CN106219532B - 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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- CN106219532B CN106219532B CN201610617315.XA CN201610617315A CN106219532B CN 106219532 B CN106219532 B CN 106219532B CN 201610617315 A CN201610617315 A CN 201610617315A CN 106219532 B CN106219532 B CN 106219532B
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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 a kind of nanometer carbon pipe array/graphite composite heat conduction films and preparation method thereof, include the following steps: (1) in 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, the deposition of macromolecule membrane carbonization, nanometer carbon pipe array is carried out after reduction treatment, obtains nanometer carbon pipe array/charcoal composite film material;(3) by the further carbonization treatment of composite film material;(4) composite film material is subjected to graphitization processing, obtains 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, to significantly improve the heat exchange amount of the surrounding enviroment such as unit area heat conducting film and air, achieve the effect that for heat to be quickly diffused into the surrounding enviroment such as air from heat conducting film.
Description
Technical field
The invention belongs to thermally conductive and technical field of heat dissipation, be related to nanometer carbon pipe array/graphite composite heat-conducting membrane material and its
Preparation method.
Background technique
In recent years, graphite film material was answered extensively because of its excellent high thermal conductivity, heat-resisting, the corrosion-resistant and characteristics such as highly conductive
For technical fields such as electronic product heat dissipation, heat-resistant seal material, heaters.And the graphite film with high thermal conductivity is even more
It is widely used under smart phone and tablet computer equidimension, in the handheld terminals such as electronic component is intensive, calorific value is big, passes through height
Thermal conductivity realizes heat sinking function.
Currently, can be had by selecting organic polymer thin-film material directly to carry out carbonization and graphitization processing
High-termal conductivity, high conductivity, the graphite film material of resistance to bend(ing) (104445174 A of CN 102838107 B, CN etc.), and
It is widely used in handheld terminal.Although the type conduction graphite film can be by heating device easy in handheld terminal
Heat conduct rapidly in entire graphite film, but being limited swept area causes it heat promptly cannot be radiated week
In collarette border, as a result, the cruising ability of heat dissipation is insufficient.Cause heat dissipation cruising ability insufficient main reason is that thermally conductive
The lesser swept area of film, and thereby result between heat conducting film and air that there are biggish interface resistances.
Carbon nanotubes has the excellent characteristics such as high heat conductance, high conductivity, high-specific surface area and high intensity, in macromolecule
The fields such as material, metal material, ceramic material play significant reinforcing effect.By the way that carbon nanotubes is mutually tied with graphite film
It closes, can effectively enhance the thermal conductive contact between substrate, and the adhesive force and splitting resistance of Heat Conduction Material can be improved
Can, so as to improve the overall performance of thin-film material.
In this regard, 104810336 A of Chinese patent CN discloses a kind of heat transmission carbon nanotube composite stone ink film, in graphite
The direct carbon nano-tube coating layer of film surface (carbon nanotube heat dissipating layer includes carbon nano-tube material, auxiliary agent and binding resin) increases
The capacity of heat transmission of vertical direction, while improving the mechanical property and flexility of heat conducting film.But due to carbon nanotubes and stone
The active force on ink film surface is poor, carbon nanotubes random distribution and cause to orient it is poor, and coating carbon nanotubes it is easy to reunite
And effective swept area cannot be increased by causing specific surface area reasons, the gained composite stone ink film such as substantially to decline.Chinese patent CN
105110312 A disclose carbon nanotube graphite composite material and preparation method thereof and device, pass through carbon using complete wet filtration method
Composite membrane is made in nanotube dispersion liquid and graphite dispersing solution, and it is thin to solve the problems, such as that natural graphite is difficult to, increases simultaneously
The capacity of heat transmission of vertical direction.However, the material has the following deficiencies: that only abutment surface adhesive force connects carbon nanotubes with graphite flake
Even, final products globality and continuity are poor;The graphite flake of carbon nanotubes and low specific surface area mutually coats and easy to reunite, leads
It causes whole specific surface area to reduce, not can increase effective swept area;Carbon nanotubes random distribution, directionality is poor, heat without
Method is conducted towards preset direction and is spread.104029461 A of Chinese patent CN discloses a kind of graphene/carbon nano-tube/graphite film
Composite material and preparation method prepares nickel Catalytic Layer in graphite film surface using magnetic control sputtering system, and be vapor-deposited graphene
With carbon nanotubes particle, the three-dimensional net structure of graphene and carbon nanotubes preferably promotes the heating conduction of material.But
Granular graphene and carbon nanotubes causes specific surface area to reduce significantly because it reunites the shortcomings that, and effective radiating area cannot get
It is obviously improved;In addition, the random distribution of graphene and carbon nanotubes causes poor directionality to cause in three-dimensional net structure
Heat radiation is difficult to carry out towards preset direction.
