CN103709757A - Insulating and heat-conducting silicone grease and preparation method thereof - Google Patents
Insulating and heat-conducting silicone grease and preparation method thereof Download PDFInfo
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Abstract
The invention discloses insulating and heat-conducting silicone grease. The insulating and heat-conducting silicone grease consists of the following raw materials in parts by weight: 10-40 parts of organic silicon oil, 50-80 parts of heat-conducting powder, 0.5-4 parts of a structure improver, 0.5-3 parts of rheological aid, 0.5-5 parts of a friction modifier and 0.1-2 parts of an antioxidant. The insulating and heat-conducting silicone grease prepared by the invention is excellent in heat-conducting performance and low in cost, and is widely applicable to heat radiators requiring effective cooling in the industry, such as heat transmission for a gap where a diode and a substrate (aluminum or copper plate) are in contact, and heat conduction and insulation of a rectifier, electric and the like.
Description
Technical field
The present invention relates to organosilicon material technical field, especially relate to a kind of heat-conducting silicone grease.
Background technology
Along with the lasting depth development of hyundai electronics industry, electronics requires microminiaturization, performance is strong, the life-span is long.The for example CPU in computer equipment, video card, its microminiaturized integrated level is higher, the heat radiation of element has been proposed to the requirement of intimate harshness.High power valve in industrial equipments, silicon controlled rectifier, be added with the electronic component of scatterer or radiator element etc., also require heat radiation to promote to increase the service life and stability.Some special occasions are as space vehicle, need to solve the problem that satellite equipment and mounting plate are shown in excessive temperature differentials of defending.
Heat-conducting silicone grease has excellent thermal conductivity and good electrical insulation properties, can within the scope of-50 ℃～+ 200 ℃, use, and nontoxic, tasteless, stable chemical performance, so be widely used at electric field.In above-mentioned device, because contact between interface not exclusively produces larger contact resistance, make hot-fluid transmission be subject to very big obstruction, cause the very large temperature difference in interface, when coat after insulating heat conductive silicon grease at these interfaces, can effectively fill up the spatial joint clearance of contact surface, thereby greatly reduce contact resistance, reduce the working temperature of electronic devices and components, improve reliability and prolongs life.
The Chinese patent of relevant heat-conducting silicone grease has CN1990819, CN1923944, CN1327025, CN101294067, CN102181271A, CN101429422.
The disclosed volatile solvent that consists of two kinds of organo-siloxanes with special construction, heat conductive filler and disperse two kinds of silicone oil of CN1990819 wherein, thermal conductivity >4.4W/mK, it is characterized in that using solvent that system viscosity is reduced and increases loading level, to reach high thermal conductivity coefficient.Disclosed two kinds of organohydrogensiloxanes, indium powder, platinum based catalyst, the addition reaction retarding agent of consisting of of CN1923944, is characterized in that providing the method for solidifying above composition, forms the thin cured product of excellent heat conductance.Disclosed methyl-silicone oil, glycerine, the aluminium nitride of consisting of of CN132705025, its thermal conductivity >1.5W/mK.Disclosed organic silicone oil, silane coupling agent, the different-grain diameter heat conduction powder of consisting of of CN101294067.It is characterized in that the composite of the surface treatment of heat conduction powder and large, medium and small different-grain diameter.The disclosed component of CN102181271A is methyl-silicone oil, Nano metal powder, heat conduction micro mist, tensio-active agent, it is characterized in that heat conduction powder used is the non-metallic material of metallic substance or conduction, application and high-power LED lamp heat radiation.CN101429422 is disclosed is by adding pretreated carbon nanotube, to improve the method for heat conductivity of heat-conduction silicone grease.
The research of above-mentioned heat-conducting silicone grease mainly concentrates in the realization of high thermal conductivity coefficient, and ignored the colloidal stability that should possess as a kind of non-Newtonian fluid, do not investigated the tremendous influence to thermal conductivity and coating property except base oil and external other auxiliary agents of conductive powder.
Summary of the invention
The problems referred to above that exist for prior art, the applicant provides a kind of insulating heat conductive silicon grease and preparation method thereof.Heat-conducting silicone grease prepared by the present invention has excellent heat conductivility, with low cost, is widely used in requiring in industry the heat abstractor of effective cooling, the heat transfer in the gap contacting with base material (aluminium, copper coin) as diode, rectifier and electric etc. heat conductive insulating.
