CN110317581A - A kind of pureed thermostable heat-conductive composite material and preparation method - Google Patents
A kind of pureed thermostable heat-conductive composite material and preparation method Download PDFInfo
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- CN110317581A CN110317581A CN201910488623.0A CN201910488623A CN110317581A CN 110317581 A CN110317581 A CN 110317581A CN 201910488623 A CN201910488623 A CN 201910488623A CN 110317581 A CN110317581 A CN 110317581A
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Abstract
The invention discloses a kind of pureed heat-conductive composite material, constituent is silicone oil, crosslinking agent, surface modifier, fire retardant, heat filling, catalyst and other auxiliary agents.Ratio calculates by weight, silicone oil 3-50%, crosslinking agent 0.1%-5%, surface modifier 0.1%-5%, fire retardant 0-20%, heat filling 50%-97%, catalyst 0.05%-0.015%.In addition, also disclosing the preparation method of above-mentioned pureed thermostable heat-conductive composite material.Pureed heat-conductive composite material of the present invention has many advantages, such as that high temperature resistance is excellent, thermal coefficient is high, thermal stability is good, oil yield is low, is convenient for extrusion, excellent storage stability, strong operability, efficiency greatly improves, and is very suitable to solve the problems, such as that electronic component generates heat.
Description
Technical field
The invention belongs to Heat Conduction Material fields, and in particular to a kind of pureed thermostable heat-conductive composite material.
Background technique
With the high speed development of electronics industry, the miniaturization of electronic component and densification degree are higher and higher, unit bodies
The heat that product comes out is also higher and higher.However, lasting high temperature meeting electron component brings very big damage, contract significantly
The service life and service efficiency of short component, thus, the heat-conductive composite material for developing a kind of stability and high efficiency, which has been carved, not to be allowed
It is slow.
Currently, the thermally conductive product in market has heat-conducting pad, heat-conducting cream, thermally conductive picture change material and thermally conductive gel.Heat conductive pad
Piece is current main product, needs to be prepared into different thickness specification and shape, and larger, higher cost is lost in production；And
The microcosmic seam-filling ability of heat-conducting pad is poor, and microcosmic gap, which is not filled, causes biggish thermal contact resistance, is unfavorable for the fast of heat
Speed transmission.Heat-conducting cream is easy fuel-displaced, easily causes circuit board to pollute in use, has greater risk that short circuit occurs, separately
It is easy to appear sedimentation and oil powder separation during storage outside, also needs to be again stirring for uniformly using preceding every time, use process is cumbersome.
Thermally conductive picture change material high temperature resistance is poor, is not suitable for being used for a long time in hot conditions.
Thermally conductive gel thermal coefficient currently on the market is relatively low, and oil yield is high, and reacts not exclusively, leads to its period of storage
It is very short；The appliance component of certain long-term golf calorific values needs Heat Conduction Material to have higher high temperature resistant and ageing-resistant requirement, at present
Thermally conductive gel in the market does not reach requirement also.
Summary of the invention
The object of the present invention is to provide a kind of pureed thermostable heat-conductive composite material, the present invention, which uses, has space three-dimensional knot
The silicone oil of structure, chemical stability is excellent, high temperature resistance is good.Meanwhile thermal coefficient of the present invention is high, facilitates operation.
A kind of pureed thermostable heat-conductive composite material, it is characterised in that its constituent is silicone oil, crosslinking agent, surface modification
Agent, fire retardant, heat filling, catalyst and other auxiliary agents.Ratio calculates by weight, silicone oil 3%-50%, and crosslinking agent is
0.1%-5%, surface modifier 0.1%-5%, fire retardant 1%-20%, heat filling 50%-97%, catalyst are
0.05%-0.015%.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the silicone oil is phenylethylene
The mixture of one or more of base silicone oil, MQ silicone resin, pheiiyldimetliyl silicone oil, vinyl silicone oil, the phenyl second
Alkenyl silicone oil is 100-10000mPa.s, preferably 300-5000mPa.s in 25 DEG C of dynamic viscosity.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: in the MQ resin of the silicone oil
M/Q is 0.5-1.5, preferably 0.8-1.2, and the MQ resin in the silicone oil is 100-10000mPa.s in 25 DEG C of dynamic viscosity,
It is preferred that 300-5000mPa.s.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the crosslinking agent is Silicon Containing Hydrogen
Oil, result are the mixture of one or more of the hydrogeneous structure of side chain, the hydrogeneous structure of the last chain in end, the hydrogeneous structure in two ends.Contain
