EP4148165B1 - 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
- Publication number
- EP4148165B1 EP4148165B1 EP21199008.0A EP21199008A EP4148165B1 EP 4148165 B1 EP4148165 B1 EP 4148165B1 EP 21199008 A EP21199008 A EP 21199008A EP 4148165 B1 EP4148165 B1 EP 4148165B1
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- EP
- European Patent Office
- Prior art keywords
- graphite
- graphene
- raw material
- heat dissipation
- graphene raw
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 181
- 229910021389 graphene Inorganic materials 0.000 title claims description 93
- 229910002804 graphite Inorganic materials 0.000 title claims description 91
- 239000010439 graphite Substances 0.000 title claims description 91
- 230000017525 heat dissipation Effects 0.000 title claims description 27
- 238000000034 method Methods 0.000 title claims description 27
- 239000000463 material Substances 0.000 title claims description 20
- 239000002994 raw material Substances 0.000 claims description 58
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 40
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 40
- 238000004140 cleaning Methods 0.000 claims description 40
- 229910052802 copper Inorganic materials 0.000 claims description 40
- 239000010949 copper Substances 0.000 claims description 40
- 238000009713 electroplating Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000012190 activator Substances 0.000 claims description 25
- 239000004094 surface-active agent Substances 0.000 claims description 17
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 14
- 230000001681 protective effect Effects 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 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
- 238000001035 drying Methods 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
- 239000002671 adjuvant Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 229910001431 copper ion Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 3
- 239000010410 layer Substances 0.000 description 44
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- RIRXDDRGHVUXNJ-UHFFFAOYSA-N [Cu].[P] Chemical compound [Cu].[P] RIRXDDRGHVUXNJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- ALKZAGKDWUSJED-UHFFFAOYSA-N dinuclear copper ion Chemical compound [Cu].[Cu] ALKZAGKDWUSJED-UHFFFAOYSA-N 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- XFYHWEFOWCRANA-UHFFFAOYSA-N 1-methylbenzotriazole Chemical compound [C]1=CC=C2N(C)N=NC2=C1 XFYHWEFOWCRANA-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 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
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 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
- 239000002135 nanosheet Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- 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
-
- 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
Definitions
- the present disclosure belong to the field of preparation of parts made of a graphite or graphene material, and relates to a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material.
- Graphite is a two-dimensional carbon nanomaterial presented with hexagonal honeycomb lattices and composed of carbon atoms in sp2 hybrid orbitals. Graphite has a very good thermal conduction performance.
- the pure and defect-free single-layer graphite has thermal conductivity up to 5300 W/mK, and is the carbon material with the highest thermal conductivity so far, and its thermal conductivity is higher than those of a single-walled carbon nanotube (3500 W/mK) and a multi-walled carbon nanotube (3000 W/mK). When it is used as a carrier, the thermal conductivity can also reach 600 W/MK.
- the ballistic thermal conductivity of graphite can lower the lower limit of the ballistic thermal conductivity of a carbon nanotube of unit circumference and length.
- CN109748267 discloses a multi-pass cleaning based preparation method of a graphene heat-dissipating component.
- the preparation method comprises the following processing steps: 1), cleaning a grapheneraw material by using ultrasonic; 2), continuing cleaning the graphene raw material by using an activator, wherein the activator comprises 10-20% of sulfuric acid, 0.05-1% of a surfactant and the balance of water; 3), continuing cleaning the graphene raw material by using deionized water; 4), electroplating the graphene raw material to form a copper layer on the surface of graphene raw material;5), continuing cleaning the copper layer-electroplated graphene raw material by using deionized water; 6), continuing to dry the copper layer-electroplated graphene raw material.
- CN108823615 discloses a preparation method of a high-heat-conductivity nanometer copper-graphite film composite material.
- the preparation method comprises the specific steps of: (1) chemical roughening of graphite films; (2) plasma treatment of the roughened graphite films; (3) copper electroplating of the plasma-treated graphite films; and (4) passivation of the graphite film after copper electroplating; and the high-heat-conductivity nanometer copper-graphite film composite material product is obtained through cleaning and drying after passivation.
- CN103943281 describes a preparation method of an electric wire and cable with a copper-graphene complex phase conductive wire core.
- the preparation method includes the steps: preparing copper sulfate, sulfuric acid, surface active agents and hydrochloric acid into copper plating liquid; adding graphene nano-sheets into the copper plating liquid to obtain electroplating liquid containing graphene; taking a phosphor copper sheet as an anode, taking a washed substrate as a cathode, placing the phosphor copper sheet and the substrate into the electroplating liquid for electroplating to obtain a plate with a copper-graphene complex phase plating layer, and rolling and drawing the plate to form the conductive wire core.
- the conductive wire core is prepared by the aid of a copper-graphene complex phase, so that the obtained electric wire and cable is light in weight, high in mechanical strength, fine in conductivity and excellent in oxidation resistance and corrosion resistance.
