CN103342896A - High temperature resistant heat-conducting silica gel sheet and preparation method thereof - Google Patents
High temperature resistant heat-conducting silica gel sheet and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high temperature resistant heat-conducting silica gel sheet and a preparation method thereof. The high temperature resistant heat-conducting silica gel sheet is characterized by comprising the following components in parts by weight: 50-80 parts of vinyl end capped polydimethylsiloxane (PDMS), 20-50 parts of vinyl end capped methyl phenyl silicone oil, 0.3-10 parts of containing hydrogen silicone oil, 2-6 parts of platinum catalyst, 0.2-0.6 parts of inhibitor, 5-100 parts of heat resistant additive and 400-1200 parts of heat-conducting powder. The preparation method of the high temperature resistant heat-conducting silica gel sheet comprises the following steps: firstly, uniformly mixing the vinyl end capped polydimethylsiloxane and the vinyl end capped methyl phenyl silicone oil in a kneading machine; adding the treated or untreated heat-conducting powder and the heat resistant additive which are added in batches, after mixing uniformly, adding the containing hydrogen silicone oil, the inhibitor and the catalyst; and mixing uniformly, and heating and solidifying in a forming machine to form a sheet. The heat resistant silica gel sheet provided by the invention is aged at 250 DEG C for 1000 hours, but still has good usability, and the changes of the hardness and the heat conductivity coefficient are within acceptable ranges.
Description
Technical field
The present invention relates to a kind of thermostable heat-conductive silica gel sheet, particularly used thermostable heat-conductive silica gel sheet in a kind of large-scale industrial equipments.
Background technology
Along with electronics and industrial equipments degree of integration are more and more higher, its thermal value is also increasing, particularly for some large-scale industrial equipments, the temperature that its accumulation of heat produces even surpass 250 ℃ for a long time, based on desirable requirement, the heat that equipment produces can scatter and disappear away as soon as possible, but these large-scale industrial equipmentss usually, the tolerance fit gap is bigger, and good heat conductivity, resistance toheat be good material also, is difficult to satisfy the requirement in big gap as graphite flake etc.So can satisfy the material of big gap heat transfer requirement still based on conducting strip.Thermal conductive silicon film resistance toheat is better, but existing thermal conductive silicon film on the market, its long-term heat resistance can only reach 160 ℃, and high also can only reach 200 ℃.A kind of long-term anti-more than 250 ℃ the conducting strip of high temperature then become a kind of urgent demand.
Summary of the invention
Purpose of the present invention just provides a kind of thermostable heat-conductive silica gel sheet, and this silica gel sheet is at 250 ℃, and 1000h is aging, still good usability can be arranged, and namely hardness, thermal conductivity change within the acceptable range.
The invention provides a kind of resistant to elevated temperatures thermal conductive silicon film, its component ratio is as follows:
The polydimethylsiloxane of ethenyl blocking: 50~80
The methyl phenyl silicone oil of ethenyl blocking: 20~50 parts
Containing hydrogen silicone oil: 0.3~10 part
Platinum catalyst: 2~6 parts
Inhibitor: 0.2~0.6 part
Heat-resisting additive: 5~100 parts
Heat conduction powder: 400~1200 parts
The polydimethylsiloxane of described ethenyl blocking, its viscosity are between 300~10000cps, between preferred 500~5000cps, more preferably between 500~2000cps.Viscosity is low, is beneficial to the filling of additive and heat conduction powder.When viscosity was lower than 300cps, the hardness that reduces conducting strip can compare difficulty.
At 2000~20000cps, contents of ethylene is between 2.5~5.5% (weight percents) in its viscosity for the methyl phenyl silicone oil of described ethenyl blocking, its viscosity, and phenyl content is between 10%~30%.The increase of phenyl content can improve the thermotolerance of final finished, but too high phenyl content can influence the consistency of the polydimethylsiloxane of itself and ethenyl blocking.
Described containing hydrogen silicone oil comprises a kind of side chain containing hydrogen silicone oil or side chain containing hydrogen silicone oil and the mixture of holding containing hydrogen silicone oil.Regulate the ratio of methyl phenyl silicone oil of polydimethylsiloxane, the ethenyl blocking of containing hydrogen silicone oil and ethenyl blocking, can regulate the thermal conductive silicon film of different hardness.
Described platinum catalyst is to make after the methyl phenyl silicone oil complexing with the polydimethylsiloxane of Platinic chloride and ethenyl blocking or ethenyl blocking.
Described inhibitor can be a kind of or their title complex in alkynol class, amide compound, the maleic acid ester compound.
Described heat-resisting additive can be aerosil, red iron oxide, iron oxide yellow, one or more in the carbon black.Preferred red iron oxide and carbon black.
Described heat conduction powder can be one or more the combination in aluminum oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, silicon nitride, silicon carbide, carbon fiber, the Graphene.Its shape can be sheet, needle-like, spherical.
The making method of thermostable heat-conductive silica gel sheet of the present invention:
Earlier the polydimethylsiloxane of ethenyl blocking and the methyl phenyl silicone oil of ethenyl blocking are mixed in kneader, add that adding was in batches handled or untreated heat conduction powder and heat-resisting additive, can heat also in the mixing process and can not heat, after treating that it mixes, at room temperature add containing hydrogen silicone oil, inhibitor, catalyzer successively.Mix and to obtain plastic sizing material.Thermofixation becomes sheet material in shaper.
In actual production, can also add fire retardant and reach the fire-retardant purpose of conducting strip, fire retardant commonly used comprises aluminium hydroxide, magnesium hydroxide, titanium oxide etc.
