CN109574668A - The manufacturing method of carbonized film - Google Patents
The manufacturing method of carbonized film Download PDFInfo
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- CN109574668A CN109574668A CN201710896134.XA CN201710896134A CN109574668A CN 109574668 A CN109574668 A CN 109574668A CN 201710896134 A CN201710896134 A CN 201710896134A CN 109574668 A CN109574668 A CN 109574668A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The present invention is a kind of manufacturing method of carbonized film, it refers in particular to carry out carbonization heat treatment by predecessor of Kapton, heat treatment condition are as follows: in 500~800 DEG C of calefactive interzones average heating rate be 2 DEG C per minute or less, highest carburizing temperature is 1000 DEG C or higher temperature, to form carbonized film.Carbonized film is subjected to graphitization heat treatment again, heat treatment condition is 2200 DEG C and is less than 3 DEG C per minute, 2500 DEG C to the average heating rate of highest graphitization temperature or higher temperature is the highest graphitization temperature of technique, to form graphite film.
Description
Technical field
The present invention relates to a kind of manufacturing methods of carbonized film, especially using polyimide film as predecessor be heat-treated with
It forms carbonized film and obtains the carbonized film of better quality by being controlled in the heating rate of specific temperature section.
Background technique
The Fast Growth of running gear makes the lightening trend as electronic product, and electronic building brick is in order to reduce volume
And component is allowed to do close accumulation, therefore the heat dissipation problem of chip, backlight module and battery etc. becomes important subject under discussion.It is leading
When heat, heat dissipation require gradually severe, artificial soft graphite film asks that city allows these problems to be able to know about certainly scheme, artificial
There is graphite film good conductibility, flexibility and heat conduction efficiency of four times better than copper to make graphite film big on running gear
Amount ground uses.
High thermal conductivity graphite film is in manufacture by high aromatic structure macromolecule membrane by a string of Pintsch process reaction and original
Son rearranges process and forms, these high-temperature process, which are referred to as, to be carbonized and be graphitized.The major function of carbonization technique is heat
Non-carbon element is cracked, treatment temperature is about between 500-1300 DEG C.Graphited function is then to push carbon atom by high temperature,
It rearranges carbon atom and forms continuous orderly layer structure, in the process can be along with foaming the phenomenon that, and form hair
Afrodite layer of ink structure, operation temperature occur between 2000-3000 DEG C.After roll to obtained foaming stone ink film and prolonging processing
It can get the graphite film with flexibility, with the heat dissipation being suitable in electronic equipment and electromagnetic shielding layer.
No matter the carbonized film shop of multi-disc (folded to burn) or web-like continous way (volume is burnt) technique production has between film surface and film surface
It is easy to produce welding and is stained with glutinous problem.This phenomenon makes be carbonized film surface generation defect or damaged probability decline.
Summary of the invention
The manufacturing method of carbonized film of the invention, the polyimides predecessor of carbonized film is in 500~800 DEG C of heating zones
Between average heating rate be 2 DEG C per minute hereinafter, highest carburizing temperature is 1000 DEG C or higher temperature.
The carbonized film made according to the present invention can reduce the even characteristic without adhesion, welding between film and film, and obtain
The carbonized film of better quality.
The manufacturing method of graphite film of the invention, carbonized film is heat-treated, in 2200 DEG C to highest graphitization temperature
Average heating digit rate be less than 3 DEG C per minute hereinafter, highest carburizing temperature be 2500 DEG C or higher temperature.
Detailed description of the invention
Fig. 1 has for carbonized film is stained with glutinous situation.
Fig. 2 is good carbonized film.
Fig. 3 has for graphite film is stained with glutinous situation.
Fig. 4 is the ripply situation of graphite film.
Fig. 5 is good graphite film.
[symbol description]
It is stained with glutinous 10
Carbonized film 12
It is stained with glutinous 14
Ripple 16
Graphite film 18
Specific embodiment
Graphite film made by the present invention is made using macromolecule thermal decomposition method, and manufacturing process includes carbonization and graphite
Change.
