CN104119627A - Heat conductive composite material with high volume fraction and preparation method thereof - Google Patents

Heat conductive composite material with high volume fraction and preparation method thereof Download PDF

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CN104119627A
CN104119627A CN201410336024.4A CN201410336024A CN104119627A CN 104119627 A CN104119627 A CN 104119627A CN 201410336024 A CN201410336024 A CN 201410336024A CN 104119627 A CN104119627 A CN 104119627A
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composite material
heat
conductive composite
heat conductive
conductive
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CN104119627B (en
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刘剑
唐榕
刘子仪
彭汝芳
楚士晋
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Southwest University of Science and Technology
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Southwest University of Science and Technology
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Abstract

The invention discloses a heat conductive composite material with a high volume fraction. The composite material is characterized by being composed of a heat conductive filling material, which is irregularly stacked to form a heat conductive network and accounts for 90 to 99% of the total weight of the composite material, and a polymer adhesive, which is dispersed in the cavities in the heat conductive network and accounts for 1 to 10% of the total weight of the composite material, wherein the heat conductive filling material is high heat conductive carbon-base micro nano powder. The moulded products can be prepared through the steps of direct mixing and hot press molding, and the preparation efficiency is high. The preparation of the composite material is simple and convenient. Moreover the content of the high heat conductive carbon-base micro nano powder filling material is high, so the composite material can meet the realistic requirements on massive production. The prepared heat conductive composite material has an excellent heat conductive performance and mechanical properties, also has a certain electric conductive performance, and can be used in fields like 3D printing materials, notebook, large power LED luminescence, panel display, digital camera, and mobile communication products and related compact and high-speed electronic elements.

Description

A kind of high-volume fractional heat-conductive composite material and preparation method thereof
Technical field
The invention belongs to carbon back heat-conductive composite material, relate to a kind of high-volume fractional heat-conductive composite material and preparation method thereof, particularly a kind ofly take high-volume fractional heat-conductive composite material that highly-conductive hot carbon based micro-nano powder is filler and preparation method thereof.High-volume fractional heat-conductive composite material of the present invention is mainly used in 3D printed material, notebook computer, high-power LED illumination, flat-panel monitor, Digital Video and mobile communication product and relevant microminiaturization and the electronic devices and components field of high speed.
Background technology
In recent years, along with microelectronics is integrated, develop rapidly with package technique, the microminiaturized degree of unicircuit is more and more higher, and the volume of electronic devices and components and logical circuit becomes thousands of times and dwindles, and the thermal value of the electronic package in integrated circuit modules unit surface is increased severely.For assurance electronic devices and components, normally work highly reliably for a long time, must stop the continuous rising of working temperature, therefore, need to effectively dispel the heat to integrated circuit modules, in the urgent need to the polymer materials of development high thermal conductivity.Carbon back micro-nano powder has high specific surface area, mechanical property, remarkable thermal characteristics, and carbon back filler wherein, as graphite (209Wm -1k -1), carbon nanotube (3100~3500Wm -1k -1), diamond (2000Wm -1k -1), Graphene (4840~5300Wm -1k -1) etc. there is the thermal conductivity of superelevation, the thermal conductivity that uses it to improve polymeric matrix enjoys the favor of academia and industry member, and gives great expectations.In prior art, people have adopted traditional heat-conductive composite material making method, by carbon nanotube (as: multi-walled carbon nano-tubes, Single Walled Carbon Nanotube), carbon nanofiber, the carbon materials such as soccerballene, as filler powder, are distributed in macromolecule matrix material, make heat-conductive composite material.Yet, adopt existing making method to prepare heat-conductive composite material and mainly have following problem: (1) is because the specific surface area of filler powder is large, increase along with filler content, reactive force between filler strengthens, and then cause detrimentally affect to the dispersion of filler, make the loading level of filler limited, directly affect the formation of heat conduction network in polymeric matrix, affect the heat conductivility of matrix material.(2) traditional heat-conductive composite material preparation method, complex steps, consumes energy larger, causes preparing matrix material cost higher, is difficult to apply in industrial production.
