CN106590549A - High-thermal conductivity graphene composite interface material and preparation method thereof - Google Patents
High-thermal conductivity graphene composite interface material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-thermal conductivity graphene composite interface material and a preparation method of the high-thermal conductivity graphene composite interface material. The high-thermal conductivity graphene composite interface material comprises the following components in percentage by mass: 5% to 10% of an organosilicon polymer, 85% to 90% of spherical heat-conductive powder, 1% to 5% of polyhedral heat-conductive powder, 1% to 5% of graphene powder and the balance of additives; raw materials in a formula ratio are dried, and then subjected to surface treatment by using a dry-wet method, and mixed and vacuumized after being placed in a planetary mixer, then heated and formed through a three-roller flattener to obtain the high-thermal conductivity composite interface material, so that the graphene powder is uniformly dispersed in the spherical heat-conductive powder and the polyhedral heat-conductive powder, and arranged in a multilayer directional manner, and excellent performances of graphene of thermal conductivity, ultra-softness and the like are used for preparing the high-thermal conductivity graphene composite interface material with high thermal conductivity and good compression and mechanical strength.
Description
Technical field
The present invention relates to Heat Conduction Material technical field, more particularly to a kind of high heat conduction Graphene compound interface material and preparation
Method.
Background technology
Radiating is always the work of one primary study of electronics industry, and the actual work temperature of electronic devices and components is to affect it
One of key factor of reliability.As electronic equipment develops towards miniaturization, high power consumption, its power dissipation density is stepped up.Electricity
The caloric value of sub- equipment is also multiplied, and this also puts forward higher requirement to the heat dispersion of system.Heat-conducting interface material is
The critical component of cooling system, is the bridge for connecting the heat transfer between chip and radiator.According to Heat Conduction Material filler with
And the difference of production technology, the thermal conductivity of heat-conducting interface material also presents larger difference.Differ primarily in that：Powder body type
Selection, including shapes and sizes；The selection of glue system, organosilicon, epoxy, acrylic acid etc.；Selection of dispersing aid etc..
Can have as the material of the heat filling of heat-conducting interface material：Metal-oxide such as Al2O3, ZnO, MgO etc.；Gold
Category nitride such as AlN, BN；Graphite；Ceramic-like powder body etc..
The production technology of heat-conducting interface material mainly has powder body pre-treatment, powder body silica gel collective stirring and evenly mixing, silica gel system
Vulcanize, cut packaging etc..At present its thermal conductivity of the heat-conducting interface material of large-scale use is mostly in below 5W/m K, existing
Under powder body system and manufacturing condition, its thermal conductivity is difficult to have a distinct increment.
Graphene is a kind of two-dimentional material with carbon element, is the general designation of single-layer graphene, bilayer graphene and few layer graphene, since
Just greatly paid close attention to since being reported first within 2004.Graphene has excellent heat conductivility, the reason of single-layer graphene
It is the decades of times of the Heat Conduction Material for being currently known best by thermal conductivity in more than 5500 W/m K.Graphene is used as thermally-conductive interface
Material conducts heat filling system prepares high-efficiency heat conduction boundary material and receives increasing concern.
The content of the invention
In order to overcome drawbacks described above, the invention provides a kind of high heat conduction Graphene compound interface material and preparation method,
Using the excellent heat conduction of Graphene and the super performance such as soft, high heat conductivity rate, compression and mechanical strength properties are prepared good
High heat conduction Graphene compound interface material.
The technical scheme that adopted to solve its technical problem of the present invention is：A kind of high heat conduction Graphene compound interface material
Material, including following component and mass percent,
Organosilicon polymer 5%-10%；
Spherical conduction powder 85%-90%；
Polyhedron conduction powder 1%-5%；
Graphene powder 1%-5%；
Adjuncts Balance.
The high heat conduction compound interface material of the present invention includes silica gel system, spherical conduction powder system, polyhedron spherical powder
Body system, Graphene filling system, dispersing aid system.The ratio sum of each component is 100%.
