KR102631465B1 - Method for preparing heat dissipation component with high flexibility made of graphite or graphene material - Google Patents
Method for preparing heat dissipation component with high flexibility made of graphite or graphene material Download PDFInfo
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- KR102631465B1 KR102631465B1 KR1020210126760A KR20210126760A KR102631465B1 KR 102631465 B1 KR102631465 B1 KR 102631465B1 KR 1020210126760 A KR1020210126760 A KR 1020210126760A KR 20210126760 A KR20210126760 A KR 20210126760A KR 102631465 B1 KR102631465 B1 KR 102631465B1
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- graphite
- graphene
- raw material
- heat dissipation
- graphene raw
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 187
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 93
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 92
- 239000010439 graphite Substances 0.000 title claims abstract description 92
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 61
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052802 copper Inorganic materials 0.000 claims abstract description 37
- 239000010949 copper Substances 0.000 claims abstract description 37
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000009713 electroplating Methods 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012190 activator Substances 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 230000001681 protective effect Effects 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000007770 graphite material Substances 0.000 claims abstract description 5
- 238000007654 immersion Methods 0.000 claims abstract description 3
- 239000013543 active substance Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims abstract 2
- QAQSNXHKHKONNS-UHFFFAOYSA-N 1-ethyl-2-hydroxy-4-methyl-6-oxopyridine-3-carboxamide Chemical compound CCN1C(O)=C(C(N)=O)C(C)=CC1=O QAQSNXHKHKONNS-UHFFFAOYSA-N 0.000 claims description 7
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 229910001431 copper ion Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- BBFCIBZLAVOLCF-UHFFFAOYSA-N pyridin-1-ium;bromide Chemical compound Br.C1=CC=NC=C1 BBFCIBZLAVOLCF-UHFFFAOYSA-N 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 45
- 238000002845 discoloration Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 230000037303 wrinkles Effects 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/02—Constructions of heat-exchange apparatus characterised by the selection of particular materials of carbon, e.g. graphite
-
- 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
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
Abstract
본 발명은 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법을 개시한다. 여기에는 1) 흑연 또는 그래핀 원료에 대해 플라즈마 세정을 수행하는 단계; 2) 황산 10-20%, OP-10 계면활성제 0.05-1%, 도데실 황산나트륨(sodium dodecyl sulfate) 0.05-1%, 나머지는 물인 중량%의 활성제를 포함한 제조 재료를 취하는 단계; 3) 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정하는 단계; 4) 탈이온수로 흑연 또는 그래핀 원료를 세정하는 단계; 5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 수행하여 구리 필름층을 형성하는 단계; 6) 흑연 또는 그래핀 원료는 탈이온수를 사용하여 계속해서 세정하는 단계; 7) 침지 방식을 통해 흑연 또는 그래핀 원료 상에 보호 필름을 형성하는 단계; 및 8) 구리 필름층을 전기 도금한 흑연 또는 그래핀 원료를 건조시키는 단계가 포함된다. 선행 기술과 비교할 때 본 발명은 활성제가 처리된 흑연 또는 그래핀 표면이 전기 도금 시 구리 필름층의 결합 품질이 우수하고 균일하며, 제조된 방열 부재의 유연성이 강화된다.The present invention discloses a method of manufacturing a heat dissipation member made of highly flexible graphite material or graphene material. These include 1) performing plasma cleaning on the graphite or graphene raw material; 2) Taking manufacturing materials containing 10-20% sulfuric acid, 0.05-1% OP-10 surfactant, 0.05-1% sodium dodecyl sulfate, and the remaining weight percent of active agents as water; 3) Continuing to clean the graphite or graphene raw material using an activator; 4) cleaning the graphite or graphene raw material with deionized water; 5) performing electroplating processing on the surface of graphite or graphene raw material to form a copper film layer; 6) Continuing to clean the graphite or graphene raw material using deionized water; 7) forming a protective film on the graphite or graphene raw material through an immersion method; and 8) drying the graphite or graphene raw material on which the copper film layer was electroplated. Compared to the prior art, in the present invention, the graphite or graphene surface treated with an activator has excellent and uniform bonding quality with the copper film layer during electroplating, and the flexibility of the manufactured heat dissipation member is enhanced.