Summary of the invention
Object of the present invention is intended to overcome deficiency of the prior art, a kind of high-volume fractional heat-conductive composite material and preparation method thereof is provided, the present invention can effectively overcome because fillers dispersed is difficult, the limited heat conduction network causing of loading level is discontinuous, makes the deficiency that thermal conductivity of composite materials is low, radiating effect is poor; Overcome in preparation process that power consumption is large, cost is high, be difficult to be applied to the technical problem in industrial production; A kind of method of easy, efficient heat-conductive composite material is provided, method of the present invention can directly be prepared the heat-conductive composite material of the micro-nano filler of high-volume fractional carbon back, significantly improve the mechanical property of polymer materials, give polymer materials many new functions simultaneously, show especially the high thermal conductivity aspect of material, realize multi-functional high-strength composite material, and can meet the actual requirement of production in enormous quantities.
Content of the present invention is: a kind of high-volume fractional heat-conductive composite material, it is characterized in that: by irregular stacking, form the heat conductive filler that heat conduction network, mass percent are 90~99%, and be scattered in described heat conduction network space, polymeric binder that mass percent is 1~10% forms;
Described heat conductive filler is highly-conductive hot carbon base micro nano powder.
In content of the present invention: described highly-conductive hot carbon base micro nano powder filler can be:
Single Walled Carbon Nanotube (can be Timestub tM-high-purity Single Walled Carbon Nanotube, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, model: TNS, outside diameter OD is 1~2nm, purity (Purity>=90wt%), length is 5~30 μ m, specific surface area SSA>=380m 2/ g, ash content≤1.5wt%, electric conductivity EC>=100s/cm, bulk density (Tap Density) is 0.14g/cm 3),
Multi-walled carbon nano-tubes (can be Timestub tM-high-purity Single Walled Carbon Nanotube, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, model: TNM1, outside diameter OD>=50nm, purity (Purity>=90wt%), length is 10~30 μ m, specific surface area SSA>=40m 2/ g, ash content≤5wt%, electric conductivity EC>=100s/cm, bulk density (Tap Density) is 0.27g/cm 3),
Graphene (can be TimesGraph tM-Graphene, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, purity (Purity>=95wt%), specific surface area SSA>=554.364m 2/ g, diameter is 0.5~3 μ m, and the number of plies is 1~10 layer, and thickness is 0.55~3.74nm; Or soccerballene C 60, purity (>=98wt%), fusing point>=280 ℃, burning-point>=94 ℃) or
(can be C-25 carbon nanofiber, Anshan Sinocrab Carbon Fiber Co., Ltd. produces carbon nanofiber, specific surface area SSA>=1000m 2/ g).
In content of the present invention: described polymeric binder can (be called for short PTFE for tetrafluoroethylene, manufacturing enterprise has: Shanghai three is liked rich, product type is: FR002A, hugeization of Zhejiang, trade mark JTC-305), polymethylmethacrylate (is called for short PMMA, manufacturing enterprise has: SUMITOMO CHEMICAL, trade mark HT03Y, France Arkema, trade mark V04l resin), (manufacturing enterprise has viton: middle Wu Chenguang chemical institute etc., trade mark FPM2606 resin), or nylon (is called for short PA, manufacturing enterprise has: Shen Ma engineering plastics company etc., nylon-66, nylon-6) resin such as, be common commercial commercialization high molecular synthetic resin.
Described polymeric binder (for example PTFE, PMMA, PA's etc.) number-average molecular weight can be 100,000~200,000.
Described polymeric binder is polymer powder, and the particle diameter of this polymer powder is 40 μ m~100 μ m preferably.
The particle diameter of described highly-conductive hot carbon base micro nano powder filler is 0.5 μ m~50 μ m preferably.
Another content of the present invention is: a kind of preparation method of high-volume fractional heat-conductive composite material, is characterized in that step is:
A, outfit raw material: the mass percent proportioning by heat conductive filler 90~99%, polymeric binder 1~10% is got heat conductive filler and polymeric binder;
B, mixing: heat conductive filler and polymer powder are uniformly mixed to (mixing time can be 1~3min) through (directly at a high speed), make modeling powder;
C, moulding: the modeling powder making is put into forming mould, after moulding, the demoulding, make high-volume fractional heat-conductive composite material.Moulding object is to make polymeric binder melt-flow in the process of compacting, fully fills the space between filler small-particle, thereby strengthens gravitation and adhesive power between small-particle, strengthens the thermal conductivity of profiled member and relevant mechanical property.
In another content of the present invention: the stir speed (S.S.) that described in step b, (at a high speed) is uniformly mixed is 25000 revs/min preferably.
In another content of the present invention: be shaped to hot-formingly described in step c, that is: will forming mould heat-insulation pressure keeping 0.5~3h under the condition of 200~400 ℃ of temperature, pressure 20~200KN of modeling powder be housed.