Technical scheme of the present invention is as follows:
An insulating heat conductive silicon grease, is comprised of the raw material of following parts by weight:
Organic silicone oil: 10-40 part, heat conduction powder: 50-80 part, Structure Improvement agent: 0.5-4 part, auxiliary rheological agents: 0.5-3 part, friction improver: 0.5-5 part, oxidation inhibitor: 0.1-2 part.
The preparation method of above-mentioned insulating heat conductive silicon grease, its concrete steps are as follows:
(1) organic silicone oil 10-40 part, heat conduction powder 50-80 part, Structure Improvement agent 0.5-4 part, auxiliary rheological agents 0.5-3 part, friction improver 0.5-5 part, oxidation inhibitor 0.1-2 part are mixed to rear grinding;
(2) in the mixture obtaining to step (1), add 5～15 parts of organic silicone oils, be then warming up to 70-120 ℃, with gauze strainer, reflux and shear 1-2 hour, in this process, adjust denseness degassed, filter and package and get product.
Described organic silicone oil is at least one in dimethyl silicone oil, polymethylphenyl siloxane fluid, vinyl silicone oil, containing hydrogen silicone oil, hydroxy silicon oil, quaternary ammonium salt alkyl modified silicon oil.Further, described organosilicon oil viscosity is at least one in kinematic viscosity 10-1000cst or 6000-100000cst at 25 ℃.
Described heat conduction powder is at least one in zinc oxide, modified zinc oxide, ball-aluminium oxide, boron nitride, nano aluminium oxide, silica powder.Described Structure Improvement agent is at least one in aerosil, organobentonite, lithium 12-hydroxy stearate, tetrafluoroethylene, CuPc.
Described auxiliary rheological agents is at least one in the surface modifiers such as high molecular weight block copolymer solution, modified organic silicon oxygen alkane, acrylate flow agent.Further, described auxiliary rheological agents is at least one in BYK161, BYK323, BYK310, BYK340, BYK390.
Described friction improver is at least one in liquid phenenyl triazole fatty amine salt, tetrafluoroethylene, oil soluble polyethers, TriMethylolPropane(TMP), pentaerythritol ester.Described oxidation inhibitor is at least one in liquid diphenylmethane amine, di-iso-octyldiphenylamine, polymer liquefied phenol.
The method of optimizing is, in the preparation method of this insulating heat conductive silicon grease, after each feed composition is mixed in pallet by parts by weight separately, by three-roll grinder or colloidal mill dispersion treatment, the sample of handling well is proceeded in stainless steel still, and heat temperature raising, is refluxed and is sheared 1-2 hour by copper wire gauze after being raised to 70-120 ℃, change the arrangement mode of powder, improve loading level.In this process, adjust denseness degassed, filter and package and get product.
The technique effect that the present invention is useful is:
The present invention is the universal industrial heat radiation product in 1.0W/mK left and right as thermal conductivity, by adding structural stabilizing agent, improved the colloidal stability of heat-conducting silicone grease, make it there is low-down minute oily and higher breakdown point, by adding friction improver, increased contacting of heat-conducting silicone grease and radiating surface, coating and heat conductivility have been improved, after grinding by three rollers, copper wire gauze refluxes and shears, and has improved heat conduction powder loading level, has strengthened the stability of heat-conducting silicone grease when guaranteeing heat conductivility.
Silicone oil in the present invention is mixed by one or more different structures, different viscosity, through silane coupling agent, coated modification has promoted loading level to heat conduction powder, structure and auxiliary rheological agents have improved the colloid stability of heat-conducting silicone grease, and friction improver has strengthened coating and heat conductivility.
Insulating heat conductive silicon grease prepared by this law has extremely low minute oil mass, outstanding colloidal stability, have good coating and oilness, thereby improved heat conductivility, simultaneously by the research to aftertreatment technology, improved the loading level of heat conduction powder, effectively controlled material cost, cost performance is high.This product thermal conductivity >0.9W/mK, volume specific resistance >1.0 * 10
14Ω cm
3.
Embodiment
Embodiment 1:
10 parts of 25 ℃ of polymethylphenyl siloxane fluids that kinematic viscosity is 500cst, 10 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 60000cst, 40 parts of modified zinc oxides, 25 parts of ball-aluminium oxides, 1 part of aerosil, 1 part of tetrafluoroethylene, 0.5 part of BYK310, 0.2 part of L135, 0.3 part of L57 mixes by three-roll grinder and grinds three times, then proceed to stainless steel still, add 12 parts of 25 ℃ of polymethylphenyl siloxane fluids that kinematic viscosity is 500cst, be warming up to 110 ℃ of insulations, filtering net fills 120 order copper wire gauze backflows and shears 1 hour, shear pressure 0.04MPa, with pump, after degassed 30 minutes, pack and get product.Physical and chemical index is in Table 1.
