CN111171578B - High-strength heat-conducting silica gel sheet and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-strength heat-conducting silica gel sheet and a preparation method thereof, belonging to the technical field of heat-conducting materials, and the preparation method comprises the following preparation steps: (1) taking heat-conducting powder, dividing the heat-conducting powder into two parts, and grinding the two parts respectively; (2) adding methyl vinyl silicone rubber into a mixing roll, wrapping the roll, sequentially adding two parts of heat-conducting powder and nano active calcium carbonate, and mixing; (3) adding silicone oil, a vulcanizing agent, hydrogen-terminated polydimethylsiloxane, polymethylhydrosiloxane and a vinyl platinum complex catalyst into a mixing roll, mixing, and thinly passing through a lower sheet to prepare a rubber compound; (4) the high-strength heat-conducting silica gel sheet has the advantages that the preparation method is simple, the prepared heat-conducting silica gel sheet has good hardness, tensile strength and tearing strength, good high-temperature resistance and moisture resistance, high strength and is beneficial to long-term use of the heat-conducting silica gel sheet.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a high-strength heat conduction silica gel sheet and a preparation method thereof.
Background
The heat-conducting silica gel sheet is a heat-conducting medium material synthesized by a special process, which is also called a heat-conducting silica gel pad, a heat-conducting silica gel sheet, a soft heat-conducting pad, a heat-conducting silica gel gasket and the like in the industry, is specially produced by a design scheme of utilizing gaps to transfer heat, can fill the gaps, and can open a heat channel between a heating part and a heat dissipation part to effectively improve the heat transfer efficiency, simultaneously has the functions of insulation, shock absorption, sealing and the like, can meet the design requirements of equipment miniaturization and ultra-thinness, and has the advantages of manufacturability and usability, wide thickness application range and excellent heat-conducting filling material. The material is used for a control main board of an electronic and electric product, a base plate and a foot pad inside and outside the motor, an electronic and electric product, automobile machinery, a computer host, a notebook computer, a DVD, a VCD and any material needing filling and heat dissipation modules.
Currently, silicone rubber is often used as a sizing material for a thermally conductive silicone sheet, but the thermal conductivity of silicone rubber is low, generally 0.2W (m.K)-1And the silicone rubber can age under the environment of high temperature and high humidity, which causes degradation and damage of a cross-linked network, and the hardness and tensile strength of the aged silicone rubber are reduced, and the tear strength of the silicone rubber is required to be improved.
Based on the above, the invention designs a high-strength heat-conducting silica gel sheet and a preparation method thereof, so as to solve the above problems.
Disclosure of Invention
The invention aims to provide a high-strength heat-conducting silica gel sheet and a preparation method thereof, and aims to solve the problems that the heat conductivity of the heat-conducting silica gel sheet made of silicon rubber is low, the silicon rubber is aged in a high-temperature and high-humidity environment to cause degradation and damage of a cross-linked network of the silicon rubber, the hardness and the tensile strength of the aged silicon rubber are reduced, and the tear strength of the silicon rubber needs to be improved.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-strength heat-conducting silica gel sheet comprises the following preparation steps:
(1) taking 80-100 parts of heat-conducting powder, and mixing the heat-conducting powder according to a mass ratio of 3: 2-2.5, grinding a larger part of the heat-conducting powder into particles with the particle size of 20-40um, and grinding a smaller part of the heat-conducting powder into particles with the particle size of 3-5 um;
(2) adding 100-120 parts of methyl vinyl silicone rubber into a mixing roll, sequentially adding the two parts of heat-conducting powder ground in the step (1) and 40-60 parts of nano active calcium carbonate after roll wrapping, and mixing for 20-30 min;
(3) then adding 10-30 parts of silicone oil, 2-5 parts of vulcanizing agent, 1-10 parts of hydrogen-terminated polydimethylsiloxane, 0.1-1 part of polymethylhydrosiloxane and 0.1-1 part of vinyl platinum complex catalyst into a mixing roll, mixing for 10-15min, and thinly passing through a lower sheet to prepare rubber compound;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 160-170 ℃, the vulcanization pressure is 6-10Mpa, and the vulcanization time is 10-30 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
According to the preparation method of the high-strength heat-conducting silica gel sheet, disclosed by the invention, further, the heat-conducting powder is zinc oxide, aluminum nitride, silicon carbide, silicon nitride or boron nitride.