In another content of the present invention: described in the raw material heat conductive filler and the polymeric binder that obtain before mixing, carry out drying treatment, that is: in convection oven, in temperature, be forced air drying 10~20h under the condition of 100~120 ℃.
In another content of the present invention: described highly-conductive hot carbon base micro nano powder filler can be:
Single Walled Carbon Nanotube (can be Timestub tM-high-purity Single Walled Carbon Nanotube, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, model: TNS, outside diameter OD is 1~2nm, purity (Purity>=90wt%), length is 5~30 μ m, specific surface area SSA>=380m 2/ g, ash content≤1.5wt%, electric conductivity EC>=100s/cm, bulk density (Tap Density) is 0.14g/cm 3),
Multi-walled carbon nano-tubes (can be Timestub tM-high-purity Single Walled Carbon Nanotube, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, model: TNM1, outside diameter OD>=50nm, purity (Purity>=90wt%), length is 10~30 μ m, specific surface area SSA>=40m 2/ g, ash content≤5wt%, electric conductivity EC>=100s/cm, bulk density (Tap Density) is 0.27g/cm 3),
Graphene (can be TimesGraph tM-Graphene, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, purity (Purity>=95wt%), specific surface area SSA>=554.364m 2/ g, diameter is 0.5~3 μ m, and the number of plies is 1~10 layer, and thickness is 0.55~3.74nm; Or soccerballene C 60, purity (>=98wt%), fusing point>=280 ℃, burning-point>=94 ℃) or
(can be C-25 carbon nanofiber, Anshan Sinocrab Carbon Fiber Co., Ltd. produces carbon nanofiber, specific surface area SSA>=1000m 2/ g).
In another content of the present invention: described polymeric binder can (be called for short PTFE for tetrafluoroethylene, manufacturing enterprise has: Shanghai three is liked rich, product type is: FR002A, hugeization of Zhejiang, trade mark JTC-305), polymethylmethacrylate (is called for short PMMA, manufacturing enterprise has: SUMITOMO CHEMICAL, trade mark HT03Y, France Arkema, trade mark V04l resin), (manufacturing enterprise has viton: middle Wu Chenguang chemical institute etc., trade mark FPM2606 resin), or nylon (is called for short PA, manufacturing enterprise has: Shen Ma engineering plastics company etc., nylon-66, nylon-6) resin such as, be common commercial commercialization high molecular synthetic resin.
For example, in another content of the present invention: described polymeric binder (PTFE, PMMA, PA's etc.) number-average molecular weight can be 100,000~200,000.
In another content of the present invention: described polymeric binder is polymer powder, the particle diameter of this polymer powder is 40 μ m~100 μ m preferably.
In another content of the present invention: the particle diameter of described highly-conductive hot carbon base micro nano powder filler is 0.5 μ m~50 μ m preferably.
Compared with prior art, the present invention has following feature and beneficial effect:
(1) the present invention adopts and is directly uniformly mixed legal system for the heat-conductive composite material of the micro-nano filler of high-volume fractional carbon back, and by hot-forming mode, make the high-volume fractional heat-conductive composite material of moulded products, preparation efficiency is high, the high-volume fractional heat-conductive composite material of preparing has excellent heat conductivility and mechanical property, has certain electroconductibility;
(2) thermal conductivity of the high-volume fractional heat-conductive composite material that employing the present invention makes is 1~30Wm -1k -1, specific conductivity is 0.5~5Sm -1, ultimate compression strength is 10~50MPa, tensile strength is 5~15MPa; Can be applied to 3D printed material, notebook computer, high-power LED illumination, flat-panel monitor, Digital Video and mobile communication product and relevant microminiaturization and the association areas such as electronic devices and components of high speed;
(3) adopt the present invention, can effectively overcome because fillers dispersed is difficult, the limited heat conduction network causing of loading level is discontinuous, make the deficiency that thermal conductivity of composite materials is low, radiating effect is poor; Overcome in preparation process that power consumption is large, cost is high, be difficult to be applied to the technical problem in industrial production; A kind of method of easy, efficient heat-conductive composite material is provided, the present invention can directly prepare the heat-conductive composite material of the micro-nano filler of high-volume fractional carbon back, significantly improve the mechanical property of polymer materials, give polymer materials many new functions simultaneously, the high thermal conductivity aspect that shows especially material, realizes multi-functional high-strength composite material; The present invention adopts and is directly uniformly mixed legal system for heat-conductive composite material, and the content of highly-conductive hot carbon based micro-nano powder stuffing is high, can reach 90~99wt%, and simple and feasible, can meet the actual requirement of production in enormous quantities, is conducive to apply in industrial production;
(4) product preparation process of the present invention is simple, and operation is easy, and feasibility is high, practical.
