods of the thermostable heat-conductive one-faced tapes the following steps are included:
S1. by 30 ~ 40 parts of hydroxy-terminated polysiloxane, 8 ~ 15 parts of epoxy resin, 35 ~ 50 parts of MQ resin, tetraethoxysilane 3 ~ 8 0.3 ~ 2 part and 30 ~ 40 parts of organic solvent part, 4,4 '-two 0.5 ~ 5 part of (propyloxy phenyl base) diphenylamines, benzotriazole addition are anti- It answers in kettle, 0.05 ~ 1 part of the metatitanic acid tert-butyl ester and 0.1 ~ 3 part of organic tin catalyst is added after being warming up to 130 ~ 135 DEG C, 140 ~ It is reacted 2 ~ 3 hours at 150 DEG C, silicone pressure sensitive glue is made after cooling;
S2. by 25 ~ 40 parts of graphene powder, 5 ~ 10 parts of nm-class boron nitride, 5 ~ 10 parts of 3- mercaptopropyltriethoxysilane, ethoxy 0.05 ~ 1 part of base acetylenic glycols and remaining organic solvent are added in stirred tank, and high speed dispersion 40 ~ 60 minutes, then will be made in S1 Silicone pressure sensitive glue be slowly added in stirred tank, stir 30 ~ 40 points, be made high-heat-conductivity glue stick;
S3. insulating coating 1 is set in the coated on one side of metal foil layer 2, it is obtained in the another side coating S2 of metal foil layer 2 High-heat-conductivity glue stick dries, is formed by curing high-heat-conductivity glue adhesion coating 3;
S4. a release film layer 4 is covered on high-heat-conductivity glue adhesion coating 3 opposite to each other in the one side of metal foil layer 2, winding obtains described Thermostable heat-conductive one-faced tapes;
The number is parts by weight, uses the total amount of solvent for 55 ~ 70 parts by weight in S1 and S2.
Further improved technical solution is as follows in above-mentioned technical proposal:
1. in above scheme, the molecular weight of the hydroxy-terminated polysiloxane is 20 ~ 300,000, the hydroxyl of the hydroxy-terminated polysiloxane Base content is 0.3 ~ 1.5%.
2. in above scheme, the organic tin catalyst is selected from dibutyl tin dilaurate, tin dilaurate dioctyl At least one of tin, dibutyl tin dilaurate or stannous octoate.
3. in above scheme, the organic solvent is the mixture of ethyl acetate and dimethylbenzene, the ethyl acetate and two The volume ratio of toluene is 1:2.
4. in above scheme, the metal foil layer is selected from one of copper foil, aluminium foil or tinfoil paper.
5. in above scheme, the high-heat-conductivity glue adhesion coating with a thickness of 5 ~ 20 μm.
Due to the application of the above technical scheme, compared with the prior art, the invention has the following advantages:
1. the preparation method of thermostable heat-conductive one-faced tapes of the present invention, high-heat-conductivity glue adhesion coating uses 25 ~ 40 parts of graphene powder With 5 ~ 10 parts of formation composite heat-conducting systems of nm-class boron nitride, and it is added to 0.05 ~ 1 part of ethyoxyl acetylenic glycols and three second of 3- mercapto propyl 5 ~ 10 parts of oxysilane are played heat filling few as far as possible with heat filling common distribution further to improve its heating conduction Additive amount achievees the effect that high thermal conductivity, and the thermal coefficient that high-heat-conductivity glue adhesion coating is made reaches 3W/ (m.K) or more, avoids Heat filling addition excessive the problem of influencing colloid mechanical property and insulation performance.
2. the preparation method of thermostable heat-conductive one-faced tapes of the present invention, base of the high-heat-conductivity glue adhesion coating in organosilicon systems On plinth, it is added to 8 ~ 15 parts of epoxy resin, 0.5 ~ 5 part of 4,4 '-two (propyloxy phenyl base) diphenylamines and benzotriazole 0.3 ~ 2 Part, the heat resistance of colloid is effectively improved, enables thermostable heat-conductive one-faced tapes prepared by the present invention for a long time higher At a temperature of work, and its adhesive property weakens without obvious, avoids the case where falling off after adhesive tape is heated for a long time, extends The service life of adhesive tape.