- the preparation process is simple, the performances of the conductive wire core can be controlled by adjusting an electroplating process, and controllability of the process is high.
- An objective of the present disclosure is to provide a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, which includes the following steps: firstly, plasma cleaning a surface of graphite or graphene, and then treating the surface of graphite or graphene with an activator compounded by sulfuric acid, an OP-10 surfactant and sodium dodecyl sulfate, so that the surface of the material has good smoothness, and it ensures a copper film layer electroplated on the surface of graphite or graphene has good binding quality and uniform, and enhances the flexibility of the prepared heat dissipation component, and the surface of the heat dissipation component is not easy to generate creases.
- a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material including the following steps:
- the graphite or graphene raw material is placed in a plasma cleaning machine for cleaning.
- the activator includes the following components in percentage by weight: 12-16% of sulfuric acid, 0.05-0.5% of an OP-10 surfactant, 0.05-0.5% of sodium dodecyl sulfate, and the balance being water.
- the activator includes the following components in percentage by weight: 15% sulfuric acid, 0.1% of the OP-10 surfactant, 0.1% of sodium dodecyl sulfate, and the balance being water.
- the graphite or graphene raw material is subjected to the electroplating process twice with an electroplating solution, and the electroplating solution includes the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of a brightener; 0.06% of an adjuvant; 0.06% of a leveling agent; and the balance being water.
- the temperature when the graphite or graphene raw material is electroplated with the electroplating solution for the first time, the temperature is 40 celsius degrees and the time is 20 minutes; and when the graphite or graphene raw material is electroplated with the electroplating solution for the second time, the temperature is 40 celsius degrees and the time is 15 minutes.
- the present disclosure has the following beneficial effects.
- This example of the present disclosure provided a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, including the following steps:
- the step 5 it included two electroplating procedures: firstly, the graphite or graphene raw material was subjected to primary electroplating with an electroplating solution; and secondly, the graphite or graphene raw material was subjected to secondary electroplating with the electroplating solution.
- the electroplating solution included the following components in percentage by weight: 5% of copper ions; 14% of sulfuric acid; 0.8% of a brightener; 0.06% of an adjuvant; 0.06% of a leveling agent; and the balance being water.
- pickling could be carried out at the same time, so that the flatness of the heat dissipation component was good.
- Example 1 Various process parameters of Example 1 were shown in the table below: Electroplating process Component name Solution concentration Temperature Time Activation sulfuric acid 15% 25°C 3 minutes Surfactant A (OP-10) 0.10% sodium dodecyl sulfate 0.10% Washing with pure water deionized water 25°C 20 seconds Pre-plating of copper Copper ions 50 g/l 40°C 20 minutes sulfuric acid 14% Additive A (brightener) 0.80% Additive B (adjuvant) 0.06% Additive C (leveling agent) 0.06% Electroplating of copper Copper ions 50 g/l 40°C 15 minutes sulfuric acid 14% Additive A (brightener) 0.80% Additive B (adjuvant) 0.06% Additive C 0.06% (leveling agent) Cleaning with pure water deionized water 25°C 20 seconds Protection 1 methyl benzotriazole 5g/l 25°C 20 seconds Protection 2 cetylpyridinium bromide 0.5g/l 25°C 20
- This example of the present disclosure provided a method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material, including the following steps:
- the method for preparing a heat dissipation component with high flexibility made of a graphite or graphene material as provided by the aforementioned examples has the following advantages.
- the graphite or graphene raw material is firstly placed in a plasma cleaning machine for plasma cleaning, and then the surface of graphite or graphene is treated with an activator compounded by sulfuric acid, the OP-10 surfactant and sodium dodecyl sulfate.
- Sulphuric acid can wash away oil stains from the graphite or graphene raw material
- the OP-10 surfactant improves the smoothness of the surface of the graphite or graphene raw material
- sodium dodecyl sulfate increases the dispersibility of graphite or graphene and further increases the smoothness of the surface of the graphite or graphene raw material, so that the electroplated copper film layer has good binding quality and is uniform, which enhances the flexibility of the prepared heat dissipation component, and the surface of the heat dissipation component is not easy to generate creases, and the heat dissipation and acid and alkali resistance performances of the heat dissipation component are improved.