It can be seen that existing graphite and the composite film material of carbon nanotubes are focused on how to promote material plane direction
Or the thermal coefficient of vertical direction, and for how heat to be quickly directionally diffused into this technology in the surrounding enviroment such as air
Problem, which then rarely has, to be related to.In the preparation method of existing graphite and carbon nanotubes composite film material, cladding process and complete wet filtration method
Since carbon nanotubes passes through the randomness that dispersion causes distribution, the nanometer carbon pipe array and graphite of high orientation cannot be formed
The composite film material of film;And the random distribution for the carbon nanotubes particle that is vapor-deposited, the astaticism of carbon nanotubes is caused, together
Sample cannot form the nanometer carbon pipe array of high orientation and the composite film material of graphite film.This has just been doomed the above material not
Effective swept area can be significantly increased, so quickly heat directionally cannot be diffused into the surrounding enviroment such as air.In addition,
The composite film material of existing graphite and carbon nanotubes introduces carbon nanotubes on the basis of molding graphite film,
Its process is complex, larger for the change of original process units, is unfavorable for continuous production.
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 in graphite film surface
Product has the nanometer carbon pipe array of 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 area heat conducting film and air, reaches that heat is fast
Speed is diffused into the effect in the surrounding enviroment such as air from heat conducting film.
The second object of the present invention is to provide a kind of one-step method to prepare nanometer carbon pipe array/graphite composite heat conduction film side
Method, by way of in the direct supported catalyst oxidant layer in high molecular film material surface or catalyst precursor layer, directly in high score
Deposition has high directivity nanometer carbon pipe array while sub- film is carbonized, and avoids macromolecule membrane carbonization and heats up, cooling,
It heats up again and deposits nanometer carbon pipe array, then the traditional handicraft process to cool down, keep this production technology production efficiency higher, saved energy
Source and production cost are suitble to large-scale batch production.
Technical scheme is as follows:
A kind of nanometer carbon pipe array/graphite composite heat conduction film, comprising: graphite film and vertical-growth are in graphite film upper surface
And/or the nanometer carbon pipe array of lower surface, wherein graphite film with a thickness of 10-100 μm, nanometer carbon pipe array with a thickness of 1-
200μm。
Preferably, the graphite film and nanometer carbon pipe array are generated using one-step method.
One-step method prepares nanometer carbon pipe array/graphite composite heat conduction film method, includes the following steps:
(1) in 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, is carried out after reduction treatment high
Molecular film carbonization, nanometer carbon pipe array deposition, obtain nanometer carbon pipe array/charcoal composite film material;
(3) nanometer carbon pipe array/charcoal composite film material is subjected to carbonization treatment;
(4) material of step (3) is subjected to graphitization processing, obtains nanometer carbon pipe array/graphite composite heat conduction film.
Specifically, high molecular film material described in step (1) is polyimides, polyamide, polyoxadiazoles, polyphenyl and dislikes
Azoles, polyphenyl and double oxazoles, polythiazole, polybenzothiozole, polyphenyl and double thiazole, poly (phenylenevinylene), polybenzimidazoles
Or polypyridobisimidazole.
