CN106185899A - A kind of preparation method of axial high thermal conductivity flexible graphite cake - Google Patents
A kind of preparation method of axial high thermal conductivity flexible graphite cake Download PDFInfo
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- CN106185899A CN106185899A CN201610540487.1A CN201610540487A CN106185899A CN 106185899 A CN106185899 A CN 106185899A CN 201610540487 A CN201610540487 A CN 201610540487A CN 106185899 A CN106185899 A CN 106185899A
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Abstract
The preparation method of a kind of axial high thermal conductivity flexible graphite cake is by expansible graphite, thermally treated expanded graphite processed, use the method for tabular prefabrication molding or block two kinds of preforming of prefabrication molding by expanded graphite prefabrication, the prefabrication prepared is put in another mould, pressurize along pressure direction when being perpendicular to prefabrication molding and prepare product.It is high that the present invention has axial thermal conductivity, and preparation cost is low, can realize advantage prepared by scale.
Description
Technical field
The present invention relates to thermal management materials preparing technical field, be specifically related to the system of a kind of axial high thermal conductivity flexible graphite cake
Preparation Method.
Background technology
Graphite is a kind of typical layer structure Carbon Materials, is connected by more weak Van der Waals force between its each aspect, so people
With chemistry or electrochemical method, other foreign peoples's particle such as atom, molecule, ion can be inserted into the interlayer of crystalline graphite, give birth to
Becoming a kind of new layered nanocomposites, this material is commonly called compound between graphite layers (Graphite
Intercalation Compounds, is called for short GIC).Wherein, receptor type-GIC be a class prepare expanded graphite important before
Body, this is the anisotropic structure feature that make use of graphite: by weak molecule bonding force i.e. Van der Waals power between graphite crystal aspect
In conjunction with, and be to be linked by strong chemical bond covalent bonding forces in aspect；The interlayer structure feature of weak link is conducive to inserting foreign peoples's grain
Son, the most beneficially insert strut graphite aspect under the effect of high temperature, are formed and a kind of have the swollen of class accordion structure feature
Swollen graphite, and when the covalent bonding power in strong aspect ensure that high temperature puffing, c-axis direction only along graphite crystal is carried out, and
Towards the feature that original graphite crystal is still fully retained.The apparent bulk density of this expanded graphite particles is about 0.003-
0.01g/cm3, except retain crystalline flake graphite properties (such as high chemical stability, high-low temperature resistant, corrosion-resistant, conduct electricity, lead
Heat, low-expansion coefficient, safety non-toxic etc.) outward, also there is bigger specific surface area and higher surface activity, it is not necessary to any viscous
Knot agent, also need not sinter, so that it may variously-shaped flexible graphite article is prepared in compression forming.The pore property master of expanded graphite
Will based in, macropore, through appropriateness compacting formed low-density soft graphite can be used as adsorbing material.Owing to there is no binding agent,
The graphite material that soft graphite is the purest, therefore has all excellent properties of graphite, but owing to native graphite is through spy
Different PROCESS FOR TREATMENT, derives again compression and resilience that native graphite does not has.Owing to its microcosmic graphite flake layer is the most vertical
In compression direction, therefore, flexible graphite platelet has preferably conduction, heat conductivity along in-plane.Honeycomb due to expanded graphite
Network structure, vertical direction more or less some connection at graphite flake layer constitutes certain conductive and heat-conductive chain, therefore, although do not have
Have towards height, but axially also there is certain electrical and thermal conductivity performance.Owing to defining many closed pores in forming process, because of
This, soft graphite has good compression and resilience.Chemical resistance, heat-resisting quantity and good heat conduction plus it
Property, therefore soft graphite is particularly suitable for sealing, heat radiation or the sandwich material doing under severe rugged environment.
