JP4930986B2 - カーボンナノチューブの製造方法 - Google Patents
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- JP4930986B2 JP4930986B2 JP2006253390A JP2006253390A JP4930986B2 JP 4930986 B2 JP4930986 B2 JP 4930986B2 JP 2006253390 A JP2006253390 A JP 2006253390A JP 2006253390 A JP2006253390 A JP 2006253390A JP 4930986 B2 JP4930986 B2 JP 4930986B2
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- carbon nanotubes
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 130
- 239000002041 carbon nanotube Substances 0.000 title claims description 122
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims description 121
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 229910052751 metal Inorganic materials 0.000 claims description 67
- 239000002184 metal Substances 0.000 claims description 67
- 239000000758 substrate Substances 0.000 claims description 64
- 238000000034 method Methods 0.000 claims description 58
- 239000003054 catalyst Substances 0.000 claims description 50
- 238000005229 chemical vapour deposition Methods 0.000 claims description 40
- 229910045601 alloy Inorganic materials 0.000 claims description 35
- 239000000956 alloy Substances 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000002079 double walled nanotube Substances 0.000 claims description 24
- 239000002109 single walled nanotube Substances 0.000 claims description 23
- 239000012298 atmosphere Substances 0.000 claims description 22
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 229910017060 Fe Cr Inorganic materials 0.000 claims description 7
- 229910002544 Fe-Cr Inorganic materials 0.000 claims description 7
- 229910003271 Ni-Fe Inorganic materials 0.000 claims description 4
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 4
- 238000005275 alloying Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 239000000463 material Substances 0.000 description 15
- 238000000059 patterning Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- 235000012431 wafers Nutrition 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 239000010409 thin film Substances 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000001307 helium Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 150000001722 carbon compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000004050 hot filament vapor deposition Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- -1 ethylene, propylene, acetylene Chemical group 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 230000001771 impaired effect Effects 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- UBAZGMLMVVQSCD-UHFFFAOYSA-N carbon dioxide;molecular oxygen Chemical compound O=O.O=C=O UBAZGMLMVVQSCD-UHFFFAOYSA-N 0.000 description 2
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910001026 inconel Inorganic materials 0.000 description 2
- 238000001459 lithography Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 229910001120 nichrome Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000000609 electron-beam lithography Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000000981 high-pressure carbon monoxide method Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- KWUUWVQMAVOYKS-UHFFFAOYSA-N iron molybdenum Chemical compound [Fe].[Fe][Mo][Mo] KWUUWVQMAVOYKS-UHFFFAOYSA-N 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000002174 soft lithography Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Description