- the graphite or graphene raw material electroplated with the copper film layer is first soaked in a 5 g/L methyl benzotriazole solution for 20-30 seconds to form a first layer of protective film on the copper film layer, and then put into a 0.5 g/L cetylpyridinium bromide solution for 20-30 seconds to form a second layer of protective film on the copper film layer, which effectively prevents the copper film layer from color changing.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (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)
- Microelectronics & Electronic Packaging (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111020365.7A CN113622007A (zh) | 2021-09-08 | 2021-09-08 | 一种高柔韧性石墨材质或石墨烯材质散热部件制备方法 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP4148165A1 EP4148165A1 (en) | 2023-03-15 |
| EP4148165C0 EP4148165C0 (en) | 2024-04-17 |
| EP4148165B1 true EP4148165B1 (en) | 2024-04-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP21199008.0A Active EP4148165B1 (en) | 2021-09-08 | 2021-09-24 | Method for preparing heat dissipation component with high flexibility made of graphite or graphene material |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20230070481A1 (ja) |
| EP (1) | EP4148165B1 (ja) |
| JP (1) | JP7187069B1 (ja) |
| KR (1) | KR102631465B1 (ja) |
| CN (1) | CN113622007A (ja) |
| TW (1) | TWI777783B (ja) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102647347B1 (ko) * | 2023-05-08 | 2024-03-15 | 가드넥(주) | 표면 활성화된 그라파이트 구리 도금방법 |
Family Cites Families (18)
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|---|---|---|---|---|
| JPH03211292A (ja) * | 1990-01-12 | 1991-09-17 | Hitachi Aic Inc | 金属表面用処理液 |
| JP3673357B2 (ja) * | 1997-01-27 | 2005-07-20 | メルテックス株式会社 | めっき用の前処理洗浄剤 |
| TW201035513A (en) * | 2009-03-25 | 2010-10-01 | Wah Hong Ind Corp | Method for manufacturing heat dissipation interface device and product thereof |
| CN102719866A (zh) * | 2012-06-12 | 2012-10-10 | 河南科技学院 | 一种不锈钢件镀前清洗活化复合剂及其生产工艺 |
| CN104593838A (zh) * | 2013-10-31 | 2015-05-06 | 青岛泰浩达碳材料有限公司 | 石墨粉表面镀铜工艺 |
| CN103943281B (zh) * | 2014-05-09 | 2016-05-04 | 浙江大学 | 一种具有铜-石墨烯复相导电线芯的电线电缆的制备方法 |
| CN104047037B (zh) * | 2014-06-16 | 2015-06-03 | 深圳市联合蓝海科技开发有限公司 | 一种硬化剂 |
| CN104562113A (zh) * | 2014-11-27 | 2015-04-29 | 镇江润德节能科技有限公司 | 一种电镀用清洗除油剂 |
| CN104861794A (zh) * | 2015-04-08 | 2015-08-26 | 安徽豪鼎金属制品有限公司 | 一种丝胶成膜金属表面处理剂 |
| CN105624747B (zh) * | 2015-12-29 | 2017-10-13 | 东莞市莞信企业管理咨询有限公司 | 一种铜/石墨烯复合多层散热膜 |
| JP6844331B2 (ja) | 2016-03-08 | 2021-03-17 | 東洋紡株式会社 | 伸縮性導体形成用ペースト、伸縮性導体シートおよび生体情報計測用プローブ |
| CN109777655A (zh) * | 2017-11-10 | 2019-05-21 | 李静 | 一种多功能除油除锈清洗剂 |
| CN108823615A (zh) * | 2018-05-23 | 2018-11-16 | 嘉兴中易碳素科技有限公司 | 高导热纳米铜—石墨膜复合材料的制备方法 |
| CN109183102B (zh) * | 2018-11-02 | 2021-03-16 | 湖南鋈鎏科技有限公司 | 一种重质粉体的分散脉冲电镀方法 |
| CN109748267B (zh) * | 2019-02-21 | 2021-05-14 | 苏州市安派精密电子有限公司 | 一种基于多道清洗的石墨烯散热部件制备方法 |
| CN110158123B (zh) * | 2019-05-10 | 2021-03-30 | 东北大学 | 一种表面金属化石墨烯及其制备方法 |
| CN110512258B (zh) * | 2019-10-11 | 2021-03-26 | 东莞市慧泽凌化工科技有限公司 | 一种无镍封孔工艺 |
| CN111593388A (zh) * | 2020-06-18 | 2020-08-28 | 江苏格优碳素新材料有限公司 | 一种镀铜石墨膜的制备方法 |
-
2021
- 2021-09-08 CN CN202111020365.7A patent/CN113622007A/zh active Pending
- 2021-09-18 US US17/448,049 patent/US20230070481A1/en active Pending
- 2021-09-21 JP JP2021153318A patent/JP7187069B1/ja active Active
- 2021-09-24 EP EP21199008.0A patent/EP4148165B1/en active Active
- 2021-09-24 KR KR1020210126760A patent/KR102631465B1/ko active IP Right Grant
- 2021-09-24 TW TW110135643A patent/TWI777783B/zh active
Also Published As
| Publication number | Publication date |
|---|---|
| JP7187069B1 (ja) | 2022-12-12 |
| KR102631465B1 (ko) | 2024-01-31 |
| EP4148165C0 (en) | 2024-04-17 |
| EP4148165A1 (en) | 2023-03-15 |
| TWI777783B (zh) | 2022-09-11 |
| CN113622007A (zh) | 2021-11-09 |
| TW202311157A (zh) | 2023-03-16 |
| KR20230036941A (ko) | 2023-03-15 |
| US20230070481A1 (en) | 2023-03-09 |
| JP2023039376A (ja) | 2023-03-20 |
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