CN102558867A - Low-trailing heat conductive silicone grease composition and preparation method thereof - Google Patents
Low-trailing heat conductive silicone grease composition and preparation method thereof Download PDFInfo
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- CN102558867A CN102558867A CN2011104131696A CN201110413169A CN102558867A CN 102558867 A CN102558867 A CN 102558867A CN 2011104131696 A CN2011104131696 A CN 2011104131696A CN 201110413169 A CN201110413169 A CN 201110413169A CN 102558867 A CN102558867 A CN 102558867A
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Abstract
The invention relates to a low-trailing heat conductive silicone grease composition and a preparation method thereof. The low-trailing heat conductive silicone grease composition consists of the following components in part by weight: 3 to 35 parts of polysiloxane, 0 to 90 parts of heat conductive filler, 1 to 75 parts of thixotropic filler and 0 to 1.5 parts of other additives. The low-trailing heat conductive silicone grease is prepared from the specific type of polysiloxane, the heat conductive filler and the additives in an appropriate formula ratio by a specific process; and the heat conductivity and other properties of the heat conductive silicone grease are the same as those of the universal heat conductive silicone grease in the market, and the heat conductive silicone grease has low wire drawing trailing property, and has the advantages of no pollution and contribution to automatic sizing when used in the process.
Description
Technical field
The present invention designs technical field of polymer materials, especially relates to a kind of heat conductive silicone grease composition of low hangover
Background technology
Because the increase of electronic apparatus power has proposed increasingly high demand to heat radiation, the thermal resistance between scatterer and thermal source is developed and be applied to reduce to multiple heat interfacial material.Heat-conducting silicone grease is wherein a kind of, and because of it has easy to usely, good heat conduction effect advantage such as is easy to reprocess and obtains widespread use.Heat-conducting silicone grease commonly used is that heat conductive filler is added in the organopolysiloxane of appropriate viscosity, and adds the additive for improving performance.Through selecting different heat conductive fillers and addition, silicone grease can obtain adjustable thermal conductivity, to satisfy demands of different.But common heat-conducting silicone grease has serious wire drawing conditions of streaking, pollutes peripheral object when taking easily, and especially on robotization applying glue equipment, serious conditions of streaking causes it normally to use.
Summary of the invention
The heat-conducting silicone grease that the purpose of this invention is to provide a kind of low hangover, the adding through specific thixotropic filler and control its consumption reaches the degree that reduces silicone grease wire drawing conditions of streaking, and the prescription of high effect can accomplish not have wire drawing does not fully have hangover.
In order to realize the object of the invention, a kind of heat conductive silicone grease composition of low hangover is proposed, said heat conductive silicone grease composition is composed of the following components by weight:
Said organopolysiloxane can be expressed as R with general formula
1 aSiO
(4-a)/2, representative has a kind of or several groups of the saturated or unsaturated alkyl of 1~18 carbon atom, and a is the positive number of 1.8≤a≤2.2, is preferably 1.9~2.2 positive number especially, and 25 ℃ kinematic viscosity is set at 50~100000mPas;
Said heat conductive filler is the material of thermal conductivity greater than 10W/mK, and heat conductive filler can be a sheet, the powder or the particulate material of spherical or amorphous, and particle diameter is between 0.1~100 micron, and filler can adopt different-grain diameter composite;
Thixotropic filler is a carbon dust, graphite, and nano aluminium oxide, zinc oxide, gas-phase silica, a kind of or several mixing of precipitated silica powder mass, its particle diameter is 10~500nm;
Other additive is anti-aging agent, coupling agent and tinting material.
Said R
1The group of representative is the alkyl group of methyl, ethyl, propyl group, decyl, dodecyl, octadecyl; The aryl of phenyl, tolyl, the naphthenic base of cyclohexyl, cyclopentyl, vinyl, allylic alkenyl; 3; 3, the halo group of 3-trifluoro propyl, rubigan is preferably methyl, phenyl and chain alkyl.
Said heat conductive filler is an aluminium powder, copper powder, and nickel powder, bronze, aluminum oxide, zinc oxide, Natural manganese dioxide, silicon oxide, aluminium nitride AlN, silicon nitride, silit, SP 1, diamond, graphite, thomel, one or more of soccerballene mix use.
The more excellent combination of several kinds of heat conductive silicone grease compositions below the present invention also proposes:
Said heat conductive silicone grease composition is to be made up of for 0.3 part 5 parts of the gas-phase silicas of 75 parts in the aluminum oxide of 19.7 parts of the methyl-silicone oils of 1000cps, 10um, 20nm and 1010A anti-aging agent.