Description
본 발명은 흑연 재질 또는 그래핀 재질 부품 제조 분야에 속하며, 더욱 상세하게는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법에 관한 것이다.The present invention belongs to the field of manufacturing components made of graphite or graphene, and more specifically, relates to a method of manufacturing a heat dissipation member made of highly flexible graphite or graphene.
흑연은 탄소 원자가 sp2 혼성 오비탈로 육각형을 구성하여 벌집 격자 모양을 띠는 2차원 탄소 나노 재료이다. 흑연은 매우 양호한 열전도 성능을 가지며, 순수한 무결함 단층 흑연의 열전도 계수는 5300W/mK이다. 이는 현재까지 열전도 계수가 가장 높은 탄소 재료로, 단일 벽 탄소 나노 튜브(3500W/mK) 및 다중 벽 탄소 나노 튜브(3000W/mK)보다 높다. 이를 캐리어로 사용할 경우 열전도 계수는 600W/mK에 도달할 수 있다. 또한 흑연의 탄도 열전도율은 단위 원주와 길이의 탄소 나노 튜브의 탄도 열전도율의 하한을 하향시킬 수 있다.Graphite is a two-dimensional carbon nanomaterial in which carbon atoms form hexagons with sp 2 hybrid orbitals, forming a honeycomb lattice shape. Graphite has very good heat conduction performance, and the heat conduction coefficient of pure defect-free single-layer graphite is 5300 W/mK. This is the carbon material with the highest thermal conductivity coefficient to date, higher than single-walled carbon nanotubes (3500 W/mK) and multi-walled carbon nanotubes (3000 W/mK). When used as a carrier, the heat conduction coefficient can reach 600W/mK. Additionally, the ballistic heat conductivity of graphite can lower the lower limit of the ballistic heat conductivity of carbon nanotubes of unit circumference and length.
전자 제품 중 각종 전자 요소는 모두 방열이 필요하다. 종래의 흑연이나 그래핀을 전자 요소의 방열에 적용할 경우, 주로 한 층의 금속층을 흑연이나 그래핀의 표면에 고정한다. 구체적으로 접착이나 전기도금 방식을 통해 금속층을 흑연 또는 그래핀 상에 고정하며, 열전도 효율 측면에서 전기도금이 접합의 방식보다 우수하다.Among electronic products, all electronic elements require heat dissipation. When conventional graphite or graphene is applied to heat dissipation of electronic elements, one metal layer is mainly fixed to the surface of graphite or graphene. Specifically, the metal layer is fixed on graphite or graphene through adhesion or electroplating, and electroplating is superior to bonding in terms of heat conduction efficiency.
흑연 또는 그래핀 재료 표면 금속층의 전기도금 품질을 보장하기 위해, 일반적으로 전기도금 전 흑연 또는 그래핀 표면에 여러 번의 세정 공정을 수행한다. 세정 공정에서 OP-10 계면활성제를 사용하여 흑연 또는 그래핀의 표면을 처리한 후, 흑연 또는 그래핀 표면의 평활도가 일반적이기 때문에 흑연 또는 그래핀 표면에 전기도금된 금속층의 결합 효과가 좋지 않고 두께가 불균일하게 된다. 이는 제조된 방열 부재의 유연성에 영향을 미치며 방열 부재 표면에 주름이 생기기 쉽다.To ensure the electroplating quality of the surface metal layer of graphite or graphene material, several cleaning processes are generally performed on the graphite or graphene surface before electroplating. After treating the surface of graphite or graphene using OP-10 surfactant in the cleaning process, the smoothness of the graphite or graphene surface is general, so the bonding effect of the electroplated metal layer on the graphite or graphene surface is not good, and the thickness becomes uneven. This affects the flexibility of the manufactured heat dissipation member and wrinkles are likely to form on the surface of the heat dissipation member.
본 발명의 목적은 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법을 제공하는 데에 있다. 먼저 흑연 또는 그래핀 표면을 플라즈마로 세정한 후, 황산, OP-10 계면활성제 및 도데실 황산나트륨으로 배합된 활성제를 이용해 흑연 또는 그래핀의 표면을 처리하여 재료 표면을 매끄럽게 만들고 흑연 또는 그래핀 표면에 전기도금된 구리 필름층의 결합 품질이 우수하고 균일하도록 보장한다. 이를 통해 제조된 방열 부재의 유연성을 강화시키고 방열 부재 표면에 쉽게 주름이 생기지 않도록 한다.The purpose of the present invention is to provide a method of manufacturing a heat dissipation member made of highly flexible graphite or graphene material. First, the surface of the graphite or graphene is cleaned with plasma, and then the surface of the graphite or graphene is treated with an activator mixed with sulfuric acid, OP-10 surfactant, and sodium dodecyl sulfate to make the material surface smooth and the surface of the graphite or graphene is treated. Ensures that the bonding quality of the electroplated copper film layer is excellent and uniform. This enhances the flexibility of the manufactured heat dissipation member and prevents wrinkles from easily forming on the surface of the heat dissipation member.
