CN104943223B - There is graphite flake and the preparation method of high thermal conductivity coefficient along plane and thickness direction simultaneously - Google Patents
There is graphite flake and the preparation method of high thermal conductivity coefficient along plane and thickness direction simultaneously Download PDFInfo
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Abstract
The present invention relates to a kind of graphite flake and preparation method simultaneously with high thermal conductivity coefficient along plane and thickness direction, the graphite flake layer in graphite flake is S-type or waveform arranges, along in-plane thermal conductivity factor 80W/ (m K)；Through-thickness thermal conductivity factor 50W/ (m K).By expanded graphite extrusion forming from a direction that expansion rate is 100～300, it is thus achieved that graphite idiosome, then from another direction, graphite idiosome is suppressed, it is thus achieved that graphite precast body；Being placed in graphite jig by graphite precast body, be placed in vacuum hotpressing stove and carry out high temperature hot pressing, hot pressing temperature is at 800～2000 DEG C, and hot pressing pressure is 5～50MPa, heat-insulation pressure keeping 0.5～4h, treats that temperature is down to less than 100 DEG C releases and is taken out sample.The matrix material expanded graphite of the present invention is easy to get, and preparation and the heat pressing process of graphite precast body are simple.Obtain the graphite flake simultaneously with high thermal conductivity coefficient along plane and thickness direction.
Description
Technical field
The present invention relates to a kind of graphite flake and preparation method simultaneously with high thermal conductivity coefficient along plane and thickness direction, specifically
It it is a kind of method that expanded graphite is carried out secondary compacting along different directions.
Background technology
Along with the fast development of the field science and technology such as computer, communication and Aero-Space, ever-increasing heat conduction, radiating requirements
Opposite heat tube reason material proposes bigger requirement.Such as microelectronic chip surface temperature must be maintained at a temperature of relatively low (such as silicon device
Part 100 DEG C) just can ensure that its high performance operation, ensure without sufficient heat management, easily cause its premature aging or damage
Bad.Therefore, the high heat conduction scattering material that heat can effectively be dredged by exploitation becomes the key issue of heat management.Traditional
Density is relatively big, thermal coefficient of expansion is higher, oxidizable, not resistance to chemical attack owing to existing for metal heat-conducting material (such as aluminium, copper etc.)
Etc. limitation, it is difficult to meet the most growing radiating requirements.Material with carbon element have higher thermal conductivity factor, relatively low density,
Low thermal coefficient of expansion, excellent mechanical property and chemical stability, be a class Heat Conduction Material the most most with prospects, because of
And have broad application prospects in fields such as the energy, communication, electronics.
Expanded graphite be by natural flake graphite through graphite intercalation, wash, be dried, one that high-temperature expansion obtains loose porous
Vermiform material.Expanded graphite is owing to having the graphitization parietal layer of regular bulk, and the obstruction of phonon conduction is less, heat transfer efficiency
The highest, thus utilize expanded graphite to prepare high conductive graphite sheet and become the research emphasis of people, also occur similar patent mandate or
Open.State Intellectual Property Office of the People's Republic of China's grant number is CN101407322B, CN100368342C,
The patents of invention such as CN101458049A disclose the technology utilizing compression-expansion graphite to prepare heat-conducting plate.