Detailed description of the invention
Attached drawing 1 is thermostable heat-conductive one-faced tapes structural schematic diagram of the present invention.
In the figures above: 1, insulating coating;2, metal foil layer;3, high-heat-conductivity glue adhesion coating;4, release film layer.
Specific embodiment
The present invention will be further described below with reference to examples:
Embodiment 1 ~ 4: a kind of preparation method of thermostable heat-conductive one-faced tapes, the thermostable heat-conductive one-faced tapes include metal The one side of layers of foil 2, this metal foil layer 2 is coated with an insulating coating 1, and the another side of metal foil layer 2 is provided with a high thermal conductivity gluing Layer 3, a release film layer 4 is covered on the high-heat-conductivity glue adhesion coating 3 opposite to each other in the one side of metal foil layer 2;
Above-mentioned metal foil layer 2 be copper foil, above-mentioned high-heat-conductivity glue adhesion coating 3 with a thickness of 10 μm;
The preparation methods of above-mentioned thermostable heat-conductive one-faced tapes the following steps are included:
S1. by 30 ~ 40 parts of hydroxy-terminated polysiloxane, 8 ~ 15 parts of epoxy resin, 35 ~ 50 parts of MQ resin, tetraethoxysilane 3 ~ 8 0.3 ~ 2 part and 30 ~ 40 parts of organic solvent part, 4,4 '-two 0.5 ~ 5 part of (propyloxy phenyl base) diphenylamines, benzotriazole addition are anti- It answers in kettle, 0.05 ~ 1 part of the metatitanic acid tert-butyl ester and 0.1 ~ 3 part of organic tin catalyst is added after being warming up to 130 ~ 135 DEG C, 140 ~ It is reacted 2 ~ 3 hours at 150 DEG C, silicone pressure sensitive glue is made after cooling;
S2. by 25 ~ 40 parts of graphene powder, 5 ~ 10 parts of nm-class boron nitride, 5 ~ 10 parts of 3- mercaptopropyltriethoxysilane, ethoxy 0.05 ~ 1 part of base acetylenic glycols and remaining organic solvent are added in stirred tank, and high speed dispersion 40 ~ 60 minutes, then will be made in S1 Silicone pressure sensitive glue be slowly added in stirred tank, stir 30 ~ 40 points, be made high-heat-conductivity glue stick;
S3. insulating coating 1 is set in the coated on one side of metal foil layer 2, it is obtained in the another side coating S2 of metal foil layer 2 High-heat-conductivity glue stick dries, is formed by curing high-heat-conductivity glue adhesion coating 3;
S4. a release film layer 4 is covered on high-heat-conductivity glue adhesion coating 3 opposite to each other in the one side of metal foil layer 2, winding obtains described Thermostable heat-conductive one-faced tapes;
High-heat-conductivity glue adhesion coating 3 in each embodiment is specifically made of following parts by weight of component:
Table 1
The molecular weight of above-mentioned hydroxy-terminated polysiloxane is 20 ~ 300,000, the hydroxy radical content of above-mentioned hydroxy-terminated polysiloxane is 0.3 ~ 1.5%。
The organic tin catalyst of above-described embodiment 1 is dibutyl tin dilaurate, the organic tin catalyst of embodiment 2 For tin dilaurate dioctyl tin, the organic tin catalyst of embodiment 3 is dibutyl tin dilaurate, the organotin of embodiment 4 Class catalyst is stannous octoate.
