WO2016175453A1 - 그라파이트 시트 및 이의 제조방법 - Google Patents
그라파이트 시트 및 이의 제조방법 Download PDFInfo
- Publication number
- WO2016175453A1 WO2016175453A1 PCT/KR2016/002876 KR2016002876W WO2016175453A1 WO 2016175453 A1 WO2016175453 A1 WO 2016175453A1 KR 2016002876 W KR2016002876 W KR 2016002876W WO 2016175453 A1 WO2016175453 A1 WO 2016175453A1
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- WIPO (PCT)
- Prior art keywords
- graphite
- graphite sheet
- fibers
- substrate
- sheet
- Prior art date
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/546—Flexural strength; Flexion stiffness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/732—Dimensional properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Definitions
- the present invention relates to a graphite sheet having excellent thermal diffusion ratio in the horizontal / vertical direction and excellent in flexibility and a method of manufacturing the same.
- heat dissipation materials are being developed, and are marketed in the form of heat dissipation pads, heat dissipation sheets, and heat dissipation paints to assist or replace heat dissipation devices such as heat dissipation fans, heat dissipation fins, and heat pipes.
- the heat dissipation sheet is manufactured in the form of graphite sheet, polymer-ceramic composite sheet, multi-layer coated metal thin film sheet, and the like. It is usefully used for the PDP etc. which comprise a plasma television etc. between a board and a board
- polymer graphite method the method of directly heat-treating a special polymer film and graphitizing was developed (henceforth a "polymer graphite method").
- the polymer film used for this purpose include polyoxadiazole, polyimide, polyphenylenevinylene, polybenzoimidazole, polybenzoxazole, polythiazole, polyamide film and the like.
- the polymer graphitization method is much simpler than the conventional expanded graphite method and is essentially a method of not incorporating impurities such as an acid, and is characterized by obtaining excellent thermal conductivity and electrical conductivity close to that of single crystal graphite. See Japanese Laid-Open Patent Publication No. 60-181129, Japanese Laid-Open Patent Publication No. Hei 7-109171, and Japanese Laid-Open Patent Publication No. 61-275116).
- the conventional graphite sheet has a high thermal diffusion rate (thermal conductivity) in the horizontal direction, but has a disadvantage in that the thermal diffusion rate in the vertical direction is low and expensive.
- the present invention provides a graphite sheet having a heat diffusion rate ratio of 300 or more in the horizontal / vertical direction.
- the present invention also provides a graphite sheet having a thermal diffusivity in the vertical direction of 2.0 mm 2 / s or less.
- the present invention provides a method comprising the steps of: (1) providing a substrate comprising natural fibers, artificial fibers or paper; (2) performing a primary coating on one or more surfaces of the substrate with a coating solution including at least one selected from the group consisting of polymer, carbonized polymer and graphite; And (3) heat treating the coated substrate to graphitize the graphite substrate.
- the present invention also provides a graphite sheet comprising an inner layer comprising graphite fibers and a graphite outer layer covering one or both sides of the inner layer.
- the graphite sheet of the present invention has a low thermal diffusion rate in the vertical direction, a high thermal diffusion rate in the horizontal direction, has excellent thermal diffusion rate ratio in the horizontal / vertical direction, and has excellent flexibility.
- the graphite sheet is manufactured using a relatively inexpensive fibrous substrate in place of an expensive polyimide film (PI film), thereby having an economic advantage that can be produced at a low manufacturing cost.
- PI film polyimide film
- FIG 1 and 2 illustrate an image obtained by observing a surface and a cross section of a substrate portion of a graphite sheet according to an embodiment of the present invention with a scanning electron microscope (SEM).
- SEM scanning electron microscope
- the present invention comprises (i) a substrate comprising natural fibers, artificial fibers or paper, and (ii) at least one selected from the group consisting of polymers, carbonized polymers and graphite, provided on one or both sides of the substrate. It relates to a graphite sheet obtained by heat treatment of the coating layer.