Embodiment
The invention will be further described for embodiment plan given below; but can not be interpreted as it is limiting the scope of the invention; some nonessential improvement and adjustment that person skilled in art makes the present invention according to the content of the invention described above, still belong to protection scope of the present invention.
Embodiment 1:
A high-volume fractional heat-conductive composite material, mass percent consists of: carbon nanotube (can be Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, rear same) 97wt%, tetrafluoroethylene 3wt%.
The preparation method of described high-volume fractional heat-conductive composite material, step is:
A, carbon back filler 97wt% and tetrafluoroethylene 3wt% are put into convection oven, forced air drying 15h at the temperature of 120 ℃;
B, fully dry carbon back filler powder and polymeric binder powder are put into high-speed multifunctional pulverizer, high-speed stirring is mixed 2min, and stir speed (S.S.) is 25000 revs/min, makes well-mixed modeling powder;
C, more well-mixed modeling powder is packed in forming mould equably, the mould that modeling powder is housed is incubated to 2h at the temperature of 340 ℃; To forming mould pressurize 2h under the pressure of 120KN of Composite modelling powder be housed simultaneously;
D, treat heat-insulation pressure keeping EO, after shaping and demoulding, make heat-conductive composite material molded article; Hot-forming object is to make polymeric binder melt-flow in the process of compacting, fully fill the space between small-particle, thereby the gravitation between enhancing small-particle and adhesive power, heat conduction, conductivity and other relevant mechanical properties etc. of enhancing profiled member.By compacting, make the molded article of high-volume fractional heat-conductive composite material.
The performance test data of the high-volume fractional heat-conductive composite material making is as follows: thermal conductivity: 15.6Wm -1k -1, ultimate compression strength: 29.47MPa, tensile strength: 8.78MPa.
Embodiment 2:
The preparation technology of the present embodiment high-volume fractional heat-conductive composite material is with reference to embodiment 1, compare with embodiment 1, its processing parameter is basic identical, just changes the proportioning of material, and the mass percent proportioning of high-volume fractional heat-conductive composite material is: carbon nanotube 94wt%, tetrafluoroethylene 6wt%.
The performance test data of the high-volume fractional heat-conductive composite material obtaining is as follows: thermal conductivity: 13.2Wm -1k -1, ultimate compression strength: 35.68MPa, tensile strength: 10.93MPa.
Embodiment 3:
The preparation technology of the present embodiment high-volume fractional heat-conductive composite material is with reference to embodiment 1, compare with embodiment 1, its processing parameter is basic identical, just changes the proportioning of material, the mass percent proportioning of high-volume fractional heat-conductive composite material is: carbon nanotube 90wt%, tetrafluoroethylene 10wt%.
The performance test data of the high-volume fractional heat-conductive composite material obtaining is as follows: thermal conductivity: 10.53Wm -1k -1, ultimate compression strength: 45.38MPa, tensile strength: 12.52MPa.
Embodiment 4:
The mass percent of the present embodiment high-volume fractional heat-conductive composite material forms with embodiment 1; Preparation technology, with reference to embodiment 1, compares with embodiment 1, and its processing parameter is basic identical, just changes the hot pressing temperature in hot-forming process, and temperature is 200 ℃.
The performance test data of the high-volume fractional heat-conductive composite material obtaining is as follows: thermal conductivity: 12.3Wm -1k -1, ultimate compression strength: 24.56MPa, tensile strength: 6.95MPa.
Embodiment 5:
The mass percent of the present embodiment high-volume fractional heat-conductive composite material forms with embodiment 1; Preparation technology, with reference to embodiment 1, compares with embodiment 1, and its processing parameter is basic identical, just changes the hot pressing temperature in hot-forming process, and temperature is 25 ℃ of room temperatures.
The performance test data of the high-volume fractional heat-conductive composite material obtaining is as follows: thermal conductivity: 9.6Wm -1k -1, ultimate compression strength: 18.64MPa, tensile strength: 4.71MPa.
