CN110092374A - A kind of preparation method and graphite film material of electrographite film - Google Patents
A kind of preparation method and graphite film material of electrographite film Download PDFInfo
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- CN110092374A CN110092374A CN201910455339.3A CN201910455339A CN110092374A CN 110092374 A CN110092374 A CN 110092374A CN 201910455339 A CN201910455339 A CN 201910455339A CN 110092374 A CN110092374 A CN 110092374A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 239000010439 graphite Substances 0.000 title claims abstract description 113
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 113
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 207
- 238000000034 method Methods 0.000 claims abstract description 95
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000011265 semifinished product Substances 0.000 claims abstract description 20
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 claims abstract description 19
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 238
- 238000010792 warming Methods 0.000 claims description 115
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000004642 Polyimide Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 21
- 238000013467 fragmentation Methods 0.000 abstract description 7
- 238000006062 fragmentation reaction Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 description 21
- 238000003763 carbonization Methods 0.000 description 16
- 239000004575 stone Substances 0.000 description 7
- 238000005087 graphitization Methods 0.000 description 6
- 239000004417 polycarbonate Substances 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 241001232787 Epiphragma Species 0.000 description 5
- 238000013461 design Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
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- 150000001875 compounds Chemical class 0.000 description 3
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- 239000012535 impurity Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000112 cooling gas Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- 239000002969 artificial stone Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 239000002113 nanodiamond Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
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- 230000001681 protective effect Effects 0.000 description 1
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- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
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Abstract
The present invention discloses the preparation method and graphite film material of a kind of electrographite film, the preparation method of the electrographite film includes: that Kapton to be roasted is carried out first time temperature-gradient method according to pre-set dimension, Kapton is set to react, then cooling obtains semi-finished product film；Semi-finished product film is subjected to second of temperature-gradient method under inert gas protection, semi-finished product film is made to react, then cooling obtains graphite film.The present invention is using Kapton as raw material, by designing double fragmentation temperature-rise period, appropriate dynamic temperature field is formed using first time temperature-gradient method process, obtaining has high-crystallinity structure, then on the basis of first time temperature-gradient method, further by means of second of temperature-gradient method process, double fragmentation temperature-rise period is set to cooperate, form the graphite film of highly oriented, high-crystallinity, high conductance energy, to make the graphite film being prepared thermal coefficient with higher, the heating conduction of graphite film is improved.
Description
Technical field
The present invention relates to graphite film manufacturing technology field, in particular to a kind of the preparation method and graphite of electrographite film
Membrane material.
Background technique
With the continuous development of science and technology, various types of electric terminals and ancillary equipment, electronic component, such as electronics
Terminal such as laptop, tablet computer, smart phone etc., ancillary equipment such as charger baby etc..For electric terminal,
The function of electric terminal is stronger and stronger, arithmetic speed is getting faster, size it is smaller and smaller cause to produce be hard to avoid
Heat dissipation problem；And more and more frequent, highly integrated, the high density of electronic component in many household electrical appliance of use of ancillary equipment
Change, this can all make, and the calorific value of electric terminal, ancillary equipment and electronic component is increasing or heat generating spot is increasingly concentrated.
In addition, in fields such as guided missile nose-cone, solid rocket motor nozzle, aerospace craft heat control system and nuclear fusion reactions,
Heat dissipation problem is also rucial scientific and technological problems urgently to be resolved.How heat dissipation problem is solved, is that the technology that all production firms are faced is difficult
Topic.Therefore graphite film is high as a kind of thermal conductivity and is widely used in the electronics industry in the Heat Conduction Material of film-form,
It can effectively transmit heat caused by electronic component to radiator bodies such as radiators, so that the heat by electronic component is fast
Speed is spread to reduce the temperature of the electronic component of fever.Charcoal, graphite material thermal conductivity with higher, excellent mechanical performance,
Low-density, low thermal coefficient of expansion etc., it is considered to be the excellent material for solving the above heat dissipation problem has very big development potentiality.
There are many ways to preparing electrographite film at present, such as using Kapton as raw material, by polyamides
It is carbonized and is graphitized in retort after imines film and graphite paper are cross layered, enhance the bending resistance of graphite film
Can, the brittleness of graphite film be reduced, but not improved significantly to the thermal conductivity of graphite film；For another example using by nanogold
Hard rock and the compound obtained laminated film of polyimides as raw material, with graphite paper it is cross layered after carry out carbonization and graphite
Change, obtain the composite stone ink film being compounded to form by Nano diamond and polyimides, improves degree of graphitization and carbonization yield, from
And the heating conduction of composite stone ink film is improved to a certain extent, but its thermal conductivity is still not ideal enough, thermal conductivity highest
Only 1056W/ (mK), it still needs further improvement.So the generally existing thermal conductivity of graphite film made from existing preparation method
Bad problem, preparation process are to be improved.
Summary of the invention
The main object of the present invention is to propose the preparation method and graphite film material of a kind of electrographite film, it is intended to be improved
The thermal coefficient of graphite film.
To achieve the above object, the present invention proposes a kind of preparation method of electrographite film, comprising the following steps:
Step S30, Kapton to be roasted is subjected to first time temperature-gradient method according to pre-set dimension, keeps polyamides sub-
Amine film reacts, and then cooling obtains semi-finished product film；
Step S40, the semi-finished product film is subjected to second of temperature-gradient method under inert gas protection, makes the semi-finished product
Film reacts, and then cooling obtains graphite film.
Preferably, the first time temperature-gradient method in step S30 includes:
Temperature T2 is warming up to by room temperature, then temperature T3 is continuously heating to by temperature T2, is then continuously heating to by temperature T3
Temperature T6, and 60~90min is kept the temperature after being warming up to temperature T6, wherein T2 is 470~490 DEG C, and T3 is 600~630 DEG C,
T6 is 1100~1550 DEG C.