Above-described patent of invention disclose only traditional expanded graphite preparation method and pressing process, only obtains heat conduction each
Heterotropic graphite heat conducting material.For graphite flake layer, the lattice vibrations of carbon atom are the bases of material conducts heat, therefore graphite material
In material, phonon transmission carries out travel at high speeds only along graphite crystal face, and between graphite wafer surface layer due to hypertelorism, serious shadow
The conduction of sound.After processing through graphite pressing process, graphite crystal face is orientated along in-plane under hot pressing function, thus
In conductive graphite sheet, only there is along in-plane high thermal conductivity (more than 100W/ (m K)), and through-thickness is being led
Heating rate is the lowest, less than 10W/ (m K) (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.).China
The through-thickness thermal conductivity of graphite heat conduction plate of the announcement such as patent application CN100368342C, CN103539111A all exist
10W/ (m K) is below.Holding up after being sheared by graphite film, the through-thickness thermal conductivity factor of mensuration is up to 75W/ (m K), so
And only have 2W/ (m K) (Qi-Zhen Liang, Xu-Xia Yao, Wei Wang, Yan Liu, and along in-plane thermal conductivity factor
Ching-Ping Wong,A three-dimensional vertically aligned functionalized multilayer graphene
architecture:an approach for graphene-based thermal interfacial materials,ACS nano,2011,5(3):
2392-2401.).The graphite flake that existing published patent of invention is obtained along the thermal conductivity factor of plane and thickness direction far from full
The foot requirement to the Heat Conduction Material capacity of heat transmission such as mainframe computer, highly integrated electronic device, opens on the basis of material with carbon element has superiority
Send out a kind of, along plane and thickness direction, there is the material of high thermal conductivity coefficient simultaneously and be particularly important.
Summary of the invention
The present invention is directed to the anisotropic heat conductivity that graphite flake prepared by existing expanded graphite is huge, i.e. can only have height in one direction
Thermal conductivity factor (more than 100W/ (m K)) and in the defect of other direction thermal conductivity factor too low (less than 10W/ (m K)), carry
For a kind of along plane and the thickness direction graphite flake with high thermal conductivity coefficient simultaneously and preparation method thereof.Lead along plane and thickness direction
Hot coefficient respectively reaches 80W/ (m K) and the graphite flake of 50W/ (m K).
The present invention is by the following technical solutions:
A kind of graphite flake along plane and thickness direction simultaneously with high thermal conductivity coefficient；Graphite flake layer in graphite flake is S-type or ripple
Shape wave arranges, along in-plane thermal conductivity factor 80W/ (m K)；Through-thickness thermal conductivity factor 50W/ (m K).Such as Fig. 1
Middle graphite flake and schematic cross-sectional view.
A kind of preparation method of the graphite flake along plane and thickness direction simultaneously with high thermal conductivity coefficient of the present invention, step is as follows:
(1) by expanded graphite extrusion forming from a direction that expansion rate is 100～300, it is thus achieved that graphite idiosome, then from separately
Graphite idiosome is suppressed by one direction, it is thus achieved that graphite precast body；
(2) being placed in graphite jig by graphite precast body, be placed in vacuum hotpressing stove and carry out high temperature hot pressing, hot pressing temperature exists
800～2000 DEG C, hot pressing pressure is 5～50MPa, heat-insulation pressure keeping 0.5～4h, treats that temperature is down to less than 100 DEG C releases and is taken out sample.
Moulding pressure in described step (1) is preferably 10～100MPa.
It is described as follows:
(1) expanded graphite is a kind of vermiform graphite material；Expansion rate refer to expansible graphite expand after with expand front volume ratio；
Can directly use commercially available prod；
(2) in the preparation process of precast body, needing to suppress expanded graphite in both direction, compacting for the first time makes to expand
The graphite flake layer of graphite is orientated along pressure at right angle direction, and second time compacting makes graphite precast body density increase and make it along another
Individual direction is orientated, and then improves its anisotropy, it is thus achieved that the graphite flake layer within precast body all have one along plane and thickness direction
Determining degree orientation, owing to graphite has high thermal conductivity coefficient along lamella i.e. crystal plane direction, the precast body after secondary compacting is along plane and thickness
All there is the graphite distribution along lamella direction in degree direction, and then precast body all has efficient hot-fluid transmission channel along both direction；
(3) precast body is carried out hot pressing, the oxygen-containing group in expanded graphite can be removed, repair the carbon backbone structure of graphite flake layer,
Make the further carbonization of graphite precast body and densified, improve the thermal conductivity factor of graphite flake；
It is compressing to the secondary of expanded graphite by above step, it is achieved that regulation and control anisotropic to expanded graphite precast body,
Make the further carbonization of expanded graphite precast body, densified through high temperature hot pressing, obtain thermal conductivity along in-plane more than or equal to 80
W/ (m K), the through-thickness high conductive graphite sheet more than or equal to 50W/ (m K).