- the substrate may be made of natural fibers, the natural fibers can be largely divided into cellulose fibers, protein fibers and mineral fibers.
- the cellulose fibers include (i) seed fibers, such as cotton or kapok, (ii) stem fibers, such as flax, hemp, hemp, or jute, (iii) fruit fibers, such as palm fibers, and (iv) manila, abaca Or leaf fibers such as sisal.
- the protein fibers may comprise (i) wool fibers, (ii) silk fibers and (iii) hair fibers.
- the natural fibers are preferably at least one natural fiber selected from the group consisting of cotton, hemp, wool and silk.
- the substrate may be made of artificial fibers
- the artificial fibers can be largely divided into organic fibers and inorganic fibers.
- the organic fibers may include (i) regenerated fibers including cellulose fibers and protein fibers such as rayon, tencel (lyocell), modal, and the like, (ii) semisynthetic fibers comprising cellulose fibers such as acetate, triacetate, or the like.
- synthetic fibers such as polyamide fiber, polyester fiber, polyurethane fiber, polyethylene fiber, polyvinyl chloride fiber, polyfluoroethylene fiber, polyvinyl alcohol fiber, acrylic fiber or polypropylene fiber It may include.
- the artificial fibers are made of nylon, polyester, polyurethane, polyethylene, polyvinyl chloride, polyfluoroethylene, polyvinyl alcohol, acrylic and polypropylene. At least one synthetic fiber selected from the group; Or one or more cellulosic fibers selected from the group consisting of rayon, acetate and triacetate.
- the substrate may be made of paper.
- the coating layer may include a polymer.
- the polymer may be at least one selected from the group consisting of polyimide, polyamic acid, polyvinyl chloride, polyester, polyurethane, polyethylene, polyfluoroethylene, polyvinyl alcohol, acrylic, and polypropylene.
- the polymer may be at least one selected from the group consisting of polyimide, polyamic acid, and polyvinyl chloride having a weight average molecular weight of 200,000 to 300,000.
- the coating layer may include a carbonized polymer.
- the carbonized polymer may be obtained by subjecting the polymer to heat treatment at 800 to 1,800 ° C., specifically 1,000 to 1,400 ° C. in an atmosphere of an inert gas such as nitrogen and argon.
- the carbonized polymer may include at least 90% by weight of carbon based on the total weight of the coating layer.
- the carbon of the carbonized polymer may be obtained in an amount of about 2 to 50% by weight of the initial polymer mass.
- the coating layer may include graphite.
- the graphite may be natural graphite or expanded graphite.
- the expanded graphite herein refers to graphite which is treated with a mixed solution of sulfuric acid, nitric acid, or the like, of natural graphite, pyrolytic graphite, and kishi graphite, and then subjected to expansion treatment at about 1,000 ° C. in an expansion furnace after washing with water and drying.
- the coating layer may include one or more of the group consisting of polyamic acid, polyimide and graphite.
- the graphite sheet of the present invention may have a thermal diffusion rate ratio of 300 or more, 400 or more, or 500 or more in the horizontal / vertical direction.
- the thermal diffusion rate ratio in the horizontal / vertical direction may be 300 to 2,000, 300 to 1,800, 300 to 1,500, 400 to 1,250, or 500 to 1,000.
- the graphite sheet of the present invention may have a thermal diffusion rate in the horizontal direction of 100 to 1,000 mm 2 / s, 200 to 800 mm 2 / s, or 400 to 600 mm 2 / s.
- the thermal diffusion rate in the vertical direction may be 2.0 mm 2 / s or less, or 1.0 mm 2 / s or less. Specifically, the thermal diffusion rate in the vertical direction may be 0.1 to 2 mm 2 / s, 0.2 to 2 mm 2 / s, or 0.3 to 2 mm 2 / s.
