CN100526386C - preparation process of thermally conductive and electrically insulating silicone rubber composite material - Google Patents
preparation process of thermally conductive and electrically insulating silicone rubber composite material Download PDFInfo
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- CN100526386C CN100526386C CNB2007101033623A CN200710103362A CN100526386C CN 100526386 C CN100526386 C CN 100526386C CN B2007101033623 A CNB2007101033623 A CN B2007101033623A CN 200710103362 A CN200710103362 A CN 200710103362A CN 100526386 C CN100526386 C CN 100526386C
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- aluminum oxide
- silicone rubber
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- alumina
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Abstract
The present invention discloses preparation process of thermally conductive and electrically insulating silicone rubber composite material. The preparation process includes the following steps: 1. mixing tabular alumina and alcohol solution of polyglycol to prepare alumina slurry or powder; 2. mixing high temperature sulfurized silicone rubber, alumina slurry, hydroxyl silicone oil and vulcanizer in certain weight proportion; 3. sulfurizing and forming through molding at certain temperature to form required product; and 4. the secondary sulfurizing of the product in a forced air drying tank. The composite material of the present invention has raised thermal conductivity coefficient, high compatibility between alumina and silicone rubber, and low cost.
Description
Technical field
The present invention relates to the preparation method of thermally conductive and electrically insulating silicone rubber composite material.
Background technology
Heat conductive rubber is a class rubber-base composite material that stresses heat conductivility, and the raising of heat conductivility is accompanied by the optimization of heat dispersion usually.Heat radiation is of crucial importance to electronic product, and statistical information shows, 2 ℃ of the every risings of electronic devices and components temperature, its reliability decrease 10%; When the life-span in the time of 50 ℃ has only 25 ℃ 1/6.Heat conductive rubber needing in Aeronautics and Astronautics, electronics, the electric field to be widely used in the position of dispelling the heat and conducting heat, with industrial production and progress of science and technology, to its demands for higher performance, wish that it can play the effect of insulation, damping again for electronic devices and components provide safe and reliable heat radiation approach.Mostly heat conductive rubber is with silicon rubber to be matrix, is used to make the parts that contact with electrical and electronic component, and it both provided required snappiness of system and thermotolerance, the heat of system can be passed rapidly again.This miniaturization, densification and improve its precision and the life-span plays a key effect for the Aeronautics and Astronautics electronics.
Unfilled silicon rubber heat conductivility is very poor, and thermal conductivity generally has only 0.165W/ (mK), can improve its heat conductivility by filling heat conductive filler.At present more for the research of the high heat conduction room temperature vulcanized silicone rubber of filled-type, and the heat conductivility of high temperature vulcanized system is studied seldom.The mineral filler aspect mainly concentrates on fibrous and particulate filler, and less research laminal filler is to the compound system Effect on Performance.
Summary of the invention
The object of the invention is to provide the method that a kind of cost is low, prepare the silicon rubber composite material with high heat conductive insulating performance.
Concrete steps are as follows:
(1) tabular alumina with 50～600 mass parts mixes with the polyoxyethylene glycol spirituous solution that accounts for aluminum oxide quality 0.5～5%, makes alumina slurry or aluminum oxide dry powder;
(2) high-temperature silicon disulfide rubber of 100 mass parts, the slurry (or aluminum oxide dry powder) that contains 50～600 mass parts aluminum oxide, the vulcanizing agent that accounts for the hydroxy silicon oil of aluminum oxide quality 0～30% and account for aluminum oxide quality 0.5～2% are carried out proportioning on demand, mix;
(3) curing temperature is 100～180 ℃, and pressure 6～10MPa under curing time 5～120min condition, adopts the compression molding sulfidization molding, makes the product of respective shapes as required;
(4) sample after the one step cure moulding carries out post vulcanization in air dry oven, and the sulfuration system is specifically determined according to practical situation, promptly rises to 100～150 ℃ with 1 hour from normal temperature, and progressively heating up then reaches 200～250 ℃, keeps constant temperature 2～20 hours.