Preferably, the step of being warming up to temperature T2 by room temperature includes: to be warming up to temperature T1 by room temperature, then by temperature T1 after
It is continuous to be warming up to temperature T2, wherein T1 is 430~465 DEG C；And/or
The step of being warming up to temperature T6 by temperature T3 includes: to be warming up to temperature T4 by temperature T3, is then continued by temperature T4
It is warming up to temperature T5, then temperature T6 is continuously heating to by temperature T5, wherein T4 is 680~720 DEG C, and T5 is 880~920 DEG C.
Preferably, during the first time temperature-gradient method in step s 30:
It is 8~12 DEG C/min by the heating rate that room temperature is warming up to T1；And/or
It is 0.5~3.5 DEG C/min by the heating rate that T1 is warming up to T2；And/or
It is 0.3~2.5 DEG C/min by the heating rate that T2 is warming up to T3；And/or
It is 1.5~3 DEG C/min by the heating rate that T3 is warming up to T4；And/or
It is 3~4 DEG C/min by the heating rate that T4 is warming up to T5；And/or
It is 3~6.5 DEG C/min by the heating rate that T5 is warming up to T6；And/or
20~30min is kept the temperature after being warming up to temperature T2.
Preferably, second of temperature-gradient method in step S40 include:
Temperature T7 is warming up to by room temperature, temperature T8 is continuously heating to by temperature T7, temperature T9 is continuously heating to by temperature T8,
Temperature T11 is continuously heating to by temperature T9, temperature T12 is continuously heating to by temperature T11, and be continuously heating to by temperature T12
Temperature T13, and after being warming up to temperature T13 keep the temperature 10~40min, wherein T7 be 1000~1200 DEG C, T8 be 1580~
1620 DEG C, T9 is 1780~1820 DEG C, and T11 is 2300 DEG C, and T12 is 2500~2520 DEG C, and T13 is 2600~2850 DEG C.
Preferably, second of temperature-gradient method in step S40 include:
Temperature T7 is warming up to by room temperature, temperature T8 is continuously heating to by temperature T7, temperature T9 is continuously heating to by temperature T8,
Temperature T10 is continuously heating to by temperature T9, temperature T11 is continuously heating to by temperature T10, temperature is continuously heating to by temperature T11
T12, and temperature T13 is continuously heating to by temperature T12, and 10~40min is kept the temperature after being warming up to temperature T13, wherein T7
It is 1000~1200 DEG C, T8 is 1580~1620 DEG C, and T9 is 1780~1820 DEG C, and T10 is 2000 DEG C, and T11 is 2200 DEG C, T12
It is 2500~2520 DEG C, T13 is 2600~2850 DEG C.
Preferably, during second of temperature-gradient method in step S40:
Temperature T10 is being warming up to by temperature T9, temperature T11 is warming up to by temperature T10 and temperature is warming up to by temperature T11
It spends in three heating steps of T12, wherein at least two heating step further includes being protected after correspondence is warming up to set temperature
Temperature, and soaking time is 10~30min；And/or
It is 8~10 DEG C/min by the heating rate that room temperature is warming up to T7；And/or
It is 5~6 DEG C/min by the heating rate that T7 is warming up to T8；And/or
It is 8~10 DEG C/min by the heating rate that T8 is warming up to T9；And/or
It is 1.5~3.5 DEG C/min by the heating rate that T9 is warming up to T10；And/or
It is 1.5~3.5 DEG C/min by the heating rate that T10 is warming up to T11；And/or
It is 1.5~3.5 DEG C/min by the heating rate that T11 is warming up to T12；And/or
It is 2~4 DEG C/min by the heating rate that T12 is warming up to T13.
Preferably, before step S30, further includes:
Step S10, it is wound after being cut Kapton raw material, between making between every adjacent two layers film
Gap is 90~180 μm, obtains fluffy Kapton；
Step S20, the fluffy Kapton is placed on roasting fixture, and is fixed using high purity graphite,
Obtain Kapton to be roasted.
Preferably, the ambient pressure during the first time temperature-gradient method in step S10 is -0.08~-0.1MPa；
And/or
The Kapton in step S10 with a thickness of 33~100 μm；And/or
The inert gas in step S20 is argon gas.
The present invention also proposes that a kind of graphite film material, the graphite film material include in the counterdie and artificial stone being stacked
Ink film, wherein the electrographite film is made by the preparation method of electrographite film as described above.
In technical solution provided by the invention, using Kapton as raw material, heated up by designing double fragmentation
The mode of journey forms appropriate dynamic temperature field using first time temperature-gradient method process, and obtaining has the half of high-crystallinity structure
Finished product, further by means of the design of second of temperature-gradient method, makes double fragmentation then on the basis of first time temperature-gradient method
Temperature-rise period cooperates, and the graphite film of highly oriented, high-crystallinity, high conductance energy is formed, to make the graphite being prepared
Film thermal coefficient with higher.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
For the thermal conductivity for improving graphite film, the present invention proposes a kind of preparation method of electrographite film, using polyimides
(Polyimide, below abbreviation PI) film improves obtained as raw material by the design of double fragmentation heating mode
Graphite film thermal conductivity.In an embodiment of the preparation method of electrographite film provided by the invention, the electrographite
The preparation method of film the following steps are included:
Step S30, PI film to be roasted is subjected to first time temperature-gradient method according to pre-set dimension, PI film occurs anti-
It answers, then cooling obtains semi-finished product film；
PI film is mainly pyrolyzed during the first time temperature-gradient method, releases CO and CO2, and N, O etc. are miscellaneous
Atom gradually releases, and fracture and recombination occur for the molecular chain structure of PI, as material film is gradually to crystal structure transition,
Graphite-like structure is derived, not expected turnover occur in mechanics and heat transfer, electrical conduction performance, this process is understood that
At be to PI film carry out carbonization treatment, correspondence obtain semi-finished product carbonized film, it is understood that at be PI film is purified,
The pretreatment such as removal of impurities or coke discharging, correspondence obtains pretreated semi-finished product film, below with the PI film in the first time
The reaction that temperature-gradient method process is occurred is considered as being illustrated for carbonization.The segmentation liter that the present invention passes through design carbonisation
Warm program forms appropriate dynamic temperature field, to successfully obtain the semi-finished product film with high-crystallinity structure after carbonization.Having
When body is implemented, the carbonisation can be capable of in the equipment of heat temperature raising in such as retort, high temperature furnace etc. to be carried out, and more excellent
It is selected as that the retort of temperature program can be set, is easy to implement during temperature-gradient method the accurate control to temperature, and by institute
It states after PI film is placed into the retort, vacuumize process is carried out to the retort, adjusts the inside of the retort
Air pressure is -0.08~-0.1MPa, so, it is possible to reduce the composition of air in the retort is influenced caused by carbonisation.
