KR20230036941A - 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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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 92
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 84
- 239000010439 graphite Substances 0.000 title claims abstract description 84
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 59
- 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 33
- 239000012190 activator Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 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 13
- 239000007770 graphite material Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract 2
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 8
- 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
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 3
- 229910001431 copper ion Inorganic materials 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- 239000013543 active substance 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
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000002791 soaking Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 43
- 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
- 239000002253 acid Substances 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 238000005282 brightening Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification 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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- 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
-
- 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
-
- 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
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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
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- 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
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- 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Electroplating Methods And Accessories (AREA)
- Inorganic Chemistry (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
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Abstract
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 parts made of graphite or graphene, and more particularly, to a method for manufacturing a heat dissipating 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 a hexagonal structure with sp 2 hybridized orbitals to form a honeycomb lattice. Graphite has very good thermal conductivity, and the thermal conductivity of pure defect-free single-layer graphite is 5300 W/mK. It is a carbon material with the highest thermal conductivity to date, higher than that of single-walled carbon nanotubes (3500 W/mK) and multi-walled carbon nanotubes (3000 W/mK). When used as a carrier, the thermal conductivity coefficient can reach 600W/mK. In addition, the ballistic thermal conductivity of graphite can lower the lower limit of the ballistic thermal 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, various electronic elements all require heat dissipation. When conventional graphite or graphene is applied to heat dissipation of an electronic element, one metal layer is mainly fixed to the surface of the 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.In order to ensure the electroplating quality of the surface metal layer of graphite or graphene material, the surface of graphite or graphene is generally subjected to several cleaning processes before electroplating. After treating the surface of graphite or graphene with OP-10 surfactant in the cleaning process, the bonding effect of the metal layer electroplated on the surface of graphite or graphene is not good, because the smoothness of the surface of graphite or graphene is common, and the thickness becomes non-uniform. This affects the flexibility of the manufactured heat radiating member and tends to cause wrinkles on the surface of the heat radiating 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.An object of the present invention is to provide a method for manufacturing a heat dissipation member made of highly flexible graphite material or graphene material. First, the surface of graphite or graphene is cleaned with plasma, and then the surface of graphite or graphene is treated using an activator formulated with sulfuric acid, OP-10 surfactant, and sodium dodecyl sulfate to make the surface of the material smooth and the graphite or graphene surface It ensures that the bonding quality of the electroplated copper film layer is good and uniform. Through this, the flexibility of the manufactured heat dissipation member is enhanced and wrinkles are not easily formed 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 adopts the following technical solution to provide a method for manufacturing a highly flexible graphite material or graphene material heat dissipation member, which includes the following steps.
1) 흑연 또는 그래핀 원료에 대해 플라즈마 세정을 수행한다.1) Plasma cleaning is performed on a graphite or graphene raw material.
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 취한다.2) Take a preparation material containing 10-20% of sulfuric acid, 0.05-1% of OP-10 surfactant, 0.05-1% of sodium dodecyl sulfate, and the rest by weight of water.
3) 상기 활성제 성분을 혼합하여 활성제를 제조하고, 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정한다.3) An activator is prepared by mixing the activator components, and the graphite or graphene raw material is continuously cleaned using the activator.
4) 탈이온수로 계속해서 흑연 또는 그래핀 원료를 세정한다.4) Continuously rinse the graphite or graphene raw material with deionized water.
5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 수행하여 구리 필름층을 형성한다.5) An electroplating process 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) The graphite or graphene raw material on which a copper film layer is electroplated on the surface is 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 an 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 is electroplated.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution will be 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 cleaned by passing through a plasma cleaner.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution will be 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 sulfuric acid 12-16%, OP-10 surfactant 0.05-0.5%, sodium dodecyl sulfate 0.05-0.5%, and the rest water components, based on weight%.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution will be 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% sulfuric acid, 0.1% OP-10 surfactant, 0.1% sodium dodecyl sulfate, and the rest water components on a weight percent basis.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution will be 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), the graphite or graphene raw material is electroplated twice through the electroplating solution. The electroplating solution contains 5% copper ions, 14% sulfuric acid, 0.8% brightening agent, 0.06% adjuvant, 0.06% leveling agent, and the balance is water, based on weight percent.