Embodiment 6:
The mass percent of the high-volume fractional heat-conductive composite material of the present embodiment forms with embodiment 1; Preparation technology, with reference to embodiment 1, compares with embodiment 1, and its processing parameter is basic identical, just changes the pressing pressure in hot-forming process, and pressure is 60KN.
The performance test data of the high-volume fractional heat-conductive composite material obtaining is as follows: thermal conductivity: 8.2Wm -1k -1, ultimate compression strength: 21.75MPa, tensile strength: 5.12MPa.
Embodiment 7:
A high-volume fractional heat-conductive composite material, forms by irregular stacking the heat conductive filler that heat conduction network, mass percent are 95%, and be scattered in described heat conduction network space, polymeric binder that mass percent is 5% forms; Described heat conductive filler is highly-conductive hot carbon base micro nano powder.
Embodiment 8~14:
A high-volume fractional heat-conductive composite material, forms by irregular stacking the heat conductive filler that heat conduction network, mass percent are 90~99%, and be scattered in described heat conduction network space, polymeric binder that mass percent is 1~10% forms; Described heat conductive filler is highly-conductive hot carbon base micro nano powder; In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
Embodiment 15:
A preparation method for high-volume fractional heat-conductive composite material, step is:
A, outfit raw material: the mass percent proportioning by heat conductive filler 95%, polymeric binder 5% is got heat conductive filler and polymeric binder;
B, mixing: heat conductive filler and polymeric binder are uniformly mixed to (mixing time can be 2min) through (directly at a high speed), make modeling powder;
C, moulding: the modeling powder making is put into forming mould, after moulding, the demoulding, make high-volume fractional heat-conductive composite material.Moulding object is to make polymeric binder melt-flow in the process of compacting, fully fills the space between filler small-particle, thereby strengthens gravitation and adhesive power between small-particle, strengthens the thermal conductivity of profiled member and relevant mechanical property;
The stir speed (S.S.) that described in step b, (at a high speed) is uniformly mixed is 25000 revs/min;
Described in step c, be shaped to hot-formingly, that is: will forming mould heat-insulation pressure keeping 1.5h under the condition of 300 ℃ of temperature, pressure 110KN of modeling powder be housed;
The described raw material heat conductive filler of obtaining and polymeric binder are carried out drying treatment before mixing, that is: in convection oven, be forced air drying 15h under the condition of 130 ℃ in temperature.
Embodiment 16:
A preparation method for high-volume fractional heat-conductive composite material, step is:
A, outfit raw material: the mass percent proportioning by heat conductive filler 90%, polymeric binder 10% is got heat conductive filler and polymeric binder;
B, mixing: heat conductive filler and polymeric binder are uniformly mixed to (mixing time can be 1min) through (directly at a high speed), make modeling powder;
C, moulding: the modeling powder making is put into forming mould, after moulding, the demoulding, make high-volume fractional heat-conductive composite material.Moulding object is to make polymeric binder melt-flow in the process of compacting, fully fills the space between filler small-particle, thereby strengthens gravitation and adhesive power between small-particle, strengthens the thermal conductivity of profiled member and relevant mechanical property;
The stir speed (S.S.) that described in step b, (at a high speed) is uniformly mixed is 25000 revs/min;
Described in step c, be shaped to hot-formingly, that is: will forming mould heat-insulation pressure keeping 3h under the condition of 200 ℃ of temperature, pressure 20KN of modeling powder be housed;
The described raw material heat conductive filler of obtaining and polymeric binder are carried out drying treatment before mixing, that is: in convection oven, be forced air drying 20h under the condition of 100 ℃ in temperature.
Embodiment 17:
A preparation method for high-volume fractional heat-conductive composite material, step is:
A, outfit raw material: the mass percent proportioning by heat conductive filler 99%, polymeric binder 10% is got heat conductive filler and polymeric binder;
B, mixing: heat conductive filler and polymeric binder are uniformly mixed to (mixing time can be 3min) through (directly at a high speed), make modeling powder;
C, moulding: the modeling powder making is put into forming mould, after moulding, the demoulding, make high-volume fractional heat-conductive composite material.Moulding object is to make polymeric binder melt-flow in the process of compacting, fully fills the space between filler small-particle, thereby strengthens gravitation and adhesive power between small-particle, strengthens the thermal conductivity of profiled member and relevant mechanical property;
The stir speed (S.S.) that described in step b, (at a high speed) is uniformly mixed is 25000 revs/min;
Described in step c, be shaped to hot-formingly, that is: will forming mould heat-insulation pressure keeping 0.5h under the condition of 400 ℃ of temperature, pressure 200KN of modeling powder be housed;
The described raw material heat conductive filler of obtaining and polymeric binder are carried out drying treatment before mixing, that is: in convection oven, be forced air drying 2h under the condition of 150 ℃ in temperature.