상기 목적을 구현하기 위해, 본 발명은 하기의 기술적 해결책을 채택하여 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법을 제공하며, 여기에는 하기 단계가 포함된다.In order to achieve the above object, the present invention provides a method for manufacturing a heat dissipation member made of highly flexible graphite material or graphene material by adopting the following technical solution, which includes the following steps.
1) 흑연 또는 그래핀 원료에 대해 플라즈마 세정을 수행한다.1) Plasma cleaning is performed on graphite or graphene raw materials.
2) 중량%를 기준으로, 황산 10-20%, OP-10 계면활성제 0.05-1%, 도데실 황산나트륨(sodium dodecyl sulfate) 0.05-1%, 나머지는 물인 활성제를 포함한 제조 재료를 취한다.2) Based on weight percent, manufacturing materials are taken including 10-20% sulfuric acid, 0.05-1% OP-10 surfactant, 0.05-1% sodium dodecyl sulfate, and the remainder is water.
3) 상기 활성제 성분을 혼합하여 활성제를 제조하고, 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정한다.3) The activator ingredients are mixed to prepare an activator, and the graphite or graphene raw material is continuously cleaned using the activator.
4) 탈이온수로 계속해서 흑연 또는 그래핀 원료를 세정한다.4) Continue cleaning the graphite or graphene raw material with deionized water.
5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 수행하여 구리 필름층을 형성한다.5) Electroplating is performed on the surface of the graphite or graphene raw material to form a copper film layer.
6) 표면에 구리 필름층이 전기도금된 흑연 또는 그래핀 원료는 탈이온수를 사용하여 계속해서 세정한다.6) Graphite or graphene raw materials with a copper film layer electroplated on the surface are continuously cleaned using deionized water.
7) 침지 방식을 통해 흑연 또는 그래핀 원료 상에 보호 필름을 형성한다.7) A protective film is formed on the graphite or graphene raw material through the immersion method.
8) 구리 필름층을 전기도금한 흑연 또는 그래핀 원료를 건조시킨다.8) Dry the graphite or graphene raw material on which the copper film layer was electroplated.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution is described in more detail.
단계 1)에서 흑연 또는 그래핀 원료를 플라즈마 세정기에 거치하여 세정한다.In step 1), the graphite or graphene raw material is placed in a plasma cleaner and cleaned.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution is described in more detail.
단계 2)에서 활성제는 중량%를 기준으로 황산 12-16%, OP-10 계면활성제 0.05-0.5%, 도데실 황산나트륨 0.05-0.5%, 나머지는 물 성분을 포함한다.In step 2), the activator includes 12-16% by weight of sulfuric acid, 0.05-0.5% of OP-10 surfactant, 0.05-0.5% of sodium dodecyl sulfate, and the remainder is water.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution is described in more detail.
단계 2)에서 활성제는 중량%를 기준으로 황산 15%, OP-10 계면활성제 0.1%, 도데실 황산나트륨 0.1%, 나머지는 물 성분을 포함한다.In step 2), the activator includes 15% by weight of sulfuric acid, 0.1% OP-10 surfactant, 0.1% sodium dodecyl sulfate, and the remainder is water.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution is described in more detail.
단계 5)에서 전기도금 용액을 통해 흑연 또는 그래핀 원료에 대해 2회 전기도금 가공을 수행한다. 전기도금 용액은 중량%를 기준으로 구리 이온 5%, 황산 14%, 광택제 0.8%, 보조제 0.06%, 평활제 0.06%, 나머지는 물 성분을 포함한다.In step 5), electroplating processing is performed twice on the graphite or graphene raw material using an electroplating solution. The electroplating solution contains, by weight, 5% copper ions, 14% sulfuric acid, 0.8% brightener, 0.06% auxiliary agent, 0.06% leveler, and the remainder is water.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution is described in more detail.