Colloidal silica therein means organosilicon polymer, and it is specially vinyl polysiloxane, benzene thiazolinyl polysiloxanes, first
The mixture of one or more in base benzene olefin(e) acid siloxanes and methylvinyl-polysiloxane, the viscosity of organosilicon polymer is
300~1000mpa.s.It functions as mixing filling powder body basic material.
Spherical conduction powder therein is the mixing of one or more in aluminium oxide, aluminium nitride, Zinc Oxide and boron nitride
Thing.The particle diameter D50 of spherical conduction powder is between 0.2 ~ 100 μm.
Polyhedron conduction powder therein is hexahedron, octahedra or dodecahedron.The particle diameter D50 of polyhedron conduction powder
Between 0.2 ~ 1.0 μm.Polyhedron conduction powder can be that polyhedron is alumina powder jointed.Polyhedron conduction powder and spherical heat conduction
Powder body plays the effect of heat conduction.
In the present invention using spherical conduction powder in combination with polyhedron conduction powder, to improve radiating efficiency.As adopted
Pure spherical conduction powder, spherical conduction powder is with spherical conduction powder thermal conductive contact model as shown in figure 1, can from figure
Go out, spherical with ball type of contact surface and little, i.e., single ball type of contact surface is less, and passage of heat has limitation.And adopt spherical heat conduction
In combination with polyhedron conduction powder, its thermal conductive contact model is as shown in Fig. 2 it can be seen that spherical and multiaspect for powder body
The contact surface increase of body, i.e., it is spherical many with polyhedral contact surface, so passage of heat increases, increase effective network knot
Structure, has been obviously improved the heat conductivility of heat-conducting interface material.As shown in figure 3, after addition Graphene, graphene uniform dispersion is more
Layer oriented alignment, it is possible to achieve more continuous thermally conductive pathways, so as to realize more preferable radiating effect.
Further, the auxiliary agent is the one kind in coupling agent, dispersant and catalyst.
Coupling agent therein is one or more in silane coupler, titanate coupling agent and aluminate coupling agent.
Its effect is the adhesion for strengthening conduction powder and colloid.
Dispersant therein is the one kind in polyethylene glycol 200 and PEG400 or two kinds.Its effect is more preferably
Powder body inside dispersion colloid.
Catalyst therein is platinum catalyst.Its effect is to solidify colloid.
Graphene powder can be the Graphene raw material that Physical or chemical method make, and can be specifically graphene sheet layer powder
Body or granule etc..
Further, the thickness of described graphene sheet layer powder body is 2 ~ 10nm, lamella length dimension is 3 ~ 50 μm, density
For 0.13 ~ 0.20g/cm3, metal ion content ＜ 1000ppm.
Graphene has that specific surface area is huge, light weight, and a small amount of addition Graphene just can form certain effective net
Network structure, is obviously improved the heat conductivility of heat-conducting interface material.Simultaneously because Graphene is very soft, heat conduction after addition Graphene
Boundary material hardness and compression performance will not receive considerable influence.Because Graphene has preferable electric conductivity, therefore
If heat-conducting interface material there are insulating properties to require, the addition for controlling Graphene is needed（Within 10%）, to control heat conduction
The breakdown voltage resistant performance of boundary material.Additionally due to dissolubility of the Graphene in common solvent is poor, it is therefore desirable to adopt
The mode added is disperseed to fill Graphene mixing filling system.
The present invention also provides a kind of preparation method of high heat conduction Graphene compound interface material as above, including step
Suddenly：After by the raw material drying of recipe ratio, it is surface-treated using wet-dry change, after placing into planetary mixer stirring evacuation,
High heat conduction compound interface material is obtained final product through the heating molding of three roller flatteners, makes graphene powder be dispersed in spherical conductive powder
In body and polyhedron conduction powder, and arranged in multi-layer oriented mode.
