CN103740108A - High-thermal-conductivity elastic composite material and preparation method thereof - Google Patents
High-thermal-conductivity elastic composite material and preparation method thereof Download PDFInfo
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Abstract
The embodiment of the invention provides a high-thermal-conductivity elastic composite material and a preparation method thereof. The composite material comprises curing type organic silicon resin and composite thermal conductive filler, wherein the composite thermal conductive filler is uniformly distributed in the curing type organic silicon resin; the weight percentage of the curing type organic silicon resin is 20% to 60%; the weight percentage of the composite thermal conductive filler is 40% to 80%; the composite thermal conductive filler comprises any one of carbon nano tubes and graphene oxide and thermal conductive powder being 0.1-100 microns. The high-thermal-conductivity elastic composite material is simple in technology, short in production period, low in product density, good in elasticity, resistant to product corrosion and good in high temperature resistance performance.
Description
Technical field
The invention belongs to field of compound material, particularly a kind of high heat conduction elastic composite and preparation method thereof.
Background technology
Along with electron device is towards thin, light, little future development, heat radiation has become the important developing direction in one, present material field.For electronic system (particularly sensitive circuit and components and parts) can be worked sustainedly and stably, it is carried out to effectively reliably heat radiation very important, therefore, research and develop high efficiency electronic radiation material and correlation technique very urgent.Heat interfacial material (Thermal Interface Material, TIM) effect is mainly the thermal contact resistance reducing between heat-generating electronic elements and scatterer, it can form effective heat transfer path between electronic devices and components and scatterer, thereby significantly reduces because air exists the large thermal contact resistance causing.
In the TIM using at present, heat-conducting elastomer has easy disassembly, reuses, facilitates by features such as size cuttings, in the situation that contact pressure is relatively low, can fully fill up the space between scatterer and electronic package surface, form effectively heat radiation and change passage.Meanwhile, it can also play to electronics the effects such as damping vibration attenuation.When TIM dispels the heat for components and parts, the effectively space between filling interface, drives away air between cold and hot interface, scatterer effect can be improved to 40% left and right.Heat-conducting elastomer TIM has extensively been used on the various electronic products such as large server, light and thin notebook computer.Because macromolecular material is isolator, and thermal conductivity is low, has limited to a great extent the application of pure polymer in these fields.Therefore, develop that to have the macromolecular material Practical significance of high heat conduction elasticity TIM and excellent combination property great.
Summary of the invention
Order of the present invention is to provide a kind of high heat conduction elastic composite and preparation method thereof.
The first aspect of the embodiment of the present invention discloses a kind of high heat conduction elastic composite, it is characterized in that, described matrix material comprises curing type silicone resin and composite heat-conducting filler, being dispersed in described curing type silicone resin of described composite heat-conducting uniform filling, the weight percent of described curing type silicone resin is 20%～60%, the weight percent of described composite heat-conducting filler is 40%～80%, and described composite heat-conducting filler comprises the heat conduction powder of any and 0.1～100 micron in carbon nanotube and graphene oxide.
In conjunction with first aspect, in the first implementation of first aspect, described heat conduction powder comprises one or the mixture in alpha-phase aluminum oxide, γ phase alumina.
In conjunction with the first implementation of first aspect or first aspect, in the second implementation of first aspect, described curing type silicone resin comprises addition curable silicone resin.
The second aspect of the embodiment of the present invention discloses a kind of preparation method of high heat conduction elastic composite, it is characterized in that, described preparation method comprises:
By mixing to curing type silicone resin, composite heat-conducting filler and vulcanizing agent even, wherein, described curing type silicone resin accounts for 20%～60% of described curing type silicone resin and described composite heat-conducting filler gross weight, described composite heat-conducting filler accounts for 40%～80% of described curing type silicone resin and described composite heat-conducting filler gross weight, and the weight percent of described vulcanizing agent and described curing type silicone resin is 1:100～2:100;
By described mixing uniform mixture, at air pressure, be that 100～300MPa temperature is to vulcanize 3～15 minutes under the condition of 160～180 ℃, obtain high heat conduction elastic composite.
