JP7427683B2 - 開放式炭素ナノ材料連続成長の装置および作製方法 - Google Patents
開放式炭素ナノ材料連続成長の装置および作製方法 Download PDFInfo
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- JP7427683B2 JP7427683B2 JP2021546443A JP2021546443A JP7427683B2 JP 7427683 B2 JP7427683 B2 JP 7427683B2 JP 2021546443 A JP2021546443 A JP 2021546443A JP 2021546443 A JP2021546443 A JP 2021546443A JP 7427683 B2 JP7427683 B2 JP 7427683B2
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- gas
- cvd
- foil strip
- metal foil
- slit
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 167
- 229910052799 carbon Inorganic materials 0.000 title claims description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 38
- 239000002086 nanomaterial Substances 0.000 title description 45
- 239000007789 gas Substances 0.000 claims description 204
- 239000011888 foil Substances 0.000 claims description 131
- 229910052751 metal Inorganic materials 0.000 claims description 127
- 239000002184 metal Substances 0.000 claims description 127
- 229910021389 graphene Inorganic materials 0.000 claims description 76
- 230000001681 protective effect Effects 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 40
- 239000012159 carrier gas Substances 0.000 claims description 38
- 238000012544 monitoring process Methods 0.000 claims description 37
- 239000002360 explosive Substances 0.000 claims description 35
- 239000002041 carbon nanotube Substances 0.000 claims description 32
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 30
- 238000000576 coating method Methods 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 26
- 238000005498 polishing Methods 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000498 cooling water Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- 239000012495 reaction gas Substances 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 8
- 238000012805 post-processing Methods 0.000 claims description 7
- 238000004891 communication Methods 0.000 claims description 6
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 239000002105 nanoparticle Substances 0.000 claims description 6
- 230000000149 penetrating effect Effects 0.000 claims description 6
- 230000007704 transition Effects 0.000 claims description 6
- 238000013459 approach Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 238000005238 degreasing Methods 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 141
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 27
- 239000011889 copper foil Substances 0.000 description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 20
- 239000010410 layer Substances 0.000 description 16
- 239000000047 product Substances 0.000 description 11
- 239000010453 quartz Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000002356 single layer Substances 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 6
- 238000004880 explosion Methods 0.000 description 6
- 229960002089 ferrous chloride Drugs 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 239000003517 fume Substances 0.000 description 6
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 4
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- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002109 single walled nanotube Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000002048 multi walled nanotube Substances 0.000 description 3
- -1 oxides Chemical class 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 230000003247 decreasing effect Effects 0.000 description 2
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- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000007665 sagging Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical group 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
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- 238000007670 refining Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
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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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
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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
- C01B32/15—Nano-sized carbon materials
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- C01B32/162—Preparation characterised by catalysts
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B32/16—Preparation
- C01B32/164—Preparation involving continuous processes
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4409—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber characterised by sealing means
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- C—CHEMISTRY; METALLURGY
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4412—Details relating to the exhausts, e.g. pumps, filters, scrubbers, particle traps
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- C—CHEMISTRY; METALLURGY
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- C23C16/4418—Methods for making free-standing articles
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45519—Inert gas curtains
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/52—Controlling or regulating the coating process
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/54—Apparatus specially adapted for continuous coating
- C23C16/545—Apparatus specially adapted for continuous coating for coating elongated substrates
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| CN109775690A (zh) * | 2019-03-25 | 2019-05-21 | 杭州英希捷科技有限责任公司 | 一种连续制备碳纳米管阵列的方法 |
| CN109898054A (zh) * | 2019-03-25 | 2019-06-18 | 杭州英希捷科技有限责任公司 | 一种基于碳纳米管阵列的新型芯片热界面材料的制备方法 |
| CN110629191A (zh) * | 2019-11-01 | 2019-12-31 | 北京大学 | 一种石墨烯薄膜卷对卷生产装置及方法 |
| CN111733400B (zh) * | 2020-07-07 | 2024-08-16 | 北京石墨烯技术研究院有限公司 | 石英支架及石英加热装置 |
| CN114433627B (zh) * | 2022-01-26 | 2024-05-17 | 重庆墨希科技有限公司 | 一种连续制备高导电石墨烯金属复合材料的方法及装置 |
| CN115108546B (zh) * | 2022-04-27 | 2024-08-06 | 东南大学 | 一种有机固废高聚物连续制备碳材料联产氢的系统和方法 |
| US20230407469A1 (en) * | 2022-06-17 | 2023-12-21 | Raytheon Technologies Corporation | Continuous atmospheric pressure cvd tow coater process with in-situ air leak monitoring |
| CN116281979B (zh) * | 2022-12-02 | 2024-05-14 | 重庆诺奖二维材料研究院有限公司 | 一种基于双重冷却控温的石墨烯喷火炉 |
| CN116469602A (zh) * | 2023-03-23 | 2023-07-21 | 闪电箭邺(上海)激光科技有限公司 | 一种高导电铜基石墨烯复合材料及其制备装置 |
| CN116332160B (zh) * | 2023-04-07 | 2023-09-12 | 重庆中润新材料股份有限公司 | 一种碳纳米管的合成装置及合成方法 |
| WO2025142961A1 (ja) * | 2023-12-27 | 2025-07-03 | Agc株式会社 | 熱cvd装置およびグラフェンの製造方法 |
| WO2025142960A1 (ja) * | 2023-12-27 | 2025-07-03 | Agc株式会社 | グラフェンの製造方法 |
| WO2025142959A1 (ja) * | 2023-12-27 | 2025-07-03 | Agc株式会社 | 熱cvd装置およびグラフェンの製造方法 |
| JP2025129911A (ja) * | 2024-02-26 | 2025-09-05 | Dowaサーモテック株式会社 | カーボンナノチューブ生成装置およびカーボンナノチューブ製造装置 |
| CN118239476B (zh) * | 2024-03-18 | 2024-10-29 | 无锡松煜科技有限公司 | 一种高纯度单壁碳纳米管的制备方法 |
| CN118343745B (zh) * | 2024-05-14 | 2025-10-28 | 江西铜业技术研究院有限公司 | 一种直流电弧放电制备单/双壁碳纳米管的方法和系统 |
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| JP2004332093A (ja) | 2003-05-08 | 2004-11-25 | Hiroshi Ashida | 連続cvd製造装置 |
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| CN109336096A (zh) | 2019-02-15 |
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| US11473192B2 (en) | 2022-10-18 |
| EP3896033A4 (en) | 2023-03-29 |
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