According to the preparation method of the high-strength heat-conducting silica gel sheet, the silicone oil is hydroxyl silicone oil or dimethyl silicone oil.
The preparation method of the high-strength heat-conducting silica gel sheet further comprises the step of preparing the nano activated calcium carbonate with the specific surface area of 16m2Per g, the particle size is 40-70 nm.
The preparation method of the high-strength heat-conducting silica gel sheet further comprises the step of adopting a double-roller mixing mill by the mixing mill, wherein the roller temperature is 30-40 ℃, and the roller spacing is 2-3 mm.
In the preparation method of the high-strength heat-conducting silica gel sheet, the vulcanizing agent is one of dicumyl peroxide, benzoyl peroxide, 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and 2, 4-dichlorobenzoyl peroxide.
The invention also provides a high-strength heat-conducting silica gel sheet which is prepared by adopting the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the heat-conducting powder is divided into two parts with different particle sizes, wherein the heat-conducting powder is stacked in the silicon rubber and contacted with each other, so that the thermal resistance is reduced, heat can be rapidly conducted among the heat-conducting particles, the heat conductivity of the silicon rubber is improved, in addition, small particles can effectively enter large particle gaps, so that contact points among the heat-conducting particles are increased, more secret stacking is formed in the silicon rubber, the density of a heat-conducting network chain is effectively increased, the heat conductivity of the silicon rubber is further improved, and meanwhile, the mechanical property of the silicon rubber is effectively improved;
decomposing the vulcanizing agent at high temperature to generate free radicals and initiate crosslinking vulcanization of the vinyl groups of the silicone rubber; both ends of a methyl vinyl silicone rubber molecular chain are provided with a certain amount of vinyl, and hydrogen-terminated polydimethylsiloxane and polymethylhydrosiloxane are used as cross-linking agents, so that the molecular chain of the silicone rubber can be multiplied during cross-linking, and meanwhile, the bridge bonds among molecular chains can be increased, so that the flexibility and the physical and mechanical properties of the silicone rubber network structure are obviously improved, and the tearing strength of the silicone rubber is effectively improved by compounding the hydrogen-terminated polydimethylsiloxane and the polymethylhydrosiloxane;
the nano active calcium carbonate is added as a reinforcing filler, wherein the specific surface area of the nano active calcium carbonate is 16m2The particle size is 40-70nm, and the hydrophobicity of the nano active calcium carbonate is utilized to be beneficial to improving the thixotropy of the silicon rubber, so that the silicon rubber has good comprehensive mechanical property and high temperature and high humidity resistance, the hardness and tensile strength of the silicon rubber are improved, and the humidity and heat resistance and aging resistance of the silicon rubber are improved;
the preparation method of the high-strength heat-conducting silica gel sheet is simple, and the prepared heat-conducting silica gel sheet has good hardness, tensile strength and tearing strength, good high-temperature resistance and moisture resistance, high strength and is beneficial to long-term use of the heat-conducting silica gel sheet.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a high-strength heat-conducting silica gel sheet is prepared by the following steps:
(1) taking 95 parts of alumina, and mixing the alumina according to a mass ratio of 3: 2, dividing the mixture into two parts, grinding a larger part of alumina into particles with the particle size of 25-30um, and grinding a smaller part of alumina into particles with the particle size of 3-5 um;
(2) adding 105 parts of methyl vinyl silicone rubber into a double-roll mixing mill, wherein the roll temperature is 35 ℃, the roll distance is 3mm, and after wrapping the rolls, sequentially adding the two parts of alumina ground in the step (1) and 55 parts of nano activated calcium carbonate, and mixing for 25 min;
(3) then adding 10 parts of simethicone, 4 parts of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 7 parts of hydrogen-terminated polydimethylsiloxane, 0.5 part of polymethylhydrosiloxane and 0.2 part of vinyl platinum complex catalyst into a mixing roll, mixing for 10min, and thinly passing through and discharging to obtain rubber compound;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 163 ℃, the vulcanization pressure is 7Mpa, and the vulcanization time is 20 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
Wherein the specific surface area of the nano active calcium carbonate is 16m2Per g, the particle size is 40-70 nm.