흑연 또는 그래핀 원료를 전기도금 용액으로 제1차 전기도금을 수행하는 경우 온도는 40도, 시간은 20분이다. 흑연 또는 그래핀 원료를 전기도금 용액으로 제2차 전기도금을 수행하는 경우 온도는 40도, 시간은 15분이다.When performing the first electroplating of graphite or graphene raw materials with an electroplating solution, the temperature is 40 degrees and the time is 20 minutes. When performing the second electroplating of graphite or graphene raw materials with an electroplating solution, the temperature is 40 degrees and the time is 15 minutes.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution is described in more detail.
단계 6)에서 흑연 또는 그래핀 원료는 먼저 5g/L 톨리트리아졸(Tolyltriazole) 용액에 20-30초 동안 침지시켜 제1층 보호 필름을 형성한 후 다시 0.5g/L의 세틸피리디늄 브로마이드(cetylpyridinium bromide) 용액에 20-30초 동안 넣어 제2층 보호 필름을 형성한다.In step 6), the graphite or graphene raw material is first immersed in a 5g/L Tolyltriazole solution for 20-30 seconds to form a first layer protective film, and then again 0.5g/L of cetylpyridinium bromide ( cetylpyridinium bromide) solution for 20-30 seconds to form a second layer protective film.
상기 내용을 종합하면, 상기 기술적 해결책을 채택함으로써 본 발명은 하기의 유익한 효과를 갖는다.Summarizing the above contents, by adopting the above technical solution, the present invention has the following beneficial effects.
1. 본 발명에서 먼저 흑연 또는 그래핀 원료를 플라즈마 세정기에 투입하여 플라즈마 세정을 수행한 후, 흑연 또는 그래핀의 표면을 황산, OP-10 계면활성제 및 도데실 황산나트륨로 배합된 활성제로 처리한다. 황산은 흑연 또는 그래핀 원료의 오일 얼룩을 씻어낼 수 있고, OP-10 계면활성제는 흑연 또는 그래핀 원료의 표면 평활성을 향상시키며, 도데실 황산나트륨은 흑연 또는 그래핀의 분산성을 증가시키고 흑연 또는 그래핀 원료 표면 평활성을 더욱 향상시킨다. 따라서 전기도금된 구리 필름층의 결합 품질이 우수하고 균일해져 제조된 방열 부재의 유연성이 강화되며, 방열 부재 표면에 주름이 쉽게 생기지 않는다. 또한 방열 부재의 방열 및 내산 성능과 내염기 성능이 향상된다.1. In the present invention, first, the graphite or graphene raw material is put into a plasma cleaner to perform plasma cleaning, and then the surface of the graphite or graphene is treated with an activator mixed with sulfuric acid, OP-10 surfactant, and sodium dodecyl sulfate. Sulfuric acid can wash away oil stains on graphite or graphene raw materials, OP-10 surfactant improves the surface smoothness of graphite or graphene raw materials, and sodium dodecyl sulfate increases the dispersibility of graphite or graphene and increases the dispersibility of graphite or graphene raw materials. Further improves the surface smoothness of graphene raw materials. Therefore, the bonding quality of the electroplated copper film layer is excellent and uniform, thereby enhancing the flexibility of the manufactured heat dissipation member, and wrinkles do not easily form on the surface of the heat dissipation member. Additionally, the heat dissipation, acid resistance, and base resistance performance of the heat dissipation member are improved.
2. 본 발명에서 흑연 또는 그래핀 원료에 구리 필름층을 전기도금한 후, 먼저 구리 필름층이 도금된 흑연 또는 그래핀 원료를 5g/L의 톨리트리아졸 용액에 20-30초간 침지하여 구리 필름층 상에 제1층 보호 필름을 형성한 후 다시 0.5g/L의 세틸피리디늄 브로마이드 용액에 20-30초간 넣어 구리 필름층 상에 제2층 보호 필름을 형성하여 구리 필름층 변색을 효과적으로 방지한다. 2. In the present invention, after electroplating a copper film layer on a graphite or graphene raw material, the graphite or graphene raw material with the copper film layer plated is first immersed in a 5 g/L tolytriazole solution for 20-30 seconds to deposit copper. After forming the first layer protective film on the film layer, put it in 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer protective film on the copper film layer, effectively preventing discoloration of the copper film layer. do.