In the present embodiment, the first time temperature-gradient method in step S30 include: temperature T2 is warming up to by room temperature, then
Temperature T3 is continuously heating to by temperature T2, temperature T6 is then continuously heating to by temperature T3, and protect after being warming up to temperature T6
60~90min of temperature, wherein T2 is 470~490 DEG C, and T3 is 600~630 DEG C, and T6 is 1100~1550 DEG C.In the first time
It after temperature-gradient method process, is cooled to room temperature and obtains the carbonized film, the type of cooling can be natural cooling, be also possible to
It is realized by being passed through cooling gas into the retort.Wherein, in step S30 after being warming up to final temperature T6 heat preservation 60~
The process of 90min is to provide temperature platform for the carbonisation of PI film, at this point, the dynamic temperature field in carbonisation and perseverance
Warm platform mating reaction is suitably buffered when so that discharging heteroatom in carbonisation, is prevented former because acutely excluding heterocycle
The defects of period of the day from 11 p.m. to 1 a.m takes away C atom, reduces intramolecular fracture finally to subtract while improving the removal of impurity of carbonation stage
The defects of having lacked molecule inner folds or fracture, obtain the carbonized structure of high-crystallinity.
Further, it during the first time temperature-gradient method, can be directly by the mode that room temperature is warming up to temperature T2
It connects and temperature T2 is warming up to by normal-temperature continuous, be also possible to be done step-by-step by multiple temperature-rise periods, and use multiple temperature-rise periods
It when the mode being done step-by-step, can operate in the following way: temperature T1 being first warming up to by room temperature, then continues to heat up by temperature T1
To temperature T2, wherein T1 is 430~465 DEG C.
Similarly, the step of being warming up to temperature T6 by temperature T3 is also possible to directly by temperature T3 continuous warming to temperature
T6, or be done step-by-step by multiple temperature-rise periods, and when in such a way that multiple temperature-rise periods being done step-by-step, it can be according to following
Mode operates: being warming up to temperature T4 by temperature T3, is then continuously heating to temperature T5 by temperature T4, then continue to heat up by temperature T5
To temperature T6, wherein T4 is 680~720 DEG C, and T5 is 880~920 DEG C.It should be noted that being warming up to temperature T2's by room temperature
Step and the step of be warming up to temperature T6 by temperature T3 in, can be any step and realized using multiple temperature-rise periods,
It can be two steps and be all made of multiple temperature-rise periods realizations, preferably two steps are all made of above-mentioned offer in the present embodiment
Multiple temperature-rise periods realize, that is, the first time temperature-gradient method process from low to high in total include six temperature rise periods, more
Be conducive to form appropriate dynamic temperature field in the carbonisation of the PI film.
Further, the heating rate during first time temperature-gradient method, during six temperature rise periods
Can according to energy conservation and product property to actual demand be configured, in the present embodiment, preferably each liter
Heating rate during thermophase is correspondingly arranged are as follows: is warming up to the heating rate of T1 by room temperature as 8~12 DEG C/min；And/or
It is 0.5~3.5 DEG C/min by the heating rate that T1 is warming up to T2；And/or being warming up to the heating rate of T3 by T2 is 0.3~2.5
℃/min；And/or the heating rate of T4 is warming up to as 1.5~3 DEG C/min by T3；And/or the heating speed of T5 is warming up to by T4
Rate is 3~4 DEG C/min；And/or the heating rate of T6 is warming up to as 3~6.5 DEG C/min by T5.It is segmented and rises in the first time
During temperature, the heating rate of any one temperature rise period in six temperature rise periods can be according to the heating speed of above-mentioned offer
Rate setting is also possible to the corresponding heating according to above-mentioned offer of heating rate of multiple temperature rise periods in six temperature rise periods
Rate setting.Preferably, in embodiments of the present invention, six heating ranks during the more preferably described first time temperature-gradient method
Section is corresponded to be arranged according to the heating rate of above-mentioned offer, in this way, improving the removal of impurity of carbonation stage.
During carrying out first time temperature-gradient method, specific heating mode can be zonal cooling heating, can also be with
By the way of gradient increased temperature, namely in corresponding one soaking zone of setting after being warming up to required temperature.Using gradient increased temperature
When mode, the wherein at least one temperature rise period can be selected to set in five temperature rise periods before the first time temperature-gradient method
Soaking zone is set, such as can choose and kept the temperature after being warming up to temperature T2, soaking time is 20~30min.
Step S40, the semi-finished product film is subjected to second of temperature-gradient method under inert gas protection, makes the semi-finished product
Film reacts, and then cooling obtains graphite film.
The semi-finished product film that carbonization obtains occurs after the first time temperature-gradient method, using further second point
Section heating treatment, is graphitized the semi-finished product film, graphite film product can be obtained, wherein the graphitization stage is compared to carbonization
Phase temperature is much higher, and carbon hexagonal network is mainly carried out ordering, and complicated three phase transition and carbon occur in reacting field again
Crystallization process.In the specific implementation, the graphitizing process carries out in graphitizing furnace, and heating journey more preferably can be set
The graphitizing furnace of sequence is easy to implement during temperature-gradient method the accurate control to temperature, and fills in the graphitizing furnace lazy
Property gas, such as helium, argon gas, xenon etc., preferably argon gas in the present embodiment, to reduce carbonization to the full extent
Side reaction of the film in graphitizing process.