Embodiment 18~24:
A preparation method for high-volume fractional heat-conductive composite material, step is:
A, outfit raw material: the mass percent proportioning by heat conductive filler 90~99%, polymeric binder 1~10% is got heat conductive filler and polymeric binder; In each embodiment, the concrete mass percent consumption of each component raw material sees the following form:
B, mixing: heat conductive filler and polymeric binder are uniformly mixed to (mixing time can be 1~3min) through (directly at a high speed), make modeling powder;
C, moulding: the modeling powder making is put into forming mould, after moulding, the demoulding, make high-volume fractional heat-conductive composite material.Moulding object is to make polymeric binder melt-flow in the process of compacting, fully fills the space between filler small-particle, thereby strengthens gravitation and adhesive power between small-particle, strengthens the thermal conductivity of profiled member and relevant mechanical property;
The stir speed (S.S.) that described in step b, (at a high speed) is uniformly mixed is 25000 revs/min;
Described in step c, be shaped to hot-formingly, that is: will forming mould heat-insulation pressure keeping 0.5~3h under the condition of 200~400 ℃ of temperature, pressure 20~200KN of modeling powder be housed;
The described raw material heat conductive filler of obtaining and polymeric binder are carried out drying treatment before mixing, that is: in convection oven, be forced air drying 10~20h under the condition of 100~150 ℃ in temperature.
In above-described embodiment 7~24: described highly-conductive hot carbon base micro nano powder filler can be:
Single Walled Carbon Nanotube (can be Timestub tM-high-purity Single Walled Carbon Nanotube, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, model: TNS, outside diameter OD is 1~2nm, purity (Purity>=90wt%), length is 5~30 μ m, specific surface area SSA>=380m 2/ g, ash content≤1.5wt%, electric conductivity EC>=100s/cm, bulk density (Tap Density) is 0.14g/cm 3),
Multi-walled carbon nano-tubes (can be Timestub tM-high-purity Single Walled Carbon Nanotube, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, model: TNM1, outside diameter OD>=50nm, purity (Purity>=90wt%), length is 10~30 μ m, specific surface area SSA>=40m 2/ g, ash content≤5wt%, electric conductivity EC>=100s/cm, bulk density (Tap Density) is 0.27g/cm 3),
Graphene (can be TimesGraph tM-Graphene, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences produces, purity (Purity>=95wt%), specific surface area SSA>=554.364m 2/ g, diameter is 0.5~3 μ m, and the number of plies is 1~10 layer, and thickness is 0.55~3.74nm; Or soccerballene C 60, purity (>=98wt%), fusing point>=280 ℃, burning-point>=94 ℃) or
(can be C-25 carbon nanofiber, Anshan Sinocrab Carbon Fiber Co., Ltd. produces carbon nanofiber, specific surface area SSA>=1000m 2/ g);
The particle diameter of described highly-conductive hot carbon base micro nano powder filler is 0.5 μ m~50 μ m.
In above-described embodiment 7~24: described polymeric binder can (be called for short PTFE for tetrafluoroethylene, manufacturing enterprise has: Shanghai three is liked rich, product type is: FR002A, hugeization of Zhejiang, trade mark JTC-305), polymethylmethacrylate (is called for short PMMA, manufacturing enterprise has: SUMITOMO CHEMICAL, trade mark HT03Y, France Arkema, trade mark V04l resin), (manufacturing enterprise has viton: middle Wu Chenguang chemical institute etc., trade mark FPM2606 resin), or nylon (is called for short PA, manufacturing enterprise has: Shen Ma engineering plastics company etc., nylon-66, nylon-6) resin such as, be common commercial commercialization high molecular synthetic resin.
Described polymeric binder (for example PMMA, PA's etc.) number-average molecular weight is 100,000~200,000.
Described polymeric binder is polymer powder, and the particle diameter of this polymer powder is 40 μ m~100 μ m.
In above-described embodiment: each component raw material adopting is commercially available prod.
In above-described embodiment: in the percentage adopting, do not indicate especially, be quality (weight) percentage or well known to a person skilled in the art percentage; Described quality (weight) part can be all gram or kilogram; Symbol wt% is weight (quality) percentage.