Beneficial effects of the present invention: the matrix material expanded graphite of the present invention is easy to get, the preparation of graphite precast body and heat pressing process letter
Single.The microstructure ordering of graphite flake in the present invention, densified and graphitization can efficiently complete, and can obtain along plane and thickness
Direction has the graphite flake of high thermal conductivity coefficient simultaneously, its comprehensive capacity of heat transmission be far superior to traditional expanded graphite hot pressing coiled material and
The compacting expanded graphite of other forms.
Accompanying drawing illustrates:
Fig. 1 is preparation flow figure and the microcosmic schematic diagram of the graphite flake of the present invention；
Detailed description of the invention
Below in conjunction with the accompanying drawings and provide 6 embodiments of the present invention, it is the present invention to be further illustrated rather than limits the present invention
Scope.
Embodiment 1
As shown in Figure 1: the expanded graphite that expansion rate is 100 is placed in mould A, under 10MPa pressure, is pressed into graphite
Idiosome, is then placed in graphite idiosome in mould B, suppresses obtaining graphite precast body under 100MPa pressure from another direction,
Graphite precast body is placed in graphite jig, is placed in vacuum hotpressing stove and carries out high temperature hot pressing, hot pressing temperature at 800 DEG C, hot pressing
Pressure is 5MPa, heat-insulation pressure keeping 0.5h, treats that temperature is down to 100 DEG C of releases and is taken out sample.Testing stone ink sheet thermal conductivity factor, its
Being 110W/ (m K) along in-plane thermal conductivity factor, through-thickness is 50W/ (m K).
A kind of preparation method of the graphite flake along plane and thickness direction simultaneously with high thermal conductivity coefficient of the present invention, step is as follows:
(1) by expanded graphite that expansion rate is 100～300 under 10～100MPa pressure compressing, it is thus achieved that graphite idiosome,
Then suppressing graphite idiosome from another direction, pressure size is 10～100MPa, it is thus achieved that graphite precast body,；
(2) being placed in graphite jig by graphite precast body, be placed in vacuum hotpressing stove and carry out high temperature hot pressing, hot pressing temperature exists
800～2000 DEG C, hot pressing pressure is 5～50MPa, heat-insulation pressure keeping 0.5～4h, treats that temperature is down to less than 100 DEG C releases and is taken out sample.
Embodiment 2
The expanded graphite that expansion rate is 300 is pressed into graphite idiosome, then from another direction 10 under 100MPa pressure
Under MPa pressure, karbate impervious graphite idiosome obtains graphite precast body, is placed in graphite jig by graphite precast body, is placed in vacuum hotpressing stove
In carry out high temperature hot pressing, hot pressing temperature is at 1000 DEG C, and hot pressing pressure is 50MPa, heat-insulation pressure keeping 4h, treats that temperature is down to 100 DEG C
Sample is taken out in release.Testing stone ink sheet thermal conductivity factor, it is 80W/ (m K) along in-plane thermal conductivity factor, and through-thickness is
80W/(m·K)。
Embodiment 3
The expanded graphite that expansion rate is 200 is pressed into graphite idiosome, then from another direction 10 under 90MPa pressure
Under MPa pressure, karbate impervious graphite idiosome obtains graphite precast body, is placed in graphite jig by graphite precast body, is placed in vacuum hotpressing stove
In carry out high temperature hot pressing, hot pressing temperature is at 800 DEG C, and hot pressing pressure is 50MPa, heat-insulation pressure keeping 4h, treats that temperature is down to 100 DEG C
Sample is taken out in release.Testing stone ink sheet thermal conductivity factor, it is 80W/ (m K) along in-plane thermal conductivity factor, and through-thickness is
70W/(m·K)。
Embodiment 4
The expanded graphite that expansion rate is 200 is pressed into graphite idiosome, then from another direction 80 under 80MPa pressure
Under MPa pressure, karbate impervious graphite idiosome obtains graphite precast body, is placed in graphite jig by graphite precast body, is placed in vacuum hotpressing stove
In carry out high temperature hot pressing, hot pressing temperature is at 1200 DEG C, and hot pressing pressure is 25MPa, heat-insulation pressure keeping 1h, treats that temperature is down to 100 DEG C
Sample is taken out in release.Testing stone ink sheet thermal conductivity factor, it is 90W/ (m K) along in-plane thermal conductivity factor, and through-thickness is
60W/(m·K)。
Embodiment 5
The expanded graphite that expansion rate is 200 is pressed into graphite idiosome, then from another direction 50 under 50MPa pressure
Under MPa pressure, karbate impervious graphite idiosome obtains graphite precast body, is placed in graphite jig by graphite precast body, is placed in vacuum hotpressing stove
In carry out high temperature hot pressing, hot pressing temperature is at 1500 DEG C, and hot pressing pressure is 50MPa, heat-insulation pressure keeping 1h, treats that temperature is down to 100 DEG C
Sample is taken out in release.Testing stone ink sheet thermal conductivity factor, it is 120W/ (m K) along in-plane thermal conductivity factor, through-thickness
For 70W/ (m K).