It when carrying out second of temperature-gradient method, can carry out in the following way: temperature T7 is warming up to by room temperature, by temperature
T7 is continuously heating to temperature T8, is continuously heating to temperature T9 by temperature T8, temperature T11 is continuously heating to by temperature T9, by temperature
T11 is continuously heating to temperature T12, and is continuously heating to temperature T13 by temperature T12, and keep the temperature after being warming up to temperature T13
10~40min, wherein T7 is 1000~1200 DEG C, and T8 is 1580~1620 DEG C, and T9 is 1780~1820 DEG C, T11 2300
DEG C, T12 is 2500~2520 DEG C, and T13 is 2600~2850 DEG C.It is cooled to room temperature that (its type of cooling is same after insulating process
Sample can be natural cooling or the mode for being passed through cooling gas), i.e., the graphite film is successfully made.
The semi-finished product film also can further exclude heteroatom at graphited initial stage in stage, and as temperature increases, C
Atomic arrangement crystallization is rapider, violent, and crystallization reaction is arranged when reaching certain high temperature and is failed again, therefore, in the present embodiment, step
The process for keeping the temperature 10~40min in rapid S40 after being warming up to final temperature can mention for the graphitizing process of the semi-finished product film
For temperature platform, so that the crystallization of C atomic arrangement is more uniform, i.e., the thickness of the graphite film obtained after the completion of graphitization is more mixed,
The probability for the defects of surface fracture, particle occur substantially reduces.
It further, can by the mode that temperature T9 is continuously heating to temperature T11 during second of temperature-gradient method
To be that in the manner described above, by the direct continuous warming of temperature T9 to temperature T11, T11 is set as 2300 DEG C at this time；It is also possible to lead to
It crosses multiple temperature-rise periods to be done step-by-step, the mode to heat up for example, by using two sections or multistage.In the present embodiment, it is heated up using two sections
Mode, specifically, at this time correspond to using second of temperature-gradient method by the way of are as follows: temperature T7 is warming up to by room temperature, by temperature
T7 is continuously heating to temperature T8, is continuously heating to temperature T9 by temperature T8, temperature T10 is continuously heating to by temperature T9, by temperature
T10 is continuously heating to temperature T11, is continuously heating to temperature T12 by temperature T11, and be continuously heating to temperature by temperature T12
T13, and 10~40min is kept the temperature after being warming up to temperature T13, wherein T7 is 1000~1200 DEG C, and T8 is 1580~1620
DEG C, T9 is 1780~1820 DEG C, and T10 is 2000 DEG C, and T11 is 2200 DEG C, and T12 is 2500~2520 DEG C, and T13 is 2600~2850
℃.That is, in the present embodiment, second of temperature-gradient method process includes seven temperature rise periods in total from low to high.
Similarly, during second of temperature-gradient method, specific heating mode can be zonal cooling heating,
A soaking zone can also be set by the way of gradient increased temperature, namely after correspondence is warming up to required temperature.Using gradient
When the mode of heating, wherein one or more can be selected in six temperature rise periods before second of temperature-gradient method
Soaking zone is arranged in temperature rise period.In the present embodiment, preferably are as follows: temperature T10 is being warming up to by temperature T9, is being heated up by temperature T10
In three heating steps for being warming up to temperature T12 to temperature T11 and by temperature T11, wherein at least two heating step is also wrapped
It includes and is kept the temperature after correspondence is warming up to set temperature, and soaking time is 10~30min, that is, being warming up to 2000 in correspondence
DEG C, after the temperature of 2200 DEG C or 2500 DEG C, the guarantor of a length of 10~30min when optionally being added in two of them heating step
Temperature section.Specifically, it can be after being warming up to T10 by T9 10~30min of heat preservation, keep the temperature 10 after being warming up to T11 by T10~
30min, and do not kept the temperature after being warming up to T12 by T11；Be also possible to after being warming up to T10 by T9 keep the temperature 10~30min, by
T10 is not kept the temperature after being warming up to T11, and 10~30min is kept the temperature after being warming up to T12 by T11；Either after being warming up to T10 by T9
It does not keep the temperature, and keeps the temperature 10~30min after being warming up to T11 by T10, and keep the temperature 10~30min after being warming up to T12 by T11；Again
Either after corresponding heat up T10, T11 and T12, the soaking zone of a length of 10~30min when being correspondingly arranged.
Further, heating during second of temperature-gradient method, during seven temperature rise periods
Rate can according to energy conservation and product property to actual demand be configured, in the present embodiment, preferably often
Heating rate during one temperature rise period is correspondingly arranged are as follows: is warming up to the heating rate of T7 by room temperature as 8~10 DEG C/min；
And/or the heating rate of T8 is warming up to as 5~6 DEG C/min by T7；And/or being warming up to the heating rate of T9 by T8 is 8~10
℃/min；And/or the heating rate of T10 is warming up to as 1.5~3.5 DEG C/min by T9；And/or the liter of T11 is warming up to by T10
Warm rate is 1.5~3.5 DEG C/min；And/or the heating rate of T12 is warming up to as 1.5~3.5 DEG C/min by T11；And/or
It is 2~4 DEG C/min by the heating rate that T12 is warming up to T13.Similarly, it during second of temperature-gradient method, can be
The heating rate of any one temperature rise period in seven temperature rise periods is arranged according to the heating rate of above-mentioned offer, is also possible to
The heating rate of multiple temperature rise periods in seven temperature rise periods is corresponded to be arranged according to the heating rate of above-mentioned offer.Preferably
Ground, in embodiments of the present invention, seven temperature rise periods during more preferably described second of temperature-gradient method correspond to according to
The heating rate of above-mentioned offer is arranged, and graphite film obtained has the characteristics that highly oriented, high-crystallinity and high conductance energy.It needs
Illustrate, is used during second of temperature-gradient method and the mode of temperature T11 is warming up to as a direct step by temperature T9
When heating mode in place, the heating rate that each warming-up section is selected in entire temperature-rise period can also be according to above-mentioned offer
Heating rate is configured, and this will not be repeated here.
