CN106219532A - A kind of nanometer carbon pipe array/graphite composite heat conduction film and preparation method thereof - Google Patents
A kind of nanometer carbon pipe array/graphite composite heat conduction film and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of nanometer carbon pipe array/graphite composite heat conduction film and preparation method thereof, comprise the steps: that (1) is at high molecular film material surface supported catalyst oxidant layer or catalyst precursor layer;(2) this high molecular film material is placed in chemical vapor deposition stove, after reduction treatment, carries out the deposition of macromolecule membrane carbonization, nanometer carbon pipe array, obtain nanometer carbon pipe array/charcoal composite film material;(3) by further for composite film material carbonization treatment;(4) composite film material is carried out graphitization processing, obtain nanometer carbon pipe array/graphite composite heat conduction film.The present invention has this specific process of high directivity nanometer carbon pipe array by surface deposition, significantly increase the effective radiating area of conduction graphite film, reduce the interface resistance between heat conducting film and air, thus significantly improve the heat exchange amount of the surrounding enviroment such as unit are heat conducting film and air, reach quickly to be diffused into heat from heat conducting film the effect the surrounding enviroment such as air.
Description
Technical field
The invention belongs to heat conduction and technical field of heat dissipation, relate to nanometer carbon pipe array/graphite composite heat-conducting membrane material and
Preparation method.
Background technology
In recent years, graphite film material, because of characteristics such as the high heat conduction of its excellence, heat-resisting, corrosion-resistant and high connductivity, extensively should
For technical fields such as electronic product heat radiation, heat-resistant seal material, heaters.And there is the graphite film of high thermal conductivity especially
It is widely used under smart mobile phone and panel computer equidimension, electronic component is intensive, caloric value is big etc. in handheld terminal, by height
Thermal conductivity realizes heat sinking function.
At present, by selecting organic polymer thin-film material directly to carry out carbonization and graphitization processing, it is possible to had
High-termal conductivity, high conductivity, the graphite film material (CN 102838107 B, CN 104445174 A etc.) of resistance to bend(ing), and
It is widely used in handheld terminal.Although this type conduction graphite film can be by heater members easy in handheld terminal
Heat conduct rapidly in whole graphite film, but limited swept area causes it that heat can not promptly be radiated week
In collarette border, its result is that the flying power of heat radiation is not enough.That causes heat radiation flying power deficiency main reason is that heat conduction
The swept area that film is less, and thereby result in and between heat conducting film and air, there is bigger interface resistance.
CNT has the characteristic that high heat conductance, high conductivity, high-specific surface area and high intensity etc. are excellent, at macromolecule
The fields such as material, metal material, ceramic material serve significant reinforced effects.By CNT is tied mutually with graphite film
Close, can effectively strengthen and thermal conductive contact between substrate, and adhesive force and the splitting resistance of Heat Conduction Material can be improved
Can such that it is able to improve the overall performance of thin-film material.
To this, Chinese patent CN 104810336 A discloses a kind of heat transmission CNT composite stone ink film, at graphite
Film surface direct carbon nano-tube coating layer (CNT heat dissipating layer includes carbon nano-tube material, auxiliary agent and binding resin), increases
The capacity of heat transmission of vertical direction, improves mechanical property and the flexility of heat conducting film simultaneously.But due to CNT and stone
The active force on ink film surface is poor, and CNT random distribution and causing orients poor, and the CNT of coating is easily reunited
And the reason such as cause that specific surface area declines to a great extent, gained composite stone ink film can not increase effective swept area.Chinese patent CN
105110312 A disclose CNT graphite composite material and preparation method thereof and device, use complete wet Filtration to pass through carbon
Nanotube dispersion liquid and graphite dispersing solution make composite membrane, solve native graphite and are difficult to thin problem, add simultaneously
The capacity of heat transmission of vertical direction.But, there is following defect in this material: CNT and graphite flake only abutment surface adhesive force connects
Even, final products globality and seriality are poor;CNT is mutually coated with the graphite flake of low specific surface area and easily reunites, and leads
Cause overall specific surface area to reduce, it is impossible to increase effective swept area;CNT random distribution, directivity is poor, heat without
Method is towards preset direction conduction diffusion.Chinese patent CN 104029461 A discloses a kind of graphene/carbon nano-tube/graphite film
Composite and preparation method thereof, uses magnetic control sputtering system to prepare nickel Catalytic Layer, vapour deposition Graphene in graphite film surface
With the heat conductivility that the three-dimensional net structure of CNT granule, Graphene and CNT preferably promotes material.But,
Shortcoming that granular Graphene and CNT are reunited because of it and cause specific surface area to be greatly reduced, effective radiating area can not get
It is obviously improved;Additionally, Graphene and the random distribution of CNT cause poor directionality to cause in three-dimensional net structure
Heat radiation is difficult to carry out towards preset direction.