Example 2:
a high-strength heat-conducting silica gel sheet is prepared by the following steps:
(1) taking 90 parts of zinc oxide, and mixing the zinc oxide with the following raw materials in a mass ratio of 3: 2.3 dividing into two parts, grinding a larger part of zinc oxide into particles with the particle size of 20-25um, and grinding a smaller part of zinc oxide into particles with the particle size of 3-4 um;
(2) adding 110 parts of methyl vinyl silicone rubber into a double-roll mixing mill, wherein the roll temperature is 40 ℃, the roll distance is 2mm, wrapping the rolls, sequentially adding the two parts of zinc oxide ground in the step (1) and 45 parts of nano activated calcium carbonate, and mixing for 23 min;
(3) adding 25 parts of hydroxyl silicone oil, 3 parts of dicumyl peroxide, 8 parts of hydrogen-terminated polydimethylsiloxane, 0.4 part of polymethylhydrosiloxane and 0.6 part of vinyl platinum complex catalyst into a mixing roll, mixing for 13min, and thinly passing through a lower sheet to obtain rubber compound;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 168 ℃, the vulcanization pressure is 8Mpa, and the vulcanization time is 18 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
Wherein the specific surface area of the nano active calcium carbonate is 16m2Per g, the particle size is 40-70 nm.
Example 3:
a high-strength heat-conducting silica gel sheet is prepared by the following steps:
(1) taking 80 parts of alumina, and mixing the alumina according to a mass ratio of 3: 2.5 dividing into two parts, grinding a larger part of alumina into 25-30um, and grinding a smaller part of alumina into 4-5 um;
(2) adding 100 parts of methyl vinyl silicone rubber into a double-roll mixing mill, wherein the roll temperature is 37 ℃, the roll distance is 3mm, and after wrapping the roll, sequentially adding the two parts of alumina ground in the step (1) and 60 parts of nano activated calcium carbonate, and mixing for 20 min;
(3) adding 22 parts of dimethyl silicone oil, 5 parts of benzoyl peroxide, 5 parts of hydrogen-terminated polydimethylsiloxane, 0.7 part of polymethylhydrosiloxane and 0.8 part of vinyl platinum complex catalyst into a mixing roll, mixing for 11min, and thinly passing through a sheet to obtain rubber compound;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 162 ℃, the vulcanization pressure is 10Mpa, and the vulcanization time is 10 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
Wherein the specific surface area of the nano active calcium carbonate is 16m2Per g, the particle size is 40-70 nm.