Embodiment 2:
15 parts of 25 ℃ of polymethylphenyl siloxane fluids that kinematic viscosity is 1000cst, 15 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 60000cst, 45 parts of modified zinc oxides, 10 parts of boron nitride, 2 parts of aerosils, 1.5 parts of liquid phenenyl triazole fatty amine salts, 1 part of BYK161, 0.3 part of L135, 0.2 part of L01 mixes by three-roll grinder and grinds three times, then proceed to stainless steel still, add 10 parts of 25 ℃ of polymethylphenyl siloxane fluids that kinematic viscosity is 500cst, be warming up to 90 ℃ of insulations, filtering net fills 120 order copper wire gauze backflows and shears 1 hour, shear pressure 0.04MPa, with pump, after degassed 30 minutes, pack and get product.Physical and chemical index is in Table 1.
Embodiment 3:
15 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 100cst, 15 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 60000cst, 30 parts of ball-aluminium oxides, 20 parts of boron nitride, 10 parts of nano aluminium oxides, 2 parts of tetrafluoroethylene, 2 parts of organobentonites, 0.5 part of BYK390, 0.2 part of L135, 0.3 part of L57 mixes by three-roll grinder and grinds three times, then proceed to stainless steel still, add 5 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 60000cst, be warming up to 90 ℃ of insulations, filtering net fills 120 order copper wire gauze backflows and shears 1 hour, shear pressure 0.04MPa, with pump, after degassed 30 minutes, pack and get product.Physical and chemical index is in Table 1.
Embodiment 4:
10 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 350cst, 5 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 10000cst, 75 parts of modified zinc oxides, 3 parts of aerosils, 0.5 part of tetrafluoroethylene, 0.5 part of BYK161, 0.5 part of BYK390, 0.2 part of L135, 0.3 part of L57 mixes by three-roll grinder and grinds three times, then proceed to stainless steel still, add 5 parts of 25 ℃ of dimethyl silicone oils that kinematic viscosity is 350cst, be warming up to 90 ℃ of insulations, filtering net fills 120 order copper wire gauze backflows and shears 1 hour, shear pressure 0.04MPa, with pump, after degassed 30 minutes, pack and get product.Physical and chemical index is in Table 1.
L135 in above-described embodiment 1～4 is liquid macroimolecule phenol, and L57 is that liquid diphenylmethane amine, L01 are di-iso-octyldiphenylamine.
Comparative example:
By the JFG-21(Yantai generation victory conductive paste of selling on market) and G746(Japan chemical company of SHIN-ETSU HANTOTAI) model heat-conducting silicone grease as a comparison case, it is carried out to physicochemical property detection, detection data are as shown in table 1.
Table 1
As can be seen from Table 1, the mean coefficient of heat conductivity of heat-conducting silicone grease prepared by the present invention is greater than currently available products, and vaporization losses is less than currently available products, and average-volume resistance is greater than currently available products, and the performance of insulation and heat conduction is very superior.Meanwhile, Stencil oil-dividing of the present invention and wear scar diameter are all less than comparative example, illustrate that Structure Improvement agent of the present invention has improved Stencil oil-dividing, and friction improver has improved wear scar diameter, and the temperature of colloidal structure is very good with friction coating.
Claims (10)
1. an insulating heat conductive silicon grease, is characterized in that being comprised of the raw material of following parts by weight:
Organic silicone oil: 10-40 part
Heat conduction powder: 50-80 part
Structure Improvement agent: 0.5-4 part
Auxiliary rheological agents: 0.5-3 part
Friction improver: 0.5-5 part
Oxidation inhibitor: 0.1-2 part.
2. a preparation method for insulating heat conductive silicon grease claimed in claim 1, is characterized in that concrete steps are as follows:
(1) organic silicone oil 10-40 part, heat conduction powder 50-80 part, Structure Improvement agent 0.5-4 part, auxiliary rheological agents 0.5-3 part, friction improver 0.5-5 part, oxidation inhibitor 0.1-2 part are mixed to rear grinding;
(2) in the mixture obtaining to step (1), add 5～15 parts of organic silicone oils, be warming up to 70-120 ℃, with gauze strainer, reflux and shear 1-2 hour, degassed, filter and package and get product.
3. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described organic silicone oil is at least one in dimethyl silicone oil, polymethylphenyl siloxane fluid, vinyl silicone oil, containing hydrogen silicone oil, hydroxy silicon oil, quaternary ammonium salt alkyl modified silicon oil.
4. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described organosilicon oil viscosity is at least one in kinematic viscosity 10-1000cst or 6000-100000cst at 25 ℃.
5. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described heat conduction powder is at least one in zinc oxide, modified zinc oxide, ball-aluminium oxide, boron nitride, nano aluminium oxide, silica powder.
6. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described Structure Improvement agent is at least one in aerosil, organobentonite, lithium 12-hydroxy stearate, tetrafluoroethylene, CuPc.
7. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described auxiliary rheological agents is at least one in the surface modifiers such as high molecular weight block copolymer solution, modified organic silicon oxygen alkane, acrylate flow agent.
8. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described auxiliary rheological agents is at least one in BYK161, BYK323, BYK310, BYK340, BYK390.
9. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described friction improver is at least one in liquid phenenyl triazole fatty amine salt, tetrafluoroethylene, oil soluble polyethers, TriMethylolPropane(TMP), pentaerythritol ester.
10. insulating heat conductive silicon grease according to claim 1 and 2 and preparation method thereof, is characterized in that: described oxidation inhibitor is at least one in liquid diphenylmethane amine, di-iso-octyldiphenylamine, polymer liquefied phenol.
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Cited By (24)
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| CN104263315A (en) * | 2014-09-28 | 2015-01-07 | 浙江时间新材料有限公司 | Acidic and transparent silicone weather-resistant sealant for construction |
| CN104387963A (en) * | 2014-12-08 | 2015-03-04 | 江苏诺飞新材料科技有限公司 | Surface dustproof coating of cell panel |
| CN104726186A (en) * | 2015-03-31 | 2015-06-24 | 中山大学 | Graphene organic silicone lubricating grease and preparation method thereof |
| CN105140137A (en) * | 2015-07-30 | 2015-12-09 | 常州银河世纪微电子有限公司 | Molding process of diode |
| CN105487625A (en) * | 2015-11-26 | 2016-04-13 | 国家电网公司 | Dampproof and dustproof computer CPU cooling fan |
| CN105860531A (en) * | 2016-05-31 | 2016-08-17 | 刘雷 | Processor heat-conduction and anti-ageing material for computer and preparation method of material |
| CN108976802A (en) * | 2018-07-11 | 2018-12-11 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of heat conductive insulating silicone grease |
| US10155894B2 (en) | 2014-07-07 | 2018-12-18 | Honeywell International Inc. | Thermal interface material with ion scavenger |
| US10174433B2 (en) | 2013-12-05 | 2019-01-08 | Honeywell International Inc. | Stannous methanesulfonate solution with adjusted pH |
| US10287471B2 (en) | 2014-12-05 | 2019-05-14 | Honeywell International Inc. | High performance thermal interface materials with low thermal impedance |
| CN109797027A (en) * | 2019-01-22 | 2019-05-24 | 东莞市港田高分子材料有限公司 | A kind of High Performance Insulation lubricating grease and preparation method thereof |
| US10312177B2 (en) | 2015-11-17 | 2019-06-04 | Honeywell International Inc. | Thermal interface materials including a coloring agent |
| US10428256B2 (en) | 2017-10-23 | 2019-10-01 | Honeywell International Inc. | Releasable thermal gel |
| US10501671B2 (en) | 2016-07-26 | 2019-12-10 | Honeywell International Inc. | Gel-type thermal interface material |
| CN111534358A (en) * | 2020-05-09 | 2020-08-14 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
| US10781349B2 (en) | 2016-03-08 | 2020-09-22 | Honeywell International Inc. | Thermal interface material including crosslinker and multiple fillers |
| CN112724677A (en) * | 2020-12-29 | 2021-04-30 | 中山大学 | Dopamine modified boron nitride heat-conducting silicone grease and preparation method thereof |
| US11041103B2 (en) | 2017-09-08 | 2021-06-22 | Honeywell International Inc. | Silicone-free thermal gel |
| US11072706B2 (en) | 2018-02-15 | 2021-07-27 | Honeywell International Inc. | Gel-type thermal interface material |
| CN113717529A (en) * | 2021-08-25 | 2021-11-30 | 广州汇纳新材料科技有限公司 | Heat-conducting silicone grease with gradually increased heat-conducting coefficient and preparation method thereof |
| CN114276790A (en) * | 2022-01-26 | 2022-04-05 | 江西宏柏新材料股份有限公司 | Preparation method of insulating high-thermal-conductivity silicone grease |