Carbonized film: by polyimides in the environment of decompression or inert gas, in addition, being passed through indifferent gas while decompression
Body is heat-treated to obtain.The heat treatment maximum temperature of carburising step is minimum to be also necessary for 1000 DEG C or more, preferably 1100 DEG C
More than, more preferably 1200 DEG C or more.
Graphite film: above-mentioned carbonized film is carried out in decompression or inert gas.The heat treatment maximum temperature of graphitization step
It is 2400 DEG C or more, preferably 2600 DEG C or more, more preferably 2800 DEG C or more.2800 DEG C or more then can get thermal diffusivity it is higher
Graphite film.
The film of carbonization and graphitization technique of the invention is put mode and is not particularly limited, for example, polyimide film is cut
For sheet, it is heat-treated with monolithic or multi-disc phase poststack for one layer, then after being separated each layer of polyimides with Graphite pad；Again
For example, the web-like film by polyimides with length greater than 5 meters is heat-treated.
The heating device and mode used needed for the present invention is not particularly limited, such as is heated with resistance-type or coil induction type
The high temperature furnace of device.In another example Acheson's method (Acheson method).
Welding between carbonization film surface be stained with it is glutinous be due to carbonization when polyimide film Pintsch process lysate out be also known as
Tar can not be successfully between discharge film and film.In addition, when remaining tar be then stained with after the process of heat treatment is carbonized it is glutinous
Phenomenon, as shown in the 10 of Fig. 1.
The ripple or crinkle mark of graphite film surface are due in carbonisation, and polyimide film is cracked while being shunk, when
Film has uneven heating to shrink uneven situation, then generates ripple.In graphitization technique, carbon occurs in 2000 DEG C to the highest temperature
Change film graphitization, when carbon structure is by SP3It is changed into SP2While occur film surface direction expansion, occur when film has uneven heating swollen
The situation of swollen unevenness, or without sufficient Bulking Time, then crinkle mark or ripple can be generated by generating film surface such as the 16 of Fig. 4, or is generated and is stained with
It is glutinous, as shown in the 14 of Fig. 3.
Carbonization film manufacturing method of the invention, the polyimides predecessor of carbonized film is in 500~800 DEG C of calefactive interzones
Average heating rate is 2 DEG C per minute hereinafter, highest carburizing temperature is 1000 DEG C or higher temperature, and preferable carbonized film can be obtained
12, as shown in Figure 2.
It is stained with glutinous criterion: A: glutinous without being stained with；It is stained at B:1~3 glutinous；DEG C: greater than 3 at be stained with it is glutinous
The criterion of film surface ripple: A: non-ripple；B: ripple area is less than 10%；C: ripple area is greater than 10%
Embodiment 1
Prepare flake graphite film.
<embodiment 1>
Sheet carbonization film preparation
Use up to the polyimides (model: TH5) for stepping science and technology production as predecessor, is sliced and is respectively for length and width
323mm and 323mm is separated using 0.25mm graphite feeding spaced papers between layers with every 5 polyimide films for one layer.Subtracting
Pressure ring heats up under border, and heating rate is divided into lower curtate: room temperature to 500 DEG C be 5 DEG C per minute, 500 to 800 DEG C are per minute
2 DEG C, 800 to the carbonization section highest temperature be 2 DEG C per minute.
Flake graphite film preparation
Above-mentioned carbonized film with normal pressure and is passed through under argon gas heating and is graphitized, heating rate are as follows: room temperature is to 2000 DEG C
Be 10 DEG C per minute, 2000 to 2200 DEG C are 5 DEG C per minute, 2200 DEG C the above are 3 DEG C per minute, the graphitization highest temperature is 2850
DEG C and constant temperature 1 hour.
Embodiment 2
The step of repeating embodiment 1, only, 500 to 800 DEG C of heating rate of carbonization are 1 DEG C per minute.