Example 4:
a high-strength heat-conducting silica gel sheet is prepared by the following steps:
(1) taking 100 parts of aluminum nitride, and mixing the aluminum nitride with the raw materials in a mass ratio of 3: 2.4 dividing into two parts, grinding a larger part of aluminum nitride into particles with the particle size of 30-35um, and grinding a smaller part of aluminum nitride into particles with the particle size of 3-5 um;
(2) adding 120 parts of methyl vinyl silicone rubber into a double-roll mixing mill, wherein the roll temperature is 32 ℃, the roll distance is 2mm, and after wrapping the rolls, sequentially adding the two parts of aluminum nitride ground in the step (1) and 40 parts of nano activated calcium carbonate, and mixing for 27 min;
(3) adding 27 parts of hydroxyl silicone oil, 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, 2 parts of hydrogen-terminated polydimethylsiloxane, 1 part of polymethylhydrosiloxane and 0.3 part of vinyl platinum complex catalyst into a mixing roll, mixing for 12min, and thinly passing through a lower sheet to prepare mixed rubber;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 165 ℃, the vulcanization pressure is 6Mpa, and the vulcanization time is 30 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
Wherein the specific surface area of the nano active calcium carbonate is 16m2Per g, the particle size is 40-70 nm.
Example 5:
a high-strength heat-conducting silica gel sheet is prepared by the following steps:
(1) taking 85 parts of silicon carbide, and mixing the silicon carbide according to a mass ratio of 3: 2, dividing the silicon carbide into two parts, grinding a larger part of the silicon carbide into particles with the particle size of 35-40um, and grinding a smaller part of the silicon carbide into particles with the particle size of 3-4 um;
(2) adding 115 parts of methyl vinyl silicone rubber into a double-roll mixing mill, wherein the roll temperature is 30 ℃, the roll distance is 3mm, wrapping the rolls, sequentially adding the two parts of silicon carbide ground in the step (1) and 47 parts of nano activated calcium carbonate, and mixing for 30 min;
(3) adding 15 parts of dimethyl silicone oil, 4 parts of 2, 4-dichlorobenzoyl peroxide, 1 part of hydrogen-terminated polydimethylsiloxane, 0.1 part of polymethylhydrosiloxane and 1 part of vinyl platinum complex catalyst into a mixing roll, mixing for 15min, and thinly passing through and discharging to obtain mixed rubber;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 170 ℃, the vulcanization pressure is 8Mpa, and the vulcanization time is 25 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
Wherein the specific surface area of the nano active calcium carbonate is 16m2Per g, the particle size is 40-70 nm.
Example 6:
a high-strength heat-conducting silica gel sheet is prepared by the following steps:
(1) taking 96 parts of silicon nitride, and mixing the silicon nitride with the raw materials in a mass ratio of 3: 2.2 dividing into two parts, grinding a larger part of silicon nitride into particles with the particle size of 30-35um, and grinding a smaller part of silicon nitride into particles with the particle size of 4-5 um;
(2) adding 113 parts of methyl vinyl silicone rubber into a double-roll mixing mill, wherein the roll temperature is 33 ℃, the roll distance is 2mm, wrapping the rolls, sequentially adding the two parts of silicon nitride ground in the step (1) and 50 parts of nano activated calcium carbonate, and mixing for 28 min;
(3) adding 24 parts of hydroxyl silicone oil, 3 parts of benzoyl peroxide, 10 parts of hydrogen-terminated polydimethylsiloxane, 0.2 part of polymethylhydrosiloxane and 0.1 part of vinyl platinum complex catalyst into a mixing roll, mixing for 14min, and thinly passing through a sheet to obtain rubber compound;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 160 ℃, the vulcanization pressure is 9Mpa, and the vulcanization time is 20 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
Wherein the specific surface area of the nano active calcium carbonate is 16m2Per g, the particle size is 40-70 nm.
The heat conductive silicone sheets obtained in examples 1 to 6 were taken, the heat conductivity was measured, they were stored at 85 ℃ under 85% relative humidity for 1000 hours, and the hardness, tensile strength and tear strength were measured before and after storage, to obtain table 1.