The tabular alumina mean particle size is between 70nm～5 μ m.The kind of vulcanizing agent and consumption are selected according to industrial practical situation.Polyoxyethylene glycol can be selected for use: PEG400, PEG1000, PEG1500, PEG6000, PEG10000, use separately or several being used.
Present method is different from the general method for preparing thermally conductive and electrically insulating silicone rubber, adopt tabular alumina slurry and high temperature silicon rubber mix, can make that tabular alumina is more uniform to be sprawled in the silicon rubber matrix, thereby form effective passage of heat, improve the thermal conductivity of matrix material.With cheap polyoxyethylene glycol is tensio-active agent, not only can strengthen the consistency of aluminum oxide and silicon rubber matrix, also can effectively reduce cost.
Embodiment
Embodiment 1:
(1) 2 gram median size is sheet α-Al of 250nm
2O
3Even with ethanolic soln (the containing 0.04 gram PEG6000) mixed grinding of polyoxyethylene glycol, make alumina slurry;
(2) 1 gram methyl vinyl silicone rubbers, 0.1 gram benzoyl peroxide, 0.3 gram hydroxy silicon oil and the alumina slurry mixed grinding of handling well are even;
(3) sizing material is placed to put into after 4 hours and is preheating to 125 ℃ mould, and matched moulds is forced into 6MPa, and heat-insulation pressure keeping 10min waits for that opening mould after the mold cools down to 90 ℃ takes out sample, and sample is the square sheet of 35mm * 35mm * 1mm;
(4) sample behind the one step cure is placed on the woven fiber glass, places the loft drier of air blast to rise to 150 ℃ through 1 hour from normal temperature, rises to 200 ℃ through 1 hour again, and 200 ℃ are incubated 2 hours down, treats baking oven cooling back taking-up sample;
(5) through UNITHERM
TMThe test of MODEL2022 type conductometer, the thermal conductivity of sample is 0.920W/ (mK).
Embodiment 2:
(1) 3 gram median size is sheet α-Al of 250nm
2O
3Even with ethanolic soln (the containing 0.06 gram PEG6000) mixed grinding of polyoxyethylene glycol, make alumina slurry;
(2) 1 gram methyl vinyl silicone rubbers, 0.1 gram benzoyl peroxide, 0.45 gram hydroxy silicon oil and the alumina slurry mixed grinding of handling well are even;
(3) sizing material is placed to put into after 4 hours and is preheating to 125 ℃ mould, and matched moulds is forced into 6MPa, and heat-insulation pressure keeping 10min waits for that opening mould after the mold cools down to 90 ℃ takes out sample, and sample is the square sheet of 35mm * 35mm * 1mm;
(4) sample behind the one step cure is placed on the woven fiber glass, places the loft drier of air blast to rise to 150 ℃ through 1 hour from normal temperature, rises to 200 ℃ through 1 hour again, and 200 ℃ are incubated 2 hours down, treats baking oven cooling back taking-up sample;
(5) through UNITHERM
TMThe test of MODEL2022 type conductometer, the thermal conductivity of sample is 1.971W/ (mK).
Embodiment 3:
(1) 2 gram median size is sheet α-Al of 250nm
2O
3Even with ethanolic soln (the containing 0.04 gram PEG6000) mixed grinding of polyoxyethylene glycol, the dry alumina powder that gets;
(2) 1 gram methyl vinyl silicone rubbers, 0.1 gram benzoyl peroxide, 0.3 gram hydroxy silicon oil and the alumina powder mixed grinding of handling well are even;
(3) sizing material is placed to put into after 4 hours and is preheating to 125 ℃ mould, and matched moulds is forced into 6MPa, and heat-insulation pressure keeping 10min waits for that opening mould after the mold cools down to 90 ℃ takes out sample, and sample is the square sheet of 35mm * 35mm * 1mm;
(4) sample behind the one step cure is placed on the woven fiber glass, places the loft drier of air blast to rise to 150 ℃ through 1 hour from normal temperature, rises to 200 ℃ through 1 hour again, and 200 ℃ are incubated 2 hours down, treats baking oven cooling back taking-up sample;
(5) through UNITHERM
TMThe test of MODEL2022 type conductometer, the thermal conductivity of sample is 0.890W/ (mK).