As can be seen here, existing graphite is focused on how promoting material plane direction with the composite film material of CNT
Or the heat conductivity of vertical direction, and for the most quickly heat being directionally diffused into this technology in the surrounding enviroment such as air
A difficult problem then rarely has and relates to.In the preparation method of existing graphite and CNT composite film material, cladding process and complete wet Filtration
Owing to CNT is through disperseing the randomness causing distribution, nanometer carbon pipe array and the graphite of high orientation therefore can not be formed
The composite film material of film;And the random distribution of vapour deposition CNT granule, cause the astaticism of CNT, with
Sample can not form the nanometer carbon pipe array of high orientation and the composite film material of graphite film.This has just been doomed above material the most not
Effective swept area can be significantly increased, so can not be quickly directionally diffused in the surrounding enviroment such as air by heat.Additionally,
Existing graphite and the composite film material of CNT, all introduce CNT on the basis of the graphite film of molding,
Its process is complex, and the change for original process units is relatively big, is unfavorable for continuous prodution.
Summary of the invention
An object of the present invention is to provide a kind of nanometer carbon pipe array/graphite composite heat conduction film, heavy on graphite film surface
The long-pending nanometer carbon pipe array with high directivity, is significantly increased the effective radiating area of conduction graphite film, reduce heat conducting film with
Interface resistance between air, significantly improves the heat exchange amount of the surrounding enviroment such as unit are heat conducting film and air, reaches that heat is fast
Speed is diffused into the effect the surrounding enviroment such as air from heat conducting film.
The two of the purpose of the present invention are to provide a kind of one-step method and prepare the side of nanometer carbon pipe array/graphite composite heat conduction film
Method, by the way of in high molecular film material surface direct supported catalyst oxidant layer or catalyst precursor layer, directly at high score
Deposition has high directivity nanometer carbon pipe array while sub-thin film carbonization, it is to avoid macromolecule membrane carbonization heats up, cooling,
The deposition that heats up again nanometer carbon pipe array, then the traditional handicraft process lowered the temperature, make this production technology production efficiency higher, saved energy
Source and production cost, be suitable for large-scale batch production.
Technical scheme is as follows:
A kind of nanometer carbon pipe array/graphite composite heat conduction film, including: graphite film and vertical-growth graphite film upper surface and/
Or the nanometer carbon pipe array of lower surface, wherein the thickness of graphite film is 10-100 μm, and the thickness of nanometer carbon pipe array is 1-200 μ
m。
As preferably, described graphite film and nanometer carbon pipe array use one-step method to generate.
One-step method prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, comprises the steps:
(1) at high molecular film material surface supported catalyst oxidant layer or catalyst precursor layer;
(2) high molecular film material of step (1) is placed in chemical vapor depsotition equipment, after reduction treatment, carries out macromolecule
Thin film carbonization, the deposition of nanometer carbon pipe array, obtain nanometer carbon pipe array/charcoal composite film material;
(3) nanometer carbon pipe array/charcoal composite film material is carried out carbonization treatment;
(4) material of step (3) is carried out graphitization processing, obtain nanometer carbon pipe array/graphite composite heat conduction film.
Specifically, high molecular film material described in step (1) be polyimides, polyamide, poly-diazole, polyphenyl also
Azoles, polybenzobisoxazole, polythiazole, polybenzothiozole, polyphenyl double thiazole, poly (phenylenevinylene), polybenzimidazoles
Or polypyridobisimidazole.
