CN106219531A - A kind of preparation method of graphite/nanometer carbon pipe array composite heat conduction film - Google Patents
A kind of preparation method of graphite/nanometer carbon pipe array composite heat conduction film Download PDFInfo
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- CN106219531A CN106219531A CN201610614188.8A CN201610614188A CN106219531A CN 106219531 A CN106219531 A CN 106219531A CN 201610614188 A CN201610614188 A CN 201610614188A CN 106219531 A CN106219531 A CN 106219531A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The present invention relates to the preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film, comprise the steps: that (1) is at graphite film surface supported catalyst oxidant layer or catalyst precursor layer;(2) graphite film of step (1) is placed in chemical vapor depsotition equipment, after reduction treatment, carries out the deposition of nanometer carbon pipe array, obtain the conduction graphite film of surface deposition nanometer carbon pipe array;(3) conduction graphite film that surface deposits nanometer carbon pipe array carries out graphitization processing, obtains graphite/nanometer carbon pipe array 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 the system of a kind of graphite/nanometer carbon pipe array composite heat conduction film
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
It is an object of the invention to provide the preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film, at graphite film
Surface deposition has the nanometer carbon pipe array of high directivity, and the effective radiating area of conduction graphite film is significantly increased, and reduction is led
Interface resistance between hotting mask and air, significantly improves the heat exchange amount of the surrounding enviroment such as unit are heat conducting film and air, reach by
Heat is quickly diffused into the effect the surrounding enviroment such as air from heat conducting film.
Technical scheme is as follows:
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film, comprises the steps:
(1) at graphite film surface supported catalyst oxidant layer or catalyst precursor layer;
(2) graphite film of step (1) is placed in chemical vapor depsotition equipment, after reduction treatment, carries out nanometer carbon pipe array
Deposition, obtains the conduction graphite film of surface deposition nanometer carbon pipe array;
(3) conduction graphite film that surface deposits nanometer carbon pipe array carries out graphitization processing, obtains graphite/nanometer carbon pipe array multiple
Close heat conducting film.
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, the loading method of catalyst or catalyst precursor described in step (1) is infusion process, sedimentation, sinks
Shallow lake method or sputtering method.
Specifically, the graphite film in step (1) is carried out following place before supported catalyst oxidant layer or catalyst precursor layer
Reason: be warming up to 200-500 DEG C in air atmosphere and keep 10-180min.
Specifically, the graphite film in step (1) is carried out following place before supported catalyst oxidant layer or catalyst precursor layer
Reason: graphite film is placed in CO2Atmosphere is warming up to 800-1200 DEG C and keeps 10-180min.
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, in step (2), the condition of 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.
Specifically, in step (2), the condition of the deposition of nanometer carbon pipe array also includes: be passed through sulfur-bearing auxiliary agent, described sulfur-bearing
Auxiliary agent is thiophene or H2S。
Specifically, step (4) described graphitization processing condition is: temperature is 2400-3300 DEG C.
Specifically, step (4) described graphitization processing condition is: temperature is 2600-3100 DEG C.
The invention has the beneficial effects as follows:
Graphite film prepared by the preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film of the present invention, at graphite film table
Face deposition has the nanometer carbon pipe array of high directivity, and the swept area of conduction graphite film is significantly increased, 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.
Accompanying drawing explanation
Fig. 1 is the structural representation of the graphite/nanometer carbon pipe array composite heat conduction film of the present invention;
In figure: 11. nanometer carbon pipe arrays, 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 graphite/nanometer carbon pipe array 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 graphite/nanometer carbon pipe array 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 a wherein surface of graphite film;This graphite film is placed in gas phase sink
Long-pending stove flat-temperature zone, at reducing atmosphere Ar/H2Lower temperature programming to 400 DEG C and keeps 2h, carries out the reduction treatment of catalyst, 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 CNT battle array
The deposition of row, switches to reducing atmosphere Ar/H after terminating2And it is down to room temperature, wherein C2H4/Ar/H2Flow be 900mL/min,
C2H4And H2Volume fraction for being 25%.
At 2600-3000 DEG C, carry out graphitization processing again, finally give graphite/nanometer carbon pipe array composite heat conduction film.
Nanometer carbon pipe array is there is on one of them surface of heat conducting film.
Understanding after tested, the graphite obtained/nanometer carbon pipe array 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%;Graphite film is completely immersed in nickel nitrate/ethanol solution
In and keep 12h;Taking-up graphite film is placed in air atmosphere and dries, and two surfaces of graphite film all support nickel nitrate.
This graphite film is placed in gaseous phase deposition stove flat-temperature zone, at reducing atmosphere Ar/H2Lower temperature programming to 450 DEG C and keeps
2h, carries 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 CNT battle array
The deposition of row, switches to reducing atmosphere Ar/H after terminating2And it is down to room temperature, wherein C2H4/He/H2Flow be 1000mL/min,
C2H4And H2Volume fraction be respectively 30% and 20%.