Embodiment 3
The step of repeating embodiment 1, only, 500 to 800 DEG C of heating rate of carbonization are 0.5 DEG C per minute.
Embodiment 4
The step of repeating embodiment 1, only, 500 to 800 DEG C of heating rate of carbonization are 0.25 DEG C per minute.
Embodiment 5
The step of repeating embodiment 3, only, the above are 2 DEG C per minute for 2200 DEG C of heating rate of graphitization.
Embodiment 6
The step of repeating embodiment 3, only, the above are 1 DEG C per minute for 2200 DEG C of heating rate of graphitization.
Embodiment 7
The step of repeating embodiment 6, only, 500 to 800 DEG C of heating rate of carbonization are 0.25 DEG C per minute.
Embodiment 8
The step of repeating embodiment 7, only, the carbonization highest temperature are 1200 DEG C.
Embodiment 9
The step of repeating embodiment 7, only, the carbonization highest temperature are 1000 DEG C.
Embodiment 10
The step of repeating embodiment 6, only, the carbonization highest temperature are 1200 DEG C.
Embodiment 11
Using the polyimide film with a thickness of 38 microns, the step of repeating embodiment 10.
Embodiment 12
Using the polyimide film with a thickness of 62 microns, the step of repeating embodiment 10, only, the graphitization highest temperature is
2750℃。
Embodiment 13
Using the polyimide film with a thickness of 75 microns, the step of repeating embodiment 10, only, the graphitization highest temperature is
2700℃。
Comparative example 1
The step of repeating embodiment 1, only, 500 to 800 DEG C of heating rate of carbonization are 3 DEG C per minute.
Comparative example 2
The step of repeating embodiment 3, only, 2200 or more DEG C of heating rate of graphitization are 4 DEG C per minute.
Comparative example 3
The step of repeating embodiment 7, only, the carbonization highest temperature are 900 DEG C.
Embodiment 14
Prepare web-like graphite film
<embodiment 14>
Web-like carbonization film preparation
The polyimides (model: TH5) up to science and technology production advanced in years is used as predecessor, by breadth 257mm length 100M's
It is 76.2mm tube core that graphite film, which is wound in an internal diameter,.Heat up under reduced pressure atmosphere, heating rate is divided into lower curtate: room temperature is extremely
500 DEG C are 5 DEG C per minute, and 500 to 800 DEG C are 0.5 DEG C per minute, and 800 to the carbonization highest temperature be 2 DEG C per minute.
Web-like graphite film preparation
Above-mentioned carbonized film with normal pressure and is passed through under argon gas heating and is graphitized, heating rate are as follows: room temperature is to 2000 DEG C
Be 10 DEG C per minute, 2000 to 2200 DEG C are 5 DEG C per minute, 2200 DEG C the above are 1 DEG C per minute, the graphitization highest temperature is 2850
DEG C and constant temperature 1 hour.
Embodiment 15
The step of repeating embodiment 14, only, 500 to 800 DEG C of heating rate of carbonization are 1 DEG C per minute.
Embodiment 16
The step of repeating embodiment 14, only, 500 to 800 DEG C of heating rate of carbonization are 2 DEG C per minute.
Embodiment 17
The step of repeating embodiment 15, only, the above are 2 DEG C per minute for 2200 DEG C of heating rate of graphitization.
Comparative example 4
The step of repeating embodiment 14, only, 500 to 800 DEG C of heating rate of carbonization are 3 DEG C per minute.
Comparative example 5
The step of repeating embodiment 15, only, the above are 3 DEG C per minute for 2200 DEG C of heating rate of graphitization.