Along with electronic equipment is to high speed, small-sized, high power, high reliability, semiconductor device is to highly integrated, extensive, many
Lamellar, high power, circuit layout develops rapidly to the direction such as fine, short-term, low resistance, high power density electronic device and logic
Thousands of times of ground of the volume of circuit reduce, and can produce substantial amounts of heat in running.In the application that some are special, right
Heat sink material has the special and requirement of harshness, such as communications satellite high power density device, nuclear fusion device with in the face of wait from
Daughter material, the high-temperature exhaust emission passage etc. produced after space flight, aircraft engine fuel burning, all face the most quickly
The amount of heat producing and accumulating in running is discharged on ground, thus ensures the stable operation of equipment, thus the heat biography to material
Lead performance and propose the highest requirement.Therefore, high-efficiency heat conduction and heat dissipation problem become restriction high power density electronic device fast
One bottleneck of speed development.The multiple excellent properties of soft graphite, particularly heat-resisting quantity, chemical resistance, good pressure
The thermal coefficient of expansion retracting elastic, low, good heat conductivity etc., providing one for the solution of various thermal control problems can
Can be with alternative.Current alternative thermal management materials mainly has: the polymer matrix composites of high heat conduction constituent element enhancing, metal material
Material, ceramic material, Carbon Materials and various composite, such as composites such as charcoal-pottery, charcoal-charcoal, charcoal-metals.Pure carbon component
High heat-conductive carbon material has diamond or diamond-film-like, highly oriented pyrolytic graphite, intermediate phase pitch-based carbon-carbon composites
With soft graphite etc..Wherein the feature of high thermal conductive resin based composites is light weight but non-refractory, and the shortcoming of metal material is
Ratio is great, perishable, and diamond, pyrolytic graphite, the shortcoming of carbon-carbon composites are complicated process of preparation, expensive, pottery
The feature of material is high temperature resistant but property is crisp, resistant to elevated temperatures metal, pottery, charcoal and carbon-carbon composites compared with soft graphite, one
Being that hardness ratio is higher, two is that compression-resilience is poor.Soft graphite quality is softer, adds good compression-resilience, especially
Be conducive to reducing the thermal resistance between interface.Because an effective radiator structure is not to be made up of single material, such as high temperature
The solution of the heat dissipation problem under environment, interior lining can use antiscour, resistant to elevated temperatures carbon-carbon composites, outside permissible
Using hardware, due to hard-firm docking, there is bigger gap in interface, effective contact area is less, can cause bigger
Thermal resistance, if one layer of soft graphite of middle folder, hardening-firm docking is hard-soft-hard bind mode.Although this bind mode solves
Determined interface resistance problem, but require soft graphite axially also should have preferable heat-conductive characteristic.The most industrial pass through
Density prepared by the mode of roll-in be the axial thermal conductivity of the soft graphite of about 1g/cm3 typically at below 5W/mK, be far below
Flexible graphite paper or plate towards thermal conductivity (150-210W/mK), this is the structure height anisotropy institute intrinsic by graphite material
Determine.Actually flexible graphite material is applied as thermal management materials, and it expands the effect of heat towards acting primarily as, and can make hot spot district
The heat in territory spreads to surrounding, thus it is too high to avoid temperatures at localized regions so that whole towards Temperature Distribution ratio more uniform.Real
Application scenario, border is more to require the axial heat radiation from flexible graphite plate, and in other words, the heat dispersion of soft graphite is main
It is embodied on Axial Thermal conductive performance.Content involved by this patent is exactly the side about improving flexible graphite plate Axial Thermal conductive performance
Method, purpose makes soft graphite have bigger design alternative leeway as thermal management materials application.
According to non-metal solid heat transfer theory, non-metal solid conduction of heat is mainly carried out with the form of lattice wave, lattice
Heat conductivity is limited, such as by causing some processes of energy exchange between lattice wave: the imperfection of different types of lattice
Scattering process, the scattering etc. to phonon of the particular case lower boundary, cause the energy exchange between lattice wave to be all reflected in average freedom
In the relation of journey and mean free path and frequency, and heat conductivity is finally restricted by mean free path of phonons.Due to flexible stone
Ink is one to be close to pure material with carbon element, affects axial mean free path and is mainly the orientation of density and graphite flake layer, and actual should
Density be typically about about 1g/cm3.Improving with the increase of density towards pyroconductivity of soft graphite, and axial
Pyroconductivity more than critical density with density relation just with towards rule contrary, say, that axial, towards thermal conductance
There is shifting relation in rate.