Hydrogen amount (weight of hydrogen group in every 100g containing hydrogen silicone oil) is 0.018%-0.18%.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the surface modifier is silicon
The mixture of one or more of alkane coupling agent, titanate coupling agent, aluminate coupling agent, stearic acid.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the silane coupling agent is 3-
(2,3 the third oxygen of epoxy) propyl trimethoxy silicane, 3- (2,3 the third oxygen of epoxy) propyl-triethoxysilicane, 3- (2,3 the third oxygen of epoxy)
Hydroxypropyl methyl diethoxy silane, 2- (3,4 7-oxa-bicyclo[4.1.0 base) ethyl trimethoxy silane, 2- (3,4 7-oxa-bicyclo[4.1.0 base)
Propyl-triethoxysilicane, 3- (2,3 the third oxygen of epoxy) hydroxypropyl methyl dimethoxysilane, vinyl trichlorosilane, vinyl three
Methoxy silane, vinyltriethoxysilane, vinyl three (b- methoxy ethoxy) silane, n-hexyl trimethoxy silicon
Alkane, n-hexyl triethoxysilane, n-octyl trimethoxy silane, n-octytriethoxysilane, positive decyl trimethoxy silicon
Alkane, positive decyl triethoxysilane, dodecyltrimethoxysilane, dodecyl triethoxysilane, cetyl front three
Oxysilane, hexadecyl, octadecyl trimethoxysilane, one in octadecyltriethoxy silane
Kind or several mixtures.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the heat filling is dioxy
One of SiClx, aluminium oxide, magnesia, magnesium hydroxide, aluminium hydroxide, aluminium nitride, silicon nitride, boron nitride and silicon carbide are several
Kind.The partial size of the heat filling is divided into large, medium and small three grades, wherein the shape of big partial size heat filling is spherical shape.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: big grain in the heat filling
The D50 of diameter conduction powder is 20-70 μm, and the D50 of middle partial size conduction powder is 1-10 μm, and the D50 of small particle conduction powder is
0.1-2μm。
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the catalyst is urged for platinum
Agent；Other auxiliary agents further include the mixture of one or more of inhibitor and plasticizer, color, antioxidant.
According to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the resistance to height of the pureed
The preparation method of warm heat-conductive composite material, its step are as follows:
Heat filling is added in kneader step 1, stirs and is warming up to 100-150 DEG C, is uniformly added into whipping process
Surfactant, then thermal-insulating sealing stirs 0.5-2h, stops stirring, stops heating and is evacuated to -0.1Mpa, 15-
60min。
Silicone oil and fire retardant are added into kneader for step 2, and 100-170 DEG C of high temperature vacuumizes stirring 1-6h, are cooled to
Room temperature is made into base-material.
The base-material being made into step 2 is put into three-roll grinder and grinds three times by step 3.
Planetary mixer is added in base-material ground in step 3 by step 4, and remaining crosslinking agent, catalyst is then added
Deng first room temperature 10-40r/min stirs 0.5-2h, then heats and vacuumize stirring 0.1-5h for 100-170 DEG C, and cooling tubulature goes out
Material.
Beneficial effects of the present invention
There is three-D space structure inside pureed heat-conductive composite material of the present invention, there is powerful cohesive force and support force,
Crosslink density is low, while having low oil yield and high rate of extrusion, is greatly improved construction efficiency.
Pureed heat-conductive composite material of the present invention has larger space steric hindrance, and thermal stability and high temperature ageing are had excellent performance,
It can be used for the heat dissipation of long-term thermal extremes environment.
Pureed heat-conductive composite material thermal coefficient of the present invention is high, contacts closely with electronic chip, and thermal contact resistance is small, and storage is steady
It is qualitative good, simple to operate, it is low in cost, it is very suitable to solve the problems, such as that electronic component generates heat.
Specific embodiment
Below with reference to embodiment to a kind of pureed thermostable heat-conductive composite material and preparation method of the invention carry out into
One step explanation:
Embodiment 1
D50 is that 1 μm of zinc oxide, 5 μm of aluminium oxide and 40 μm of aluminium oxide are added in kneader by step 1, and stirring is simultaneously
120 DEG C are warming up to, (b- methoxy ethoxy) silane of vinyl three and stearic acid are uniformly added into whipping process, is then kept the temperature close
Envelope stirring 0.5h, stops stirring, stops heating and is evacuated to -0.1Mpa, 25min.
Step 2, into kneader be added 25 DEG C at dynamic viscosity be 1000mPa.s phenyl-vinyl silicon oil,
The vinyl silicone oil and fire retardant of 350mPa.s, 135 DEG C of high temperature vacuumize stirring 3h, are cooled to room temperature, are made into base-material.
The base-material being made into step 2 is put into three-roll grinder and grinds three times by step 3.
Planetary mixer is added in base-material ground in step 3 by step 4, and then the end side chain of addition 0.18% is hydrogeneous
Silicone oil, 0.1% liang of end containing hydrogen silicone oil, catalyst and other auxiliary agents, first room temperature 10r/min stir 0.5h, then 110 DEG C of heating
And stirring 1h is vacuumized, cooling tubulature discharging.