이하에서는 본 발명의 예시적 실시예를 보다 상세하게 설명한다. 본 발명의 예시적인 실시예를 도시하였으나, 본 발명은 여기에서 설명하는 실시예에 의해 제한되지 않고 다양한 형태로 구현될 수 있음을 이해해야 한다. 반면 이러한 실시예들은 본 발명을 보다 철저하게 이해하고 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에게 본 발명의 범위를 충분히 전달하기 위해 제공되는 것이다.Hereinafter, exemplary embodiments of the present invention will be described in more detail. Although exemplary embodiments of the present invention have been shown, it should be understood that the present invention is not limited to the embodiments described herein and may be implemented in various forms. On the other hand, these embodiments are provided to understand the present invention more thoroughly and to sufficiently convey the scope of the present invention to those skilled in the art.
실시예 1Example 1
본 발명의 실시예에서 제공하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법은 하기 단계를 포함한다.The method for manufacturing a heat dissipation member made of highly flexible graphite or graphene material provided in an embodiment of the present invention includes the following steps.
1) 흑연 또는 그래핀 원료를 플라즈마 세정기에 넣고 플라즈마 세정을 수행하며, 플라즈마 세정기의 압력은 2MPa, 전력은 550-600W, 시간은 30분이다.1) Graphite or graphene raw materials are placed in a plasma cleaner and plasma cleaning is performed. The pressure of the plasma cleaner is 2MPa, the power is 550-600W, and the time is 30 minutes.
2) 중량%를 기준으로, 황산 15%, OP-10 계면활성제 0.1%, 도데실 황산나트륨 0.1%, 나머지는 물인 활성제를 포함한 제조 재료를 취한다.2) Based on weight percent, take manufacturing materials including 15% sulfuric acid, 0.1% OP-10 surfactant, 0.1% sodium dodecyl sulfate, and the remainder being water.
3) 상기 활성제 성분을 혼합하여 활성제를 제조하고, 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정한다.3) The activator ingredients are mixed to prepare an activator, and the graphite or graphene raw material is continuously cleaned using the activator.
4) 탈이온수로 계속해서 흑연 또는 그래핀 원료를 세정한다.4) Continue cleaning the graphite or graphene raw material with deionized water.
5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 2회 수행하여 구리 필름층을 형성한다.5) Electroplating is performed twice on the surface of the graphite or graphene raw material to form a copper film layer.
6) 표면에 구리 필름층이 전기도금된 흑연 또는 그래핀 원료는 탈이온수를 사용하여 계속해서 세정한다.6) Graphite or graphene raw materials with a copper film layer electroplated on the surface are continuously cleaned using deionized water.
7) 먼저 구리 필름층이 도금된 흑연 또는 그래핀 원료를 5g/L 톨리트리아졸 용액에 20-30초 동안 침지시켜 구리 필름층 상에 제1층 보호 필름을 형성한 후, 다시 0.5g/L의 세틸피리디늄 브로마이드 용액에 20-30초 동안 넣어 구리 필름층 상에 제2층 보호 필름을 형성하여, 구리 필름층 변색을 효과적으로 방지한다.7) First, the graphite or graphene raw material on which the copper film layer was plated was immersed in a 5g/L tolytriazole solution for 20-30 seconds to form a first layer protective film on the copper film layer, and then again 0.5g/L. It is placed in the cetylpyridinium bromide solution of L for 20-30 seconds to form a second layer protective film on the copper film layer, effectively preventing discoloration of the copper film layer.
8) 구리 필름층을 전기도금한 흑연 또는 그래핀 원료를 건조시킨다.8) Dry the graphite or graphene raw material on which the copper film layer was electroplated.
단계 5)는 두 차례의 전기도금 절차가 포함된다. 먼저 전기도금 용액을 이용해 흑연 또는 그래핀 원료에 대해 1차 전기도금을 수행한다. 그 다음 전기도금 용액을 이용해 흑연 또는 그래핀 원료에 대해 2차 전기도금을 수행한다. 전기도금 용액에는 중량%를 기준으로 구리 이온 5%, 황산 14%, 광택제 0.8%, 보조제 0.06%, 평활제 0.06%, 나머지는 물 성분이 포함된다. 전기도금 과정 중에서 산세척을 동시에 수행하여 방열 부재의 평탄도가 우수하게 만들 수 있다.Step 5) involves two electroplating procedures. First, first electroplating is performed on graphite or graphene raw materials using an electroplating solution. Next, secondary electroplating is performed on the graphite or graphene raw material using an electroplating solution. The electroplating solution contains, by weight, 5% copper ions, 14% sulfuric acid, 0.8% brightener, 0.06% auxiliary agent, 0.06% leveler, and the remainder is water. Pickling can be performed simultaneously during the electroplating process to improve the flatness of the heat dissipation member.