At present soft graphite is applied as thermal management materials, mainly by its towards highly thermally conductive property, act the work expanding heat
With；And occasion of more dispelling the heat is desirable with its axial thermal conductance, due to the high anisotropy of soft graphite, particularly
The flexible graphite sheet material of more than 2mm, is difficult to obtain the highest thermal conductivity by existing continuous rolling mode.To this end, people
Attempted various method and improved its axial thermal conductivity performance, as fine with mesophase asphalt carbon fiber, CNT, vapor grown carbon
Dimension, Graphene contour heat conduction constituent element by being combined without binding agent, the fragility intrinsic due to expanded graphite and apparent close
Spend low feature, be difficult to uniformly mix with other material and combine closely, the most do not lose the compression resilience of its excellence simultaneously.I
Test result indicate that, the addition of foreign material, only useful in terms of intensity raising, and be unprofitable to improve axial thermal conductivity
Can, this is caused by the reason of interface increase.
Summary of the invention
It is an object of the invention to provide a kind of axial thermal conductivity high, preparation cost is low, and can realize prepared by scale is axial
The preparation method of high thermal conductivity flexible graphite cake.
The apparent density of the expanded graphite that the present invention uses is 3.0 × 10-3-1.0 × 10-2g/cm3, and apparent density is low
Expanded graphite worm compressibility is big, and the sheet material tensile strength prepared is higher；The expanded graphite worm compressibility that apparent density is high
Little, the tensile strength of the sheet material prepared is relatively low, but is prone to filling material when preparing prefabrication, is drawing the highest the answering of strong requirement
With the density requirements of occasion or end article in the case of 1.2g/cm3, it is recommended to use highdensity expanded graphite worm.Just
The apparent density of anthelmintic is for the heat conductivility of end article, and between the graphite worm that granule is little, contact probability increases, easy shape
Becoming heat conduction chain, and the bigger anthelmintic surface homogeneity of granule is bad, intergranular space is big, the air adsorption easily remained, material
Thermal conductivity the highest.But too small granule is also unfavorable for increasing the thermal conductivity of material.Forming the heat conduction chain time institute of equal length
Need fine particle number to increase, i.e. add intergranular contact point.When hot-fluid flows through material, material internal contact point dissipates
Range degree increases, and reduces the thermal conductivity of material on the contrary.
The preparation method of the present invention comprises the steps:
(1) prepared by expanded graphite
By the industrial goods expansible graphite of outsourcing, through 900-1200 DEG C of heat treatment expanded graphite, it is 3.0 that its apparent density controls
×10-3-1.0×10-2g/cm3；
(2) high-purity expanded graphite preforming
The present invention is in order to improve the axial thermal conductivity of soft graphite, and thinking is sacrificed a part exactly and exchanged axle towards heat conductivility for
To the raising of heat conductivility.It is axially to improve the pressing direction that is parallel to of the i.e. flexible graphite sheet material of expanded graphite stampings
Thermal conductivity, technical scheme have employed the method for two kinds of preforming, the i.e. molding of tabular prefabrication and block prefabrication
Molding.Both approaches is respectively arranged with feature, and the mould of tabular prefabrication is lightweight, volume is little, and charging is few, is suitable for preparation few
The goods of amount, and be difficult to charging by graphite worm and limited, the slit width of preforming tool should be not less than 4mm.This side
Method is primarily directed to prepare the flexible graphite sheet material of more than thickness 2mm.In view of the characteristic that expanded graphite apparent density is little, in order to just
In charging, under conditions of charge and prefabrication length and width size are certain, the width of slit is the biggest, and the density of prefabrication is the least；