In conjunction with second aspect, in the first implementation of second aspect, described composite heat-conducting filler comprises the heat conduction powder of carbon nanotube and 0.1～100 micron, and described composite heat-conducting filler preparation method comprises:
Heat conduction powder described in 20g is distributed in the aqueous solution that 100ml concentration is 1Mol/L Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and obtains the first mixing solutions, by even post-heating to 70～90 ℃ of described the first mixing solutions supersound process in ultrasonic oscillator, in heat-processed, described the first mixing solutions is carried out to mechanical stirring, then in described the first mixing solutions, dropwise add ammoniacal liquor to obtain the second mixing solutions, until described the second mixing solutions pH value is more than or equal to 12, described the second mixing solutions is heated one hour and stirred simultaneously at the temperature of 70～90 ℃, then from described the second mixing solutions, filter out solids, and water rinses described solids repeatedly to neutrality, finally by rinsing extremely neutral solids, more than 100 ℃, dry and grind to form micro mist,
The described micro mist grinding to form is put into the reactor of 600～800 ℃, in described reactor, pass into pure nitrogen gas, by after emptying the air in described reactor, pass into the mixed gas that comprises nitrogen and acetylene gas, nitrogen in described mixed gas and the throughput ratio of acetylene are 3:1～10:1, wherein acetylene flow is 0.3L/MIN, thereby catalytic pyrolysis acetylene gas, make carbon laydown in acetylene in described micro mist Surface Creation carbon nanotube, surface coverage has the micro mist of carbon nanotube to be described composite heat-conducting filler.
In conjunction with second aspect, in the second implementation of second aspect, described composite heat-conducting filler comprises the heat conduction powder of carbon nanotube and 0.1～100 micron, and described composite heat-conducting filler preparation method comprises:
Heat conduction powder described in 20g is distributed in the aqueous solution that 100ml concentration is 1Mol/L Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and obtains the first mixing solutions, by even post-heating to 70～90 ℃ of described the first mixing solutions supersound process in ultrasonic oscillator, in heat-processed, described the first mixing solutions is carried out to mechanical stirring, then in described the first mixing solutions, dropwise add ammoniacal liquor to obtain the second mixing solutions, until described the second mixing solutions pH value is more than or equal to 12, described the second mixing solutions is heated one hour and stirred simultaneously at the temperature of 70～90 ℃, then from described the second mixing solutions, filter out solids, and water rinses described solids repeatedly to neutrality, finally by rinsing extremely neutral solids, more than 100 ℃, dry and grind to form micro mist,
The described micro mist grinding to form is put into the reactor of 600～800 ℃, in described reactor, pass into pure nitrogen gas, by after emptying the air in described reactor, pass into the mixed gas that comprises nitrogen and acetylene gas, nitrogen in described mixed gas and the throughput ratio of acetylene are 3:1～10:1, wherein acetylene flow is 0.3L/MIN, thereby catalytic pyrolysis acetylene gas, make carbon laydown in acetylene in described micro mist Surface Creation carbon nanotube, surface coverage has the micro mist of carbon nanotube to be described composite heat-conducting filler.
In conjunction with the first implementation of second aspect or second aspect or the second implementation of second aspect, in the third implementation of second aspect, described vulcanizing agent comprises 2,5-dimethyl-2,5-di-t-butyl peroxy hexane.
In conjunction with the third mode of the first implementation of second aspect or second aspect or the second implementation of second aspect or second aspect, in the 4th kind of implementation of second aspect, described heat conduction powder comprises one or the mixture in alpha-phase aluminum oxide, γ phase alumina.
In conjunction with the third mode of the first implementation of second aspect or second aspect or the second implementation of second aspect or second aspect or the 4th kind of implementation of second aspect, in the 5th kind of implementation of second aspect, described curing type silicone resin comprises addition curable silicone resin.