- the graphite sheet according to the present invention is a MIT bendability test results under a bending radius (R) of 5 mm, a bending angle of 180 degrees, a load of 0.98 N and a bending speed of 90 times / minute, reciprocating bending until fracture
- the number may be 10,000 or more times.
- the graphite sheet according to the present invention is characterized in that the shape of the cross section of the substrate portion is the same as that of the natural fiber, artificial fiber or paper constituting it.
- the cross section of the substrate portion of the graphite sheet is the same as that of the cellulose fibers.
- the present invention comprises the steps of (1) providing a substrate comprising natural fibers, artificial fibers or paper; (2) first coating one or both sides of the substrate with a coating solution containing a polymer, a carbonized polymer or graphite; And (3) heat treating the coated substrate to graphitize the graphite substrate.
- Step (2) of the present invention may be applied to the method commonly used in the coating process, for example, a rolling process, a bar coating process, a dip coating process, a spray coating process and the like can be used.
- a rolling process or a bar coating process may be used.
- a rolling process when using a high viscosity liquid polyamic acid as the coating liquid, it is preferable to use a rolling process to coat the substrate effectively.
- the method for producing the graphite sheet may further comprise the step of performing a secondary coating on the primary coating layer with the same coating liquid after the primary coating.
- the primary coating is the main purpose of filling the polymer between the cotton fabric
- the secondary coating is the main purpose to adjust the thickness.
- the secondary coating may be performed by repeating 1 to 3 times.
- the graphite sheet manufacturing method may further include a rolling step after the primary coating.
- the rolling is to improve the uniformity of the thickness of the coating layer.
- the coating solution may include a polyamic acid, and may further include an imidization step after the first coating.
- Step (3) of the present invention may include a carbonization process, a graphitization process and a post treatment process.
- the carbonization process may carbonize the substrate and the coating layer by heating at 800 to 1,800 ° C., specifically 1,000 to 1,400 ° C., more specifically at about 1,000 ° C. for 1 to 20 hours.
- the graphite sheet may be obtained by graphitizing the carbonized base layer and the coating layer by heating at 2,000 to 2,900 ° C., specifically, at about 2,850 ° C. for 1 to 20 hours.
- the graphite sheet prepared in the graphitization step may be post-treated with acid or pressure to impart flexibility to the graphite sheet.
- the acid can be used as long as it can expand the C-axis direction of the graphite crystal by entering the graphite layer to generate acidic ions (anions), preferably sulfuric acid, more preferably at least 95% by weight
- Concentrated concentrated sulfuric acid can be used. For example, by immersing the graphite sheet in a sulfuric acid solution and heating to a normal temperature as necessary, it is possible to obtain a graphite sheet having a flexibility by expanding the graphite interlayer C-axis direction.
- the pressing may be performed using a roll press.
- the present invention provides a graphite sheet comprising an inner layer comprising graphite fibers and a graphite outer layer covering one or both sides of the inner layer.
- the inner layer may be made of a fiber bundle comprising a plurality of graphite fibers.
- the fiber bundle may comprise a void formed between a plurality of graphite fibers.
- the inner layer may comprise a weft and warp woven fabric form consisting of graphite fibers or graphite fiber bundles.
- the graphite outer layer may include a first graphite outer layer coated on one surface of the graphite inner layer and a second graphite outer layer coated on the other surface of the graphite inner layer, and a portion of the first graphite outer layer and the second graphite outer layer may be connected to each other. .
- the base material consisting of cellulose-based fibers prepared 100 cotton fabrics (150 mm ⁇ 100 mm) (origin: China).
- Liquid polyamic acid manufactured by KOLON PI, product name: PAA varnish, weight average molecular weight: 250,000
- KOLON PI product name: PAA varnish, weight average molecular weight: 250,000
- a secondary coating was performed to a thickness of 150 ⁇ m on the coating layer to prepare a base film.
