KR101809641B1 - Method for preparing roll type graphite sheet - Google Patents
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- KR101809641B1 KR101809641B1 KR1020150184035A KR20150184035A KR101809641B1 KR 101809641 B1 KR101809641 B1 KR 101809641B1 KR 1020150184035 A KR1020150184035 A KR 1020150184035A KR 20150184035 A KR20150184035 A KR 20150184035A KR 101809641 B1 KR101809641 B1 KR 101809641B1
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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
- C01B32/21—After-treatment
- C01B32/23—Oxidation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H37/00—Article or web delivery apparatus incorporating devices for performing specified auxiliary operations
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
- H05K7/20436—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing
- H05K7/20445—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing the coupling element being an additional piece, e.g. thermal standoff
- H05K7/20472—Sheet interfaces
- H05K7/20481—Sheet interfaces characterised by the material composition exhibiting specific thermal properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H2301/00—Handling processes for sheets or webs
- B65H2301/50—Auxiliary process performed during handling process
- B65H2301/51—Modifying a characteristic of handled material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H2301/00—Handling processes for sheets or webs
- B65H2301/50—Auxiliary process performed during handling process
- B65H2301/51—Modifying a characteristic of handled material
- B65H2301/516—Securing handled material to another material
- B65H2301/5162—Coating, applying liquid or layer of any material to material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H2701/00—Handled material; Storage means
- B65H2701/10—Handled articles or webs
- B65H2701/17—Nature of material
- B65H2701/171—Physical features of handled article or web
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H2701/00—Handled material; Storage means
- B65H2701/10—Handled articles or webs
- B65H2701/17—Nature of material
- B65H2701/174—Textile, fibre
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65H—HANDLING THIN OR FILAMENTARY MATERIAL, e.g. SHEETS, WEBS, CABLES
- B65H2701/00—Handled material; Storage means
- B65H2701/10—Handled articles or webs
- B65H2701/17—Nature of material
- B65H2701/177—Fibrous or compressible material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
- C01P2006/37—Stability against thermal decomposition
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- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Carbon And Carbon Compounds (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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Abstract
The present invention provides a process for producing a graphite sheet in the form of a roll, in which a curing step is carried out in a heat treatment apparatus and a coating and curing step is a continuous process. The present invention also relates to a process for producing a graphite sheet in the form of a roll, wherein the curing step, the carbonization step and the graphitization step are continuously performed in a heat treatment apparatus, and the coating step, the curing step, A process for producing a roll-shaped graphite sheet comprising a continuous process.
The method of producing a roll-shaped graphite sheet according to the present invention is a method in which a curing, carbonization and / or graphitization process is continuously performed in one heat treatment apparatus, thereby not only improving productivity but also suppressing surface irregularities, A graphite sheet can be obtained. By producing the graphite sheet in the form of a roll, it is excellent in storage and transportability, and it is economical because loss can be reduced during punching. By using fibers such as cotton fibers or rayon as the base component, it is possible to produce a graphite sheet which is excellent in thermal conductivity in the horizontal and vertical directions, can be produced at a low manufacturing cost, is economically advantageous, have.
Description
The present invention relates to a process for producing a graphite sheet in the form of a roll using fibers as a base component and more particularly to a process for producing a graphite sheet comprising a curing step, a carbonization step and / or a graphitization step, Which is carried out continuously.
In recent years, electronic devices have become highly integrated with thin, thin and multifunctional devices, and heat dissipation has been demanded. It is also important that the release of heat is closely related to the reliability and lifetime of the device. Accordingly, a variety of heat dissipation materials have been developed and marketed in the form of a heat dissipation pad, a heat dissipation sheet, and a heat dissipation paint, thereby supplementing or replacing existing heat dissipation fans, heat dissipation fins, and heat pipes.
Among them, the heat-radiating sheet is manufactured in the form of a graphite sheet, a polymer-ceramic composite sheet, a multilayered coating metal thin film sheet, etc. In the case of a graphite sheet, lightweight, slim and thermal conductivity is extremely high, And a PDP constituting a plasma television or the like.
