CN104961464B - Through-thickness has high resilience and high thermal conductivity coefficient C-base composte material and preparation method - Google Patents
Through-thickness has high resilience and high thermal conductivity coefficient C-base composte material and preparation method Download PDFInfo
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Abstract
The present invention relates to the preparation method that a kind of through-thickness has high resilience and high thermal conductivity coefficient C-base composte material simultaneously, the graphite flake layer in expanded graphite is connected by array carbon nano tube, and the space between graphite flake layer is filled by array carbon nano tube；The hot Xi Shuo of through-thickness Dao≤25W/ (mK)；Resilience Shuai≤90% after compression 10%.Using ferrocene carbon source solution growth array carbon nano tube, ferrocene is cracked into iron atom and is attached to the graphite flake layer of expanded graphite, carbon source solution is cracked into carbon atom and adsorbs on iron atom surface, so as to grow array carbon nano tube between the graphite flake layer of expanded graphite, the transmission of graphite layers hot-fluid in expanded graphite is realized using the high thermal conductivity of CNT, graphite flake layer can be that horizontal direction is orientated along vertical hot pressing direction, array carbon nano tube connects and fills lamella and the space of expanded graphite in thickness direction, obtaining through-thickness has high resilience and high thermal conductivity coefficient C-base composte material.
Description
Technical field
The present invention relates to the preparation that a kind of through-thickness has high resiliency and high thermal conductivity coefficient C-base composte material simultaneously
The preparation method of method, specifically a kind of expanded graphite and array carbon nano tube composite.
Background technology
With the fast development of science and technology, the key issue of efficient heat conduction and radiating as field of heat management.For example
With the continuous improvement of the electrical installation electronic component integration degree such as computer, mobile phone, its unit area electronic device is improved constantly
Caloric value make system produce heat abruptly increase.If without sufficient heat management guarantee, easily causing related device to shift to an earlier date always
Change or damage.Many electronic units need the ability normal work at a temperature of 40~60 DEG C, and this is proposed to Heat Conduction Material
Higher and higher requirement.Density is larger, specific heat conductance (thermal conductivity system due to existing for traditional metal heat-conducting material (such as aluminium, copper)
Number is the ratio between with material volume density) limitation such as relatively low, thermal coefficient of expansion is higher, oxidizable, be difficult satisfaction and increasingly increased at present
Radiating requirements long.Carbon material has thermal conductivity factor higher, relatively low density and preferable chemical resistance, is in recent years
Carry out a class Heat Conduction Material most with prospects, thus had broad application prospects in fields such as the energy, communication, electronics.
Expanded graphite is a kind of loose porous vermiform material obtained by intercalation, expansion by natural flake graphite.
Expanded graphite is less due to the graphitization parietal layer with regular bulk, the obstruction of phonon conduction, and heat transfer efficiency is very high, thus utilizes
Expanded graphite prepares research emphasis of the carbon-based highly heat-conductive material as people, mandate or the disclosure of similar patent also occurs.China
State Intellectual Property Office of people's republic grant number is the invention such as CN101407322B, CN100368342C, CN101458049A
Patent disclosure prepares using compression-expansion graphite the technology of heat-conducting plate.
Above-described patent of invention disclose only traditional expanded graphite preparation method and pressing process, only obtain
The graphite heat conducting material of anisotropic heat conductivity, and the compression resilience of material is poor.For graphite flake layer, the lattice of carbon atom
Vibrations are the bases of material conducts heat, therefore phonon transmission can only carry out travel at high speeds along graphite crystal face in graphite material, and right
Due to hypertelorism between graphite wafer surface layer, the conduction of phonon is had a strong impact on.After being processed by graphite pressing process, graphite wafer
Face is orientated under hot pressing function along in-plane, thus only has high heat conduction system along in-plane in graphite heat-conducting fin
Number (be more than 100W/ (mK)), and through-thickness thermal conductivity factor is very low, less than 10W/ (mK) (Zhi-Hai Feng,
Tong-Qi Li,Zi-Jun Hu,Gao-Wen Zhao,Jun-Shan Wang,Bo-Yun Huang,Low cost
preparation of high thermal conductivity carbon blocks with ultra-high
anisotropy from a commercial graphite paper,Carbon,2012,50(10):3947–3948.).In
The through-thickness thermal conductivity factor of the graphite heat conduction plate of the announcements such as patent application CN100368342C, CN103539111A of state is all
In 10W/ (mK) below, compression resilience is poor.Therefore, existing published patent of invention obtains graphite material along thickness
The compression resilience and thermal conductivity factor in direction far from meeting requirement of the highly integrated electronic device to the Heat Conduction Material capacity of heat transmission,
A kind of through-thickness is developed on the basis of carbon material is advantageous, and there is high resilience and the material of high thermal conductivity coefficient to seem particularly
It is important.