Embodiment 6
The expanded graphite that expansion rate is 200 is pressed into graphite idiosome, then from another direction 100 under 10MPa pressure
Under MPa pressure, karbate impervious graphite idiosome obtains graphite precast body, is placed in graphite jig by graphite precast body, is placed in vacuum hotpressing stove
In carry out high temperature hot pressing, hot pressing temperature is at 2000 DEG C, and hot pressing pressure is 50MPa, heat-insulation pressure keeping 1h, treats that temperature is down to 100 DEG C
Sample is taken out in release.Testing stone ink sheet thermal conductivity factor, it is 150W/ (m K) along in-plane thermal conductivity factor, through-thickness
For 80W/ (m K).
Present invention disclosure and graphite flake and the preparation method along plane and thickness direction simultaneously with high thermal conductivity coefficient that propose, ability
Field technique personnel can be by using for reference present disclosure, and the link such as suitable feed change and process route realizes, although the method for the present invention
Being described by preferred embodiment with technology of preparing, person skilled substantially can be without departing from present invention, essence
In god and scope, methods and techniques described herein route is modified or reconfigures, realize final technology of preparing.Special
Not it is pointed out that all similar replacements and change apparent to those skilled in the art, they all by
It is considered as being included in present invention spirit, scope and content.
Claims (2)
1. have a preparation method for the graphite flake of high thermal conductivity coefficient along plane and thickness direction, step is as follows simultaneously:
(1) by expanded graphite extrusion forming from a direction that expansion rate is 100～300, it is thus achieved that graphite idiosome, then
From another direction, graphite idiosome is suppressed, it is thus achieved that graphite precast body；
(2) being placed in graphite jig by graphite precast body, be placed in vacuum hotpressing stove and carry out high temperature hot pressing, hot pressing temperature exists
800～2000 DEG C, hot pressing pressure is 5～50MPa, heat-insulation pressure keeping 0.5～4h, treats that temperature is down to less than 100 DEG C releases and is taken out
Sample；Graphite flake layer in the graphite flake of preparation is S-type or waveform arranges, along in-plane thermal conductivity factor 80W/ (m
·K)；Through-thickness thermal conductivity factor 50W/ (m K).
2. preparation method as claimed in claim 1, is characterized in that the moulding pressure in described step (1) is 10～100MPa.
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Cited By (1)
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| CN109554168A (en) * | 2017-09-22 | 2019-04-02 | 天津大学 | Carbon nano pipe array/graphene heat-conductive composite material and preparation method thereof |
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| CN105859291B (en) * | 2016-03-30 | 2018-07-13 | 天津大学 | The preparation method of three-dimensional highly-conductive hot carbon based composites |
| CN106185899A (en) * | 2016-07-11 | 2016-12-07 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of axial high thermal conductivity flexible graphite cake |
| CN107602122A (en) * | 2016-07-11 | 2018-01-19 | 佛山市顺德区美的电热电器制造有限公司 | The hot press forming technology and graphite pan of graphite pan |
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| CN116082047B (en) * | 2021-11-05 | 2024-05-07 | 天津大学 | Preparation method of heat dissipation in plane and high heat conduction orientation graphite plate outside plane constructed by hot pressing method |
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