However, the graphite sheet is generally produced by pyrolysis of a polymer film. Since the graphite sheet is similar to a single crystal, its breaking strength and tensile strength are low, and the heat transfer is made in the horizontal direction by the principle of thermal diffusion, There is a problem that the heat radiation effect is not sufficiently obtained because the thermal conductivity in the vertical direction (thickness direction) is low. In addition, shrinkage and expansion occur in the heat treatment process. When a gap or space is generated between raw film layers at the time of shrinkage and unevenness is generated on the surface through such a gap or space at the time of expansion, surface roughness becomes poor and physical properties of the graphite sheet There was a problem of deterioration.
Thus, the inventors of the present invention have succeeded in obtaining a graphite sheet which not only has improved productivity but also has surface unevenness suppressed and is excellent in flatness, by continuously performing the hardening step, the carbonization step and / or the graphitization step in one heat treatment apparatus, It has been found that, by making the graphite sheet in the form of a roll, it is excellent in storability and transportability, and it is economical because loss can be reduced during punching. Further, it has been found that by using cotton fibers or fibers such as rayon as the base component, it is possible to produce a product having a high thermal conductivity in the horizontal and vertical directions at a low manufacturing cost, thereby being economically advantageous and also excellent in flexibility.
Accordingly, an object of the present invention is to provide a process for producing a graphite sheet in the form of a roll, which not only improves productivity, but also has excellent storability and transportability, suppresses surface irregularities and has excellent flatness and excellent thermal conductivity in horizontal and vertical directions, And to provide a graphite sheet produced therefrom.
In order to accomplish the above object, the present invention provides a method for producing a sheet, comprising the steps of: (1) coating a cross-section or both sides of a fiber substrate with a polymer resin to produce a sheet; (2) a curing step of curing the polymer resin coated on the fiber substrate to produce a cured sheet; (3) carbonizing the cured sheet to produce a carbonized sheet; And (4) a graphitizing step of graphitizing, the curing step being carried out in a heat treatment apparatus, and the coating and curing step being a continuous process.
(1) a coating step of coating a cross-section or both sides of the fiber substrate with a polymer resin to produce a sheet; (2) a curing step of curing the polymer resin coated on the fiber substrate to produce a cured sheet; (3) carbonizing the cured sheet to produce a carbonized sheet; And (4) a graphitizing step, wherein the curing step, the carbonization step and the graphitization step are continuously performed in a heat treatment apparatus, and the coating step, the curing step, the carbonization step and the graphitization step are continuously performed The present invention provides a method for producing a graphite sheet in the form of a roll.
The method of producing a graphite sheet in the form of a roll according to the present invention is advantageous in that not only the productivity is improved but also the surface irregularity is suppressed and the flatness is improved by continuously performing the hardening step, the carbonization step and / or the graphitization step in one heat treatment apparatus An excellent graphite sheet can be obtained. By making the graphite sheet in the form of a roll, it is excellent in storability and transportability, and it is economical because loss can be reduced in punching. By using fibers such as cotton fibers or rayon as the base component, it is possible to produce a graphite sheet which is excellent in thermal conductivity in the horizontal and vertical directions, can be produced at a low manufacturing cost, is economically advantageous, have.
Figs. 1 and 2 schematically show a method of producing a roll-shaped graphite sheet according to an embodiment of the present invention.
3 schematically shows a state in which the winding core is rotated in a direction opposite to the winding direction after the cured sheet is wound, according to an embodiment of the present invention.
Figs. 4 and 5 schematically show a state in which a wound film is charged into a crucible and carbonized and graphitized, according to an embodiment of the present invention.
Fig. 6 schematically shows the appearance of a cured sheet wound with a cured sheet and a graphite powder wound together with a masking film or a separator in an embodiment of the present invention. Fig.
7 schematically shows a state in which an induction heating coil is disposed outside a crucible in which a wound cured sheet is loaded, according to an embodiment of the present invention.
Fig. 8 shows the temperature distribution in the crucible depending on the presence or absence of the center column when the crucible is inductively heated, according to an embodiment of the present invention.
(1) a coating step of coating a cross-section or both sides of a fiber substrate with a polymer resin to produce a sheet; (2) a curing step of curing the polymer resin coated on the fiber substrate to produce a cured sheet; (3) carbonizing the cured sheet to produce a carbonized sheet; And (4) a graphitizing step of graphitizing, the curing step being carried out in a heat treatment apparatus, and the coating and curing step being a continuous process.