Under normal conditions, if it is desired to obtain the high graphite film of carbonizing degree, then the thickness of raw material cannot be too thick, and this
When be unable to satisfy requirement to sintered density again；, whereas if pursuing sintered density, then the thickness of raw material must increase, this
When again can due to sintering process deficiency and the carbonizing degree for sacrificing graphite film of having to.That is, existing use PI film
It is prepared in the technique of graphite film for raw material, the thickness of the thickness of PI film and final graphite film product obtained exists certain
Corresponding relationship, for example, it is desired to which the thickness of the corresponding PI film selected is generally most when preparing the graphite film that target thickness is 17 μm
It is 37~38 μm；When needing to prepare the graphite film that target thickness is 25 μm, the thickness of the corresponding PI film selected generally is up to
49~50 μm；When needing to prepare the graphite film that target thickness is 32 μm, the thickness of the corresponding PI film selected generally is up to 61
~63 μm；When needing to prepare the graphite film that target thickness is 40 μm, the thickness of the corresponding PI film selected generally up to 74~
75μm；By above-mentioned corresponding relationship it is found that in the prior art, when needing to prepare the graphite film of fixed target thickness, PI film
Optional thickness range is very narrow, and about the ratio between thickness of the thickness of PI film and graphite film is (1.88~2.12): 1, make
It obtains more harsh to the thickness requirement of raw material.
And when preparing graphite film using method provided by the invention, carbonization and stone are carried out by using the mode of temperature-gradient method
The technique of inkization, so that the ratio between the thickness of raw material PI film and the target thickness of graphite film product obtained selected is closed
System's broadening has been arrived (1.56~2.35): 1, compared to existing technologies, the optional thickness range of raw material PI film is bigger, especially
When the thickness of raw material PI film increases, be conducive to the sintered density for further increasing graphite film, while can guarantee graphite film
Conductive performance.Under normal circumstances, the graphite film products application that thickness specification is 17 μm, 25 μm, 32 μm, 40 μm and 50 μm is more wide
It is general, for the target thickness of above-mentioned graphite film, selected PI film with a thickness of 33~100 μm.In other realities of the invention
It applies in example, when needing to prepare the graphite film product of other thickness, according to the raw material PI film thickness and stone of above-mentioned offer
Proportionate relationship between ink film product thickness is adjusted the thickness of the raw material PI film of selection.
Further, in specific embodiment provided by the invention, the thickness regulation of graphite film product obtained can lead to
Each of adjustment double fragmentation temperature-rise period temperature rise period and its heating rate are crossed to realize, wherein through this embodiment
When the method for offer carries out the preparation of electrographite film, between the target thickness of graphite film product and the thickness of raw material PI film
Corresponding relationship is as follows: when the target thickness of graphite film product is 17 μm, the thickness range of selected PI film is 38 ± 5 μ
m；When the target thickness of graphite film product is 25 μm, the thickness range of selected PI film is 38 ± 5 μm or 50 ± 5 μm；
When the target thickness of graphite film product is 32 μm, the thickness range of selected PI film is 62.5 ± 5 μm or 50 ± 5 μm；
When the target thickness of graphite film product is 40 μm, the thickness range of selected PI film be 75 ± 5 μm or 62.5 ± 5 μm or
67.5±5μm；When the target thickness of graphite film product be 50 μm when, selected PI film with a thickness of 100 ± 7 μm.
Due to being usually directly to buy from market as the PI film for preparing the electrographite film, usually wind non-
The PI film coil of Chang Mishi, basic gapless before every adjacent two layers film, is unfavorable at the charing and graphitization of PI film
Therefore reason in the present embodiment, more preferably before step S30, also re-starts winding processing to PI film, specific
When implementation the following steps are included:
Step S10, it is wound after being cut Kapton raw material, between making between every adjacent two layers film
Gap is 90~180 μm, obtains fluffy PI film；
Step S20, the fluffy PI film is placed on roasting fixture, and is fixed using high purity graphite, obtain to
The Kapton of roasting.
It takes the PI film of corresponding thickness to be cut according to production requirement first, cuts into required width, cut
At the PI film to be roasted of pre-set dimension, then PI film is wound again, the PI film after control winding is in puffy, and
The gap of every adjacent two layers film is consistent, is 90~180 μm, obtains fluffy PI film, then the fluffy PI film is put
It is put on specific roasting fixture, and is fixed using high purity graphite, obtain PI film to be roasted.Wherein, using high purity graphite
The mode of fixed PI film, which can be, is wound PI film using graphite paper, such as can be high purity graphite paper is direct
It is wrapped in the outermost layer of the fluffy PI film, or is wound together with the PI film, keeps every adjacent two layers PI thin
Graphite paper is wound with before film；It can also be carried out by graphite tube using the mode of the fixed PI film of high purity graphite, directly will
Graphite tube is socketed the outermost layer that the fluffy PI film is arranged in.Pass through the side of the fixed PI film of high purity graphite
Formula can play fixed protective effect to the PI film in roasting process, facilitate obtained electrographite after improvement roasting
Film strength avoids causing cracked equal scarce in roasting process since the PI thin film raw material self performance is bad
It falls into.
The preparation method of electrographite film provided by the invention has at least the following advantages: (1) passing through design double fragmentation
The mode of temperature-rise period forms appropriate dynamic temperature field using first time temperature-gradient method process, and obtaining has high-crystallinity knot
The semi-finished product of structure, further by means of the design of second of temperature-gradient method, make two then on the basis of first time temperature-gradient method
Secondary temperature-gradient method process cooperates, and the graphite film of highly oriented, high-crystallinity, high conductance energy is formed, to make to be prepared
Graphite film thermal coefficient with higher, improve the heating conduction of graphite film, the thermal coefficient of 17 μm of graphite films obtained
Greater than 1700W/ (mK), the thermal coefficient of 25 μm of graphite films is greater than 1500W/ (mK), and the thermal coefficient of 32 μm of graphite films is big
It is greater than 1200W/ (mK) in the thermal coefficient of 1300W/ (mK), 40 μm of graphite films, the thermally conductive system of 50 μm and 60 μm graphite films
Number is greater than 1100W/ (mK)；(2) preparation method is reproducible, it can be achieved that the quantization of different-thickness graphite film produces；(3) work as stone
When the target thickness of ink film product is identical, the optional thickness range of raw material PI film is bigger compared to the prior art, can pass through
The thickness for increasing PI film reaches the effect for further increasing the sintered density of graphite film while guaranteeing the conductive performance of graphite film
Fruit.