In above-described embodiment: the processing parameter in each step (temperature, time, concentration, pressure etc.) and each amounts of components numerical value etc. are scope, and any point is all applicable.
The not concrete same prior art of technology contents of narrating in content of the present invention and above-described embodiment.
The invention is not restricted to above-described embodiment, all can implement and have described good result described in content of the present invention.

Claims (10)

1. a high-volume fractional heat-conductive composite material, it is characterized in that: by irregular stacking, form the heat conductive filler that heat conduction network, mass percent are 90~99%, and be scattered in described heat conduction network space, polymeric binder that mass percent is 1~10% forms;
Described heat conductive filler is highly-conductive hot carbon base micro nano powder.
2. by high-volume fractional heat-conductive composite material claimed in claim 1, it is characterized in that: described highly-conductive hot carbon base micro nano powder filler is: Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, Graphene or carbon nanofiber.
3. by the high-volume fractional heat-conductive composite material described in claim 1 or 2, it is characterized in that: described polymeric binder is tetrafluoroethylene, polymethylmethacrylate, viton or nylon.
4. by high-volume fractional heat-conductive composite material claimed in claim 3, it is characterized in that: described polymeric binder number-average molecular weight is 100,000~200,000.
5. by high-volume fractional heat-conductive composite material described described in claim 3, it is characterized in that: described polymeric binder is polymer powder, the particle diameter of this polymer powder is 40 μ m~100 μ m.
6. by the high-volume fractional heat-conductive composite material described in claim 1 or 2, it is characterized in that: the particle diameter of described highly-conductive hot carbon base micro nano powder filler is 0.5 μ m~50 μ m.
7. by the preparation method of high-volume fractional heat-conductive composite material described in claim 1, it is characterized in that step is:
A, outfit raw material: the mass percent proportioning by heat conductive filler 90~99%, polymeric binder 1~10% is got heat conductive filler and polymeric binder;
B, mixing: heat conductive filler and polymeric binder, through being uniformly mixed, are made to modeling powder;
C, moulding: the modeling powder making is put into forming mould, after moulding, the demoulding, make high-volume fractional heat-conductive composite material.
8. by the preparation method of high-volume fractional heat-conductive composite material described in claim 7, it is characterized in that: the stir speed (S.S.) being uniformly mixed described in step b is 25000 revs/min.
9. by the preparation method of high-volume fractional heat-conductive composite material described in claim 7, it is characterized in that: described in step c, be shaped to hot-formingly, that is: will forming mould heat-insulation pressure keeping 0.5~3h under the condition of 200~400 ℃ of temperature, pressure 20~200KN of modeling powder be housed.
10. by the preparation method of high-volume fractional heat-conductive composite material described in claim 7, it is characterized in that: described in the raw material heat conductive filler and the polymeric binder that obtain before mixing, carry out drying treatment, that is: in convection oven, in temperature, be forced air drying 10~20h under the condition of 100~120 ℃.
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105255004A (en) * 2015-10-26 2016-01-20 四川大学 Graphite resin composite material of core-shell structure and preparation method thereof
CN107337881A (en) * 2017-06-29 2017-11-10 华中科技大学鄂州工业技术研究院 Fluororesin interfacial agents, method of preparation and use for LED encapsulation
CN109796720A (en) * 2018-12-25 2019-05-24 中国科学院福建物质结构研究所 A kind of 3D printing product and preparation method thereof with high thermal conductivity coefficient
CN111517692A (en) * 2020-04-26 2020-08-11 广州视源电子科技股份有限公司 Non-metal heat conductor and its manufacturing method
CN111655010A (en) * 2020-06-29 2020-09-11 广州视源电子科技股份有限公司 Radiator and preparation method thereof
CN112574468A (en) * 2019-09-30 2021-03-30 天津理工大学 Heat-conducting polymer composite material with multi-layer continuous network structure and preparation method thereof