| US11373921B2 (en) | 2019-04-23 | 2022-06-28 | Honeywell International Inc. | Gel-type thermal interface material with low pre-curing viscosity and elastic properties post-curing |
| CN114957996A (en) * | 2022-05-17 | 2022-08-30 | 北京科技大学广州新材料研究院 | Flexible silicon rubber substrate with high thermal conductivity and preparation method thereof |
| WO2023197698A1 (en) * | 2022-04-14 | 2023-10-19 | 华南理工大学 | Heat-conduction-enhanced phase-change nanocapsule composite material, and preparation method therefor and use thereof |
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| US10174433B2 (en) | 2013-12-05 | 2019-01-08 | Honeywell International Inc. | Stannous methanesulfonate solution with adjusted pH |
| US10155894B2 (en) | 2014-07-07 | 2018-12-18 | Honeywell International Inc. | Thermal interface material with ion scavenger |
| US10428257B2 (en) | 2014-07-07 | 2019-10-01 | Honeywell International Inc. | Thermal interface material with ion scavenger |
| CN104263315B (en) * | 2014-09-28 | 2016-01-27 | 浙江时间新材料有限公司 | A kind of acid transparent silicone weather proofing sealant for building |
| CN104263315A (en) * | 2014-09-28 | 2015-01-07 | 浙江时间新材料有限公司 | Acidic and transparent silicone weather-resistant sealant for construction |
| US10287471B2 (en) | 2014-12-05 | 2019-05-14 | Honeywell International Inc. | High performance thermal interface materials with low thermal impedance |
| CN104387963A (en) * | 2014-12-08 | 2015-03-04 | 江苏诺飞新材料科技有限公司 | Surface dustproof coating of cell panel |
| CN104726186A (en) * | 2015-03-31 | 2015-06-24 | 中山大学 | Graphene organic silicone lubricating grease and preparation method thereof |
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| US10781349B2 (en) | 2016-03-08 | 2020-09-22 | Honeywell International Inc. | Thermal interface material including crosslinker and multiple fillers |
| CN105860531A (en) * | 2016-05-31 | 2016-08-17 | 刘雷 | Processor heat-conduction and anti-ageing material for computer and preparation method of material |
| US10501671B2 (en) | 2016-07-26 | 2019-12-10 | Honeywell International Inc. | Gel-type thermal interface material |
| US11041103B2 (en) | 2017-09-08 | 2021-06-22 | Honeywell International Inc. | Silicone-free thermal gel |
| US10428256B2 (en) | 2017-10-23 | 2019-10-01 | Honeywell International Inc. | Releasable thermal gel |
| US11072706B2 (en) | 2018-02-15 | 2021-07-27 | Honeywell International Inc. | Gel-type thermal interface material |
| CN108976802B (en) * | 2018-07-11 | 2020-12-11 | 江苏科兴电器有限公司 | Preparation method of heat-conducting insulating silicone grease |
| CN108976802A (en) * | 2018-07-11 | 2018-12-11 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of heat conductive insulating silicone grease |
| CN109797027A (en) * | 2019-01-22 | 2019-05-24 | 东莞市港田高分子材料有限公司 | A kind of High Performance Insulation lubricating grease and preparation method thereof |
| CN109797027B (en) * | 2019-01-22 | 2021-11-09 | 东莞市港田高分子材料有限公司 | High-performance insulating lubricating grease and preparation method thereof |
| US11373921B2 (en) | 2019-04-23 | 2022-06-28 | Honeywell International Inc. | Gel-type thermal interface material with low pre-curing viscosity and elastic properties post-curing |
| CN111534358A (en) * | 2020-05-09 | 2020-08-14 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
| CN111534358B (en) * | 2020-05-09 | 2022-03-29 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
| CN112724677A (en) * | 2020-12-29 | 2021-04-30 | 中山大学 | Dopamine modified boron nitride heat-conducting silicone grease and preparation method thereof |
| CN113717529A (en) * | 2021-08-25 | 2021-11-30 | 广州汇纳新材料科技有限公司 | Heat-conducting silicone grease with gradually increased heat-conducting coefficient and preparation method thereof |
| CN114276790A (en) * | 2022-01-26 | 2022-04-05 | 江西宏柏新材料股份有限公司 | Preparation method of insulating high-thermal-conductivity silicone grease |
| WO2023197698A1 (en) * | 2022-04-14 | 2023-10-19 | 华南理工大学 | Heat-conduction-enhanced phase-change nanocapsule composite material, and preparation method therefor and use thereof |
| CN114957996A (en) * | 2022-05-17 | 2022-08-30 | 北京科技大学广州新材料研究院 | Flexible silicon rubber substrate with high thermal conductivity and preparation method thereof |
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Application publication date: 20140409 |