A kind of preparation method of high heat conduction Graphene compound interface material as above, by the raw material drying of recipe ratio
Afterwards, it is surface-treated using wet-dry change, after placing into planetary mixer stirring evacuation, through three roller flatteners molding is heated
Obtaining final product high heat conduction compound interface material makes graphene powder be dispersed in spherical conduction powder and polyhedron conduction powder, and
And arranged in multi-layer oriented mode.
The invention has the beneficial effects as follows：The present invention is using the excellent heat conduction of Graphene and the super performance such as soft, and coordinates
Polyhedron conduction powder, prepares the compound boundary of high heat conduction Graphene that heat conductivity rate is high, compression and mechanical strength properties are good
Facestock material.
Description of the drawings
Fig. 1 is contact surface schematic diagram between spherical conduction powder and spherical conduction powder in the present invention；
Fig. 2 is contact surface schematic diagram between spherical conduction powder and polyhedron conduction powder in the present invention；
Fig. 3 is contact surface schematic diagram between Graphene and spherical conduction powder and polyhedron conduction powder in the present invention.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, should
Embodiment is only used for the explanation present invention, does not constitute limiting the scope of the present invention.
Embodiment 1
Prepare following material：
Methylvinyl-polysiloxane 8g, spherical conduction powder（Including ball-aluminium oxide powder 3g and, ball-aluminium oxide and spherical
The mixed-powder 86g of aluminium nitride）, silane coupler help 1g.Wherein, particle diameter D50=0.4 ~ 0.8 μm of 3g ball-aluminium oxides powder,
Particle diameter D50=1 ~ 70 μm of 86g mixed-powders.In 86g mixed-powders, the mass ratio of ball-aluminium oxide and spherical aluminum nitride is 7:
3。
After above-mentioned raw materials are dried, proportioning is proportionally carried out, the raw material after proportioning is carried out at surface using wet-dry change
Reason, makes powder surface wrap up one layer of coupling agent.After planetary mixer stirring evacuation is put into, the heating molding of the roller flatteners of Jing tri-
Obtain final product high heat conduction gasket material.It is 5.0W/m that Jing tests the heat-conducting interface material its thermal conductivity in the case where pressure is for the pressure of 10Psi
K, specific insulation is 1013Ω•cm.Wet-dry change therein refers to and stirred together with other raw materials after silane coupler is hydrolyzed,
Mixing speed is 85 turns/min, and mixing time is 10min, and temperature is less than 25 DEG C（Such as 20 DEG C）.Stir planetary mixer is put into
Mixing the process conditions of evacuation is：Mixing speed is 30 ~ 85 turns/min（Such as 50 turns/min）, the time is not higher than 60min（For example
50min）, temperature is less than 25 DEG C（Such as 20 DEG C）.Three roller flatteners heat the process conditions of molding：Control thickness and wide cut,
Adjustment suitable tension, temperature is set as 80 ~ 130 DEG C（Such as 100 DEG C）, speed is 0.8 ~ 1.4m/min（Such as 1m/min）.
Embodiment 2
Prepare following material：
Methylvinyl-polysiloxane 8g, polyhedron conduction powder（Polyhedron alumina powder, D50=0.4 ~ 0.8 μm）3g, ball
Shape conduction powder（The mixed-powder of ball-aluminium oxide and spherical aluminum nitride, D50=1 ~ 70 μm）88g, silane coupler 1g.88g is mixed
In closing powder, the mass ratio of ball-aluminium oxide and spherical aluminum nitride is 7:3.
After above-mentioned raw materials are dried, proportioning is proportionally carried out, the raw material after proportioning is carried out at surface using wet-dry change
Reason, makes powder surface wrap up one layer of coupling agent.After planetary mixer stirring evacuation is put into, the heating molding of the roller flatteners of Jing tri-
Obtain final product high heat conduction gasket material.It is 5.5W/m that Jing tests the heat-conducting interface material its thermal conductivity in the case where pressure is for the pressure of 10Psi
K, specific insulation is 1013Ω•cm.Wet-dry change therein refers to and stirred together with other raw materials after silane coupler is hydrolyzed,
Mixing speed is 85 turns/min, and mixing time is 10min, and temperature is less than 25 DEG C（Such as 20 DEG C）.Stir planetary mixer is put into
Mixing the process conditions of evacuation is：Mixing speed is 30 ~ 85 turns/min（Such as 50 turns/min）, the time is not higher than 60min（For example
50min）, temperature is less than 25 DEG C（Such as 20 DEG C）.Three roller flatteners heat the process conditions of molding：Control thickness and wide cut,
Adjustment suitable tension, temperature is set as 80 ~ 130 DEG C（Such as 100 DEG C）, speed is 0.8 ~ 1.4m/min（Such as 1m/min）.