Above-mentioned organic solvent is the mixture of ethyl acetate and dimethylbenzene, and the volume ratio of above-mentioned ethyl acetate and dimethylbenzene is 1:2。
Comparative example 1 ~ 3, a kind of preparation method of thermally conductive one-faced tapes, the thermally conductive one-faced tapes include metal foil layer 2, this The one side of metal foil layer 2 is coated with an insulating coating 1, and the another side of metal foil layer 2 is provided with a high-heat-conductivity glue adhesion coating 3, one from Type film layer 4 is covered on the high-heat-conductivity glue adhesion coating 3 opposite to each other in the one side of metal foil layer 2;
Above-mentioned metal foil layer 2 be copper foil, above-mentioned high-heat-conductivity glue adhesion coating 3 with a thickness of 10 μm;
The preparation methods of above-mentioned thermally conductive one-faced tapes the following steps are included:
S1. by hydroxy-terminated polysiloxane, epoxy resin, MQ resin, tetraethoxysilane, 4,4 '-two (propyloxy phenyl base) hexichol Amine, benzotriazole and part organic solvent are added in reaction kettle, and the metatitanic acid tert-butyl ester and organic is added after being warming up to 130 ~ 135 DEG C Tin catalyst is reacted 2 ~ 3 hours at 140 ~ 150 DEG C, and silicone pressure sensitive glue is made after cooling;
S2. by graphene powder, nm-class boron nitride, 3- mercaptopropyltriethoxysilane, ethyoxyl acetylenic glycols and remaining organic Solvent is added in stirred tank, and high speed dispersion 40 ~ 60 minutes, then silicone pressure sensitive glue obtained in S1 is slowly added to stir In kettle, 30 ~ 40 points are stirred, high-heat-conductivity glue stick is made;
S3. insulating coating 1 is set in the coated on one side of metal foil layer 2, it is obtained in the another side coating S2 of metal foil layer 2 High-heat-conductivity glue stick dries, is formed by curing high-heat-conductivity glue adhesion coating 3;
S4. a release film layer 4 is covered on high-heat-conductivity glue adhesion coating 3 opposite to each other in the one side of metal foil layer 2, winding obtains described Thermally conductive one-faced tapes;
High-heat-conductivity glue adhesion coating 3 in each comparative example is specifically made of following parts by weight of component:
Table 2
The molecular weight of above-mentioned hydroxy-terminated polysiloxane is 20 ~ 300,000, the hydroxy radical content of above-mentioned hydroxy-terminated polysiloxane is 0.3 ~ 1.5%。
The organic tin catalyst of above-mentioned comparative example 1 is dibutyl tin dilaurate, the organic tin catalyst of comparative example 2 For tin dilaurate dioctyl tin, the organic tin catalyst of comparative example 3 is stannous octoate.
Above-mentioned organic solvent is the mixture of ethyl acetate and dimethylbenzene, and the volume ratio of above-mentioned ethyl acetate and dimethylbenzene is 1:2。
The high-heat-conductivity glue adhesion coating performance of thermally conductive one-faced tapes made from above-described embodiment 1 ~ 4 and comparative example 1 ~ 3 such as 3 institute of table Show:
Table 3
As shown in the evaluation result of table 3, the glue-line of the thermostable heat-conductive one-faced tapes of various embodiments of the present invention preparation is either led Hot property or heat aging property, are all significantly better than each comparative example, and one-faced tapes obtained can be for a long time in higher temperature Lower work, adhesive property weaken without obvious at high temperature, effectively prevent the case where falling off after adhesive tape is heated for a long time.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (6)

1. a kind of preparation method of thermostable heat-conductive one-faced tapes, it is characterised in that: the thermostable heat-conductive one-faced tapes include The one side of metal foil layer (2), this metal foil layer (2) is coated with an insulating coating (1), and the another side of metal foil layer (2) is provided with One high-heat-conductivity glue adhesion coating (3), a release film layer (4) are covered on the high-heat-conductivity glue adhesion coating (3) opposite to each other in the one of metal foil layer (2) Face;
The preparation methods of the thermostable heat-conductive one-faced tapes the following steps are included:
S1. by 30 ~ 40 parts of hydroxy-terminated polysiloxane, 8 ~ 15 parts of epoxy resin, 35 ~ 50 parts of MQ resin, tetraethoxysilane 3 ~ 8 0.3 ~ 2 part and 30 ~ 40 parts of organic solvent part, 4,4 '-two 0.5 ~ 5 part of (propyloxy phenyl base) diphenylamines, benzotriazole addition are anti- It answers in kettle, 0.05 ~ 1 part of the metatitanic acid tert-butyl ester and 0.1 ~ 3 part of organic tin catalyst is added after being warming up to 130 ~ 135 DEG C, 140 ~ It is reacted 2 ~ 3 hours at 150 DEG C, silicone pressure sensitive glue is made after cooling;
S2. by 25 ~ 40 parts of graphene powder, 5 ~ 10 parts of nm-class boron nitride, 5 ~ 10 parts of 3- mercaptopropyltriethoxysilane, ethoxy 0.05 ~ 1 part of base acetylenic glycols and remaining organic solvent are added in stirred tank, and high speed dispersion 40 ~ 60 minutes, then will be made in S1 Silicone pressure sensitive glue be slowly added in stirred tank, stir 30 ~ 40 points, be made high-heat-conductivity glue stick;
S3. insulating coating (1) is set in the coated on one side of metal foil layer (2), in the another side coating S2 of metal foil layer (2) High-heat-conductivity glue stick obtained dries, is formed by curing high-heat-conductivity glue adhesion coating (3);
S4. a release film layer (4) is covered on high-heat-conductivity glue adhesion coating (3) opposite to each other in the one side of metal foil layer (2), winding is made Obtain the thermostable heat-conductive one-faced tapes;
The number is parts by weight, uses the total amount of solvent for 55 ~ 70 parts by weight in S1 and S2.