In actual production, can also use coupling agent to carry out the surface treatment of heat conduction powder to improve the addition of heat conduction powder in silicone oil, coupling agent commonly used comprises γ-(2,3-epoxy, third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxy silane, vinyltriethoxysilane, octyl group trimethoxy silicone oil etc.
In actual production, can use mixing equipment such as planetary mixer, kneader to carry out the mixing of sizing material, then use rolling press or vulcanizing press, form, and thermofixation.
Testing method:
With the conducting strip after the moulding, conducting strip is the aluminium sheet of surfacing up and down, puts into thermostatic drying chamber, and 250 ℃ are aging, respectively at 100h, and 200h, 500h, 750h takes out its hardness of partial test during 1000h and thermal resistance changes.
The testing method of hardness is with reference to " ASTM D2240-2005 rubber hardness testing standard "
The testing method of thermal resistance is with reference to " ASTM D5470-2006 thermal conduction solid electrical isolation thin material heat-conductive characteristic testing method (10.02) "
The invention beneficial effect:
High temperature resistant silicon film provided by the invention after 1000h is aging, still can have good usability at 250 ℃, and namely hardness, thermal conductivity change within the acceptable range.
Specific embodiment
The preparation of heat conduction sizing material
The polydimethylsiloxane of the ethenyl blocking of specified amount and the methyl phenyl silicone oil of ethenyl blocking are added in the planetary mixer, mix, then divide auxiliary agents such as adding heat conduction powder and heat-resisting additive, coupling agent for three times to stir, temperature is risen to 150 ℃ simultaneously, stir begin after 3 hours the cooling.At room temperature add containing hydrogen silicone oil, inhibitor successively.After stirring, standby.
Be shaped
Use two rod rolling presss or multi-rolling mill, the sizing material for preparing is put on the PET that scribbles parting agent, the upper strata also is covered with the PET that scribbles parting agent simultaneously, is calendered to the thickness of requirement, adds baking shaping in the heat tunnel in separate type or integral type.
Utilize different ingredients to carry out the preparation of thermostable heat-conductive silica gel sheet and respectively at 100h, 200h, 500h, 750h takes out its hardness of partial test during 1000h and thermal resistance changes.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (10)
1. thermostable heat-conductive silica gel sheet and preparation method thereof is characterized in that component ratio is as follows:
20~50 parts of the methyl phenyl silicone oils of 50~80 parts of the polydimethylsiloxanes of ethenyl blocking, ethenyl blocking, 0.3~10 part of containing hydrogen silicone oil, 2~6 parts of platinum catalysts, 0.2~0.6 part in inhibitor, 5~100 parts of heat-resisting additives, heat conduction powder: 400~1200 parts.
2. resistant to elevated temperatures thermal conductive silicon film according to claim 1 is characterized in that the polydimethylsiloxane of described ethenyl blocking, and its viscosity is at 300~10000cps.
3. resistant to elevated temperatures thermal conductive silicon film according to claim 1, the methyl phenyl silicone oil that it is characterized in that described ethenyl blocking, at 2000~20000cps, contents of ethylene is 2.5~5.5% in its viscosity for its viscosity, and phenyl content is between 10%~30%.
4. resistant to elevated temperatures thermal conductive silicon film according to claim 1 is characterized in that described containing hydrogen silicone oil comprises a kind of side chain containing hydrogen silicone oil or side chain containing hydrogen silicone oil and the mixture of holding containing hydrogen silicone oil.
5. resistant to elevated temperatures thermal conductive silicon film according to claim 1 is characterized in that described platinum catalyst is to make after the methyl phenyl silicone oil complexing with the polydimethylsiloxane of Platinic chloride and ethenyl blocking or ethenyl blocking;
Described resistant to elevated temperatures thermal conductive silicon film is characterized in that described inhibitor can be a kind of or their title complex in alkynol class, amide compound, the maleic acid ester compound.
6. resistant to elevated temperatures thermal conductive silicon film according to claim 1 is characterized in that described heat-resisting additive can be aerosil, red iron oxide, iron oxide yellow, one or more in the carbon black;
Described heat conduction powder can be one or more the combination in aluminum oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, silicon nitride, silicon carbide, carbon fiber, the Graphene, and its shape can be sheet, needle-like, spherical.
7. the preparation method of resistant to elevated temperatures thermal conductive silicon film according to claim 1 is characterized in that comprising following steps: earlier the polydimethylsiloxane of ethenyl blocking and the methyl phenyl silicone oil of ethenyl blocking are mixed in kneader; Add that adding was in batches handled or untreated heat conduction powder and heat-resisting additive, can heat also in the mixing process and can not heat; After treating that it mixes, at room temperature add containing hydrogen silicone oil, inhibitor, catalyzer successively; Mix and to obtain plastic sizing material; Thermofixation becomes sheet material in shaper.
8. the preparation method of resistant to elevated temperatures thermal conductive silicon film according to claim 7 is characterized in that adding fire retardant and reaches the fire-retardant purpose of conducting strip, and described fire retardant is aluminium hydroxide, magnesium hydroxide or titanium oxide.
9. the preparation method of resistant to elevated temperatures thermal conductive silicon film according to claim 7, it is characterized in that using coupling agent to carry out the surface treatment of heat conduction powder to improve the addition of heat conduction powder in silicone oil, described coupling agent comprises γ-(2,3-epoxy, third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxy silane, vinyltriethoxysilane and octyl group trimethoxy silicone oil.
10. the preparation method of resistant to elevated temperatures thermal conductive silicon film according to claim 7, it is characterized in that in dispersion process, adding coupling agent or dispersion agent, coupling agent can be any one in the commercial coupling agent that can share with the platinum vulcanizer, and dispersion agent is fluorine-containing siloxanes.
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