Table 1:
as can be seen from Table 1, the heat conductive silicone sheets obtained in examples 1 to 6 had good hardness, tensile strength and tear strength, and had thermal conductivities of 5.2 to 5.6W (m.K)-1After the double eighty-five test, the reduction of the hardness, the tensile strength and the tear strength is small.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (3)
1. The preparation method of the high-strength heat-conducting silica gel sheet is characterized by comprising the following preparation steps:
(1) taking 80-100 parts of heat-conducting powder, and mixing the heat-conducting powder according to a mass ratio of 3: 2-2.5, grinding a larger part of the heat-conducting powder into particles with the particle size of 20-40um, and grinding a smaller part of the heat-conducting powder into particles with the particle size of 3-5 um; the heat conducting powder is zinc oxide, aluminum nitride, silicon carbide, silicon nitride or boron nitride;
(2) adding 100-120 parts of methyl vinyl silicone rubber into a mixing roll, sequentially adding the two parts of heat-conducting powder ground in the step (1) and 40-60 parts of nano active calcium carbonate after roll wrapping, and mixing for 20-30 min; the specific surface area of the nano active calcium carbonate is 16m2Per g, the particle size is 40-70 nm;
(3) then adding 10-30 parts of silicone oil, 2-5 parts of vulcanizing agent, 1-10 parts of hydrogen-terminated polydimethylsiloxane, 0.1-1 part of polymethylhydrosiloxane and 0.1-1 part of vinyl platinum complex catalyst into a mixing roll, mixing for 10-15min, and thinly passing through a lower sheet to prepare rubber compound; the silicone oil is hydroxyl silicone oil or dimethyl silicone oil; the vulcanizing agent is one of dicumyl peroxide, benzoyl peroxide, 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and 2, 4-dichlorobenzoyl peroxide;
(4) placing the rubber compound into a mold, and vulcanizing on a flat vulcanizing machine, wherein the first-stage vulcanization comprises the following steps: the vulcanization temperature is 160-170 ℃, the vulcanization pressure is 6-10Mpa, and the vulcanization time is 10-30 min; secondary vulcanization: vulcanizing at 190 ℃ for 1h, vulcanizing at 250 ℃ for 2h, and cooling to obtain the heat-conducting silica gel sheet.
2. The preparation method of the high-strength heat-conducting silica gel sheet according to claim 1, wherein the preparation method comprises the following steps: the mixing roll adopts a double-roll mixing roll, the roll temperature is 30-40 ℃, and the roll distance is 2-3 mm.
3. A high-strength heat-conducting silica gel sheet prepared by the preparation method according to claim 1 or 2.
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| CN112646377A (en) * | 2020-12-24 | 2021-04-13 | 江门威富新材料科技有限公司 | Conductive silicone rubber for electromagnetic shielding and preparation method thereof |
| CN112831187A (en) * | 2021-01-28 | 2021-05-25 | 天津泽希新材料有限公司 | High-temperature vulcanized heat-conducting silicone rubber composite material |
| CN114736522A (en) * | 2022-05-24 | 2022-07-12 | 无锡市百合花胶粘剂厂有限公司 | High-heat-conductivity silica gel sheet and preparation method thereof |
| CN116063853A (en) * | 2023-01-31 | 2023-05-05 | 安徽迈腾新材料有限公司 | Platinum vulcanization type heat-conductive silicone rubber composite material |
| CN116120890B (en) * | 2023-02-23 | 2023-08-18 | 东莞市富颖电子材料有限公司 | Heat-conducting adhesive tape and preparation method thereof |
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| US6306957B1 (en) * | 1999-03-11 | 2001-10-23 | Shin-Etsu Chemical Co., Ltd. | Thermal conductive silicone rubber compositions and making method |
| JP2003080640A (en) * | 2001-09-12 | 2003-03-19 | Fuji Kobunshi Kogyo Kk | Heat-softened sheet |
| CN108659549A (en) * | 2018-05-30 | 2018-10-16 | 深圳市零度智控科技有限公司 | The preparation method and silica gel material of high thermal conductive silicon glue material |
| CN111073591A (en) * | 2019-12-13 | 2020-04-28 | 深圳市丰盛源科技有限公司 | Single-component room temperature curing liquid silicone rubber and preparation method thereof |
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