In conjunction with the first implementation of first aspect, in the third implementation of first aspect,
Described carbon nanotube and described heat conduction micro mist form composite heat-conducting filler, and described composite heat-conducting filler forming process comprises:
Choose granularity at the heat conduction powder of 0.1～100 micron;
The heat conduction powder of choosing is placed in the High Temperature Furnaces Heating Apparatus of 1200～1600 ℃ and is incubated 2～8 hours, atmosphere surrounding is air, then carries out naturally cooling, obtains pure heat conduction powder;
Pure heat conduction powder described in 20g is scattered in the cetyl trimethylammonium bromide aqueous solution that 1 liter of concentration is 1%, and high-speed stirring evenly obtains dispersion;
The ultrasonic concussion at normal temperatures of described graphene oxide or high speed shear are become to dispersion soln, and the concentration of described dispersion soln is 0.1～2g/L;
Described dispersion soln is joined in described dispersion to dispersed with stirring 30 minutes, and then filtering drying then heats, thereby obtains composite heat-conducting filler in 200～300 degree air.
In conjunction with the third implementation of the first implementation of first aspect or the second implementation of first aspect or first aspect, in the 4th kind of implementation of first aspect, described heat conduction powder is one or the mixture in alpha-phase aluminum oxide, γ phase alumina.
In conjunction with the third implementation of the first implementation of first aspect or first aspect or the second implementation first aspect of first aspect or the 4th kind of implementation of first aspect, in the 5th kind of implementation of first aspect, described high heat conduction elastic composite preparation method comprises:
On mixing roll or kneader, mix the rubber of organo-silicone rubber, by the weight percent of 1:100～2:100, add after vulcanizing agent and described high heat conductive filler, mixing even;
Described mixing uniform mixture is put into vulcanizing press, is that 100～300MPa temperature is to vulcanize 3～15 minutes under the condition of 160～180 ℃ at air pressure, obtains high heat conduction elastic composite.
In conjunction with the 5th kind of implementation of first aspect, in the 7th kind of implementation of first aspect, described vulcanizing agent is 2,5-dimethyl-2,5-di-t-butyl peroxy hexane.
In conjunction with the 4th kind of implementation of the third implementation of the first implementation of first aspect or first aspect or the second implementation first aspect of first aspect or first aspect or the 5th kind of implementation of first aspect, in the 6th kind of implementation of first aspect, described curing type silicone resin is addition curable organosilicon material.
From the above, the high heat conduction elastic composite that the embodiment of the present invention provides comprises aluminum oxide, carbon nanotube and Graphene, and wherein, aluminum oxide hardness is high, good stability of the dimension, particularly improves material thermal conductivity energy aspect particularly remarkable; Meanwhile, carbon nanotube is the one-dimensional carbon nano material that degree of graphitization is high, and covalent bonds is conducive to phonon transport, and its heat conductivility is also very high; Aluminum oxide form is particulate state, need larger volume content could realize the perforation of passage of heat, and carbon nanotube diameter is little, and length is long.The two realizes combination, and namely carbon nano tube growth, on the surface of alpha-phase aluminum oxide particle, is compared with the two physical mixed, can obtain more thermal conducting path, further improves the overall thermal conductivity energy of matrix material; Graphene has high thermal conductivity, and Graphene and alumina composite can not only improve thermal conduction characteristic, can also improve the anti-corrosion capability of material.
Accompanying drawing explanation
Fig. 1 is the SEM figure (scanning electron microscope, scanning electronic microscope) that is deposited on alumina surface carbon nanotube in the embodiment of the present invention one;
Fig. 2 is the SEM figure that is deposited on alumina surface carbon nanotube in the embodiment of the present invention two.
Embodiment
embodiment mono-
The embodiment of the present invention provides a kind of high heat conduction elastic composite, this high heat conduction elastic composite comprises curing type silicone resin and composite heat-conducting filler, being dispersed in this curing type silicone resin of this composite heat-conducting uniform filling, the weight percent of this curing type silicone resin is 20%～60%, and the weight percent of this composite heat-conducting filler is 40%～80%.This high heat conduction elastic composite technique is simple, with short production cycle, product density is little, good springiness, product erosion resistance, resistance to elevated temperatures are good.
Wherein, this curing type silicone resin comprises addition curable silicone resin, and for example molecular weight is at 40～600,000 methyl vinyl silicone rubber.