The content of the invention
The present invention for existing expanded graphite prepare graphite heat-conducting fin through-thickness thermal conductivity factor is too low and resilience
Poor defect, there is provided a kind of through-thickness has C-base composte material and its preparation side of high resilience and high thermal conductivity coefficient
Method.Through-thickness thermal conductivity factor reaches 25W/ (mK), carbon-based composite wood of the rebound degree more than or equal to 90% after compression 10%
Material, as shown in Figure 1.
The present invention uses following technical scheme：
A kind of through-thickness has the C-base composte material of high resilience and high thermal conductivity coefficient；Graphite in expanded graphite
Lamella is connected by array carbon nano tube, and the space between graphite flake layer is filled by array carbon nano tube；Through-thickness heat conduction system
Shuo≤25W/ (mK)；Resilience Shuai≤90% after compression 10%.
A kind of through-thickness of the invention has the preparation side of the C-base composte material of high resilience and high thermal conductivity coefficient
Method, step is as follows：
(1) by absolute ethyl alcohol and dimethylbenzene in mass ratio 0.1~10：1 is uniformly mixed preparation carbon source solution, Jiang Ermao
Iron is dissolved in above-mentioned carbon source solution, the ferrocene carbon source solution of configuration quality fraction 1~5%；
(2) expanded graphite that expansion rate is 100~300 is positioned in tube furnace, is passed through argon gas protection, heated Tube-furnace
700~900 DEG C are warming up to, ferrocene carbon source solution are injected into tube furnace and are used to grow array carbon nanometer on expanded graphite
Pipe；
(3) expanded graphite for growing array carbon nano tube is placed in graphite jig, being placed in vacuum hotpressing stove carries out high temperature
Hot pressing, in 200~300 DEG C/h, hot pressing temperature is 1500~2000 DEG C for programming rate control, and hot pressing pressure is 5~40MPa, is protected
The warm dwell time is 0.5~1h, treats that temperature is down to 100 DEG C of releases and takes out sample.
In the step (2), the injection speed of ferrocene carbon source solution is 10~30mL/h, growth time is 30~
120min, growth terminates to be cooled to room temperature taking-up under the protection of inert gas.
It is described as follows：
(1) expanded graphite is a kind of vermiform graphite material；Expansion rate refer to expansible graphite expansion after with expansion before
Volume ratio；Commercially available prod can directly be used；
(2) effect of ferrocene carbon source solution is that, for growing array carbon nano tube, ferrocene splits in high temperature process furnances
Solution is into iron atom and is attached to the graphite flake layer of expanded graphite, and carbon source solution is cracked into carbon atom and adsorbs on iron atom surface,
So as to grow array carbon nano tube, such as Fig. 2 between the graphite flake layer of expanded graphite；
(3) the array carbon nano tube Main Function being grown between the graphite flake layer of expanded graphite is using the height of CNT
Heat conductivility realizes the transmission of graphite layers hot-fluid in expanded graphite, specifically, such as Fig. 1 and 2, vertical-growth is in Expandable graphite sheet
The array carbon nano tube of layer, connect the graphite flake layer of expanded graphite, the space between filling graphite flake layer, due to CNT
There is high thermal conductivity factor (~2000W/ (mK)) along tube axial direction, the array carbon nano tube of dense arrangement is in expanded graphite
Graphite flake layer between a large amount of passages of heat are provided so that the hot-fluid between the graphite flake layer of expanded graphite can be by the battle array of interlayer
Row CNT is transmitted, and then improves the thermal conductivity factor between the graphite flake layer of expanded graphite, simultaneously because highdensity array
Space between the carbon nano-tube filled graphite flake layer of expanded graphite, and then improve its compression resilience；
(4) under hot pressing condition, the graphite flake layer of expanded graphite can be that horizontal direction is orientated along vertical hot pressing direction, now
Array carbon nano tube connects and fills lamella and the space of expanded graphite in thickness direction, and then obtains through-thickness with height
Resilience and high thermal conductivity coefficient C-base composte material.