Kenji Hata et al, Water-Assisted Highly Efficient Synthesis of Impurity-Free Single-Walled Carbon Nanotubes, SCIENCE, 2004.11.19, vol.306, p.1362-1364
ンナノチューブを大量且つきわめて安価に製造することができる技術を提供することを課題としている。
Pa以上3×105Pa(3大気圧)以下がさらに好ましく、5×10Pa以上9×10
Pa以下が特に好ましい。
コストについて調べた。その結果を表1に示す。
*配向カーボンナノチューブ・バルク集合体中のカーボンナノチューブ(フィラメント)の品質はラマン分光を測定することにより評価できる。ラマンGバンドとDバンドについて調べた。Dバンドは小さいことより、欠陥が少ない、高品質の良いグラファイト層が存在することがわかる。
雰囲気(ガス)(Pa):ヘリウム、水素混合ガス;供給速度1000sccm
圧力1大気圧
水蒸気添加量(ppm):150ppm
反応温度(℃):750℃
反応時間(分):10分
金属触媒(存在量):鉄薄膜;厚さ1nm
基板:材料は表1に記載(膜厚0.3mm)
なお、基板上への触媒の配置はスパッタ蒸着装置を用いた。
ューブ選択性(多層カーボンナノチューブの発現)、という問題があったりするため、さらに材料選定に検討を要することを確認した。
囲気中での基板の耐久性)を○、△、×で示す。
成された二層配向カーボンナノチューブ・バルク集合体の像を示す平面図、(b)は該二層カーボンナノチューブ・バルク集合体を斜め上方向からやや拡大して示す走査電子顕微鏡図、(c)は(b)の四角形で囲んだ部分を拡大して示す走査電子顕微鏡図、(d)は該二層カーボンナノチューブ・バルク集合体を水溶液に分散し、透過型電子顕微鏡(TEM)で観察した顕微鏡像を示す図、(e)は(d)の拡大図である。
以下の条件において、CVD法により配向カーボンナノチューブ・バルク集合体を成長させた。
雰囲気(ガス)(Pa):ヘリウム、水素混合ガス;供給速度1000sccm
圧力1大気圧
水蒸気添加量(ppm):150ppm
反応温度(℃):750℃
反応時間(分):10分
金属触媒(存在量):鉄薄膜;厚さ1nm
基板:実施例1〜7はそれぞれ表2に示す組成のNiCr、
Inconel(登録商標) 601、YEF50、
YEF426、SUS310S
なお、基板上への触媒の配置はスパッタ蒸着装置を用い、厚さ1nmの鉄金属を蒸着することにより行った。
以下の条件において、CVD法により二層配向カーボンナノチューブ・バルク集合体を成長させた。
雰囲気(ガス)(Pa):ヘリウム、水素混合ガス;供給速度1000sccm
圧力1大気圧
水蒸気添加量(ppm):150ppm
反応温度(℃):750℃
反応時間(分):10分
金属触媒(存在量):鉄薄膜;厚さ1.8nm
基板:表2に示す組成のYEF426のカーソードグリッド
なお、基板上への触媒の配置はスパッタ蒸着装置を用い、厚さ1.8nmの鉄金属を蒸着することにより行った。
上記実施例において、基板として、表2のNi、SUS304、SUS430、Feを用いた以外は同様にして配向カーボンナノチューブ・バルク集合体を得た。
Claims (7)
- 金属触媒を備え、Ni20原子%以上を含有するNi基合金を用いてなる金属基板上に該金属触媒の存在下に単層カーボンナノチューブを化学気相成長(CVD)させる方法を用い、反応雰囲気下に複数の単層カーボンナノチューブを成長させることを特徴とするカーボンナノチューブの製造方法。
- 金属触媒を備え、Ni20原子%以上を含有するNi基合金を用いてなる金属基板上に該金属触媒の存在下に二層カーボンナノチューブを化学気相成長(CVD)させる方法を用い、反応雰囲気下に複数の二層カーボンナノチューブを成長させることを特徴とするカーボンナノチューブの製造方法。
- 金属触媒を備え、Ni20原子%以上を含有するNi基合金を用いてなる金属基板上に該金属触媒の存在下にカーボンナノチューブを化学気相成長(CVD)させる方法を用い、反応雰囲気下に複数の単層カーボンナノチューブと二層及び三層カーボンナノチューブが混在したカーボンナノチューブを成長させることを特徴とするカーボンナノチューブの製造方法。
- 金属触媒を備え、Ni20原子%以上を含有するNi基合金を用いてなる金属基板上に該金属触媒の存在下に単層カーボンナノチューブを化学気相成長(CVD)させる方法を用い、反応雰囲気下に複数の単層カーボンナノチューブを配向カーボンナノチューブ・バルク集合体として成長させることを特徴とするカーボンナノチューブの製造方法。
- 金属触媒を備え、Ni20原子%以上を含有するNi基合金を用いてなる金属基板上に該金属触媒の存在下に二層カーボンナノチューブを化学気相成長(CVD)させる方法を用い、反応雰囲気下に複数の二層カーボンナノチューブを配向カーボンナノチューブ・バルク集合体として成長させることを特徴とするカーボンナノチューブの製造方法。
- 金属触媒を備え、Ni20原子%以上を含有するNi基合金を用いてなる金属基板上に該金属触媒の存在下にカーボンナノチューブを化学気相成長(CVD)させる方法を用い、反応雰囲気下に複数の単層カーボンナノチューブと二層及び三層カーボンナノチューブが混在したカーボンナノチューブを配向カーボンナノチューブ・バルク集合体として成長させることを特徴とするカーボンナノチューブの製造方法。
- 前記Ni基合金は、Ni−Fe、Ni−Cr、Ni−Fe−Crよりなる群から選ばれる1種の合金であることを特徴とする請求項1から6のいずれか1項記載のカーボンナノチューブの製造方法。
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JP2010099572A (ja) * | 2008-10-22 | 2010-05-06 | Sumitomo Electric Ind Ltd | 触媒基材およびこれを用いたカーボンナノ構造体の製造方法 |
KR102166230B1 (ko) | 2013-08-01 | 2020-10-15 | 세키스이가가쿠 고교가부시키가이샤 | 전도성 필러 및 그의 제조 방법, 및 전도성 페이스트 및 그의 제조 방법 |
JP6039534B2 (ja) | 2013-11-13 | 2016-12-07 | 東京エレクトロン株式会社 | カーボンナノチューブの生成方法及び配線形成方法 |
KR101756453B1 (ko) * | 2014-01-09 | 2017-07-10 | 주식회사 제이오 | 다중벽 탄소나노튜브 합성을 위한 촉매, 그 촉매의 제조 방법 및 그 촉매로 합성된 다중벽 탄소나노튜브 |
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