(1) a coating step of coating a cross-section or both sides of the fiber substrate with a polymer resin to produce a sheet; (2) a curing step of curing the polymer resin coated on the fiber substrate to produce a cured sheet; (3) carbonizing the cured sheet to produce a carbonized sheet; And (4) a graphitizing step, wherein the curing step, the carbonization step and the graphitization step are continuously performed in a heat treatment apparatus, and the coating step, the curing step, the carbonization step and the graphitization step are continuously performed The present invention provides a method for producing a graphite sheet in the form of a roll.
Fiber substrate
In the method of producing a graphite sheet in the form of a roll according to the present invention, the fiber substrate may comprise natural fibers, artificial fibers or paper.
The fibrous base material may be made of natural fibers, and natural fibers constituting the fibrous base material may be roughly divided into cellulose fibers, protein fibers and mineral fibers. The cellulosic fibers may be selected from the group consisting of (i) seed fibers such as cotton or kapok, (ii) stem fibers such as flax, hemp, hemp or jute, (iii) fruit fibers such as coconut fibers, and (iv) Or leaf fibers such as sisal. In addition, the protein fibers include (i) wool fibers, (ii) silk fibers, and (iii) hair fibers. When the base material constituting the graphite sheet according to the present invention is made of natural fibers, it is preferable that the natural fibers are at least one natural fiber selected from the group consisting of cotton, hemp, wool and silk.
The fibrous base material may be formed of a synthetic fiber, and the synthetic fibers constituting the fibrous base material may be roughly divided into an organic fiber and an inorganic fiber. The organic fibers may be selected from the group consisting of (i) regenerated fibers including cellulose-based fibers and protein-based fibers such as rayon, tencel (lyocell), or modal, (ii) semisynthetic fibers including cellulosic fibers such as acetate or triacetate, (iii) a synthetic fiber such as a polyamide fiber, a polyester fiber, a polyurethane fiber, a polyethylene fiber, a polyvinyl chloride fiber, a polyfluoroethylene fiber, a polyvinyl alcohol fiber, an acrylic fiber or a polypropylene fiber . In the case where the fiber substrate constituting the graphite sheet according to the present invention is made of a synthetic fiber, the synthetic fiber is preferably composed of nylon, polyester, polyurethane, polyethylene, polyvinyl chloride, polyfluoroethylene, polyvinyl alcohol, acrylic and polypropylene And at least one synthetic fiber selected from the group consisting of When the base material constituting the graphite sheet according to the present invention is made of artificial fiber, it is preferable that the artificial fiber is at least one kind of cellulose fiber selected from the group consisting of rayon, acetate and triacetate.
The fibrous substrate may be paper.
Polymer resin
In the graphite sheet according to the present invention, the polymer is not particularly limited, but may be polyamic acid, polyimide, polyamide, polyvinyl chloride, polyester, polyurethane, polyethylene, polypropylene, polyfluoroethylene, polyvinyl alcohol, Acrylic, polyoxadiazole, polybenzoxazole, polyacrylonitrile, and the like, preferably polyamic acid, polyimide, polyamide or polyvinyl chloride.
In addition, the polymer resin may include a carbonized polymer. The carbonized polymer is prepared by heat-treating the polymer resin in an atmosphere of an inert gas such as nitrogen or argon, and contains carbon in an amount of 90 wt% or more.
Coating step
In the process for producing a graphite sheet according to the present invention, the coating may be carried out in various conventional coating processes, for example, a roll coating process, a rolling process, a bar coating process, a dip coating (immersion coating) process , A spray coating process, a cast coating process, an extrusion coating process, or the like. In one embodiment of the present invention, when a liquid polyamic acid having a high viscosity is used, a rolling process may be used to effectively coat the fibrous substrate, but the present invention is not limited thereto. Can be used.
In addition, in the coating step, the thickness ratio of the fibrous base material and the coated polymer resin is preferably 1: 9 to 9: 1. Further, in one embodiment of the present invention, after the coating step, a rolling step of rolling the sheet may be further included to improve the uniformity of the coating thickness.
Further, when tensile force is applied to the fibrous substrate in the coating step, the pulling tension (N / m) applied to the fibrous substrate may be 1 to 10 N / m.