By the array carbon nano tube of above step in the growth of the graphite layers of expanded graphite and hot-forming, realize
High heat conduction array carbon nano tube obtains through-thickness heat conduction system to the connection of the graphite flake layer of expanded graphite and the filling in space
Number is more than or equal to 25W/ (mK), C-base composte material of the rebound degree more than or equal to 90% after compression 10%.
Beneficial effects of the present invention：Matrix material expanded graphite of the invention is easy to get, the growthform of array carbon nano tube
It is controllable.The ordering of C-base composte material microstructure and densification can be completed efficiently in the present invention, can obtain through-thickness tool
There is the C-base composte material of high resilience and high thermal conductivity coefficient, the resilience and the capacity of heat transmission of its through-thickness are far superior to pass
The expanded graphite hot pressing coiled material and other expanded graphites and carbon nano tube compound material of system.
Brief description of the drawings：
Fig. 1 is the microcosmic schematic diagram of C-base composte material of the invention；
Fig. 2 is the scanning electron microscopic picture that array carbon nano tube grows in expanded graphite interlayer.
Specific embodiment
Embodiments of the invention are given below, are further illustrated to of the invention, rather than limitation the scope of the present invention.
Embodiment 1
1.8g and 18g is configured to carbon source solution respectively with dimethylbenzene to choose absolute ethyl alcohol, and 0.2g is added in carbon source solution
Ferrocene is configured to the ferrocene carbon source solution of mass fraction 1%.The expanded graphite that expansion rate is 100 is positioned over tube furnace
In, argon gas protection is passed through, heated Tube-furnace is warming up to 700 DEG C, injects above-mentioned ferrocene carbon source solution, and the ferrocene carbon source is molten
The injection speed of liquid is controlled in 10mL/h, and growth time is 120min, and growth stops injection ferrocene carbon source solution after terminating, and
Room temperature taking-up is cooled under the protection of inert gas.The expanded graphite for growing array carbon nano tube is placed in graphite jig,
Being placed in vacuum hotpressing stove carries out high temperature hot pressing, and programming rate is 200 DEG C/h, and hot pressing temperature is 1500 DEG C, and hot pressing pressure is 5MPa,
Heat-insulation pressure keeping 0.5h, treats that temperature is down to 100 DEG C of releases and takes out sample.Test sample through-thickness thermal conductivity factor is 25W/ (m
K), rebound degree is 95% after sample through-thickness being compressed into 10%.
Embodiment 2
Choose absolute ethyl alcohol and be configured to carbon source solution with each 9.5g of dimethylbenzene, the configuration of 1g ferrocene is added in carbon source solution
Into the ferrocene carbon source solution of mass fraction 5%.The expanded graphite that expansion rate is 300 is positioned in tube furnace, argon gas is passed through
Protection, heated Tube-furnace is warming up to 900 DEG C, injects above-mentioned ferrocene carbon source solution, the injection speed of the ferrocene carbon source solution
In 30mL/h, growth time is 30min for degree control, and growth stops injection ferrocene carbon source solution after terminating, and in inert gas
Protection under be cooled to room temperature taking-up.The expanded graphite for growing array carbon nano tube is placed in graphite jig, Vacuum Heat is placed in
Pressure stove carries out high temperature hot pressing, and programming rate is 300 DEG C/h, and hot pressing temperature is 2000 DEG C, and hot pressing pressure is 40MPa, heat-insulation pressure keeping
1h, treats that temperature is down to 100 DEG C of releases and takes out sample.Test sample through-thickness thermal conductivity factor is 35W/ (mK), by sample
Rebound degree is 98% after through-thickness compression 10%.
Embodiment 3
Choose absolute ethyl alcohol and be configured to carbon source solution with each 9.6g of dimethylbenzene, add 0.8g ferrocene to match somebody with somebody in carbon source solution
It is set to the ferrocene carbon source solution of mass fraction 4%.The expanded graphite that expansion rate is 200 is positioned in tube furnace, argon is passed through
Gas shielded, heated Tube-furnace is warming up to 800 DEG C, injects above-mentioned ferrocene carbon source solution, the injection of the ferrocene carbon source solution
In 20mL/h, growth time is 60min to speed control, and growth stops injection ferrocene carbon source solution after terminating, and in indifferent gas
Room temperature taking-up is cooled under the protection of body.The expanded graphite for growing array carbon nano tube is placed in graphite jig, vacuum is placed in
Hot pressing furnace carries out high temperature hot pressing, and programming rate is 260 DEG C/h, and hot pressing temperature is 1600 DEG C, and hot pressing pressure is 30MPa, and insulation is protected
Pressure 0.6h, treats that temperature is down to 100 DEG C of releases and takes out sample.Test sample through-thickness thermal conductivity factor is 27W/ (mK), will
Rebound degree is 90% after sample through-thickness compression 10%.