Embodiment 4:
(1) 20 gram median size is sheet α-Al of 250nm
2O
3Even with ethanolic soln (the containing 0.4 gram PEG6000) mixed grinding of polyoxyethylene glycol, the dry alumina powder that gets;
(2) 10 gram methyl vinyl silicone rubbers, 1 gram benzoyl peroxide, 3 gram hydroxy silicon oils and the alumina powder of handling well are mixing evenly;
(3) sizing material is placed to put into after 4 hours and is preheating to 125 ℃ mould, and matched moulds is forced into 6MPa, and heat-insulation pressure keeping 10min waits for that opening mould after the mold cools down to 90 ℃ takes out sample, and sample is the square sheet of 35mm * 35mm * 1mm;
(4) sample behind the one step cure is placed on the woven fiber glass, places the loft drier of air blast to rise to 150 ℃ through 1 hour from normal temperature, rises to 200 ℃ through 1 hour again, and 200 ℃ are incubated 2 hours down, treats baking oven cooling back taking-up sample;
(5) through UNITHERM
TMThe test of MODEL2022 type conductometer, the thermal conductivity of sample is 0.890W/ (mK).
Claims (1)
1. the preparation method of a thermally conductive and electrically insulating silicone rubber composite material is characterized in that concrete steps are:
(1) tabular alumina with 50～600 mass parts mixes with the polyoxyethylene glycol spirituous solution that accounts for aluminum oxide quality 0.5～5%, makes alumina slurry or aluminum oxide dry powder; Described tabular alumina mean particle size is 70nm～5 μ m;
(2) high-temperature silicon disulfide rubber of 100 mass parts, the slurry that contains 50～600 mass parts aluminum oxide or aluminum oxide dry powder, the vulcanizing agent that accounts for the hydroxy silicon oil of aluminum oxide quality 0～30% and account for aluminum oxide quality 0.5～2% are carried out proportioning, mix;
(3) curing temperature is 100～180 ℃, and pressure 6～10MPa under curing time 5～120min condition, adopts the compression molding sulfidization molding, makes the product of respective shapes as required;
(4) sample after the one step cure moulding carries out post vulcanization in air dry oven, and the sulfuration system is specifically determined according to practical situation, promptly rises to 100～150 ℃ with 1 hour from normal temperature, and progressively heating up then reaches 200～250 ℃, keeps constant temperature 2～20 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101033623A CN100526386C (en) | 2007-05-16 | 2007-05-16 | preparation process of thermally conductive and electrically insulating silicone rubber composite material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101033623A CN100526386C (en) | 2007-05-16 | 2007-05-16 | preparation process of thermally conductive and electrically insulating silicone rubber composite material |
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| Publication Number | Publication Date |
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| CN101067044A CN101067044A (en) | 2007-11-07 |
| CN100526386C true CN100526386C (en) | 2009-08-12 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659790B (en) * | 2009-09-23 | 2011-08-10 | 广东工业大学 | Method for preparing composite material of heat conduction silicon rubber of carbon aluminum-wrapping composite nano filler |
| CN101941262B (en) * | 2010-08-19 | 2014-01-01 | 浙江三元电子科技有限公司 | Process for producing high performance heat conducting fin |
| WO2013147229A1 (en) * | 2012-03-30 | 2013-10-03 | 日立化成株式会社 | Method for manufacturing thermally conductive sheet |
| CN103073893A (en) * | 2013-01-25 | 2013-05-01 | 阿特斯(中国)投资有限公司 | Potting adhesive for photovoltaic connecting box |
| CN106751910A (en) * | 2017-01-24 | 2017-05-31 | 大连东信微波技术有限公司 | A kind of heat conduction electromagnetic-wave absorbing rubber material and preparation method thereof |
| CN108776214A (en) * | 2017-10-16 | 2018-11-09 | 中国电力科学研究院有限公司武汉分院 | A kind of determination method of excellent electromechanical properties HTV insulating materials curing parameters |
| CN110305368B (en) * | 2019-06-20 | 2021-03-26 | 杭州师范大学 | Flame-retardant foaming agent and preparation method and application thereof |
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