Said heat conductive silicone grease composition is made up of for 5 parts 20 parts of the methyl-silicone oils of 1000cps, 50 parts in the aluminum oxide of 10um, 25 parts in the aluminum oxide of 1um and the gas-phase silica of 20nm.
Said heat conductive silicone grease composition is made up of for 4 parts 50 parts in the aluminum oxide of 20 parts of 1000cps methyl-silicone oils, 10um, 25 parts of the aluminium nitride AlN of 2um and the gas-phase silica of 20nm.
Said heat conductive silicone grease composition is made up of for 72 parts 28 parts of zinc oxide with 40nm of 100cps methyl-silicone oil.
Said heat conductive silicone grease composition is by being made up of for 8 parts 40 parts in the aluminum oxide of 22 parts of 100cps methyl-silicone oils, 10um, 30 parts of the ball aluminum powder of 10um and the nano aluminium oxide of 200nm.
Said heat conductive silicone grease composition is made up of for 1 part 85 parts in the aluminum oxide of 14 parts of 100cps methyl-silicone oils, 10um and the gas-phase silica of 20nm.
The present invention also proposes to prepare the method for above-mentioned low hangover heat-conducting silicone grease, is made up of following steps successively:
(a) organopolysiloxane, other additive were at room temperature mixed 5~20 minutes;
(b) divide and to add heat conductive filler for 1-3 time and at room temperature mixed 30~90 minutes, use the homodisperse of high speed dispersing device, cause stirring at need, can heat to viscosity reduction below 130 ℃ and stir at the viscosity height with powder;
(c) add thixotropic filler, at room temperature stirred 30~90 minutes, use high speed dispersing device to guarantee the homodisperse of powder, cause stirring at need, can heat to viscosity reduction below 130 ℃ and stir at the viscosity height;
(d) vacuum defoamation 20-50 minute, be cooled to 20-60 ℃ of left and right sides plastic emitting.
The present invention selects the organopolysiloxane of particular types, heat conductive filler, and additive according to suitable prescription ratio, goes out to hang down the heat-conducting silicone grease of hangover with specific prepared.Heat conductivity of heat-conduction silicone grease and other performances are identical with general on the market heat-conducting silicone grease, but it has the performance of low wire drawing hangover, in technology is used, have pollution-freely, are convenient to the advantage of robotization applying glue.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, to further explain of the present invention.
The heat conductive silicone grease composition of low hangover of the present invention is composed of the following components by weight:
3~35 parts of A organopolysiloxane
0~90 part of B heat conductive filler
1~75 part of C thixotropic filler
0~1.5 part of other additive of D
With above composition thorough mixing.
Above-mentioned organopolysiloxane can be expressed as R with general formula
1 aSiO
(4-a)/2, R
1Representative has a kind of or several groups of the saturated or unsaturated alkyl of 1~18 carbon atom.Usually the group of representative is alkyl groups such as methyl, ethyl, propyl group, decyl, dodecyl, octadecyl; Aryl such as phenyl, tolyl, naphthenic base such as cyclohexyl, cyclopentyl, alkenyls such as vinyl, allyl group; 3; 3, halo groups such as 3-trifluoro propyl, rubigan are preferably methyl, phenyl and chain alkyl especially.
A is the positive number of 1.8≤a≤2.2, is preferably 1.9~2.2 positive number especially.
25 ℃ kinematic viscosity of above-mentioned organopolysiloxane is set at 50~100000mPas, and viscosity is lower than this scope, and the silicone grease that makes is prone to oily from phenomenon, is higher than this scope, and the silicone grease viscosity that makes is too high, is difficult to use.
Heat conductive filler is the filler with certain capacity of heat transmission, is generally the material of thermal conductivity greater than 10W/mK, and commonly used is aluminium powder, copper powder, nickel powder; Bronze, aluminum oxide, zinc oxide, Natural manganese dioxide, silicon oxide; Aluminium nitride AlN, silicon nitride, silit, SP 1, diamond; Graphite, thomel, powder or particulate materials such as soccerballene are a kind of during filling or several mix use.Heat conductive filler can be a sheet, and spherical or amorphous, particle diameter concentrate between 0.1~100 micron.Filler can adopt greatly, in, small particle size makes silicone grease reach higher thermal conductivity and flowing property according to certain composite raising filling ratio of ratio.
Thixotropic filler is a carbon dust, graphite, nano aluminium oxide, zinc oxide, gas-phase silica, powder masss such as precipitated silica, its particle diameter 10~500nm.Be a kind of during filling or several mixing uses.
Other additive is generally anti-aging agent for improving the auxiliary agent that the silicone grease performance is used, coupling agent, and tinting materials etc. are prerequisite not influence performance of products of the present invention.