- the substrate film prepared in step (2) was heated at a rate of 1 ° C./min in a nitrogen atmosphere (pressure of about 100 torr), and heated at about 400 ° C. for about 10 hours to form an imidized substrate having a thickness of 140 to 160 ⁇ m.
- a film was prepared.
- the imidized base film prepared in step (3) was carbonized by heating at a rate of 1 ° C./min in nitrogen or an inert gas atmosphere (pressure of about 100 torr) and heating at about 1,000 ° C. for 3 hours. After heating at a rate of 5 °C / min and graphitized by heating at about 2,600 °C for 1 hour, using a roll press as a post-treatment by applying a force of 10 tons load to give flexibility, about 40 ⁇ m thick graphite Sheets were prepared.
- Example 2 In place of the cotton fabric of Example 1, except that rayon was used, the same process as in Example 1 was performed to prepare a graphite sheet having a thickness of about 40 ⁇ m.
- Example 2 The same carbonization, graphitization, and post-treatment steps as in Example 1, except that a polyimide film (thickness: 75 ⁇ m, manufacturer: KOLON PI, product name: PI Film 75 ⁇ m) as the base film of Example 1
- a polyimide film thickness: 75 ⁇ m, manufacturer: KOLON PI, product name: PI Film 75 ⁇ m
- the horizontal and vertical thermal diffusivities of the graphite sheets prepared in the above Examples and Comparative Examples were measured using a thermal diffusivity measuring device ("LFA447 Nanoflash” manufactured by Netsch) by the light exchange method. Specifically, the horizontal and vertical thermal diffusivities were measured by cutting the prepared graphite sheets into ⁇ 25.4 mm and ⁇ 12.6 mm, respectively, and measuring five or more times at a temperature of 25 ° C., respectively.
- the flexibility of the graphite sheets prepared in Examples and Comparative Examples was evaluated by the MIT flexibility test.
- the MIT flexural test was made of square specimens of 20 mm width and then conducted at 5 mm radius of curvature R, 180 degree bending angle, 0.98 N load and 90 times / min bending rate conditions. Flexibility was assessed by the number of reciprocating bends until fracture in the MIT flexural test.
- the graphite sheet according to the present invention has an excellent horizontal / vertical thermal diffusivity ratio by lowering the thermal diffusivity in the vertical direction while maintaining the excellent thermal diffusion rate in the horizontal direction.
- the graphite sheet according to the present invention has excellent thermal diffusivity ratio in the horizontal / vertical direction and at the same time excellent flexibility.
- the graphite sheet according to the present invention can be produced at a low manufacturing cost by using fibers such as cotton or rayon as the base component, it is economically advantageous.
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Abstract
Description
구분 | 기재성분 | 코팅층성분 | 시트의두께(㎛) | 수평방향 열확산율(㎟/s) | 수직방향 열확산율(㎟/s) | 수평/수직방향 열확산율비 | 유연성 |
실시예 1 | 면직물 | 폴리아믹산 | 40 | 500 | 0.5 | 1000 | 12311 |
실시예 2 | 레이온 | 폴리아믹산 | 40 | 450 | 0.8 | 562.5 | 13456 |
비교예 1 | 폴리이미드 필름 | - | 40 | 520 | 2.7 | 193 | 8760 |
Claims (17)
- 수평/수직 방향의 열확산율비가 300 이상인 그라파이트 시트.
- 제1항에 있어서,상기 수평/수직 방향의 열확산율비가 500 이상인 그라파이트 시트.
- 제1항에 있어서,5mm의 곡률 반경(R), 180도의 절곡 각도, 0.98 N의 하중 및 90 회/분의 절곡 속도 조건에서 수행한 MIT 왕복 절곡 횟수가 10,000회 이상인, 그라파이트 시트.
- 수직 방향의 열확산율이 2.0 ㎟/s 이하인 그라파이트 시트.
- 제4항에 있어서,상기 수직 방향의 열확산율이 1.0 ㎟/s 이하인 그라파이트 시트.