The graphite film product prepared using method provided by the invention, thermal coefficient is higher, and heating conduction is excellent, is suitable for
It applies on the radiating element in the fields such as various types of electric terminals and ancillary equipment, electronic component, also can be applied to
In heat conducting film, conductive film, signal shielding film and/or wear-resistant material, there is preferable application effect.And in order to avoid stone obtained
Ink film is mechanically damaged during transport or storage or occurs deforming, will be described more preferably after graphite film is made
Graphite film and a counterdie are compound, and the counterdie plays the role of carrying and the support graphite film, are combined with graphite film as stone
One of the product of ink film material, and in graphite film in use, only needing to take off the counterdie.As a result, the present invention also into
One step proposes a kind of graphite film material, including in the counterdie and electrographite film that are stacked, wherein the electrographite film by
The preparation method of electrographite film provided by the above embodiment is made.
The material of the counterdie is not specifically limited, and mechanical strength is selected to be higher than the membrane material of the graphite film, example
Such as PET (polyethylene terephthalate) film, it is described in a preferred embodiment of graphite film material provided by the invention
The material of counterdie is PC/PET composite membrane (wherein PC is polycarbonate), and it is preferable to be easier to and protecting effect compound with graphite film.Into
One step, in the other embodiments of graphite film material provided by the invention, one layer of epiphragma can also be added again, that is, described
Graphite film material includes in the counterdie, electrographite film and the epiphragma that are stacked, and the electrographite film is set to the bottom
Between film and the epiphragma, contacted in this way, further reducing the electrographite film with the direct of external environment, to reduce
There is the probability of the problems such as mechanical damage or deformation in the electrographite film.At this point, the more preferably described counterdie and the lid
The material of film is PC/PET composite membrane, and in the graphite film in use, only needing to take off the counterdie and the epiphragma
?.Further, after the electrographite film is combined with the PC/PET counterdie and/or PC/PET epiphragma, pressure can be passed through
The mode prolonged is fabricated to coiled material or the form of sheet material is applied.
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, it should be understood that following real
It applies example to be only used to explain the present invention, be not intended to limit the present invention.
Embodiment 1
(1) first time temperature-gradient method: using the PI film with a thickness of 38 ± 5 μm as raw material, be placed in air pressure inside be-
In the retort of 0.08MPa, following temperature-gradient method program is used to carry out first time temperature-gradient method: with the heating rate of 8 DEG C/min
From room temperature to 440 DEG C, 480 DEG C then are continuously heating to the heating rate of 0.5 DEG C/min, then with the liter of 0.5 DEG C/min
Warm rate is continuously heating to 620 DEG C, then is continuously heating to 690 DEG C with the heating rate of 1.5 DEG C/min, then with the liter of 3 DEG C/min
Warm rate is continuously heating to 890 DEG C, is finally continuously heating to 1300 DEG C again with the heating rate of 3 DEG C/min, cold after constant temperature 60min
But, carbonized film is obtained；
(2) second of temperature-gradient method: the carbonized film that step (1) obtains is placed in the graphitizing furnace filled with argon gas,
Use following temperature-gradient method program to carry out second of temperature-gradient method: being warming up to 1150 DEG C with the heating rate of 8 DEG C/min, then with
The heating rate of 5 DEG C/min is continuously heating to 1580 DEG C, is warming up to 1780 DEG C followed by the heating rate with 8 DEG C/min, then with 2
DEG C/heating rate of min is continuously heating to 2000 DEG C, then is continuously heating to 2200 DEG C with the heating rate of 2 DEG C/min, then with 2
DEG C/heating rate of min is continuously heating to 2500 DEG C, 2800 DEG C finally are continuously heating to the heating rate of 2 DEG C/min, constant temperature
It is cooling after 10min, obtain graphite film.
Embodiment 2
(1) first time temperature-gradient method: using the PI film with a thickness of 38 ± 5 μm as raw material, be placed in air pressure inside be-
In the retort of 0.09MPa, following temperature-gradient method program is used to carry out first time temperature-gradient method: with the heating rate of 10 DEG C/min
From room temperature to 450 DEG C, 470 DEG C then are continuously heating to the heating rate of 1.5 DEG C/min, then with the heating of 1 DEG C/min
Rate is continuously heating to 610 DEG C, then is continuously heating to 680 DEG C with the heating rate of 2 DEG C/min, then with the heating of 3.5 DEG C/min
Rate is continuously heating to 900 DEG C, is finally continuously heating to 1100 DEG C with the heating rate of 4 DEG C/min, cools down after constant temperature 80min,
Obtain carbonized film；
(2) second of temperature-gradient method: the carbonized film that step (1) obtains is placed in the graphitizing furnace filled with argon gas,
Use following temperature-gradient method program to carry out second of temperature-gradient method: being warming up to 1200 DEG C with the heating rate of 9 DEG C/min, then with
The heating rate of 5.5 DEG C/min is continuously heating to 1600 DEG C, is warming up to 1800 DEG C followed by the heating rate with 9 DEG C/min, then
2000 DEG C are continuously heating to the heating rate of 2.5 DEG C/min, then is continuously heating to 2200 with the heating rate of 2.5 DEG C/min
DEG C, then 2500 DEG C are continuously heating to the heating rate of 2.5 DEG C/min, finally it is continuously heating to the heating rate of 3 DEG C/min
It is 2700 DEG C, cooling after constant temperature 20min, obtain graphite film.