Specifically, described in step (1), catalyst is one or more in ferrum, cobalt, nickel, copper, platinum, palladium, gold and silver, institute
Stating catalyst precursor is one or more in the oxide of metal, inorganic salt and organo-metallic compound.
Specifically, in step (1), the loading method of catalyst or catalyst precursor is infusion process, sedimentation, the sedimentation method
Or sputtering method.
Specifically, in macromolecule membrane upper surface and/or lower surface supported catalyst oxidant layer or catalyst carrier in step (1)
Layer.
Specifically, in step (2), reduction treatment condition is: temperature is 300-600 DEG C, and reducing atmosphere is Ar/H2、He/H2Or
N2/H2, the recovery time is 0.5-20h.
Specifically, the condition of the deposition of macromolecule membrane carbonization in step (2), nanometer carbon pipe array is: temperature is 400-
1200 DEG C, atmosphere is CH4、C2H4、C2H6、C3H8、C6H6、C2H5One or more in OH or CO gas and the mixing of reducing atmosphere
Gas, sedimentation time is 0.5-20h.
Specifically, the condition of the deposition of macromolecule membrane carbonization in step (2), nanometer carbon pipe array also includes: is passed through and contains
Sulfur auxiliary agent, described sulfur-bearing auxiliary agent is thiophene or H2S。
Specifically, the nanometer carbon pipe array/charcoal composite film material of step (2) gained is carried out following process: at air
Atmosphere is warming up to 200-500 DEG C and keeps 10-180min.
Specifically, step (3) described carbonization treatment condition is: temperature is 1800-2400 DEG C.Preferable temperature 1900-2300
℃。
Specifically, step (4) described graphitization processing condition is: temperature is 2400-3300 DEG C.Preferable temperature is 2600-
3100℃。
The invention has the beneficial effects as follows:
A kind of nanometer carbon pipe array/graphite the composite heat conduction film of the present invention, on graphite film surface, deposition has high directivity
Nanometer carbon pipe array, is significantly increased the swept area of conduction graphite film, reduces the interface resistance between heat conducting film and air, significantly carries
The heat exchange amount of the surrounding enviroment such as high unit are heat conducting film and air, reaches quickly from heat conducting film, heat is diffused into air isoperimetric
Effect in surrounding environment.
A kind of one-step method of the present invention prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, by macromolecule
Thin-film material surface direct supported catalyst oxidant layer or the mode of catalyst precursor layer, directly while macromolecule membrane carbonization
Deposition has high directivity nanometer carbon pipe array, it is to avoid macromolecule membrane carbonization heats up, and cooling is, then the deposition nano-sized carbon that heats up
Pipe array, then the traditional handicraft process lowered the temperature, make this production technology production efficiency higher, saved the energy and production cost, suitable
Close large-scale batch production.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of nanometer carbon pipe array/graphite composite heat conduction film of the present invention;In figure: 11. receive
Rice array carbon nanotube, 12. graphite films.
Detailed description of the invention
In order to make the object of the invention, technical scheme and advantage clearer, below in conjunction with example, the present invention is carried out
Further describe in detail.
Embodiment I
As shown in Fig. 1 (a), a kind of nanometer carbon pipe array/graphite composite heat conduction film, including: graphite film 12 and vertical-growth exist
The nanometer carbon pipe array of graphite film upper surface, wherein the thickness of graphite film can be 10-100 μm, the thickness of nanometer carbon pipe array
Can be 1-200 μm, in this specific embodiment, the thickness of graphite film be 100 μm, and the thickness of nanometer carbon pipe array is 200 μm.
Embodiment II
As it is shown in figure 1, a kind of nanometer carbon pipe array/graphite composite heat conduction film, including: graphite film 12 and vertical-growth are at graphite
The nanometer carbon pipe array of film upper and lower surface, wherein the thickness of graphite film can be 10-100 μm, nanometer carbon pipe array
Thickness can be 1-200 μm, and in this specific embodiment, the thickness of graphite film is 10 μm, and the thickness of nanometer carbon pipe array is 1 μ
m。
As preferably, graphite film and nanometer carbon pipe array use one-step method to generate.