CN109897177B (en) * 2019-02-27 2021-04-06 中国科学院福建物质结构研究所 Workpiece with multi-scale three-dimensional heat conduction network and preparation method thereof
WO2021125049A1 (en) * 2019-12-18 2021-06-24 Agc株式会社 Coated substrate, heat exchanger, coated substrate production method, and liquid composition
CN113278406A (en) * 2020-02-19 2021-08-20 国家能源投资集团有限责任公司 Heat-conducting film composite material and preparation method thereof
WO2022033481A1 (en) * 2020-08-14 2022-02-17 中兴通讯股份有限公司 Heat dissipation structure, heat dissipation component and mounting method therefor, and foldable terminal

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101134837A (en) * 2007-09-03 2008-03-05 四川大学 Method for preparing filling type high polymer conductive porous composite material
CN101550330A (en) * 2009-05-18 2009-10-07 浙江大学 Lightweight high heat conductive composite material and preparation method thereof
WO2013051707A1 (en) * 2011-10-05 2013-04-11 独立行政法人産業技術総合研究所 Carbon nanotube composite material and heat conductor
CN103122075A (en) * 2013-03-19 2013-05-29 苏州格瑞丰纳米科技有限公司 High heat-conducting thin graphene-based composite material, as well as preparation method and application thereof
KR101343997B1 (en) * 2011-11-18 2013-12-31 강형식 Thermal conductive composite comprising nano metal powder and method of preparation the same
CN104386948A (en) * 2013-10-30 2015-03-04 长沙理工大学 Fast preparation method of graphite composite material with high thermal conductivity

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101134837A (en) * 2007-09-03 2008-03-05 四川大学 Method for preparing filling type high polymer conductive porous composite material
CN101550330A (en) * 2009-05-18 2009-10-07 浙江大学 Lightweight high heat conductive composite material and preparation method thereof
WO2013051707A1 (en) * 2011-10-05 2013-04-11 独立行政法人産業技術総合研究所 Carbon nanotube composite material and heat conductor
KR101343997B1 (en) * 2011-11-18 2013-12-31 강형식 Thermal conductive composite comprising nano metal powder and method of preparation the same
CN103122075A (en) * 2013-03-19 2013-05-29 苏州格瑞丰纳米科技有限公司 High heat-conducting thin graphene-based composite material, as well as preparation method and application thereof
CN104386948A (en) * 2013-10-30 2015-03-04 长沙理工大学 Fast preparation method of graphite composite material with high thermal conductivity

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
HUANG WU ET AL: ""Graphene nanoplatelet paper as a light-weight composite with excellent electrical and thermal conductivity and good gas barrier properties"", 《CARBON》 *
于伟等: ""高导热含石墨烯纳米片尼龙6复合材料"", 《工程热物理学报》 *
汪文等: ""石墨烯微片/聚丙烯导热复合材料的制备与性能"", 《复合材料学报》 *
郭文满等: ""聚合物/碳基导热复合材料研究进展"", 《塑料》 *

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105255004B (en) * 2015-10-26 2018-06-01 四川大学 A kind of graphite resin composite material with nucleocapsid and preparation method thereof
CN105255004A (en) * 2015-10-26 2016-01-20 四川大学 Graphite resin composite material of core-shell structure and preparation method thereof
CN107337881B (en) * 2017-06-29 2020-05-08 华中科技大学鄂州工业技术研究院 Fluororesin interface agent for LED packaging, preparation and use method
CN107337881A (en) * 2017-06-29 2017-11-10 华中科技大学鄂州工业技术研究院 Fluororesin interfacial agents, method of preparation and use for LED encapsulation
CN109796720B (en) * 2018-12-25 2021-05-11 中国科学院福建物质结构研究所 Workpiece with high heat conductivity coefficient and preparation method thereof
CN109796720A (en) * 2018-12-25 2019-05-24 中国科学院福建物质结构研究所 A kind of 3D printing product and preparation method thereof with high thermal conductivity coefficient
CN109897177B (en) * 2019-02-27 2021-04-06 中国科学院福建物质结构研究所 Workpiece with multi-scale three-dimensional heat conduction network and preparation method thereof
CN112574468A (en) * 2019-09-30 2021-03-30 天津理工大学 Heat-conducting polymer composite material with multi-layer continuous network structure and preparation method thereof
CN112574468B (en) * 2019-09-30 2022-07-15 天津理工大学 Heat-conducting polymer composite material with multi-layer continuous network structure and preparation method thereof
WO2021125049A1 (en) * 2019-12-18 2021-06-24 Agc株式会社 Coated substrate, heat exchanger, coated substrate production method, and liquid composition
CN113278406A (en) * 2020-02-19 2021-08-20 国家能源投资集团有限责任公司 Heat-conducting film composite material and preparation method thereof
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WO2022033481A1 (en) * 2020-08-14 2022-02-17 中兴通讯股份有限公司 Heat dissipation structure, heat dissipation component and mounting method therefor, and foldable terminal

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