Embodiment 4
18g and 1.8g is configured to carbon source solution respectively with dimethylbenzene to choose absolute ethyl alcohol, and 0.2g is added in carbon source solution
Ferrocene is configured to the ferrocene carbon source solution of mass fraction 1%.The expanded graphite that expansion rate is 100 is positioned over tube furnace
In, argon gas protection is passed through, heated Tube-furnace is warming up to 750 DEG C, injects above-mentioned ferrocene carbon source solution, and the ferrocene carbon source is molten
The injection speed of liquid is controlled in 15mL/h, and growth time is 50min, and growth stops injection ferrocene carbon source solution after terminating, and
Room temperature taking-up is cooled under the protection of inert gas.The expanded graphite for growing array carbon nano tube is placed in graphite jig,
Being placed in vacuum hotpressing stove carries out high temperature hot pressing, and programming rate is 200 DEG C/h, and hot pressing temperature is 1800 DEG C, and hot pressing pressure is
30MPa, heat-insulation pressure keeping 0.8h, treat that temperature is down to 100 DEG C of releases and takes out sample.Test sample through-thickness thermal conductivity factor is
26W/ (mK), rebound degree is 98% after sample through-thickness is compressed into 10%.
Embodiment 5
Choose absolute ethyl alcohol and be configured to carbon source solution with each 9.8g of dimethylbenzene, add 0.4g ferrocene to match somebody with somebody in carbon source solution
It is set to the ferrocene carbon source solution of mass fraction 2%.The expanded graphite that expansion rate is 200 is positioned in tube furnace, argon is passed through
Gas shielded, heated Tube-furnace is warming up to 750 DEG C, injects above-mentioned ferrocene carbon source solution, the injection of the ferrocene carbon source solution
In 15mL/h, growth time is 60min to speed control, and growth stops injection ferrocene carbon source solution after terminating, and in indifferent gas
Room temperature taking-up is cooled under the protection of body.The expanded graphite for growing array carbon nano tube is placed in graphite jig, vacuum is placed in
Hot pressing furnace carries out high temperature hot pressing, and programming rate is 280 DEG C/h, and hot pressing temperature is 2000 DEG C, and hot pressing pressure is 30MPa, and insulation is protected
Pressure 1h, treats that temperature is down to 100 DEG C of releases and takes out sample.Test sample through-thickness thermal conductivity factor is 32W/ (mK), by sample
Rebound degree is 95% after product through-thickness compression 10%.
Embodiment 6
Choose absolute ethyl alcohol and be configured to carbon source solution with each 9.5g of dimethylbenzene, the configuration of 1g ferrocene is added in carbon source solution
Into the ferrocene carbon source solution of mass fraction 5%.The expanded graphite that expansion rate is 100 is positioned in tube furnace, argon gas is passed through
Protection, heated Tube-furnace is warming up to 700 DEG C, injects above-mentioned ferrocene carbon source solution, the injection speed of the ferrocene carbon source solution
In 20mL/h, growth time is 60min for degree control, and growth stops injection ferrocene carbon source solution after terminating, and in inert gas
Protection under be cooled to room temperature taking-up.The expanded graphite for growing array carbon nano tube is placed in graphite jig, Vacuum Heat is placed in
Pressure stove carries out high temperature hot pressing, and programming rate is 200 DEG C/h, and hot pressing temperature is 2000 DEG C, and hot pressing pressure is 35MPa, heat-insulation pressure keeping
1h, treats that temperature is down to 100 DEG C of releases and takes out sample.Test sample through-thickness thermal conductivity factor is 36W/ (mK), by sample
Rebound degree is 96% after through-thickness compression 10%.
The present invention is disclosed and the through-thickness that proposes is while have high resiliency and high thermal conductivity coefficient C-base composte material
Preparation method, those skilled in the art can be by using for reference present disclosure, and the link such as appropriate feed change and process route is realized, to the greatest extent
The pipe method of the present invention and technology of preparing are described by preferred embodiment, and person skilled can substantially not take off
Methods and techniques described herein route is modified in present invention, spirit and scope or reconfigured to realize
Final technology of preparing.In particular, all similar replacements and change be for a person skilled in the art
It will be apparent that they are considered as being included in spirit of the invention, scope and content.