Specifically, catalyst described in step (1) is one or more of iron, cobalt, nickel, copper, platinum, palladium, Jin Heyin, institute
State one or more of oxide, inorganic salts and the organo-metallic compound that catalyst precursor is metal.
Specifically, the loading method of catalyst or catalyst precursor is infusion process, sedimentation, the precipitation method in step (1)
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, reduction treatment condition in step (2) are as follows: temperature is 300-600 DEG C, reducing atmosphere Ar/H2、He/H2Or
N2/H2, recovery time 0.5-20h.
Specifically, in step (2) macromolecule membrane carbonization, nanometer carbon pipe array deposition condition are as follows: temperature 400-
1200 DEG C, atmosphere CH4、C2H4、C2H6、C3H8、C6H6、C2H5The mixing of one or more of OH or CO gas and reducing atmosphere
Gas, sedimentation time 0.5-20h.
Specifically, in step (2) macromolecule membrane carbonization, nanometer carbon pipe array deposition condition further include: be passed through and contain
Sulphur auxiliary agent, the sulfur-bearing auxiliary agent are thiophene or H2S。
Specifically, the resulting nanometer carbon pipe array of step (2)/charcoal composite film material is carried out the following processing: in air
It is warming up to 200-500 DEG C in atmosphere and keeps 10-180min.
Specifically, step (3) the carbonization treatment condition are as follows: temperature is 1800-2400 DEG C.Preferable temperature 1900-2300
℃。
Specifically, step (4) the graphitization processing condition are as follows: temperature is 2400-3300 DEG C.Preferable temperature is 2600-
3100℃。
The beneficial effects of the present invention are:
A kind of nanometer carbon pipe array/graphite composite heat conduction film of the invention has high orientation in graphite film surface deposition
Property nanometer carbon pipe array, be significantly increased the swept area of conduction graphite film, reduce the interface resistance between heat conducting film and air, show
The heat exchange amount for improving the surrounding enviroment such as unit area heat conducting film and air is write, reaches and heat is quickly diffused into air from heat conducting film
Etc. effect in surrounding enviroment.
A kind of one-step method of the invention prepares nanometer carbon pipe array/graphite composite heat conduction film method, by macromolecule
The mode of the direct supported catalyst oxidant layer of thin-film material surface or catalyst precursor layer, directly while macromolecule membrane is carbonized
Deposition has high directivity nanometer carbon pipe array, avoids macromolecule membrane carbonization heating, cooling, then heat up and deposit nano-sized carbon
Pipe array, then the traditional handicraft process to cool down, keep this production technology production efficiency higher, have saved the energy and production cost, fit
Close large-scale batch production.
Detailed description of the invention
Fig. 1 is a kind of nanometer carbon pipe array/graphite composite heat conduction film structural schematic diagram of the invention;In figure: 11. receive
Rice array carbon nanotube, 12. graphite films.
Specific embodiment
In order to which the object of the invention, technical solution and advantage is more clearly understood, below in conjunction with example, the present invention is carried out
It is further to be described in detail.
Embodiment I
As shown in Fig. 1 (a), a kind of nanometer carbon pipe array/graphite composite heat conduction film, comprising: graphite film 12 and vertical life
The nanometer carbon pipe array in graphite film upper surface is grown, wherein the thickness of graphite film can be 10-100 μm, nanometer carbon pipe array
Thickness can be 1-200 μm, in this embodiment, graphite film with a thickness of 100 μm, nanometer carbon pipe array with a thickness of
200μm。
Embodiment II
As shown in Figure 1, a kind of nanometer carbon pipe array/graphite composite heat conduction film, comprising: graphite film 12 and vertical-growth exist
The nanometer carbon pipe array of graphite film upper and lower surfaces, wherein the thickness of graphite film can be 10-100 μm, carbon nanotubes battle array
The thickness of column can be 1-200 μm, in this embodiment, graphite film with a thickness of 10 μm, the thickness of nanometer carbon pipe array
It is 1 μm.