실시예 1의 각 공정 파라미터는 하기 표와 같다.Each process parameter of Example 1 is shown in the table below.
실시예 2Example 2
본 발명의 실시예에서 제공하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법은 하기 단계를 포함한다.The method for manufacturing a heat dissipation member made of highly flexible graphite or graphene material provided in an embodiment of the present invention includes the following steps.
1) 흑연 또는 그래핀 원료를 플라즈마 세정기에 넣고 플라즈마 세정을 수행하며, 플라즈마 세정기의 압력은 2MPa, 전력은 550-600W, 시간은 30분이다.1) Graphite or graphene raw materials are placed in a plasma cleaner and plasma cleaning is performed. The pressure of the plasma cleaner is 2MPa, the power is 550-600W, and the time is 30 minutes.
2) 중량%를 기준으로, 황산 16%, OP-10 계면활성제 0.2%, 도데실 황산나트륨 0.2%, 나머지는 물인 활성제를 포함한 제조 재료를 취한다.2) Based on weight percent, manufacturing materials are taken including 16% sulfuric acid, 0.2% OP-10 surfactant, 0.2% sodium dodecyl sulfate, and the remainder being water.
3) 상기 활성제 성분을 혼합하여 활성제를 제조하고, 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정한다.3) The activator ingredients are mixed to prepare an activator, and the graphite or graphene raw material is continuously cleaned using the activator.
4) 탈이온수로 계속해서 흑연 또는 그래핀 원료를 세정한다.4) Continue cleaning the graphite or graphene raw material with deionized water.
5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 2회 수행하여 구리 필름층을 형성한다.5) Electroplating is performed twice on the surface of the graphite or graphene raw material to form a copper film layer.
6) 표면에 구리 필름층이 전기도금된 흑연 또는 그래핀 원료는 탈이온수를 사용하여 계속해서 세정한다.6) Graphite or graphene raw materials with a copper film layer electroplated on the surface are continuously cleaned using deionized water.
7) 먼저 구리 필름층이 도금된 흑연 또는 그래핀 원료를 5g/L 톨리트리아졸 용액에 20-30초 동안 침지시켜 구리 필름층 상에 제1층 보호 필름을 형성한 후, 다시 0.5g/L의 세틸피리디늄 브로마이드 용액에 20-30초간 넣어 구리 필름층 상에 제2층 보호 필름을 형성하여, 구리 필름층 변색을 효과적으로 방지한다.7) First, the graphite or graphene raw material on which the copper film layer was plated was immersed in a 5g/L tolytriazole solution for 20-30 seconds to form a first layer protective film on the copper film layer, and then again 0.5g/L. It is placed in the cetylpyridinium bromide solution of L for 20-30 seconds to form a second layer protective film on the copper film layer, effectively preventing discoloration of the copper film layer.
8) 구리 필름층을 전기도금한 흑연 또는 그래핀 원료를 건조시킨다.8) Dry the graphite or graphene raw material on which the copper film layer was electroplated.