Wherein, this composite heat-conducting filler comprises the heat conduction powder of any and 0.1～100 micron in carbon nanotube and graphene oxide.This heat conduction powder comprises one or the mixture in alpha-phase aluminum oxide, γ phase alumina.
embodiment bis-
The embodiment of the present invention provides a kind of preparation method of high heat conduction elastic composite, and this preparation method comprises: on machine, by mixing to curing type silicone resin, composite heat-conducting filler and vulcanizing agent even, wherein, machine can be mixing roll or kneader; Wherein, this curing type silicone resin accounts for 20%～60% of curing type silicone resin and composite heat-conducting filler gross weight, this composite heat-conducting filler accounts for 40%～80% of curing type silicone resin and composite heat-conducting filler gross weight, the weight percent of this vulcanizing agent and this curing type silicone resin is 1:100～2:100, this vulcanizing agent can be 2,5-dimethyl-2,5-di-t-butyl peroxy hexane;
By described mixing uniform mixture, at air pressure, be that 100～300MPa temperature is to vulcanize 3～15 minutes under the condition of 160～180 ℃, obtain high heat conduction elastic composite, wherein, described mixing uniform mixture can be put into vulcanizing press and vulcanize.
embodiment tri-
Composite heat-conducting filler as depicted in figs. 1 and 2, this composite heat-conducting filler is related in embodiment bis-, the embodiment of the present invention provides a kind of preparation method of composite heat-conducting filler, this composite heat-conducting filler comprises the heat conduction powder of carbon nanotube and 0.1～100 micron, and this composite heat-conducting filler is preparation method comprise:
Heat conduction powder described in 20g is distributed in the aqueous solution that 100ml concentration is 1Mol/L Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and obtains the first mixing solutions, by even post-heating to 70～90 ℃ of described the first mixing solutions supersound process in ultrasonic oscillator, in heat-processed, described the first mixing solutions is carried out to mechanical stirring, then in described the first mixing solutions, dropwise add ammoniacal liquor to obtain the second mixing solutions, until described the second mixing solutions pH value is more than or equal to 12, described the second mixing solutions is heated one hour and stirred simultaneously at the temperature of 70～90 ℃, then from described the second mixing solutions, filter out solids, and water rinses described solids repeatedly to neutrality, finally by rinsing extremely neutral solids, more than 100 ℃, dry and grind to form micro mist,
The described micro mist grinding to form is put into the reactor of 600～800 ℃, in described reactor, pass into pure nitrogen gas, by after emptying the air in described reactor, pass into the mixed gas that comprises nitrogen and acetylene gas, nitrogen in described mixed gas and the throughput ratio of acetylene are 3:1～10:1, wherein acetylene flow is 0.3L/MIN, thereby catalytic pyrolysis acetylene gas, make carbon laydown in acetylene in described micro mist Surface Creation carbon nanotube, surface coverage has the micro mist of carbon nanotube to be described composite heat-conducting filler.
embodiment tetra-
In another embodiment of the present invention, the preparation method of the composite heat-conducting filler that the high heat conduction elastic composite manufacture method of describing according to embodiment bis-and embodiment tri-describe, makes high heat conduction elastic composite concrete steps and is:
Selecting D50 is 25 microns of alpha-phase aluminum oxides, through 1300 degree calcining 8 hours, on its surface, carries out after catalyst deposit, under 750 degree, after cracking acetylene, obtains carbon nanotube/alumina composite heat conductive filler.After this composite heat-conducting filler (weight percent is 50%) is mixed with the trade mark 110 methyl vinyl silicone rubbers (weight percent is 50%) and vulcanizing agent, in vacuum 180, spend under 100MPa pressure and vulcanize moulding in 10 minutes, obtain high heat conduction elastic composite.The thermal conductivity of measuring its vertical hot-press vulcanization direction is 0.67W/mK.
Another concrete steps that make high heat conduction elastic composite are:
Selecting D50 is 5 microns of γ phase alumina, through 1200 degree calcining 2 hours, on its surface, carries out after catalyst deposit, under 700 degree, after cracking acetylene, obtains carbon nanotube/alumina composite heat conductive filler.After its (weight percent is 60%) mixed with the trade mark 110 methyl vinyl silicone rubbers (weight percent is 40%) and vulcanizing agent, in vacuum 160, spend under 100MPa pressure and vulcanize moulding in 3 minutes, obtain high heat conduction elastic composite.The thermal conductivity of measuring its vertical hot-press vulcanization direction is 0.78W/mK.