On the contrary, under conditions of slit width and prefabrication length and width size are certain, charge is the most, and the density of prefabrication is the highest.Often
In actual application, the density of flexible graphite sheet material and dimensional requirement are certain, say, that charge is certain, at this
In the case of Zhong, the density of prefabrication can only be improved by reducing the width of slit.Briquetting pressure is 38-62MPa, and prefabrication is close
Degree is 0.3-0.5g/cm3。
And the advantage of the method for bulk prefabrication is that filling graphite worm is easy, it is suitable for preparing flexible graphite plate in a large number, because of
Being that one piece of block prefabrication can cut out many block tabulars, shortcoming is that the mould of prefabrication is bulky, Heavy Weight,
Need the press that work top is bigger.Briquetting pressure is 38-100MPa, and prefabrication density is 0.3-0.8g/cm3。
(3) prepared by flexible graphite sheet material
The prefabrication prepared is put in another mould, pressurize along pressure direction when being perpendicular to prefabrication molding, molding
Pressure is 100-150MPa.Accordingly.In secondary pressing process, originally in prefabrication, the lamella of graphite microcrystal was main along hanging down
Directly it is orientated in precompression direction, during post forming, when along after being perpendicular to precompression pressuring direction, although quite a few graphite
Crystallite lamella is along pressurized vertical direction again preferred orientation, but still some maintains and is axially oriented, and this is to improve flexibility
The key point of graphite sheet axial thermal conductivity performance.
The density of the axial high thermal conductivity flexible graphite cake of the present invention is 0.8-1.2g/cm3, axial thermal conductivity rate is 43-120W/
MK, is 208-238W/mK towards thermal conductivity.
The present invention compared with prior art has the advantage that
1, the axial thermal conductivity of flexible graphite plate prepared by the present invention is higher than the flexible graphite plate of presently commercially available all size
Axial thermal conductivity；
2, the thermal management materials design that the present invention can be actual provides more preferable choice；
3, the present invention can regulate and control flexible graphite sheet material easily towards, the thermal conductivity of axial both direction；
4, flexible graphite sheet material prepared by the present invention acts not only as heat sink along towards expanding heat, it is also possible to as heat sink edge
Axially heat radiation.
Detailed description of the invention
Embodiment 1
Expansible graphite is hot expanding treatment at 1200 DEG C, and the apparent density of the expanded graphite of preparation is 3.0 × 10-3g/cm3；Profit
With 300mm × 300mm × 1200mm cube of mould, the press face of mould is 300mm × 300mm face, in briquetting pressure 100MPa
Under, by block prefabrication pre-shaping method, prepare prefabrication a size of 300mm × 300mm × 300mm, apparent density is
0.8g/cm3Prefabrication, then cut out 300mm × 300mm × 3mm sheet material along prefabrication pressure surface, put into 300mm × 300mm
In × 40mm mould, along being perpendicular to 300mm × 300mm planar pressing, briquetting pressure 150Mpa, compacting thickness is 2mm, density is
1.2g/cm3Flexible graphite sheet material, its axial thermal conductivity rate is 120W/mK, is 230W/mK towards thermal conductivity.
Embodiment 2
Expansible graphite is hot expanding treatment at 1000 DEG C, and the apparent density of the expanded graphite of preparation is 4.0 × 10-3g/cm3；Profit
With 300mm × 300mm × 1200mm cube of mould, the press face of mould is 300mm × 300mm face, in briquetting pressure 62MPa
Under, by block prefabrication pre-shaping method, prepare prefabrication a size of 300mm × 300mm × 300mm, apparent density is
0.5g/cm3Prefabrication, then cut out 300mm × 300mm × 3mm sheet material along prefabrication pressure surface, put into 300mm × 300mm
In × 40mm mould, along being perpendicular to 300mm × 300mm planar pressing, briquetting pressure 125MPa, compacting thickness is 1.5mm, density
For 1.0g/cm3Flexible graphite sheet material, its axial thermal conductivity rate is 75W/mK, is 215W/mK towards thermal conductivity.