Embodiment 3
Prepare following material：
Methylvinyl-polysiloxane 8g, polyhedron conduction powder（Polyhedron alumina powder, D50=0.4 ~ 0.8 μm）4g, ball
Shape conduction powder（The mixed-powder of ball-aluminium oxide and spherical aluminum nitride, D50=1 ~ 70 μm）87g, silane coupler 1g.87g is mixed
In closing powder, the mass ratio of ball-aluminium oxide and spherical aluminum nitride is 7:3.
After above-mentioned raw materials are dried, proportioning is proportionally carried out, the raw material after proportioning is carried out at surface using wet-dry change
Reason, makes powder surface wrap up one layer of coupling agent.After planetary mixer stirring evacuation is put into, the heating molding of the roller flatteners of Jing tri-
Obtain final product high heat conduction gasket material.It is 6.2W/m that Jing tests the heat-conducting interface material its thermal conductivity in the case where pressure is for the pressure of 10Psi
K, specific insulation is 1013Ω•cm.Wet-dry change therein refers to and stirred together with other raw materials after silane coupler is hydrolyzed,
Mixing speed is 85 turns/min, and mixing time is 10min, and temperature is less than 25 DEG C（Such as 20 DEG C）.Stir planetary mixer is put into
Mixing the process conditions of evacuation is：Mixing speed is 30 ~ 85 turns/min（Such as 50 turns/min）, the time is not higher than 60min（For example
50min）, temperature is less than 25 DEG C（Such as 20 DEG C）.Three roller flatteners heat the process conditions of molding：Control thickness and wide cut,
Adjustment suitable tension, temperature is set as 80 ~ 130 DEG C（Such as 100 DEG C）, speed is 0.8 ~ 1.4m/min（Such as 1m/min）.
Embodiment 4
Methylvinyl-polysiloxane 8g, polyhedron conduction powder（Polyhedron alumina powder, D50=0.4 ~ 0.8 μm）4g, ball
Shape conduction powder（The mixed-powder of ball-aluminium oxide and spherical aluminum nitride, D50=1 ~ 70 μm）85g, graphene powder（Lamella is tied
Structure, thickness is 2 ~ 10nm, lamella length dimension is 3 ~ 50 μm, such as 25 μm）2g, silane coupler 1g.
After above-mentioned raw materials are dried, proportioning is proportionally carried out, the raw material after proportioning is carried out at surface using wet-dry change
Reason, makes powder surface wrap up one layer of coupling agent.After planetary mixer stirring evacuation is put into, the heating molding of the roller flatteners of Jing tri-
Obtain final product high heat conduction gasket material.It is 7.2W/m that Jing tests the heat-conducting interface material its thermal conductivity in the case where pressure is for the pressure of 10Psi
K, so its thermal conductivity increased relative to the result of previous embodiment, that is, improves heat-conducting effect；The heat conduction that test is obtained
The specific insulation of boundary material is 1010Ω cm, so add after grapheme material, the heat-conducting interface material for preparing, its
Insulation characterisitic decreases.Wet-dry change therein refers to and stirred together with other raw materials after silane coupler is hydrolyzed that stirring is fast
Spend for 85 turns/min, mixing time is 10min, temperature is less than 25 DEG C（Such as 20 DEG C）.Take out true planetary mixer stirring is put into
Empty process conditions are：Mixing speed is 30 ~ 85 turns/min（Such as 50 turns/min）, the time is not higher than 60min（For example
50min）, temperature is less than 25 DEG C（Such as 20 DEG C）.Three roller flatteners heat the process conditions of molding：Control thickness and wide cut,
Adjustment suitable tension, temperature is set as 80 ~ 130 DEG C（Such as 100 DEG C）, speed is 0.8 ~ 1.4m/min（Such as 1m/min）.