2. the preparation method of thermostable heat-conductive one-faced tapes according to claim 1, it is characterised in that: the terminal hydroxy group is poly- The molecular weight of siloxanes is 20 ~ 300,000, and the hydroxy radical content of the hydroxy-terminated polysiloxane is 0.3 ~ 1.5%.
3. the preparation method of thermostable heat-conductive one-faced tapes according to claim 1, it is characterised in that: the organic tin Catalyst is in dibutyl tin dilaurate, tin dilaurate dioctyl tin, dibutyl tin dilaurate or stannous octoate It is at least one.
4. the preparation method of thermostable heat-conductive one-faced tapes according to claim 1, it is characterised in that: the organic solvent For the mixture of ethyl acetate and dimethylbenzene, the volume ratio of the ethyl acetate and dimethylbenzene is 1:2.
5. the preparation method of thermostable heat-conductive one-faced tapes according to claim 1, it is characterised in that: the metal foil layer (2) selected from one of copper foil, aluminium foil or tinfoil paper.
6. the preparation method of thermostable heat-conductive one-faced tapes according to claim 1, it is characterised in that: the high-heat-conductivity glue Adhesion coating (3) with a thickness of 5 ~ 20 μm.
CN201910103918.1A 2019-02-01 2019-02-01 The preparation method of thermostable heat-conductive one-faced tapes Pending CN109880545A (en)

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CN113214755A (en) * 2021-05-24 2021-08-06 深圳日高胶带新材料有限公司 Adhesive tape with high thermal conductivity coefficient and preparation method thereof
CN115104940A (en) * 2022-07-25 2022-09-27 陕西天柔华创电子科技有限公司 Heating toilet seat cushion and preparation process thereof
CN115710472A (en) * 2022-10-31 2023-02-24 福建友谊胶粘带集团有限公司 High-thermal-conductivity adhesive tape with good heat dissipation effect and preparation method thereof
CN117089291A (en) * 2023-10-09 2023-11-21 昆山汉品电子有限公司 Method for preparing high-temperature high-viscosity metal film by taking metal film as base material

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113214755A (en) * 2021-05-24 2021-08-06 深圳日高胶带新材料有限公司 Adhesive tape with high thermal conductivity coefficient and preparation method thereof
CN115104940A (en) * 2022-07-25 2022-09-27 陕西天柔华创电子科技有限公司 Heating toilet seat cushion and preparation process thereof
CN115104940B (en) * 2022-07-25 2023-09-01 陕西天柔华创电子科技有限公司 Heating toilet seat cushion and preparation process thereof
CN115710472A (en) * 2022-10-31 2023-02-24 福建友谊胶粘带集团有限公司 High-thermal-conductivity adhesive tape with good heat dissipation effect and preparation method thereof
CN115710472B (en) * 2022-10-31 2024-06-18 福建友谊胶粘带集团有限公司 High-heat-conductivity adhesive tape with good heat dissipation effect and preparation method thereof
CN117089291A (en) * 2023-10-09 2023-11-21 昆山汉品电子有限公司 Method for preparing high-temperature high-viscosity metal film by taking metal film as base material
CN118085682A (en) * 2023-10-09 2024-05-28 昆山汉品电子有限公司 Method for preparing high-temperature high-viscosity metal film by taking metal film as base material
CN118085682B (en) * 2023-10-09 2024-10-18 昆山汉品电子有限公司 Method for preparing high-temperature high-viscosity metal film by taking metal film as base material

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Application publication date: 20190614