Heat treatment apparatus
In the process for producing a graphite sheet according to the present invention, the curing step, the carbonization step and / or the graphitization step may be continuously performed in one
The
Further, in order to gently heat the
Further, the
<When the curing step is performed continuously in one heat treatment apparatus>
Curing step
In one embodiment of the present invention, when the curing step is carried out continuously in a heat treatment apparatus, it may be carried out in a heat treatment apparatus having a temperature range of 80 to 400 DEG C, 0.0 > g., ≪ / RTI >
The pulling tension applied to the sheet in the curing step is preferably 1 to 10 N / m so as to suppress generation of wrinkles due to heat and to prevent breakage due to excessive tension.
Coiling step
In the method of producing a rolled graphite sheet according to the present invention, after the curing step, it may include a winding step of winding the cured sheet in the form of a roll, and may optionally further include a rolling step before the winding step have. The winding
As shown in Fig. 3, in the winding step, the winding
Carbonization step
In the method for producing a graphite sheet according to the present invention, the wound cured sheet is formed into a graphite sheet through a heat treatment process through a carbonization and / or a graphitization step. The heat treatment step in the carbonization step can be carried out after the wound cured sheet is charged into the crucible. The crucible is provided with pressing means for preventing a phenomenon that a rolled rolled cured sheet is shrunk during heat treatment to cause a gap or a space between the cured sheet layers, Can be mounted.
The wound cured sheet charged into the crucible is charged into the crucible with the winding
The carbonization step of the present invention is preferably carried out in an inert gas such as nitrogen or argon, and may be carried out at a temperature ranging from 400 to 2500 ° C. In one embodiment of the present invention, the carbonization step is performed at a temperature in the range of 800 ° C to 1800 ° C, more specifically, in a temperature range of 1000 ° C to 1400 ° C for about 30 minutes For 20 hours, more specifically about 1 to 4 hours, to carbonize the cured sheet.
Graphitization step
The graphitization step is preferably performed in an inert gas such as nitrogen or argon, and may be performed at a temperature of about 2500 DEG C or higher or a temperature of about 3200 DEG C or lower. In one embodiment of the present invention, the graphitization step may be carried out at a temperature of about 2500 ° C to 3000 ° C, specifically at a temperature of about 2600 ° C to 2900 ° C, more specifically about 2600 ° C to 2700 ° C . As the heat treatment temperature is increased, the degree of graphitization is improved, but the process cost is increased. Further, the heat treatment in the graphitization step may be performed for about 30 minutes to 20 hours, more specifically about 30 minutes to 4 hours, and the pressure condition may be in the range of 700 to 760 torr, but is not limited thereto.
The carbonization and / or graphitization step may be performed by resistance heating, arc heating or induction heating, so that the carbonization and / or graphitization step may proceed in a resistance heating furnace, an arc heating furnace, or an induction heating furnace.
The induction heating is an electromagnetic induction principle in which a current flows in a closed circuit by a temporally varying magnetic field. When a coil is disposed around a heating object such as a conductor to allow an alternating current to flow, It is a phenomenon that heat is generated by heat loss and loss of hysteresis. As an embodiment of the present invention, the induction heating may be performed by disposing an
≪ Curing, Carbonization and Graphitization Steps are Performed Successively in One Heat Treatment Apparatus >
Hardening, carbonization and Graphitization step
In one embodiment of the present invention, the curing step, the carbonization step and the graphitization step may be performed continuously in the heat treatment apparatus, in which case the temperature range may be 80 to 3200 占 폚. In addition, the temperature in the heat treatment apparatus may have a gentle temperature gradient over the entire temperature range.
The pulling tension applied to the sheet during the curing, carbonization and graphitization steps is preferably 1 to 10 N / m so as to suppress generation of wrinkles due to heat and to prevent breakage due to excessive tension.
Coiling step
In the method of producing a graphite sheet in the form of a roll according to the present invention, after the curing, carbonization and graphitization steps, it may include a winding step of winding the sheet 13 'into a roll form, A rolling step may be further included. The winding
Hereinafter, the present invention will be described in more detail with reference to the following examples. The following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example
Example 1
(1) Preparation step of description
100 plain yarn (150X100) (origin: China) was prepared as a fiber base material.