From the above, the high heat conduction elastic composite that the embodiment of the present invention provides comprises aluminum oxide, carbon nanotube, and wherein, aluminum oxide hardness is high, good stability of the dimension, particularly improves material thermal conductivity energy aspect particularly remarkable; Meanwhile, carbon nanotube is the one-dimensional carbon nano material that degree of graphitization is high, and covalent bonds is conducive to phonon transport, and its heat conductivility is also very high;
Further, aluminum oxide form is particulate state, need larger volume content could realize the perforation of passage of heat, and carbon nanotube diameter is little, and length is long.The two realizes combination, and namely carbon nano tube growth, on the surface of alpha-phase aluminum oxide particle, is compared with the two physical mixed, can obtain more thermal conducting path, further improves the overall thermal conductivity energy of matrix material.
embodiment five
Composite heat-conducting filler as depicted in figs. 1 and 2, this composite heat-conducting filler is related in embodiment bis-, the embodiment of the present invention provides the preparation method of another kind of composite heat-conducting filler, the heat conduction powder of this composite heat-conducting filler graphene oxide and 0.1～100 micron, this composite heat-conducting filler is preparation method comprise:
Heat conduction powder described in 20g is scattered in the cetyl trimethylammonium bromide aqueous solution that 1 liter of concentration is 1%, and high-speed stirring evenly obtains dispersion;
The ultrasonic concussion at normal temperatures of described graphene oxide or high speed shear are become to dispersion soln, and the concentration of described dispersion soln is 0.1～2g/L;
Described dispersion soln is joined in described dispersion and stirred 30 minutes, and then filtering drying obtains solids, then described solids is heated in 200～300 degree air, thereby obtains described composite heat-conducting filler.
embodiment six
In another embodiment of the present invention, the preparation method of the composite heat-conducting filler that the high heat conduction elastic composite manufacture method of describing according to embodiment bis-and embodiment five describe, makes high heat conduction elastic composite concrete steps and is:
Selecting D50 is 5 microns of γ phase alumina, through 1400 degree calcining 4 hours, on its surface, deposits after graphene oxide, under 200 degree, heats, and obtains Graphene/alumina composite heat conductive filler.After its (weight percent is 60%) mixed with the trade mark 110 methyl vinyl silicone rubbers (weight percent is 40%) and vulcanizing agent, in vacuum 170, spend under 100MPa pressure and vulcanize moulding in 5 minutes, obtain high heat conduction elastic composite.The thermal conductivity of measuring its vertical hot-press vulcanization direction is 0.82W/mK.
Another concrete steps that make high heat conduction elastic composite are:
Selecting D50 is 25 microns of alpha-phase aluminum oxides, through 1500 degree calcining 8 hours, after its surface deposition graphene oxide, under 300 degree, heats, and obtains Graphene/alumina composite heat conductive filler.After its (weight percent is 50%) mixed with the trade mark 110 methyl vinyl silicone rubbers (weight percent is 50%) and vulcanizing agent, in vacuum 180, spend under 100MPa pressure and vulcanize moulding in 8 minutes, obtain high heat conduction elastic composite.The thermal conductivity of measuring its vertical hot-press vulcanization direction is 0.72W/mK.
From the above, the high heat conduction elastic composite that the embodiment of the present invention provides comprises aluminum oxide and Graphene, and wherein, aluminum oxide hardness is high, good stability of the dimension, particularly improves material thermal conductivity energy aspect particularly remarkable; Graphene has high thermal conductivity, and Graphene and alumina composite can not only improve thermal conduction characteristic, can also improve the anti-corrosion capability of material.
Below by embodiment, the present invention is specifically described; the present embodiment is only for the present invention is described further; can not be interpreted as limiting the scope of the invention; those skilled in the art's content according to the present invention is made some nonessential change and adjustment, all belongs to protection scope of the present invention.