상기 내용을 요약하면, 상기 실시예에서 제공하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법은, 종래 기술과 비교할 때 다음의 장점이 있다. 즉, 구리 필름층을 전기도금할 때 먼저 흑연 또는 그래핀 원료를 플라즈마 세정기에 넣고 플라즈마 세정을 수행한 후, 황산, OP-10 계면활성제 및 도데실 황산나트륨로 배합된 활성제를 사용하여 흑연 또는 그래핀 표면을 처리한다. 황산은 흑연 또는 그래핀 원료의 오일 얼룩을 씻어낼 수 있고, OP-10 계면활성제는 흑연 또는 그래핀 원료의 표면 평활성을 향상시키며, 도데실 황산나트륨은 흑연 또는 그래핀의 분산성을 증가시키고 흑연 또는 그래핀 원료 표면 평활성을 더욱 향상시킨다. 따라서 전기도금된 구리 필름층의 결합 품질이 우수하고 균일해져 제조된 방열 부재의 유연성이 강화되며, 방열 부재 표면에 주름이 쉽게 생기지 않는다. 또한 방열 부재의 방열 및 내산 성능과 내염기 성능이 향상된다. 흑연 또는 그래핀 원료에 구리 필름층을 전기도금한 후, 먼저 구리 필름층이 도금된 흑연 또는 그래핀 원료를 5g/L의 톨리트리아졸 용액에 20-30초간 침지하여 구리 필름층 상에 제1층 보호 필름을 형성한 후 다시 0.5g/L의 세틸피리디늄 브로마이드 용액에 20-30초간 넣어 구리 필름층 상에 제2층 보호 필름을 형성하여 구리 필름층 변색을 효과적으로 방지한다.To summarize the above, the method for manufacturing a heat dissipation member made of highly flexible graphite or graphene material provided in the above embodiment has the following advantages compared to the prior art. That is, when electroplating a copper film layer, graphite or graphene raw materials are first placed in a plasma cleaner, plasma cleaning is performed, and then an activator mixed with sulfuric acid, OP-10 surfactant, and sodium dodecyl sulfate is used to produce graphite or graphene. Treat the surface. Sulfuric acid can wash away oil stains on graphite or graphene raw materials, OP-10 surfactant improves the surface smoothness of graphite or graphene raw materials, and sodium dodecyl sulfate increases the dispersibility of graphite or graphene and increases the dispersibility of graphite or graphene raw materials. Further improves the surface smoothness of graphene raw materials. Therefore, the bonding quality of the electroplated copper film layer is excellent and uniform, thereby enhancing the flexibility of the manufactured heat dissipation member, and wrinkles do not easily form on the surface of the heat dissipation member. Additionally, the heat dissipation, acid resistance, and base resistance performance of the heat dissipation member are improved. After electroplating a copper film layer on a graphite or graphene raw material, the graphite or graphene raw material on which the copper film layer was plated was first immersed in a 5 g/L tolytriazole solution for 20-30 seconds to deposit on the copper film layer. After forming the first layer protective film, it is placed in a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer protective film on the copper film layer, effectively preventing discoloration of the copper film layer.
상기 내용은 본 발명의 비교적 바람직한 구체적인 실시예에 불과하나, 본 발명의 보호 범위는 이에 한정되지 않는다. 본 발명이 개시하는 기술적 범위 내에서 당해 기술 분야에 정통한 자가 본 발명의 기술적 해결책 및 그 발명의 사상에 따라 수행한 균등한 대체 또는 변경은 모두 본 발명의 보호 범위에 포함된다.The above is only a relatively preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent replacement or change made by a person skilled in the art according to the technical solution and idea of the present invention within the technical scope disclosed by the present invention is included in the protection scope of the present invention.
Claims (7)
하기의 단계,
1) 흑연 또는 그래핀 원료에 대해 플라즈마 세정을 수행하는 단계;
2) 중량%를 기준으로, 황산 10-20%, OP-10 계면활성제 0.05-1%, 도데실 황산나트륨(sodium dodecyl sulfate) 0.05-1%, 나머지는 물인 활성제를 포함한 제조 재료를 취하는 단계;
3) 상기 활성제 성분을 혼합하여 활성제를 제조하고, 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정하는 단계;
4) 탈이온수로 계속해서 흑연 또는 그래핀 원료를 세정하는 단계;
5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 수행하여 구리 필름층을 형성하는 단계;
6) 표면에 구리 필름층이 전기도금된 흑연 또는 그래핀 원료는 탈이온수를 사용하여 계속해서 세정하는 단계;
7) 침지 방식을 통해 흑연 또는 그래핀 원료 상에 보호 필름을 형성하는 단계;
8) 구리 필름층을 전기도금한 흑연 또는 그래핀 원료를 건조시키는 단계;를 포함하는 것을 특징으로 하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법.In the method of manufacturing a heat dissipation member made of highly flexible graphite material or graphene material,
The following steps,
1) performing plasma cleaning on graphite or graphene raw material;
2) Taking manufacturing materials including activators that are 10-20% by weight sulfuric acid, 0.05-1% OP-10 surfactant, 0.05-1% sodium dodecyl sulfate, and the remainder is water;
3) mixing the activator components to prepare an activator and continuously cleaning the graphite or graphene raw material using the activator;
4) Continuing to wash the graphite or graphene raw material with deionized water;
5) performing electroplating processing on the surface of graphite or graphene raw material to form a copper film layer;
6) continuously washing the graphite or graphene raw material with a copper film layer electroplated on the surface using deionized water;
7) forming a protective film on the graphite or graphene raw material through an immersion method;
8) A method of manufacturing a heat dissipation member made of a highly flexible graphite material or graphene material, comprising the step of drying the graphite or graphene raw material on which the copper film layer was electroplated.