Embodiment 3
Step is same as Example 2, the difference is that, the PI film used in step (1) with a thickness of 50 ± 5 μm.
Embodiment 4
(1) first time temperature-gradient method: using the PI film with a thickness of 50 ± 5 μm as raw material, be placed in air pressure inside be-
In the retort of 0.1MPa, following temperature-gradient method program is used to be carbonized: with the heating rate of 12 DEG C/min from room temperature
To 465 DEG C, 490 DEG C then are continuously heating to the heating rate of 3.5 DEG C/min, then continue with the heating rate of 1.5 DEG C/min
600 DEG C are warming up to, then is continuously heating to 700 DEG C with the heating rate of 2.5 DEG C/min, then continue with the heating rate of 3 DEG C/min
920 DEG C are warming up to, is finally continuously heating to 1400 DEG C with the heating rate of 5 DEG C/min, cooling after constant temperature 90min is carbonized
Film；
(2) second of temperature-gradient method: the carbonized film that step (1) obtains is placed in the graphitizing furnace filled with argon gas,
It uses following temperature-gradient method program to be graphitized: 1100 DEG C is warming up to the heating rate of 10 DEG C/min, then with 6 DEG C/min
Heating rate be continuously heating to 1620 DEG C, be warming up to 1820 DEG C followed by the heating rate with 10 DEG C/min, then with 3.5 DEG C/
The heating rate of min is continuously heating to 2000 DEG C, then is continuously heating to 2200 DEG C with the heating rate of 3.5 DEG C/min, then with 3.5
DEG C/heating rate of min is continuously heating to 2510 DEG C, 2600 DEG C finally are continuously heating to the heating rate of 4 DEG C/min, constant temperature
It is cooling after 30min, obtain graphite film.
Embodiment 5
Step is same as Example 2, the difference is that, the PI film used in step (1) with a thickness of 62.5 ± 5 μ
m。
Embodiment 6
(1) first time temperature-gradient method: using the PI film with a thickness of 62.5 ± 5 μm as raw material, be placed in air pressure inside be-
In the retort of 0.1MPa, following temperature-gradient method program is used to be carbonized: with the heating rate of 9 DEG C/min from room temperature to
430 DEG C, 485 DEG C then are continuously heating to the heating rate of 3 DEG C/min, then continue to heat up with the heating rate of 2.5 DEG C/min
720 DEG C are continuously heating to 630 DEG C, then with the heating rate of 3 DEG C/min, then continues to heat up with the heating rate of 6.5 DEG C/min
To 920 DEG C, 1500 DEG C finally are continuously heating to the heating rate of 4 DEG C/min, cooling after constant temperature 70min obtains carbonized film；
(2) second of temperature-gradient method: the carbonized film that step (1) obtains is placed in the graphitizing furnace filled with argon gas,
It uses following temperature-gradient method program to be graphitized: 1000 DEG C is warming up to the heating rate of 10 DEG C/min, then with 6 DEG C/min
Heating rate be continuously heating to 1600 DEG C, be warming up to 1800 DEG C followed by the heating rate with 8 DEG C/min, then with 1.5 DEG C/
The heating rate of min is continuously heating to 2000 DEG C, then is continuously heating to 2200 DEG C with the heating rate of 1.5 DEG C/min, then with 1.5
DEG C/heating rate of min is continuously heating to 2520 DEG C, 2850 DEG C finally are continuously heating to the heating rate of 4 DEG C/min, constant temperature
It is cooling after 40min, obtain graphite film.
Embodiment 7
Step is same as Example 2, the difference is that, the PI film used in step (1) with a thickness of 67.5 ± 5 μ
m。
Embodiment 8
Step is same as Example 2, the difference is that, the PI film used in step (1) with a thickness of 75 ± 5 μm.
Embodiment 9
Step is same as Example 2, the difference is that, the PI film used in step (1) with a thickness of 80 ± 7 μm.
Embodiment 10
Step is same as Example 2, the difference is that, the PI film used in step (1) with a thickness of 100 ± 7 μm.
Graphitization thickness and graphite thickness prepared in the above embodiments are tested below, and thousand points are used after graphitization is come out of the stove
Ruler, tenthousandth micrometer or the measurement of hand-held finger gauge；The thermal coefficient of graphite film: thermal coefficient=close is calculated according to the following equation
Spend the * thermal diffusion of * specific heat, wherein density is measured using volumetric method or real density instrument, and specific heat is measured using differential scanning calorimeter,
Thermal diffusion is measured using TA33 (thermal analyzer), and test result is as follows shown in table 1 for thickness test and thermal coefficient.
The performance test results of the graphite film of each embodiment of table 1 preparation
By the test result in table 1 it is found that preparing graphite film, raw material PI film using method provided in an embodiment of the present invention
Proportionate relationship broadening between the target thickness of graphite film product has been arrived (1.56~2.35): 1, it can be by increasing PI film
Thickness improve the sintered density of graphite film, and can guarantee the good conductive performance of graphite film, and 17 μm of graphite films obtained
Thermal coefficient is greater than 1700W/ (mK), and the thermal coefficients of 25 μm of graphite films is greater than 1500W/ (mK), and 32 μm of graphite films are led
Hot coefficient is greater than 1200W/ (mK), and the thermal coefficient of 40 μm of graphite films is greater than 1300W/ (mK), 50 μm and 60 μm of graphite films
Thermal coefficient can also reach the level greater than 1100W/ (mK), thermal coefficient is higher than the thermally conductive of graphite film in the prior art
Rate highest only has 1056W/ (mK), and the thermal coefficient of the graphite film of preparation of the embodiment of the present invention is higher, significantly improves graphite
The heating conduction of film.
The above is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc. should all be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of electrographite film, which comprises the following steps:
Step S30, Kapton to be roasted is subjected to first time temperature-gradient method according to pre-set dimension, keeps polyimides thin
Film reacts, and then cooling obtains semi-finished product film；
Step S40, the semi-finished product film is subjected to second of temperature-gradient method under inert gas protection, sends out the semi-finished product film
Raw reaction, then cooling obtains graphite film.