Preferably, graphite film and nanometer carbon pipe array are generated using one-step method.
A kind of specific embodiment of the preparation method of nanometer carbon pipe array/graphite composite heat conduction film is as follows:
Embodiment 1
In this example, it uses iron for catalyst, it is as follows to support implementation process:
Iron catalyst layer is supported on polyamide film material wherein a surface using magnetron sputtering technique;By this macromolecule
Thin-film material is placed in gaseous phase deposition stove flat-temperature zone, in reducing atmosphere Ar/H2Lower temperature programming is to 400 DEG C and keeps 2h, is urged
The reduction treatment of agent, wherein Ar/H2Flow be 900mL/min, H2Volume fraction be 20%.
Gas is switched to carbon-source gas C to after 800 DEG C by temperature programming2H4/Ar/H22h is kept, macromolecule membrane is carried out
Carbonization and nanometer carbon pipe array deposition, after switch to reducing atmosphere Ar/H2And it is down to room temperature, obtain carbon nanotubes battle array
Column/charcoal laminated film, wherein C2H4/Ar/H2Flow be 900mL/min, C2H4And H2Volume fraction be 25%.
This composite film material is subjected to further carbonization treatment in 1900-2200 DEG C, and at 2600-3000 DEG C into
Row graphitization processing finally obtains nanometer carbon pipe array/graphite composite heat conduction film.Exist on one of surface of heat conducting film and receives
Rice array carbon nanotube.
After tested it is found that obtained nanometer carbon pipe array/graphite composite heat conduction film, the thermal coefficient of horizontal direction are
1863-1879 W/ (K m), the thermal coefficient of vertical direction are 453-461 W/ (K m), effective radiating area 178-188
m2/g。
Embodiment 2
In this example, used catalyst precursor is nickel nitrate, and it is as follows to support implementation process:
Nickel nitrate is dissolved in ethanol solution, control content is 10wt%;Polyimide film material is completely immersed in nitre
In sour nickel/ethanol solution and keep 12h;It takes out high molecular film material and is placed in air atmosphere and dry, the two of macromolecule membrane
Nickel nitrate is supported on a surface.
This high molecular film material is placed in gaseous phase deposition stove flat-temperature zone, in 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 is switched to carbon-source gas C to after 850 DEG C by temperature programming2H4/He/H22h is kept, macromolecule membrane is carried out
Carbonization and nanometer carbon pipe array deposition, after switch to reducing atmosphere Ar/H2And it is down to room temperature, obtain carbon nanotubes battle array
Column/charcoal laminated film, wherein C2H4/He/H2Flow be 1000mL/min, C2H4And H2Volume fraction be respectively 30% He
20%。
This composite film material is subjected to further carbonization treatment in 2000-2300, and is carried out at 2600-3000 DEG C
Graphitization processing finally obtains nanometer carbon pipe array/graphite composite heat conduction film.There is nano-sized carbon on two surfaces of heat conducting film
Pipe array.
After tested it is found that obtained nanometer carbon pipe array/graphite composite heat conduction film, the thermal coefficient of horizontal direction are
1883-1902 W/ (K m), the thermal coefficient of vertical direction are 468-485 W/ (K m), effective radiating area 204-219
m2/g。
Embodiment 3
In this example, used catalyst precursor is ferrocene, and it is as follows to support implementation process:
Ferrocene is supported in a manner of being vapor-deposited on two surfaces of polyimides, by this high molecular film material
It is placed in gaseous phase deposition stove flat-temperature zone, in reducing atmosphere Ar/H2Lower temperature programming is to 500 DEG C and keeps 1.5h, carries out catalyst
Reduction treatment, wherein N2/H2Flow be 2000mL/min, H2Volume fraction be 30%.