- (1) 천연 섬유, 인조 섬유 또는 종이를 포함하는 기재를 제공하는 단계;(2) 상기 기재의 단면 또는 양면을 고분자, 탄소화된 고분자 및 흑연으로 이루어진 군 중 1종 이상을 포함하는 코팅액으로 1차 코팅을 하는 단계; 및(3) 상기 코팅된 기재를 열처리하여 흑연화시키는 단계를 포함하는, 그라파이트 시트의 제조방법.
- 제6항에 있어서,상기 1차 코팅 후, 동일한 코팅액으로 1차 코팅층 상에 2차 코팅을 수행하는 단계를 추가로 포함하는, 그라파이트 시트의 제조방법.
- 제6항에 있어서,상기 1차 코팅 후, 압연 단계를 추가로 포함하는, 그라파이트 시트의 제조방법.
- 제6항에 있어서,상기 코팅액이 폴리아믹산을 포함하고, 1차 코팅 후, 이미드화 단계가 추가로 포함되는, 그라파이트 시트의 제조방법.
- 제6항에 있어서,상기 기재가 면, 마, 모 및 견으로 구성된 군으로부터 선택되는 1종 이상의 천연 섬유인, 그라파이트 시트의 제조방법.
- 제6항에 있어서,상기 기재가 레이온, 아세테이트 및 트리아세테이트로 이루어진 군으로부터 선택되는 1종 이상의 셀룰로오스계 섬유인, 그라파이트 시트의 제조방법.
- 제6항에 있어서,상기 기재가 나일론, 폴리에스테르, 폴리우레탄, 폴리에틸렌, 폴리염화비닐, 폴리플루오로에틸렌, 폴리비닐알코올, 아크릴 및 폴리프로필렌으로 이루어진 군으로부터 선택되는 1종 이상의 합성섬유인 그라파이트 시트의 제조방법.
- 흑연 섬유를 포함하는 내층 및 상기 내층의 단면 또는 양면을 덮는 흑연 외층을 포함하는 그라파이트 시트.
- 제13항에 있어서,상기 내층이 복수의 흑연 섬유를 포함하는 섬유 다발로 이루어진, 그라파이트 시트.
- 제14항에 있어서,상기 섬유 다발이 복수의 흑연 섬유 사이에 형성된 공극을 포함하는, 그라파이트 시트.
- 제13항에 있어서,상기 흑연 외층은 흑연 내층의 일면을 피복하는 제1 흑연 외층과 상기 흑연 내층의 다른 일면을 피복하는 제2 흑연 외층으로 구성되며, 상기 제1 흑연 외층과 제2 흑연 외층의 일부가 서로 연결된, 그라파이트 시트.
- 제13항에 있어서,상기 내층은 흑연 섬유 또는 흑연 섬유 다발로 이루어진, 위사와 경사가 직조된 직물 형태를 포함하는, 그라파이트 시트.
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US15/532,544 US11040516B2 (en) | 2015-04-30 | 2016-03-22 | Graphite sheet and method for manufacturing same |
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JP2017531842A JP6495456B2 (ja) | 2015-04-30 | 2016-03-22 | 黒鉛シートおよびその製造方法 |
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US11040516B2 (en) | 2021-06-22 |
TW201700403A (zh) | 2017-01-01 |
JP6495456B2 (ja) | 2019-04-03 |
CN107108227B (zh) | 2020-08-14 |
KR101669204B1 (ko) | 2016-10-25 |
JP6759322B2 (ja) | 2020-09-23 |
US20200223700A1 (en) | 2020-07-16 |
US11541634B2 (en) | 2023-01-03 |
TWI727945B (zh) | 2021-05-21 |
US20180265362A1 (en) | 2018-09-20 |
JP2019073438A (ja) | 2019-05-16 |
JP2018506492A (ja) | 2018-03-08 |
CN107108227A (zh) | 2017-08-29 |
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