Claims (3)
1. a kind of through-thickness has the C-base composte material of high resilience and high thermal conductivity coefficient；It is characterized in that, expanded graphite
In graphite flake layer connected by array carbon nano tube, array carbon nano tube vertical-growth in expanded graphite lamella, graphite flake layer it
Between space filled by array carbon nano tube；The hot Xi Shuo of through-thickness Dao≤25W/ (mK)；Compression 10% after resilience Shuai≤
90%；
The through-thickness has the preparation method of the C-base composte material of high resilience and high thermal conductivity coefficient, and step is as follows：
(1) by absolute ethyl alcohol and dimethylbenzene in mass ratio 0.1~10：1 is uniformly mixed preparation carbon source solution, and ferrocene is molten
In above-mentioned carbon source solution, the ferrocene carbon source solution of configuration quality fraction 1~5%；
(2) expanded graphite that expansion rate is 100~300 is positioned in tube furnace, is passed through argon gas protection, heated Tube-furnace heats up
To 700~900 DEG C, ferrocene carbon source solution is injected into tube furnace to grow array carbon nano tube on expanded graphite；
(3) expanded graphite for growing array carbon nano tube is placed in graphite jig, being placed in vacuum hotpressing stove carries out high temperature hot pressing,
In 200~300 DEG C/h, hot pressing temperature is 1500~2000 DEG C for programming rate control, and hot pressing pressure is 5~40MPa, heat-insulation pressure keeping
Time is 0.5~1h, treats that temperature is down to 100 DEG C of releases and takes out sample.
2. a kind of through-thickness has the preparation method of the C-base composte material of high resilience and high thermal conductivity coefficient, and step is such as
Under：
(1) by absolute ethyl alcohol and dimethylbenzene in mass ratio 0.1~10：1 is uniformly mixed preparation carbon source solution, and ferrocene is molten
In above-mentioned carbon source solution, the ferrocene carbon source solution of configuration quality fraction 1~5%；
(2) expanded graphite that expansion rate is 100~300 is positioned in tube furnace, is passed through argon gas protection, heated Tube-furnace heats up
To 700~900 DEG C, ferrocene carbon source solution is injected into tube furnace to grow array carbon nano tube on expanded graphite；
(3) expanded graphite for growing array carbon nano tube is placed in graphite jig, being placed in vacuum hotpressing stove carries out high temperature hot pressing,
In 200~300 DEG C/h, hot pressing temperature is 1500~2000 DEG C for programming rate control, and hot pressing pressure is 5~40MPa, heat-insulation pressure keeping
Time is 0.5~1h, treats that temperature is down to 100 DEG C of releases and takes out sample.
3. method as claimed in claim 2, it is characterized in that in the step (2), the injection speed of ferrocene carbon source solution is
10~30mL/h, growth time is 30~120min, and growth terminates to be cooled to room temperature taking-up under the protection of inert gas.
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| CN105439124B (en) * | 2015-12-17 | 2019-08-06 | 山西大同大学 | A method of growing carbon nanotubes in expanded graphite hole |
| CN105859291B (en) * | 2016-03-30 | 2018-07-13 | 天津大学 | The preparation method of three-dimensional highly-conductive hot carbon based composites |
| CN106116580B (en) * | 2016-06-30 | 2018-07-17 | 东华大学 | A kind of flexibility carbon film and preparation method thereof |
| CN106276859B (en) * | 2016-08-15 | 2018-11-30 | 天津大学 | A kind of preparation method for the carbon nanotube microballoon being coated with carbon film |
| CN108968703A (en) * | 2017-06-01 | 2018-12-11 | 佛山市顺德区美的电热电器制造有限公司 | Pot and cooking apparatus in ceramic inserts metal |
| CN110344020A (en) * | 2018-04-03 | 2019-10-18 | 江苏先丰纳米材料科技有限公司 | A kind of device and method preparing composite material using chemical vapor deposition |
| CN110871270B (en) * | 2018-09-04 | 2021-07-20 | 天津大学 | Preparation method of high-elasticity high-heat-conductivity three-dimensional carbon nanotube composite material |
| CN115637158A (en) * | 2022-12-23 | 2023-01-24 | 华北理工大学 | Expanded graphite/carbon nanotube composite material and preparation method and application thereof |
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