(2) Coating step
A liquid polyamic acid was coated on one side of the fiber substrate using a roll coating process at 25 캜 to prepare a sheet.
(3) Curing step
The sheet thus prepared was dried and cured for 30 minutes by a hot air curing method in a heat treatment apparatus having a temperature gradient of 80 ° C to 250 ° C to prepare a cured sheet.
(4) Coiling step
The thus-prepared cured sheet was wound 10 times and then unwound by one turn.
(5) Carbonization and graphitization step
The rolled sheet was charged into a graphite crucible, carbonized at a temperature of 1200 ° C for 2 hours, and then graphitized at a temperature of 2800 ° C for 1 hour to prepare a graphite sheet having a thickness of 40 μm.
Example 2
A graphite sheet having a thickness of 40 占 퐉 was produced in the same manner as in Example 1 except that 140 carbon fibers were used instead of 100 cotton fabrics of Example 1. [
Experimental Example 1: Heat diffusion test
The graphite sheets prepared in the above examples were measured for thermal diffusivity using a laser flash method (NEIZCH LFA447). The results are summarized in Table 1 below.
As shown in the above table, the graphite sheet according to the present invention exhibits a thermal diffusivity of about 520 to 530 mm 2 / s, and exhibits the same or superior thermal diffusivity as that of the conventional graphite sheet. In addition, since the graphite sheet according to the present invention uses relatively inexpensive cotton fiber as a base component, it can be produced at a considerably lower production cost than the conventional graphite sheet, and the manufacturing cost can be greatly reduced, which is economical.
11:
20: Coating device 30: Rolling device
40:
50: winding device 51: winding core
60: Crucible 61: Crucible cap
62: induction heating coil
Claims (20)
Wherein the curing step is performed in a heat treatment apparatus, the coating and curing step is a continuous process,
Wherein the carbonization of the wound cured sheet is carried out in a crucible and a center pillar having a diameter of 70 to 90% is located at the center of the crucible on the basis of the inner diameter of the wound cured sheet, Way.
Wherein the fiber base material is natural fiber, artificial fiber or paper.
Wherein the fiber base material is at least one natural fiber selected from the group consisting of cotton, hemp, wool, and silk.
Wherein the polymer resin comprises a polyamic acid.
Wherein the thickness ratio of the fibrous base material to the coated polymer resin is 1: 9 to 9: 1.
Further comprising a rolling step of rolling the sheet after the coating step.
Wherein the pulling tension applied in the coating step and the curing step is 1 to 10 N / m.
Wherein the curing step is performed in a heat treatment apparatus in a temperature range of 80 to 400 占 폚.
Wherein the pulling tension applied to the cured sheet in the winding step is 1 to 10 N / m or less.
Wherein the rate of change of the pulling tension is less than +/- 5%.
And in the winding step, the cured sheet is wound together with a masking film or a separator.
Wherein the rolled sheet is rolled while spraying graphite powder on one side of the cured sheet in the winding step.
Wherein the carbonization step is carried out at a temperature in the range of 400 to 2500 占 폚.
Wherein the graphitization step is performed in a temperature range of 2500 to 3200 캜.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004299937A (en) | 2003-03-28 | 2004-10-28 | Kanegafuchi Chem Ind Co Ltd | Method of producing graphite film |
JP2010064391A (en) * | 2008-09-11 | 2010-03-25 | Kaneka Corp | Graphite composite film |
JP5602956B2 (en) | 2011-11-30 | 2014-10-08 | 株式会社カネカ | Graphite film and method for producing graphite film |
KR101554912B1 (en) | 2014-08-13 | 2015-09-22 | 에스케이씨 주식회사 | Method for preparing graphite and furnace therefor |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004299937A (en) | 2003-03-28 | 2004-10-28 | Kanegafuchi Chem Ind Co Ltd | Method of producing graphite film |
JP2010064391A (en) * | 2008-09-11 | 2010-03-25 | Kaneka Corp | Graphite composite film |
JP5602956B2 (en) | 2011-11-30 | 2014-10-08 | 株式会社カネカ | Graphite film and method for producing graphite film |
KR101554912B1 (en) | 2014-08-13 | 2015-09-22 | 에스케이씨 주식회사 | Method for preparing graphite and furnace therefor |
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