Embodiment 3
Expansible graphite is hot expanding treatment at 900 DEG C, and the apparent density of the expanded graphite of preparation is 4.3 × 10-3g/cm3；Profit
With 300mm × 300mm × 1200mm cube of mould, the press face of mould is 300mm × 300mm face, at briquetting pressure 38 MPa
Under, by block prefabrication pre-shaping method, prepare prefabrication a size of 300mm × 300mm × 300mm, apparent density is
0.3g/cm3Prefabrication, then cut out 300mm × 300mm × 2.7mm sheet material along prefabrication pressure surface, put into 300mm ×
In 300mm × 40mm mould, along being perpendicular to 300mm × 300mm planar pressing, briquetting pressure 100MPa, compacting thickness is
1.0mm, density are 0.8g/cm3Flexible graphite sheet material, its axial thermal conductivity rate is 43W/mK, is 208W/mK towards thermal conductivity.
Embodiment 4
Expansible graphite is hot expanding treatment at 1200 DEG C, and the apparent density of the expanded graphite of preparation is 3.0 × 10-3g/cm3；Profit
With 300mm × 6mm × 1700mm cube of mould, die slit width is 6mm, and press face is 300mm × 6mm face, in molding pressure
Under power 62MPa, by tabular prefabrication pre-shaping method, prepare prefabrication a size of 300mm × 300mm × 6mm, apparent density
For 0.5g/cm3Prefabrication, be then placed in 300mm × 300mm × 40mm mould, along being perpendicular to 300mm × 300mm plane
Pressure, briquetting pressure 150Mpa, compacting thickness is 2.5mm, density is 1.2g/cm3Flexible graphite sheet material, its axial thermal conductivity rate
For 68W/mK, it is 238W/mK towards thermal conductivity.
Embodiment 5
Expansible graphite is hot expanding treatment at 1000 DEG C, and the apparent density of the expanded graphite of preparation is 4.0 × 10-3g/cm3；Profit
With 300mm × 6mm × 1200mm cube of mould, die slit width is 6mm, and press face is 300mm × 6mm face, in molding pressure
Under power 50 MPa, prepare prefabrication a size of 300mm × 300mm × 6mm, apparent density is 0.4g/cm3Prefabrication, so
After put in 300mm × 300mm × 40mm mould, along being perpendicular to 300mm × 300mm planar pressing, briquetting pressure 125MPa, pressure
Thickness processed is 2.4mm, density is 1.0g/cm3Flexible graphite sheet material, its axial thermal conductivity rate is 66W/mK, towards thermal conductivity is
220W/mK。
Embodiment 6
Expansible graphite is hot expanding treatment at 900 DEG C, and the apparent density of the expanded graphite of preparation is 4.3 × 10-3g/cm3；Profit
With 300mm × 6mm × 1700mm cube of mould, die slit width is 6mm, and press face is 300mm × 6mm face, in molding pressure
Under power 38 MPa, prepare prefabrication a size of 300mm × 300mm × 6mm, apparent density is 0.3g/cm3Prefabrication, so
Tailing edge prefabrication pressure surface cuts out 300mm × 300mm × 2.2mm sheet material, puts in 300mm × 300mm × 40mm mould, along hanging down
Straight in 300mm × 300mm planar pressing, briquetting pressure 100MPa, compacting thickness is 1.0mm, density is 0.8g/cm3Flexibility
Graphite sheet, its axial thermal conductivity rate is 43W/mK, is 208W/mK towards thermal conductivity.