It is stained with glutinous criterion: A: glutinous without being stained with；It is stained at B:1~3 glutinous；It is stained at C: greater than 3 glutinous
The criterion of ripple: A: non-ripple；B: ripple area is less than 10%；C: ripple area is greater than 10%
1~embodiment of embodiment 4 and comparative example 1 are compared, will carbonization 500 DEG C~800 DEG C heating rates by 3 DEG C/
Min drops to 0.25 DEG C/min, and A can be promoted to by C by being stained with stickiness, is that sufficient cracking and enough is obtained due to polyimide film
Time, tar was discharged.
5~embodiment of embodiment 6 and comparative example 2 are compared, 2200 DEG C will be graphitized to the liter for being graphitized the highest temperature
Warm rate drops to 1 DEG C/min by 4 DEG C/min, and graphite film ripple is promoted to A by C, is to carry out stone due to obtaining sufficient thermal energy
Mo Hua.
7~embodiment of embodiment 9 and comparative example 3 are compared, it, can sufficiently will be high with the promotion of carbonization maximum temperature
Warm lysate cracks completely, obtains high-quality carbonized film, as shown in the 12 of Fig. 2, and obtains the diffusible stone of high fever after graphitization
Ink film, such as the 18 of Fig. 5.
10~embodiment of embodiment 13 is that different-thickness polyimide film is graphitized, and obtains good appearance and high fever
The graphite film of diffusion property.
14~embodiment of embodiment 16 and comparative example 4 are compared, by 500 DEG C~800 DEG C heating rates of carbonization by 3
DEG C/min drops to 0.5 DEG C/min, A can be promoted to by C by being stained with stickiness, be obtained due to web-like polyimide film sufficient cracking and
Tar is discharged time enough.
Embodiment 15, embodiment 17 and comparative example 5 are compared, by 2200 DEG C of graphite or more heating rates by 3 DEG C/
Min drops to 1 DEG C/min, and 2 DEG C/min can be obtained good film surface state, 1 DEG C/min due to there is more sufficient heating,
There are preferable heat diffusion properties.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
It describes in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (5)
1. a kind of manufacturing method of carbonized film comprising there is the following steps:
There is provided a polyimide film is predecessor；And
Carbonization heat treatment is carried out to the polyimide film, in the average heating rate of carbonization 500~800 DEG C of calefactive interzones of heat treatment
For 2 DEG C per minute hereinafter, highest carburizing temperature is 1000 DEG C or more.
2. the manufacturing method of carbonized film as described in claim 1 is heat-treated being averaged for 500~800 DEG C of calefactive interzones in carbonization
Heating rate is 1 DEG C per minute or less.
3. the manufacturing method of carbonized film as described in claim 1 is heat-treated being averaged for 500~800 DEG C of calefactive interzones in carbonization
Heating rate is 0.5 DEG C per minute.
4. the manufacturing method of carbonized film as described in claim 1, wherein the polyimide film is stacked or web-like.
5. the manufacturing method of carbonized film as described in claim 1, wherein the highest carburizing temperature is 1300 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451965A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | The production technology of the artificial synthesized graphite film of super thick |
| CN114853001A (en) * | 2021-11-22 | 2022-08-05 | 广东一纳科技有限公司 | Preparation method of heat dissipation film |
| CN115520862A (en) * | 2022-10-10 | 2022-12-27 | 中汇睿能凤阳新材料科技有限公司 | Preparation method of artificial high-thermal-conductivity ultrathin graphite film |
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| JP2008024571A (en) * | 2006-07-25 | 2008-02-07 | Kaneka Corp | Graphite film and method for manufacturing graphite film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110451965A (en) * | 2019-09-10 | 2019-11-15 | 北京中石伟业科技无锡有限公司 | The production technology of the artificial synthesized graphite film of super thick |
| CN114853001A (en) * | 2021-11-22 | 2022-08-05 | 广东一纳科技有限公司 | Preparation method of heat dissipation film |
| CN115520862A (en) * | 2022-10-10 | 2022-12-27 | 中汇睿能凤阳新材料科技有限公司 | Preparation method of artificial high-thermal-conductivity ultrathin graphite film |
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