The method for preparing above-mentioned a kind of low hangover heat-conducting silicone grease is made up of following steps successively:
(a) organopolysiloxane, other additive were at room temperature mixed 5~20 minutes.
(b) divide and to add heat conductive filler for 1-3 time and at room temperature mixed 30~90 minutes, need high speed dispersing device to guarantee the homodisperse of powder, cause stirring can heat at need to viscosity reduction below 130 ℃ like the viscosity height and stir.
(c) add thixotropic filler, at room temperature stirred 30~90 minutes, need high speed dispersing device to guarantee the homodisperse of powder, cause stirring to heat at need to viscosity reduction below 130 ℃ like the viscosity height and stir.
(d) vacuum defoamation 20-50 minute, be cooled to 20-60 ℃ of left and right sides plastic emitting
Below be the embodiment that the contriver provides, but the present invention is not limited to these embodiment.
Embodiment 1
Buy and use following product
A1 methyl-silicone oil 1000cps
A2 methyl-silicone oil 100cps
B1 aluminum oxide 10um
B2 aluminum oxide 1um
B3 aluminium nitride AlN 2um
B4 ball aluminum powder 10um
C1 zinc oxide 40nm
C2 nano aluminium oxide 200nm
C3 gas-phase silica 20nm
D anti-aging agent 1010A
Above-mentioned raw materials is produced the silicone grease mixture according to aforesaid production technique, measure its thermal conductivity and hangover performance.
With preferred embodiment openly as above they are not to be used for limiting the present invention though the present invention is own, and the content that protection scope of the present invention should be defined with the application's claim protection domain is as the criterion.Anyly have the knack of present technique field person, do not breaking away from the spirit and scope of the present invention, various variations of being done or be equal to replacement all should belong to protection scope of the present invention.
Claims (10)
1. one kind is hanged down the heat conductive silicone grease composition that trails, and it is characterized in that said heat conductive silicone grease composition is composed of the following components by weight:
Said organopolysiloxane can be expressed as R with general formula
1 aSiO
(4-a)/2, representative has a kind of or several groups of the saturated or unsaturated alkyl of 1~18 carbon atom, and a is the positive number of 1.8≤a≤2.2, is preferably 1.9~2.2 positive number especially, and 25 ℃ kinematic viscosity is set at 50~100000mPas;
Said heat conductive filler is the material of thermal conductivity greater than 10W/mK, and heat conductive filler can be a sheet, the powder or the particulate material of spherical or amorphous, and particle diameter is between 0.1~100 micron, and filler can adopt different-grain diameter composite;
Thixotropic filler is a carbon dust, graphite, and nano aluminium oxide, zinc oxide, gas-phase silica, a kind of or several mixing of precipitated silica powder mass, its particle diameter is 10~500nm;
Other additive is anti-aging agent, coupling agent and tinting material.
2. heat conductive silicone grease composition according to claim 1 is characterized in that, said R
1The group of representative is the alkyl group of methyl, ethyl, propyl group, decyl, dodecyl, octadecyl; The aryl of phenyl, tolyl, the naphthenic base of cyclohexyl, cyclopentyl, vinyl, allylic alkenyl; 3; 3, the halo group of 3-trifluoro propyl, rubigan is preferably methyl, phenyl and chain alkyl.
3. heat conductive silicone grease composition according to claim 1 is characterized in that, heat conductive filler is an aluminium powder, copper powder, nickel powder; Bronze, aluminum oxide, zinc oxide, Natural manganese dioxide, silicon oxide; Aluminium nitride AlN, silicon nitride, silit, SP 1; Diamond, graphite, thomel, one or more of soccerballene mix use.
4. heat conductive silicone grease composition according to claim 4 is characterized in that, said heat conductive silicone grease composition is made up of for 0.3 part 19.7 parts of the methyl-silicone oils of 1000cps, 75 parts in the aluminum oxide of 10um, 5 parts of gas-phase silicas and the 1010A anti-aging agent of 20nm.
5. heat conductive silicone grease composition according to claim 4 is characterized in that, said heat conductive silicone grease composition is made up of for 5 parts 20 parts of the methyl-silicone oils of 1000cps, 50 parts in the aluminum oxide of 10um, 25 parts in the aluminum oxide of 1um and the gas-phase silica of 20nm.
6. heat conductive silicone grease composition according to claim 4 is characterized in that, said heat conductive silicone grease composition is made up of for 4 parts 50 parts in the aluminum oxide of 20 parts of 1000cps methyl-silicone oils, 10um, 25 parts of the aluminium nitride AlN of 2um and the gas-phase silica of 20nm.