Gas is switched to carbon-source gas CH to after 830 DEG C by temperature programming4/ N2/H21h is kept, macromolecule membrane is carried out
Carbonization and nanometer carbon pipe array deposition, after switch to reducing atmosphere Ar/H2And it is down to room temperature, obtain carbon nanotubes battle array
Column/charcoal laminated film, wherein CH4/N2/H2Flow be 2000mL/min, CH4And H2Volume fraction be respectively 35% and 20%.
This composite film material is subjected to further carbonization treatment in 2000-2300, and is carried out at 2600-3000 DEG C
Graphitization processing finally obtains nanometer carbon pipe array/graphite composite heat conduction film.There is nano-sized carbon on two surfaces of heat conducting film
Pipe array.
After tested it is found that obtained nanometer carbon pipe array/graphite composite heat conduction film, the thermal coefficient of horizontal direction are
1948-1975 W/ (K m), the thermal coefficient of vertical direction are 474-492 W/ (K m), effective radiating area 238-253
m2/g。
Embodiment 4
In this example, used catalyst precursor is ferric carbonate, and it is as follows to support implementation process:
Ferric nitrate is dissolved in deionized water, control content is 15wt%;Polybenzimidazoles thin-film material is completely immersed in
In nickel nitrate/aqueous solution, after being gradually added into ammonium bicarbonate aqueous solution under magnetic stirring, stand for 24 hours;It is thin to take out polybenzimidazoles
Membrane material drying, has supported ferric carbonate on two surfaces of film.
This high molecular film material is placed in gaseous phase deposition stove flat-temperature zone, in 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 is switched to carbon-source gas C to after 750 DEG C by temperature programming3H6/Ar/H21h is kept, macromolecule membrane is carried out
Carbonization and nanometer carbon pipe array deposition, after switch to reducing atmosphere Ar/H2And it is down to room temperature, obtain carbon nanotubes battle array
Column/charcoal laminated film, wherein C3H6/Ar/H2Flow be 1800mL/min, C3H6And H2Volume fraction be respectively 20% He
30%。
This composite film material is subjected to further carbonization treatment in 2000-2300, and is carried out at 2600-3000 DEG C
Graphitization processing finally obtains nanometer carbon pipe array/graphite composite heat conduction film.There is carbon nanotubes on two surfaces in heat conducting film
Array.
After tested it is found that obtained nanometer carbon pipe array/graphite composite heat conduction film, the thermal coefficient of horizontal direction are
1898-1915 W/ (K m), the thermal coefficient of vertical direction are 464-482 W/ (K m), effective radiating area 198-223
m2/g。
As a comparison, 104810336 A of patent CN is respectively adopted, in 104029461 A of CN 105110312 A and CN
The method prepares carbon nanotubes/graphite composite heat conduction film respectively, and answers with prepared in embodiment 1-4 in simultaneously patent
It closes heat conducting film and carries out performance comparison, the results are shown in tables 1.
By the comparison of table 1 it is found that high-specific surface area, high directionality nanometer carbon pipe array and the stone obtained through the invention
The composite heat-conducting thin-film material of ink not only both horizontally and vertically has apparent advantage, but also its effective radiating surface
Product is with more the advantage on the order of magnitude.
Table 1
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (8)
1. one-step method prepares nanometer carbon pipe array/graphite composite heat conduction film method, it is characterised in that include the following steps:
(1) in 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, macromolecule is carried out after reduction treatment
Film carbonization, nanometer carbon pipe array deposition, obtain nanometer carbon pipe array/charcoal composite film material;
(3) nanometer carbon pipe array/charcoal composite film material is subjected to carbonization treatment;
(4) material of step (3) is subjected to graphitization processing, obtains nanometer carbon pipe array/graphite composite heat conduction film;
Reduction treatment condition in step (2) are as follows: temperature is 300-600 DEG C, reducing atmosphere Ar/H2、He/H2Or N2/H2, when reduction
Between be 0.5-20h;
In step (2) macromolecule membrane carbonization, nanometer carbon pipe array deposition condition are as follows: temperature be 400-1200 DEG C, atmosphere
For CH4、C2H4、C2H6、C3H8、C6H6、C2H5The mixed gas of one or more of OH or CO gas and reducing atmosphere, deposition
Time is 0.5-20h;
Step (3) the carbonization treatment condition are as follows: temperature is 1800-2400 DEG C;
Step (4) the graphitization processing condition are as follows: temperature is 2400-3300 DEG C.