상기 단계 1)에서 흑연 또는 그래핀 원료를 플라즈마 세정기에 거치하여 세정하는 것을 특징으로 하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법.According to paragraph 1,
A method of manufacturing a heat dissipation member made of highly flexible graphite or graphene material, characterized in that in step 1), the graphite or graphene raw material is placed in a plasma cleaner and cleaned.
상기 단계 2)에서, 상기 활성제는 중량%를 기준으로, 황산 12-16%, OP-10 계면활성제 0.05-0.5%, 도데실 황산나트륨 0.05-0.5%, 나머지는 물 성분을 포함하는 것을 특징으로 하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법.According to paragraph 1,
In step 2), the active agent is characterized in that it contains 12-16% by weight of sulfuric acid, 0.05-0.5% of OP-10 surfactant, 0.05-0.5% of sodium dodecyl sulfate, and the remainder is water. Method of manufacturing a heat dissipation member made of highly flexible graphite or graphene material.
상기 단계 2)에서, 상기 활성제는 중량%를 기준으로, 황산 15%, OP-10 계면활성제 0.1%, 도데실 황산나트륨 0.1%, 나머지는 물 성분을 포함하는 것을 특징으로 하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법.According to paragraph 3,
In step 2), the activator is a highly flexible graphite material or graphite, characterized in that it contains 15% by weight of sulfuric acid, 0.1% of OP-10 surfactant, 0.1% of sodium dodecyl sulfate, and the remainder is water. Method of manufacturing fin material heat dissipation member.
상기 단계 5)에서, 전기도금 용액을 통해 흑연 또는 그래핀 원료에 대해 2회 전기도금 가공을 수행하고, 상기 전기도금 용액은 중량%를 기준으로, 구리 이온 5%, 황산 14%, 광택제 0.8%, 보조제 0.06%, 평활제 0.06%, 나머지는 물 성분을 포함하는 것을 특징으로 하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법.According to paragraph 1,
In step 5), electroplating processing is performed twice on the graphite or graphene raw material using an electroplating solution, and the electroplating solution contains 5% copper ions, 14% sulfuric acid, and 0.8% brightener based on weight percent. , a method of manufacturing a heat dissipation member made of highly flexible graphite or graphene material, characterized in that it contains 0.06% of an auxiliary agent, 0.06% of a leveling agent, and the remainder is a water component.
상기 단계 5)에서, 흑연 또는 그래핀 원료를 전기도금 용액으로 제1차 전기도금을 수행하는 경우, 온도는 40도, 시간은 20분이고; 흑연 또는 그래핀 원료를 전기도금 용액으로 제2차 전기도금을 수행하는 경우, 온도는 40도, 시간은 15분인 것을 특징으로 하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법.According to clause 5,
In step 5), when performing the first electroplating of graphite or graphene raw material with an electroplating solution, the temperature is 40 degrees and the time is 20 minutes; When performing secondary electroplating of graphite or graphene raw materials with an electroplating solution, a method of manufacturing a heat dissipation member made of highly flexible graphite or graphene material, characterized in that the temperature is 40 degrees and the time is 15 minutes.
상기 단계 6)에서, 상기 흑연 또는 그래핀 원료는 먼저 5g/L 톨리트리아졸(Tolyltriazole) 용액에 20-30초 동안 침지시켜 제1층 보호 필름을 형성한 후, 다시 0.5g/L의 세틸피리디늄 브로마이드(cetylpyridinium bromide) 용액에 20-30초 동안 넣어 제2층 보호 필름을 형성하는 것을 특징으로 하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법.According to paragraph 1,
In step 6), the graphite or graphene raw material is first immersed in a 5 g/L tolyltriazole solution for 20-30 seconds to form a first layer protective film, and then again in 0.5 g/L of cetyl. A method of manufacturing a heat dissipation member made of highly flexible graphite or graphene material, characterized in that it is placed in a pyridinium bromide (cetylpyridinium bromide) solution for 20-30 seconds to form a second layer protective film.
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