Claims (9)
1. one kind high heat conduction elastic composite, it is characterized in that, described matrix material comprises curing type silicone resin and composite heat-conducting filler, being dispersed in described curing type silicone resin of described composite heat-conducting uniform filling, the weight percent of described curing type silicone resin is 20%～60%, the weight percent of described composite heat-conducting filler is 40%～80%, and described composite heat-conducting filler comprises the heat conduction powder of any and 0.1～100 micron in carbon nanotube and graphene oxide.
2. high heat conduction elastic composite as claimed in claim 1, is characterized in that, described heat conduction powder comprises one or the mixture in alpha-phase aluminum oxide, γ phase alumina.
3. high heat conduction elastic composite as claimed in claim 1 or 2, is characterized in that, described curing type silicone resin comprises addition curable silicone resin.
4. a preparation method for high heat conduction elastic composite, is characterized in that, described preparation method comprises:
By mixing to curing type silicone resin, composite heat-conducting filler and vulcanizing agent even, wherein, described curing type silicone resin accounts for 20%～60% of described curing type silicone resin and described composite heat-conducting filler gross weight, described composite heat-conducting filler accounts for 40%～80% of described curing type silicone resin and described composite heat-conducting filler gross weight, and the weight percent of described vulcanizing agent and described curing type silicone resin is 1:100～2:100;
By described mixing uniform mixture, at air pressure, be that 100～300MPa temperature is to vulcanize 3～15 minutes under the condition of 160～180 ℃, obtain high heat conduction elastic composite.
5. preparation method as claimed in claim 4, is characterized in that, described composite heat-conducting filler comprises the heat conduction powder of carbon nanotube and 0.1～100 micron, and described composite heat-conducting filler preparation method comprises:
Heat conduction powder described in 20g is distributed in the aqueous solution that 100ml concentration is 1Mol/L Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and obtains the first mixing solutions, by even post-heating to 70～90 ℃ of described the first mixing solutions supersound process in ultrasonic oscillator, in heat-processed, described the first mixing solutions is carried out to mechanical stirring, then in described the first mixing solutions, dropwise add ammoniacal liquor to obtain the second mixing solutions, until described the second mixing solutions pH value is more than or equal to 12, described the second mixing solutions is heated one hour and stirred simultaneously at the temperature of 70～90 ℃, then from described the second mixing solutions, filter out solids, and water rinses described solids repeatedly to neutrality, finally by rinsing extremely neutral solids, more than 100 ℃, dry and grind to form micro mist,
The described micro mist grinding to form is put into the reactor of 600～800 ℃, in described reactor, pass into pure nitrogen gas, by after emptying the air in described reactor, pass into the mixed gas that comprises nitrogen and acetylene gas, nitrogen in described mixed gas and the throughput ratio of acetylene are 3:1～10:1, wherein acetylene flow is 0.3L/MIN, thereby catalytic pyrolysis acetylene gas, make carbon laydown in acetylene in described micro mist Surface Creation carbon nanotube, surface coverage has the micro mist of carbon nanotube to be described composite heat-conducting filler.
6. preparation method as claimed in claim 4, is characterized in that, described composite heat-conducting filler comprises the heat conduction powder of graphene oxide and 0.1～100 micron, and described composite heat-conducting filler preparation method comprises:
Heat conduction powder described in 20g is scattered in the cetyl trimethylammonium bromide aqueous solution that 1 liter of concentration is 1%, and high-speed stirring evenly obtains dispersion;
The ultrasonic concussion at normal temperatures of described graphene oxide or high speed shear are become to dispersion soln, and the concentration of described dispersion soln is 0.1～2g/L;
Described dispersion soln is joined in described dispersion and stirred 30 minutes, and then filtering drying obtains solids, then described solids is heated in 200～300 degree air, thereby obtains described composite heat-conducting filler.
7. according to the arbitrary described preparation method of claim 4 to 6, it is characterized in that, described vulcanizing agent comprises 2,5-dimethyl-2,5-di-t-butyl peroxy hexane.
8. the preparation method as described in as arbitrary in claim 4 to 7, is characterized in that, described heat conduction powder comprises one or the mixture in alpha-phase aluminum oxide, γ phase alumina.
9. the preparation method as described in as arbitrary in claim 4 to 8, is characterized in that, described curing type silicone resin comprises addition curable silicone resin.
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