Embodiment 2
D50 is that 0.5 μm of aluminium oxide, 2 μm of aluminium nitride and 70 μm of aluminium oxide are added in kneader by step 1, stirring
And 110 DEG C are warming up to, hexadecyl trimethoxy silane is uniformly added into whipping process, then thermal-insulating sealing stirs 2h, stops
Stirring stops heating and is evacuated to -0.1Mpa, 30min.
Step 2, into kneader be added 25 DEG C at dynamic viscosity be 500mPa.s pheiiyldimetliyl silicone oil,
The MQ silicone resin and fire retardant that the M/Q of 1500mPa.s is 0.9,150 DEG C of high temperature vacuumize stirring 3h, are cooled to room temperature, are made into
Base-material.
The base-material being made into step 2 is put into three-roll grinder and grinds three times by step 3.
Planetary mixer is added in base-material ground in step 3 by step 4, and 0.18% side chain Silicon Containing Hydrogen is then added
Oil, 0.1% liang of end containing hydrogen silicone oil, catalyst and other auxiliary agents, first room temperature 30r/min stir 0.5h, then heat simultaneously for 110 DEG C
Vacuumize stirring 0.5h, cooling tubulature discharging.
Embodiment 3
D50 is that 0.5 μm of aluminium oxide, 7 μm of aluminium oxide and 40 μm of boron nitride are added in kneader by step 1, stirring
And 110 DEG C are warming up to, 2- (3,4 7-oxa-bicyclo[4.1.0 base) propyl-triethoxysilicane and n-hexyl three are uniformly added into whipping process
Ethoxysilane, then thermal-insulating sealing stirs 1h, stops stirring, stops heating and is evacuated to -0.1Mpa, 30min.
Vinyl base silicone oil, 1000mPa.s that dynamic viscosity at 25 DEG C is 350mPa.s are added into kneader for step 2
M/Q be 1.1 MQ silicone resin and fire retardant, 130 DEG C of high temperature, vacuumize stirring 2.5h, be cooled to room temperature, be made into base-material.
The base-material being made into step 2 is put into three-roll grinder and grinds three times by step 3.
Planetary mixer is added in base-material ground in step 3 by step 4, and then the end side chain of addition 0.18% is hydrogeneous
Silicone oil, 0.05% side chain containing hydrogen silicone oil, catalyst and other auxiliary agents, first room temperature 30r/min stir 20min, then 150 DEG C of heating
And stirring 0.5h is vacuumized, cooling tubulature discharging.Proportion is as shown in the table in the present invention for specific each component.
Embodiment 1, embodiment 2 and embodiment 3 are carried out to squeeze out the rate that hastens, thermal coefficient, high temperature ageing performance, vertical fluidity
It can be carried out test, specific performance data are as shown in the table:
Test result shows that pureed thermostable heat-conductive composite material of the invention has that high temperature resistance is excellent, thermally conductive system
Number is high, thermal stability is good, oil yield is low, is convenient for the advantages that extrusion, excellent storage stability, and strong operability, efficiency greatly improves,
It is very suitable to solve the problems, such as that electronic component generates heat.
The above, is section Example of the invention, and protection scope of the present invention includes above-described embodiment but is not limited to
Above-described embodiment, protection scope of the present invention are subject to the protection scope that the claims are defined.
Claims (10)
1. a kind of pureed thermostable heat-conductive composite material, it is characterised in that its constituent is silicone oil, crosslinking agent, surface modification
Agent, fire retardant, heat filling, catalyst and other auxiliary agents.Ratio calculates by weight, silicone oil 3%-50%, and crosslinking agent is
0.1%-5%, surface modifier 0.1%-5%, fire retardant 1%-20%, heat filling 50%-97%, catalyst are
0.05%-0.015%.
2. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the silicone oil is phenyl vinyl
The mixture of one or more of silicone oil, MQ silicone resin, pheiiyldimetliyl silicone oil, vinyl silicone oil, the phenylethylene
Base silicone oil is 100-10000mPa.s, preferably 300-5000mPa.s in 25 DEG C of dynamic viscosity.
3. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: M/ in the MQ resin of the silicone oil
Q is 0.5-1.5, preferably 0.8-1.2, and the MQ resin in the silicone oil is 100-10000mPa.s in 25 DEG C of dynamic viscosity, excellent
Select 300-5000mPa.s.
4. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the crosslinking agent is Silicon Containing Hydrogen
Oil, result are the mixture of one or more of the hydrogeneous structure of side chain, the hydrogeneous structure of the last chain in end, the hydrogeneous structure in two ends.Contain
Hydrogen amount (weight of hydrogen group in every 100g containing hydrogen silicone oil) is 0.018%-0.18%.
5. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the surface modifier is silane
The mixture of one or more of coupling agent, titanate coupling agent, aluminate coupling agent, stearic acid.
6. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the silane coupling agent is 3-
(2,3 the third oxygen of epoxy) propyl trimethoxy silicane, 3- (2,3 the third oxygen of epoxy) propyl-triethoxysilicane, 3- (2,3 the third oxygen of epoxy)
Hydroxypropyl methyl diethoxy silane, 2- (3,4 7-oxa-bicyclo[4.1.0 base) ethyl trimethoxy silane, 2- (3,4 7-oxa-bicyclo[4.1.0 base)
Propyl-triethoxysilicane, 3- (2,3 the third oxygen of epoxy) hydroxypropyl methyl dimethoxysilane, vinyl trichlorosilane, vinyl three
Methoxy silane, vinyltriethoxysilane, vinyl three (b- methoxy ethoxy) silane, n-hexyl trimethoxy silicon
Alkane, n-hexyl triethoxysilane, n-octyl trimethoxy silane, n-octytriethoxysilane, positive decyl trimethoxy silicon
Alkane, positive decyl triethoxysilane, dodecyltrimethoxysilane, dodecyl triethoxysilane, cetyl front three
Oxysilane, hexadecyl, octadecyl trimethoxysilane, one in octadecyltriethoxy silane
Kind or several mixtures.
7. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the heat filling is titanium dioxide
One of silicon, aluminium oxide, magnesia, magnesium hydroxide, aluminium hydroxide, aluminium nitride, silicon nitride, boron nitride and silicon carbide are several
Kind.The partial size of the heat filling is divided into large, medium and small three grades, wherein the shape of big partial size heat filling is spherical shape.
8. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: big partial size in the heat filling
The D50 of conduction powder is 20-70 μm, and the D50 of middle partial size conduction powder is 1-10 μm, and the D50 of small particle conduction powder is 0.1-2
μm。
9. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the catalyst is platinum catalysis
Agent；Other auxiliary agents further include the mixture of one or more of inhibitor and plasticizer, color, antioxidant.
10. according to pureed thermostable heat-conductive composite material described in right 1, it is characterised in that: the pureed thermostable heat-conductive
The preparation method of composite material, its step are as follows:
Heat filling is added in kneader step 1, stirs and is warming up to 100-150 DEG C, is uniformly added into surface in whipping process
Activating agent, then thermal-insulating sealing stirs 0.5-2h, stops stirring, stops heating and is evacuated to -0.1Mpa, 15-60min.
Silicone oil and fire retardant are added into kneader for step 2, and 100-170 DEG C of high temperature vacuumizes stirring 1-6h, are cooled to room temperature,
It is made into base-material.
The base-material being made into step 2 is put into three-roll grinder and grinds three times by step 3.
Planetary mixer is added in base-material ground in step 3 by step 4, remaining crosslinking agent, catalyst etc. is then added, first
Room temperature 10-40r/min stirs 0.5-2h, then heats and vacuumize stirring 0.1-5h, cooling tubulature discharging for 100-170 DEG C.
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| CN110982277A (en) * | 2019-12-23 | 2020-04-10 | 成都硅宝科技股份有限公司 | Single-component temperature-resistant heat-conducting silicon mud composition and preparation method thereof |
| CN111171575A (en) * | 2020-01-16 | 2020-05-19 | 广东桑泰科技有限公司 | Heat-conducting gel with high heat conductivity and low oil-yielding performance and preparation process thereof |
| CN111944498A (en) * | 2020-08-20 | 2020-11-17 | 广东鼎泰新材料科技有限公司 | Heat-conducting gel with ultralow oil extraction amount and high flow rate performance and preparation method thereof |
| CN112552882A (en) * | 2020-12-02 | 2021-03-26 | 上海阿莱德实业股份有限公司 | Single-component muddy interface heat conduction material and application thereof |
| CN112608722A (en) * | 2020-12-16 | 2021-04-06 | 上海阿莱德实业股份有限公司 | Muddy interface heat conduction material and application thereof |
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| CN111171575A (en) * | 2020-01-16 | 2020-05-19 | 广东桑泰科技有限公司 | Heat-conducting gel with high heat conductivity and low oil-yielding performance and preparation process thereof |
| CN111944498A (en) * | 2020-08-20 | 2020-11-17 | 广东鼎泰新材料科技有限公司 | Heat-conducting gel with ultralow oil extraction amount and high flow rate performance and preparation method thereof |
| CN112552882A (en) * | 2020-12-02 | 2021-03-26 | 上海阿莱德实业股份有限公司 | Single-component muddy interface heat conduction material and application thereof |
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Application publication date: 20191011 |