상기 기술적 해결책을 더욱 상세하게 설명한다.The above technical solution will be 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.In the case of performing the first electroplating of the graphite or graphene raw material with an electroplating solution, the temperature is 40 degrees and the time is 20 minutes. In the case of performing the second electroplating of the graphite or graphene raw material 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 will be 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 5 g/L Tolyltriazole solution for 20-30 seconds to form a first layer protective film, and then 0.5 g/L 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.Taken together, by adopting the above technical solution, the present invention has the following advantageous 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 formulated with sulfuric acid, OP-10 surfactant, and sodium dodecyl sulfate. Sulfuric acid can wash off the oil stains of graphite or graphene raw material, OP-10 surfactant improves the surface smoothness of graphite or graphene raw material, sodium dodecyl sulfate increases the dispersibility of graphite or graphene, and graphite or graphene or Graphene raw material surface smoothness is further improved. Therefore, the bonding quality of the electroplated copper film layer is excellent and uniform, so that the flexibility of the manufactured heat radiating member is enhanced, and wrinkles are not easily formed on the surface of the heat radiating member. In addition, heat dissipation and acid resistance performance and salt 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 the copper film layer on the graphite or graphene raw material, first, the graphite or graphene raw material plated with the copper film layer is immersed in a 5 g / L tolytriazole solution for 20-30 seconds to obtain copper After forming the first layer protective film on the film layer, put it 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 to effectively prevent 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.In the following, exemplary embodiments of the present invention are described in more detail. Although exemplary embodiments of the present invention have been shown, it should be understood that the present invention may be implemented in various forms without being limited by the embodiments described herein. On the other hand, these embodiments are provided to more thoroughly understand the present invention and sufficiently convey the scope of the present invention to those skilled in the art to which the present invention belongs.
실시예 1Example 1
본 발명의 실시예에서 제공하는 고유연성 흑연 재질 또는 그래핀 재질 방열 부재 제조 방법은 하기 단계를 포함한다.The method of 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) Plasma cleaning is performed by putting the graphite or graphene raw material into a plasma cleaner, the pressure of the plasma cleaner is 2MPa, the power is 550-600W, and the time is 30 minutes.
2) 황산 15%, OP-10 계면활성제 0.1%, 도데실 황산나트륨 0.1%, 나머지는 물인 중량%의 활성제를 포함한 제조 재료를 취한다.2) Take a preparation material containing 15% of sulfuric acid, 0.1% of OP-10 surfactant, 0.1% of sodium dodecyl sulfate, and the rest by weight of an activator with water.
3) 상기 활성제 성분을 혼합하여 활성제를 제조하고, 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정한다.3) An activator is prepared by mixing the activator components, and the graphite or graphene raw material is continuously cleaned using the activator.
4) 탈이온수로 계속해서 흑연 또는 그래핀 원료를 세정한다.4) Continuously rinse the graphite or graphene raw material with deionized water.
5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 2회 수행하여 구리 필름층을 형성한다.5) An electroplating process 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) The graphite or graphene raw material on which a copper film layer is electroplated on the surface is 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 is plated is immersed in a 5 g/L tolytriazole solution for 20-30 seconds to form a first layer protective film on the copper film layer, and then again 0.5 g/L tolytriazole solution. L into the cetylpyridinium bromide solution for 20-30 seconds to form a second 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 is 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, primary electroplating is performed on a graphite or graphene raw material using an electroplating solution. Secondary electroplating is then performed on the graphite or graphene raw material using the electroplating solution. The electroplating solution contains 5% copper ions, 14% sulfuric acid, 0.8% brightening agent, 0.06% adjuvant, 0.06% leveling agent, balance by weight of water. During the electroplating process, pickling is performed simultaneously to make the heat dissipation member excellent in flatness.
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 of 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) Plasma cleaning is performed by putting the graphite or graphene raw material into a plasma cleaner, the pressure of the plasma cleaner is 2MPa, the power is 550-600W, and the time is 30 minutes.
2) 황산 16%, OP-10 계면활성제 0.2%, 도데실 황산나트륨 0.2%, 나머지는 물인 중량%의 활성제를 포함한 제조 재료를 취한다.2) Take a preparation material containing an activator in weight percent of 16% sulfuric acid, 0.2% OP-10 surfactant, 0.2% sodium dodecyl sulfate, and the balance being water.
3) 상기 활성제 성분을 혼합하여 활성제를 제조하고, 활성제를 사용하여 흑연 또는 그래핀 원료를 계속해서 세정한다.3) An activator is prepared by mixing the activator components, and the graphite or graphene raw material is continuously cleaned using the activator.
4) 탈이온수로 계속해서 흑연 또는 그래핀 원료를 세정한다.4) Continuously rinse the graphite or graphene raw material with deionized water.