The detailed description of the invention of the preparation method of a kind of nanometer carbon pipe array/graphite composite heat conduction film is as follows:
Embodiment 1
In this example, employing ferrum is catalyst, and it is as follows that it supports implementation process:
Magnetron sputtering technique is used to support iron catalyst layer on polyamide film material wherein a surface;By this macromolecule membrane
Material is placed in gaseous phase deposition stove flat-temperature zone, at reducing atmosphere Ar/H2Lower temperature programming to 400 DEG C and keeps 2h, carries out catalyst
Reduction treatment, wherein Ar/H2Flow be 900mL/min, H2Volume fraction be 20%.
Gas, to after 800 DEG C, is switched to carbon-source gas C by temperature programming2H4/Ar/H2Keep 2h, carry out macromolecule membrane
Carbonization and the deposition of nanometer carbon pipe array, switch to reducing atmosphere Ar/H after terminating2And it is down to room temperature, obtain CNT battle array
Row/charcoal laminated film, wherein C2H4/Ar/H2Flow be 900mL/min, C2H4And H2Volume fraction for being 25%.
This composite film material is carried out further carbonization treatment in 1900-2200 DEG C, and enters at 2600-3000 DEG C
Row graphitization processing, finally gives nanometer carbon pipe array/graphite composite heat conduction film.Exist on one of them surface of heat conducting film and receive
Rice array carbon nanotube.
Understanding after tested, the nanometer carbon pipe array obtained/graphite composite heat conduction film, the heat conductivity of its horizontal direction is
1863-1879 W/ (K m), the heat conductivity of vertical direction is 453-461 W/ (K m), and effective radiating area is 178-188
m2/g。
Embodiment 2
In this example, the catalyst precursor used is nickel nitrate, and it is as follows that it supports implementation process:
Being dissolved in ethanol solution by nickel nitrate, control content is 10wt%;Polyimide film material is completely immersed in nitric acid
In nickel/ethanol solution and keep 12h;Taking-up high molecular film material is placed in air atmosphere and dries, two of macromolecule membrane
Nickel nitrate is all supported on surface.
This high molecular film material is placed in gaseous phase deposition stove flat-temperature zone, at reducing atmosphere Ar/H2Lower temperature programming is to 450
DEG C and keep 2h, carry out the reduction treatment of catalyst, wherein He/H2Flow be 1000mL/min, H2Volume fraction be 30%.
Gas, to after 850 DEG C, is switched to carbon-source gas C by temperature programming2H4/He/H2Keep 2h, carry out macromolecule membrane
Carbonization and the deposition of nanometer carbon pipe array, switch to reducing atmosphere Ar/H after terminating2And it is down to room temperature, obtain CNT battle array
Row/charcoal laminated film, wherein C2H4/He/H2Flow be 1000mL/min, C2H4And H2Volume fraction be respectively 30% He
20%。
This composite film material is carried out further carbonization treatment in 2000-2300, and carries out at 2600-3000 DEG C
Graphitization processing, finally gives nanometer carbon pipe array/graphite composite heat conduction film.Nano-sized carbon is all there is on two surfaces of heat conducting film
Pipe array.
Understanding after tested, the nanometer carbon pipe array obtained/graphite composite heat conduction film, the heat conductivity of its horizontal direction is
1883-1902 W/ (K m), the heat conductivity of vertical direction is 468-485 W/ (K m), and effective radiating area is 204-219
m2/g。
Embodiment 3
In this example, the catalyst precursor used is ferrocene, and it is as follows that it supports implementation process:
Ferrocene is supported in the way of vapour deposition on two surfaces of polyimides, this high molecular film material is placed in
Gaseous phase deposition stove flat-temperature zone, at reducing atmosphere Ar/H2Lower temperature programming to 500 DEG C and keeps 1.5h, carries out the reduction of catalyst
Process, wherein N2/H2Flow be 2000mL/min, H2Volume fraction be 30%.