Claims (2)
1. the preparation method of an axial high thermal conductivity flexible graphite cake, it is characterised in that comprise the steps:
(1) prepared by expanded graphite
By industrial goods expansible graphite, through 900-1200 DEG C of heat treatment expanded graphite, it is 3.0 × 10 that its apparent density controls-3-
1.0×10-2g/cm3；
(2) high-purity expanded graphite preforming
Employing tabular prefabrication molding or the method for block two kinds of preforming of prefabrication molding:
When using tabular prefabrication molding, the slit width of preforming tool should be not less than 4mm, and briquetting pressure is 38-62MPa,
Prefabrication density is 0.3-0.5g/cm3；
When using block prefabrication molding, briquetting pressure is 38-100MPa, and prefabrication density is 0.3-0.8g/cm3；
(3) prepared by flexible graphite sheet material
The prefabrication prepared is put in another mould, pressurize along pressure direction when being perpendicular to prefabrication molding, molding
Pressure is 100-150Mpa.
Product prepared by the preparation method of a kind of axial high thermal conductivity flexible graphite cake the most as claimed in claim 1, its feature exists
It is 0.8-1.2g/cm in density3, axial thermal conductivity rate is 43-120W/mK, is 208-238W/mK towards thermal conductivity.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109802149A (en) * | 2019-03-19 | 2019-05-24 | 上海神力科技有限公司 | A kind of flexible graphite sheet material inside synusia direction-controlling method |
| CN109808222A (en) * | 2019-01-16 | 2019-05-28 | 北京航空航天大学 | A kind of compression-expansion graphite heat conducting material and preparation method thereof |
| CN109921052A (en) * | 2019-03-19 | 2019-06-21 | 上海神力科技有限公司 | A kind of preparation method of vertical lamellar structure flexible graphite polar plate |
| CN111211315A (en) * | 2020-02-26 | 2020-05-29 | 中国科学院山西煤炭化学研究所 | Asphalt substrate layer carbon material and preparation method and application thereof |
| CN114656939A (en) * | 2022-05-10 | 2022-06-24 | 华南理工大学 | Expanded graphite-based composite phase-change material with anisotropic thermal conductivity and preparation method thereof |
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| CN104495795A (en) * | 2014-11-24 | 2015-04-08 | 云南云天化股份有限公司 | Graphite flake and preparation method thereof |
| CN104943223A (en) * | 2015-06-17 | 2015-09-30 | 天津大学 | Graphite sheet with high heat conductivity coefficients along plane and thickness directions at the same time and preparation method |
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Patent Citations (2)
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| CN104495795A (en) * | 2014-11-24 | 2015-04-08 | 云南云天化股份有限公司 | Graphite flake and preparation method thereof |
| CN104943223A (en) * | 2015-06-17 | 2015-09-30 | 天津大学 | Graphite sheet with high heat conductivity coefficients along plane and thickness directions at the same time and preparation method |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109808222A (en) * | 2019-01-16 | 2019-05-28 | 北京航空航天大学 | A kind of compression-expansion graphite heat conducting material and preparation method thereof |
| CN109802149A (en) * | 2019-03-19 | 2019-05-24 | 上海神力科技有限公司 | A kind of flexible graphite sheet material inside synusia direction-controlling method |
| CN109921052A (en) * | 2019-03-19 | 2019-06-21 | 上海神力科技有限公司 | A kind of preparation method of vertical lamellar structure flexible graphite polar plate |
| CN109802149B (en) * | 2019-03-19 | 2023-07-21 | 上海神力科技有限公司 | Method for controlling direction of internal lamellar sheet of flexible graphite sheet |
| CN111211315A (en) * | 2020-02-26 | 2020-05-29 | 中国科学院山西煤炭化学研究所 | Asphalt substrate layer carbon material and preparation method and application thereof |
| CN111211315B (en) * | 2020-02-26 | 2023-02-28 | 中国科学院山西煤炭化学研究所 | Asphalt substrate layer carbon material and preparation method and application thereof |
| CN114656939A (en) * | 2022-05-10 | 2022-06-24 | 华南理工大学 | Expanded graphite-based composite phase-change material with anisotropic thermal conductivity and preparation method thereof |
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Application publication date: 20161207 |