At 2600-3000 DEG C, carry out graphitization processing again, finally give graphite/nanometer carbon pipe array composite heat conduction film.
Nanometer carbon pipe array is all there is on two surfaces of heat conducting film.
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 graphite film, this graphite film material is placed in gas phase and sinks
Long-pending stove flat-temperature zone, at reducing atmosphere Ar/H2Lower temperature programming to 500 DEG C and keeps 1.5h, carries out the reduction treatment of catalyst, its
Middle 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 CNT battle array
The deposition of row, switches to reducing atmosphere Ar/H after terminating2And it is down to room temperature, wherein CH4/N2/H2Flow be 2000mL/min,
CH4And H2Volume fraction be respectively 35% and 20%.
At 2600-3000 DEG C, carry out graphitization processing again, finally give graphite/nanometer carbon pipe array composite heat conduction film.
Nanometer carbon pipe array is all there is on two surfaces of heat conducting film.
Understanding after tested, the graphite obtained/nanometer carbon pipe array 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%;Graphite film material is completely immersed in nickel nitrate/water-soluble
In liquid, after being gradually added into ammonium bicarbonate aqueous solution under magnetic stirring, stand 24h;Taking-up graphite film material is dried, at graphite film
Two surfaces all supported ferric carbonate.
This graphite film 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 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 CNT battle array
The deposition of row, switches to reducing atmosphere Ar/H after terminating2And it is down to room temperature, wherein C3H6/Ar/H2Flow be 1800mL/min,
C3H6And H2Volume fraction be respectively 20% and 30%.
At 2600-3000 DEG C, carry out graphitization processing again, finally give graphite/nanometer carbon pipe array composite heat conduction film.
Nanometer carbon pipe array is all there is in heat conducting film on two surfaces.
Understanding after tested, the graphite obtained/nanometer carbon pipe array 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 graphite/nanometer carbon pipe array composite heat conduction film respectively, and prepared with embodiment 1-4 in also patent
Composite heat conduction film 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 (10)
1. the preparation method of graphite/nanometer carbon pipe array composite heat conduction film, it is characterised in that comprise the steps:
(1) at graphite film surface supported catalyst oxidant layer or catalyst precursor layer;
(2) graphite film of step (1) is placed in chemical vapor depsotition equipment, after reduction treatment, carries out nanometer carbon pipe array
Deposition, obtains the conduction graphite film of surface deposition nanometer carbon pipe array;
(3) conduction graphite film that surface deposits nanometer carbon pipe array carries out graphitization processing, obtains graphite/nanometer carbon pipe array multiple
Close heat conducting film.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 1, 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.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 1, its feature exists
In: described in step (1), the loading method of catalyst or catalyst precursor is infusion process, sedimentation, the sedimentation method or sputtering method.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 1, its feature exists
In: the graphite film in step (1) is carried out following process before supported catalyst oxidant layer or catalyst precursor layer: at air atmosphere
In be warming up to 200-500 DEG C and keep 10-180min.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 1, its feature exists
In: the graphite film in step (1) is carried out following process before supported catalyst oxidant layer or catalyst precursor layer: put by graphite film
In CO2Atmosphere is warming up to 800-1200 DEG C and keeps 10-180min.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 1, 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.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 1, its feature exists
In: in step (2), the condition of 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 is 0.5-20h.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 7, its feature exists
In: in step (2), the condition of the deposition of nanometer carbon pipe array also includes: be passed through sulfur-bearing auxiliary agent, described sulfur-bearing auxiliary agent be thiophene or
H2S。
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 1, its feature exists
In: step (4) described graphitization processing condition is: temperature is 2400-3300 DEG C.
The preparation method of a kind of graphite/nanometer carbon pipe array composite heat conduction film the most according to claim 9, its feature exists
In: step (4) described graphitization processing condition is: temperature is 2600-3100 DEG C.
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CN107059004A (en) * | 2017-04-19 | 2017-08-18 | 江苏联科纳米科技有限公司 | A kind of high radiant rate heat radiating metal paper tinsel and preparation method and application |
CN110777532A (en) * | 2019-11-29 | 2020-02-11 | 山东大学 | Control method for uniformly growing carbon nanotubes on surface of graphite fiber film cloth |
CN111925735A (en) * | 2020-08-18 | 2020-11-13 | 南京工程学院 | Directional heat dissipation composite adhesive film and preparation method thereof |
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CN111925735A (en) * | 2020-08-18 | 2020-11-13 | 南京工程学院 | Directional heat dissipation composite adhesive film and preparation method thereof |
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