Gas, to after 830 DEG C, is switched to carbon-source gas CH by temperature programming4/ N2/H2Keep 1h, carry out macromolecule membrane
Carbonization and the deposition of nanometer carbon pipe array, switch to reducing atmosphere Ar/H after terminating2And it is down to room temperature, obtain CNT battle array
Row/charcoal laminated film, wherein CH4/N2/H2Flow be 2000mL/min, CH4And H2Volume fraction be respectively 35% and 20%.
This composite film material is carried out further carbonization treatment in 2000-2300, and carries out at 2600-3000 DEG C
Graphitization processing, finally gives nanometer carbon pipe array/graphite composite heat conduction film.Nano-sized carbon is all there is on two surfaces of heat conducting film
Pipe array.
Understanding after tested, the nanometer carbon pipe array obtained/graphite composite heat conduction film, the heat conductivity of its horizontal direction is
1948-1975 W/ (K m), the heat conductivity of vertical direction is 474-492 W/ (K m), and effective radiating area is 238-253
m2/g。
Embodiment 4
In this example, the catalyst precursor used is ferric carbonate, and it is as follows that it supports implementation process:
Being dissolved in deionized water by ferric nitrate, control content is 15wt%;Polybenzimidazoles thin-film material is completely immersed in nitric acid
In nickel/aqueous solution, after being gradually added into ammonium bicarbonate aqueous solution under magnetic stirring, stand 24h;Take out polybenzimidazoles thin film material
Material is dried, and has all supported ferric carbonate on two surfaces of thin film.
This high molecular film material is placed in gaseous phase deposition stove flat-temperature zone, at reducing atmosphere Ar/H2Lower temperature programming is to 500
DEG C and keep 1.5h, carry out the reduction treatment of catalyst, wherein Ar/H2Flow be 1800mL/min, H2Volume fraction be
30%。
Gas, to after 750 DEG C, is switched to carbon-source gas C by temperature programming3H6/Ar/H2Keep 1h, carry out macromolecule membrane
Carbonization and the deposition of nanometer carbon pipe array, switch to reducing atmosphere Ar/H after terminating2And it is down to room temperature, obtain CNT battle array
Row/charcoal laminated film, wherein C3H6/Ar/H2Flow be 1800mL/min, C3H6And H2Volume fraction be respectively 20% He
30%。
This composite film material is carried out further carbonization treatment in 2000-2300, and carries out at 2600-3000 DEG C
Graphitization processing, finally gives nanometer carbon pipe array/graphite composite heat conduction film.CNT is all there is in heat conducting film on two surfaces
Array.
Understanding after tested, the nanometer carbon pipe array obtained/graphite composite heat conduction film, the heat conductivity of its horizontal direction is
1898-1915 W/ (K m), the heat conductivity of vertical direction is 464-482 W/ (K m), and effective radiating area is 198-223
m2/g。
As a comparison, patent CN 104810336 A, CN 105110312 it is respectively adopted in A and CN 104029461 A
Described method, prepares CNT/graphite composite heat conduction film respectively, and with and patent in prepared answering in embodiment 1-4
Closing heat conducting film and carry out performance comparison, its result is listed in table 1.
By the contrast of table 1, high-specific surface area, high directionality nanometer carbon pipe array and the stone obtained by the present invention
The composite heat-conducting thin-film material of ink the most both horizontally and vertically has an obvious advantage, and its effective radiating surface
Amass and have more the advantage on the order of magnitude.
Table 1
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, relevant staff completely may be used
With in the range of without departing from this invention technological thought, carry out various change and amendment.The technical model of this invention
Enclose the content being not limited in description, it is necessary to determine its technical scope according to right.
Claims (13)
1. nanometer carbon pipe array/graphite composite heat conduction film, it is characterised in that including: graphite film and vertical-growth are at graphite
Film upper surface and/or the nanometer carbon pipe array of lower surface, wherein the thickness of graphite film is 10-100 μm, the thickness of nanometer carbon pipe array
Degree is 1-200 μm.
A kind of nanometer carbon pipe array/graphite composite heat conduction film the most according to claim 1, it is characterised in that: described graphite
Film and nanometer carbon pipe array use one-step method to generate.