2. the preparation method of electrographite film as described in claim 1, which is characterized in that the first time in step S30
Temperature-gradient method includes:
Temperature T2 is warming up to by room temperature, then temperature T3 is continuously heating to by temperature T2, temperature is then continuously heating to by temperature T3
T6, and 60~90min is kept the temperature after being warming up to temperature T6, wherein T2 is 470~490 DEG C, and T3 is 600~630 DEG C, and T6 is
1100~1550 DEG C.
3. the preparation method of electrographite film as claimed in claim 2, which is characterized in that be warming up to the step of temperature T2 by room temperature
Suddenly include: that temperature T1 is warming up to by room temperature, temperature T2 is then continuously heating to by temperature T1, wherein T1 is 430~465 DEG C；
And/or
The step of being warming up to temperature T6 by temperature T3 includes: to be warming up to temperature T4 by temperature T3, then continues to heat up by temperature T4
Temperature T6 is continuously heating to temperature T5, then by temperature T5, wherein T4 is 680~720 DEG C, and T5 is 880~920 DEG C.
4. the preparation method of electrographite film as claimed in claim 3, which is characterized in that in step s 30 described first
During secondary temperature-gradient method:
It is 8~12 DEG C/min by the heating rate that room temperature is warming up to T1；And/or
It is 0.5~3.5 DEG C/min by the heating rate that T1 is warming up to T2；And/or
It is 0.3~2.5 DEG C/min by the heating rate that T2 is warming up to T3；And/or
It is 1.5~3 DEG C/min by the heating rate that T3 is warming up to T4；And/or
It is 3~4 DEG C/min by the heating rate that T4 is warming up to T5；And/or
It is 3~6.5 DEG C/min by the heating rate that T5 is warming up to T6；And/or
20~30min is kept the temperature after being warming up to temperature T2.
5. the preparation method of electrographite film as described in claim 1, which is characterized in that described second in step S40
Temperature-gradient method includes:
Temperature T7 is warming up to by room temperature, temperature T8 is continuously heating to by temperature T7, temperature T9 is continuously heating to by temperature T8, by temperature
Degree T9 is continuously heating to temperature T11, is continuously heating to temperature T12 by temperature T11, and be continuously heating to temperature by temperature T12
T13, and 10~40min is kept the temperature after being warming up to temperature T13, wherein T7 is 1000~1200 DEG C, and T8 is 1580~1620
DEG C, T9 is 1780~1820 DEG C, and T11 is 2300 DEG C, and T12 is 2500~2520 DEG C, and T13 is 2600~2850 DEG C.
6. the preparation method of electrographite film as described in claim 1, which is characterized in that described second in step S40
Temperature-gradient method includes:
Temperature T7 is warming up to by room temperature, temperature T8 is continuously heating to by temperature T7, temperature T9 is continuously heating to by temperature T8, by temperature
Degree T9 is continuously heating to temperature T10, is continuously heating to temperature T11 by temperature T10, is continuously heating to temperature T12 by temperature T11,
And temperature T13 is continuously heating to by temperature T12, and 10~40min is kept the temperature after being warming up to temperature T13, wherein T7 is
1000~1200 DEG C, T8 is 1580~1620 DEG C, and T9 is 1780~1820 DEG C, and T10 is 2000 DEG C, and T11 is 2200 DEG C, and T12 is
2500~2520 DEG C, T13 is 2600~2850 DEG C.
7. the preparation method of electrographite film as claimed in claim 6, which is characterized in that described second in step S40
During temperature-gradient method:
Temperature T10 is being warming up to by temperature T9, temperature T11 is warming up to by temperature T10 and temperature T12 is warming up to by temperature T11
Three heating steps in, wherein at least two heating step further include it is corresponding be warming up to set temperature after kept the temperature, and
Soaking time is 10~30min；And/or
It is 8~10 DEG C/min by the heating rate that room temperature is warming up to T7；And/or
It is 5~6 DEG C/min by the heating rate that T7 is warming up to T8；And/or
It is 8~10 DEG C/min by the heating rate that T8 is warming up to T9；And/or
It is 1.5~3.5 DEG C/min by the heating rate that T9 is warming up to T10；And/or
It is 1.5~3.5 DEG C/min by the heating rate that T10 is warming up to T11；And/or
It is 1.5~3.5 DEG C/min by the heating rate that T11 is warming up to T12；And/or
It is 2~4 DEG C/min by the heating rate that T12 is warming up to T13.
8. the preparation method of electrographite film as described in claim 1, which is characterized in that before step S30, further includes:
Step S10, it is wound after being cut Kapton raw material, makes gap between every adjacent two layers film
90~180 μm, obtain fluffy Kapton；
Step S20, the fluffy Kapton is placed on roasting fixture, and is fixed using high purity graphite, obtained
Kapton to be roasted.
9. the preparation method of electrographite film as described in claim 1, which is characterized in that the first time in step S10
Ambient pressure during temperature-gradient method is -0.08~-0.1MPa；And/or
The Kapton in step S10 with a thickness of 33~100 μm；And/or
The inert gas in step S20 is argon gas.
10. a kind of graphite film material, which is characterized in that the graphite film material includes in the counterdie and electrographite being stacked
Film, wherein the electrographite film is made by the preparation method of electrographite film as claimed in any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110451500A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | Graphite film carbonization technique |
| CN112897522A (en) * | 2021-03-26 | 2021-06-04 | 浙江华熔科技有限公司 | Ultrathin heat-conducting graphite film and preparation method thereof |
| WO2022198661A1 (en) * | 2021-03-26 | 2022-09-29 | 浙江华熔科技有限公司 | Ultrathin thermally-conductive graphite film and manufacturing method therefor |
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| CN110451500A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | Graphite film carbonization technique |
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| WO2022198661A1 (en) * | 2021-03-26 | 2022-09-29 | 浙江华熔科技有限公司 | Ultrathin thermally-conductive graphite film and manufacturing method therefor |
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