5) 흑연 또는 그래핀 원료의 표면에 전기 도금 가공을 2회 수행하여 구리 필름층을 형성한다.5) An electroplating process 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) The graphite or graphene raw material on which a copper film layer is electroplated on the surface is 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 is plated is immersed in a 5 g/L tolytriazole solution for 20-30 seconds to form a first layer protective film on the copper film layer, and then again 0.5 g/L tolytriazole solution. L into the 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.
8) 구리 필름층을 전기도금한 흑연 또는 그래핀 원료를 건조시킨다.8) Dry the graphite or graphene raw material on which the copper film layer is 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.Summarizing the above, the method for manufacturing a heat dissipating member made of highly flexible graphite material 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, first, a graphite or graphene raw material is put into a plasma cleaner, plasma cleaning is performed, and then graphite or graphene is formed using an activator formulated with sulfuric acid, OP-10 surfactant, and sodium dodecyl sulfate. treat the surface Sulfuric acid can wash off the oil stains of graphite or graphene raw material, OP-10 surfactant improves the surface smoothness of graphite or graphene raw material, sodium dodecyl sulfate increases the dispersibility of graphite or graphene, and graphite or graphene or Graphene raw material surface smoothness is further improved. Therefore, the bonding quality of the electroplated copper film layer is excellent and uniform, so that the flexibility of the manufactured heat radiating member is enhanced, and wrinkles are not easily formed on the surface of the heat radiating member. In addition, heat dissipation and acid resistance performance and salt resistance performance of the heat dissipation member are improved. After electroplating the copper film layer on the graphite or graphene raw material, first, the graphite or graphene raw material plated with the copper film layer is immersed in a 5 g/L tolytriazole solution for 20-30 seconds to remove the copper film layer. After forming the first-layer protective film, put it in a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second protective film on the copper film layer to effectively prevent 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 protection scope of the present invention is not limited thereto. Within the technical scope disclosed in the present invention, all equivalent replacements or modifications made by a person skilled in the art according to the technical solutions of the present invention and the spirit of the present invention shall be included in the protection scope of the present invention.
Claims (7)
하기의 단계,
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) 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 highly flexible graphite material or graphene material heat dissipation member,
the following steps,
1) performing plasma cleaning on a graphite or graphene raw material;
2) taking a manufacturing material containing an activator in weight percent of 10-20% sulfuric acid, 0.05-1% OP-10 surfactant, 0.05-1% sodium dodecyl sulfate, and the balance being water;
3) preparing an activator by mixing the activator components, and continuously cleaning the graphite or graphene raw material using the activator;
4) continuously washing the graphite or graphene raw material with deionized water;
5) forming a copper film layer by performing an electroplating process on the surface of the graphite or graphene raw material;
6) continuing to clean the graphite or graphene raw material on which the copper film layer is electroplated using deionized water;
7) forming a protective film on the graphite or graphene raw material through an immersion method;
8) drying the graphite or graphene raw material obtained by electroplating the copper film layer; a highly flexible graphite material or graphene material heat dissipation member manufacturing method comprising the.
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 claim 1,
In step 1), a highly flexible graphite material or graphene material heat dissipation member manufacturing method, characterized in that for washing the graphite or graphene raw material in a plasma cleaner.
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 claim 1,
In step 2), the activator comprises 12-16% sulfuric acid, 0.05-0.5% OP-10 surfactant, 0.05-0.5% sodium dodecyl sulfate, and the rest is water, based on weight%. A method for manufacturing a highly flexible graphite material or graphene material heat dissipation member.
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 claim 3,
In step 2), the activator is a highly flexible graphite material or graphite material, characterized in that the active agent contains 15% sulfuric acid, 0.1% OP-10 surfactant, 0.1% sodium dodecyl sulfate, and the rest is water, based on weight%. A method of manufacturing a 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 claim 1,
In step 5), the graphite or graphene raw material is electroplated twice through an electroplating solution, and the electroplating solution contains, by weight, 5% copper ions, 14% sulfuric acid, and 0.8% brightener. , auxiliaries 0.06%, leveling agent 0.06%, the remainder is a highly flexible graphite material or graphene heat dissipation member manufacturing method characterized in that it comprises 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 claim 5,
In step 5), when the first electroplating is performed on the graphite or graphene raw material with an electroplating solution, the temperature is 40 degrees and the time is 20 minutes; When the second electroplating is performed on the graphite or graphene raw material with an electroplating solution, 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 claim 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 0.5 g/L cetyl A method of manufacturing a highly flexible graphite material or graphene material heat dissipation member, characterized in that by putting it in a pyridinium bromide (cetylpyridinium bromide) solution for 20-30 seconds to form a second layer protective film.
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