3. the method that one-step method prepares nanometer carbon pipe array/graphite composite heat conduction film, it is characterised in that comprise the steps:
(1) at high molecular film material surface supported catalyst oxidant layer or catalyst precursor layer;
(2) high molecular film material of step (1) is placed in chemical vapor depsotition equipment, after reduction treatment, carries out macromolecule
Thin film carbonization, the deposition of nanometer carbon pipe array, obtain nanometer carbon pipe array/charcoal composite film material;
(3) nanometer carbon pipe array/charcoal composite film material is carried out carbonization treatment;
(4) material of step (3) is carried out graphitization processing, obtain nanometer carbon pipe array/graphite composite heat conduction film.
One-step method the most according to claim 3 prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, and its feature exists
It is polyimides, polyamide, poly-diazole, polybenzoxazole, polyphenyl double in: high molecular film material described in step (1)
Azoles, polythiazole, polybenzothiozole, polyphenyl double thiazole, poly (phenylenevinylene), polybenzimidazoles or polyphenyl double miaow
Azoles.
One-step method the most according to claim 3 prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, and its feature exists
In: described in step (1), catalyst is one or more in ferrum, cobalt, nickel, copper, platinum, palladium, gold and silver, described complex catalyst precursor
Body is one or more in the oxide of metal, inorganic salt and organo-metallic compound.
One-step method the most according to claim 3 prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, and its feature exists
In: in step (1), the loading method of catalyst or catalyst precursor is infusion process, sedimentation, the sedimentation method or sputtering method.
One-step method the most according to claim 3 prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, and its feature exists
In: in macromolecule membrane upper surface and/or lower surface supported catalyst oxidant layer or catalyst support layer in step (1).
One-step method the most according to claim 3 prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, and its feature exists
In: in step (2), reduction treatment condition is: temperature is 300-600 DEG C, and reducing atmosphere is Ar/H2、He/H2Or N2/H2, during reduction
Between be 0.5-20h.
One-step method the most according to claim 3 prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, and its feature exists
Condition in: macromolecule membrane carbonization in step (2), the deposition of nanometer carbon pipe array is: temperature is 400-1200 DEG C, and atmosphere is
CH4、C2H4、C2H6、C3H8、C6H6、C2H5One or more in OH or CO gas and the mixed gas of reducing atmosphere, sedimentation time
For 0.5-20h.
One-step method the most according to claim 9 prepares the method for nanometer carbon pipe array/graphite composite heat conduction film, its feature
It is: macromolecule membrane carbonization in step (2), the condition of deposition of nanometer carbon pipe array also include: be passed through sulfur-bearing auxiliary agent, described
Sulfur-bearing auxiliary agent is thiophene or H2S。
11. one-step method according to claim 3 prepare the method for nanometer carbon pipe array/graphite composite heat conduction film, its feature
It is: the nanometer carbon pipe array/charcoal composite film material of step (2) gained is carried out following process: heat up in air atmosphere
To 200-500 DEG C and keep 10-180min.
12. one-step method according to claim 3 prepare the method for nanometer carbon pipe array/graphite composite heat conduction film, its feature
It is: step (3) described carbonization treatment condition is: temperature is 1800-2400 DEG C.
13. one-step method according to claim 3 prepare the method for nanometer carbon pipe array/graphite composite heat conduction film, its feature
It is: step (4) described graphitization processing condition is: temperature is 2400-3300 DEG C.
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CN110423432A (en) * | 2019-01-14 | 2019-11-08 | 上海大学 | A kind of vertically-oriented carbon nano pipe array and graphene epoxy resin composite film material and preparation method thereof |
CN110723724A (en) * | 2018-07-16 | 2020-01-24 | 天津大学 | Three-dimensional graphene-carbon nanotube network structure and preparation method thereof |
CN111925735A (en) * | 2020-08-18 | 2020-11-13 | 南京工程学院 | Directional heat dissipation composite adhesive film and preparation method thereof |
CN114980651A (en) * | 2021-11-29 | 2022-08-30 | 图达通智能科技(上海)有限公司 | Heat-conducting vibration-isolating interface material |
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