7. heat conductive silicone grease composition according to claim 4 is characterized in that, said heat conductive silicone grease composition is made up of for 72 parts 28 parts of zinc oxide with 40nm of 100cps methyl-silicone oil.
8. heat conductive silicone grease composition according to claim 4 is characterized in that, said heat conductive silicone grease composition is by being made up of for 8 parts 40 parts in the aluminum oxide of 22 parts of 100cps methyl-silicone oils, 10um, 30 parts of the ball aluminum powder of 10um and the nano aluminium oxide of 200nm.
9. heat conductive silicone grease composition according to claim 4 is characterized in that, said heat conductive silicone grease composition is made up of for 1 part 85 parts in the aluminum oxide of 14 parts of 100cps methyl-silicone oils, 10um and the gas-phase silica of 20nm.
10. prepare the method for above-mentioned low hangover heat-conducting silicone grease, it is characterized in that, said method is made up of following steps successively:
(a) organopolysiloxane, other additive were at room temperature mixed 5~20 minutes;
(b) divide and to add heat conductive filler for 1-3 time and at room temperature mixed 30~90 minutes, use the homodisperse of high speed dispersing device, cause stirring at need, can heat to viscosity reduction below 130 ℃ and stir at the viscosity height with powder;
(c) add thixotropic filler, at room temperature stirred 30~90 minutes, use high speed dispersing device to guarantee the homodisperse of powder, cause stirring at need, can heat to viscosity reduction below 130 ℃ and stir at the viscosity height;
(d) vacuum defoamation 20-50 minute, be cooled to 20-60 ℃ of left and right sides plastic emitting.
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CN102924923A (en) * | 2012-10-24 | 2013-02-13 | 江苏大学 | High thermal conductive magnetic metal fiber/silicon rubber composite material and preparation method thereof |
CN103194067A (en) * | 2013-04-25 | 2013-07-10 | 汕头市骏码凯撒有限公司 | Ultra-low thermal-resistance heat-conducing silicon grease and preparation method thereof |
CN104672911A (en) * | 2015-03-03 | 2015-06-03 | 矽照光电(厦门)有限公司 | Preparation method of carbon nanotube doped weather-proof heat conductive silicone grease for LED |
CN105950100A (en) * | 2016-05-31 | 2016-09-21 | 江苏创景科技有限公司 | {0><}0{>Organosilicon pouring sealant with high curing speed and low wiredrawing capability and preparation method thereof<0} |
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CN112251139A (en) * | 2020-10-27 | 2021-01-22 | 深圳市誉隆新材料有限公司 | Fire-resistant flame-retardant liquid polyorganosiloxane composition |
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CN115558293A (en) * | 2022-10-12 | 2023-01-03 | 杭州之江有机硅化工有限公司 | Heat-conducting silicone grease composition and application thereof |
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WO2011083880A1 (en) * | 2010-01-07 | 2011-07-14 | Dow Corning Toray Co., Ltd. | Thermally conductive silicone grease composition |
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Patent Citations (1)
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WO2011083880A1 (en) * | 2010-01-07 | 2011-07-14 | Dow Corning Toray Co., Ltd. | Thermally conductive silicone grease composition |
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CN102924923B (en) * | 2012-10-24 | 2014-12-03 | 江苏大学 | High thermal conductive magnetic metal fiber/silicon rubber composite material and preparation method thereof |
CN103194067A (en) * | 2013-04-25 | 2013-07-10 | 汕头市骏码凯撒有限公司 | Ultra-low thermal-resistance heat-conducing silicon grease and preparation method thereof |
CN103194067B (en) * | 2013-04-25 | 2015-03-11 | 汕头市骏码凯撒有限公司 | Ultra-low thermal-resistance heat-conducing silicon grease and preparation method thereof |
CN104672911B (en) * | 2015-03-03 | 2017-07-28 | 矽照光电(厦门)有限公司 | A kind of preparation method based on carbon nano tube-doped weather resistant LED heat-conducting silicone greases |
CN104672911A (en) * | 2015-03-03 | 2015-06-03 | 矽照光电(厦门)有限公司 | Preparation method of carbon nanotube doped weather-proof heat conductive silicone grease for LED |
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CN107602915A (en) * | 2017-02-14 | 2018-01-19 | 广州奥翼电子科技股份有限公司 | A kind of composite heat-conducting silicone grease |
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CN107603224A (en) * | 2017-09-14 | 2018-01-19 | 中国科学院工程热物理研究所 | A kind of heat conductive silicone grease composition of high heat conductance low viscosity and preparation method thereof |
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Application publication date: 20120711 |