2. one-step method according to claim 1 prepares nanometer carbon pipe array/graphite composite heat conduction film method, feature exists
In: nanometer carbon pipe array/graphite composite heat conduction film includes: graphite film and vertical-growth in graphite film upper surface and/or following table
The nanometer carbon pipe array in face, wherein graphite film with a thickness of 10-100 μm, nanometer carbon pipe array with a thickness of 1-200 μm.
3. one-step method according to claim 1 prepares nanometer carbon pipe array/graphite composite heat conduction film method, feature exists
In: high molecular film material described in step (1) is polyimides, polyamide, polyoxadiazoles, polybenzoxazoles, polyphenyl are simultaneously double
Oxazole, polythiazole, polybenzothiozole, polyphenyl and double thiazole, poly (phenylenevinylene), polybenzimidazoles or polyphenyl and double miaows
Azoles.
4. one-step method according to claim 1 prepares nanometer carbon pipe array/graphite composite heat conduction film method, feature exists
In: catalyst described in step (1) is one or more of iron, cobalt, nickel, copper, platinum, palladium, Jin Heyin, the complex catalyst precursor
Body is one or more of oxide, inorganic salts and the organo-metallic compound of metal.
5. one-step method according to claim 1 prepares nanometer carbon pipe array/graphite composite heat conduction film method, feature exists
In: the loading method of catalyst or catalyst precursor is infusion process, sedimentation, the precipitation method or sputtering method in step (1).
6. one-step method according to claim 1 prepares nanometer carbon pipe array/graphite composite heat conduction film method, feature exists
In: in macromolecule membrane upper surface and/or lower surface supported catalyst oxidant layer or catalyst precursor layer in step (1).
7. one-step method according to claim 1 prepares nanometer carbon pipe array/graphite composite heat conduction film method, feature exists
In: in step (2) macromolecule membrane carbonization, nanometer carbon pipe array deposition condition further include: be passed through sulfur-bearing auxiliary agent, it is described to contain
Sulphur auxiliary agent is thiophene or H2S。
8. one-step method according to claim 1 prepares nanometer carbon pipe array/graphite composite heat conduction film method, feature exists
In: the resulting nanometer carbon pipe array of step (2)/charcoal composite film material is carried out the following processing: being warming up in air atmosphere
200-500 DEG C and keep 10-180min.
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CN105110312A (en) * | 2015-08-21 | 2015-12-02 | 昆明纳太科技有限公司 | Carbon nanotube graphite composite material and preparation method and device thereof |
CN105236384A (en) * | 2015-09-25 | 2016-01-13 | 天津工业大学 | Method for preparing three dimensional graphene/carbon nanotube ultra-light structure |
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CN1112086A (en) * | 1993-06-09 | 1995-11-22 | 中国科学院山西煤炭化学研究所 | High crystallinity graphite film material and its preparing method |
CN104029461A (en) * | 2014-06-13 | 2014-09-10 | 江苏悦达新材料科技有限公司 | Graphene/carbon nano tube/graphite film composite material and preparation method thereof |
CN105110312A (en) * | 2015-08-21 | 2015-12-02 | 昆明纳太科技有限公司 | Carbon nanotube graphite composite material and preparation method and device thereof |
CN105236384A (en) * | 2015-09-25 | 2016-01-13 | 天津工业大学 | Method for preparing three dimensional graphene/carbon nanotube ultra-light structure |
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