In sum, the filling of graphene powder has more contact effects and realizes more passages of heat, than tradition
Higher heat conductivity is obtained on the basis of powder body.The present invention using the excellent heat conduction of Graphene and the super performance such as soft, and
Coordinate polyhedron conduction powder, prepare the high heat conduction Graphene that heat conductivity rate is high, compression and mechanical strength properties are good and answer
Close boundary material.Simultaneously the production technology of heat-conducting interface material is practical.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, and for those of ordinary skills, can
To be improved according to the above description or be converted, all these modifications and variations should all belong to the guarantor of claims of the present invention
Shield scope.
Claims (8)
1. a kind of high heat conduction Graphene compound interface material, it is characterised in that：Including following component and mass percent,
Organosilicon polymer 5%-10%；
Spherical conduction powder 85%-90%；
Polyhedron conduction powder 1%-5%；
Graphene powder 1%-5%；
Adjuncts Balance；
The polyhedron conduction powder is hexahedron, octahedra or dodecahedron；
The graphene powder is graphene sheet layer powder body.
2. high heat conduction Graphene compound interface material according to claim 1, it is characterised in that：The organosilicon polymer
For the one kind in vinyl polysiloxane, benzene thiazolinyl polysiloxanes, methylbenzene olefin(e) acid siloxanes and methylvinyl-polysiloxane
Or various mixture.
3. high heat conduction Graphene compound interface material according to claim 1, it is characterised in that：The spherical conduction powder
For the mixture of one or more in aluminium oxide, aluminium nitride, Zinc Oxide and boron nitride.
4. high heat conduction Graphene compound interface material according to claim 1, it is characterised in that：The auxiliary agent is coupling
One kind in agent, dispersant and catalyst.
5. high heat conduction Graphene compound interface material according to claim 1, it is characterised in that：The coupling agent is silane
One or more in coupling agent, titanate coupling agent and aluminate coupling agent.
6. high heat conduction Graphene compound interface material according to claim 1, it is characterised in that：The dispersant is poly- second
One kind in glycol 200 and PEG400 or two kinds.
7. high heat conduction Graphene compound interface material according to claim 1, it is characterised in that：The catalyst is platinum
Catalyst.
8. a kind of preparation method of high heat conduction Graphene compound interface material as above, it is characterised in that：By recipe ratio
After raw material drying, it is surface-treated using wet-dry change, after placing into planetary mixer stirring evacuation, through three roller flatteners
Heating molding obtains final product high heat conduction compound interface material makes graphene powder be dispersed in spherical conduction powder and polyhedron heat conduction
In powder body, and arranged in multi-layer oriented mode.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861620A (en) * | 2021-09-25 | 2021-12-31 | 中建材蚌埠玻璃工业设计研究院有限公司 | Polyhedral single-crystal alumina/aluminum nitride/epoxy resin heat-conducting composite material and preparation method thereof |
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| CN105658715A (en) * | 2013-10-24 | 2016-06-08 | Dic株式会社 | Resin composition, heat-dissipating material, and heat-dissipating member |
| CN106554626A (en) * | 2015-09-29 | 2017-04-05 | 中兴通讯股份有限公司 | A kind of high heat conduction Graphene compound interface material and preparation method thereof |
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| CN101787178A (en) * | 2010-03-09 | 2010-07-28 | 王全胜 | Heat-conduction electric insulation composite material component and manufacturing method thereof |
| CN103408939A (en) * | 2013-08-02 | 2013-11-27 | 昆山市中迪新材料技术有限公司 | Insulation pad and preparation method thereof |
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Application publication date: 20170426 |