JP5002960B2 - ナノ構造炭素材料の製造方法、前記製造方法により形成されたナノ構造炭素材料および前記ナノ構造炭素材料を有する基板 - Google Patents
ナノ構造炭素材料の製造方法、前記製造方法により形成されたナノ構造炭素材料および前記ナノ構造炭素材料を有する基板 Download PDFInfo
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- JP5002960B2 JP5002960B2 JP2005515470A JP2005515470A JP5002960B2 JP 5002960 B2 JP5002960 B2 JP 5002960B2 JP 2005515470 A JP2005515470 A JP 2005515470A JP 2005515470 A JP2005515470 A JP 2005515470A JP 5002960 B2 JP5002960 B2 JP 5002960B2
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- 235000015243 ice cream Nutrition 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002527 isonitriles Chemical class 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
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 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
- 229910052763 palladium Inorganic materials 0.000 description 1
- JZRYQZJSTWVBBD-UHFFFAOYSA-N pentaporphyrin i Chemical compound N1C(C=C2NC(=CC3=NC(=C4)C=C3)C=C2)=CC=C1C=C1C=CC4=N1 JZRYQZJSTWVBBD-UHFFFAOYSA-N 0.000 description 1
- 229920011301 perfluoro alkoxyl alkane Polymers 0.000 description 1
- 229920013653 perfluoroalkoxyethylene Polymers 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical class N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- LOAUVZALPPNFOQ-UHFFFAOYSA-N quinaldic acid Chemical compound C1=CC=CC2=NC(C(=O)O)=CC=C21 LOAUVZALPPNFOQ-UHFFFAOYSA-N 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 229910052704 radon Inorganic materials 0.000 description 1
- SYUHGPGVQRZVTB-UHFFFAOYSA-N radon atom Chemical compound [Rn] SYUHGPGVQRZVTB-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000007767 slide coating Methods 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- AYNNSCRYTDRFCP-UHFFFAOYSA-N triazene Chemical compound NN=N AYNNSCRYTDRFCP-UHFFFAOYSA-N 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Images
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Description
(1)基板上に、有機金属化合物を含む溶液を塗布した後、当該有機金属化合物の有機成分を分解除去して金属微粒子を付着させる金属微粒子付着工程と、
大気圧又は大気圧近傍の圧力下で、対向する電極間に少なくとも放電ガスとしてN2ガス、Arガスから選ばれるガスを導入し、前記電極間に高周波電圧を印加することにより放電プラズマを発生させ、ナノ構造炭素材料を形成する原料ガスを前記放電プラズマと共存させて活性化した原料ガスとし、前記金属微粒子が付着した基板を前記活性化した原料ガスに晒すことで、前記基板上にナノ構造炭素材料を形成するナノ構造炭素材料形成工程と、を有し、
前記ナノ構造炭素材料形成工程は、電極温度が400℃以下で行うことを特徴とするナノ構造炭素材料の製造方法。
(2)電極間に印加する電圧が周波数0.5kHz〜100MHzであることを特徴とする(1)に記載のナノ構造炭素材料の製造方法。
(3)少なくとも一方の電極が誘電体で被覆されていることを特徴とする(1)に記載のナノ構造炭素材料の製造方法。
(4)前記電極間に導入するガスの50体積%以上がArガス及び/又はN2ガスであることを特徴とする(1)記載のナノ構造炭素材料の製造方法。
(5)前記ナノ構造炭素材料形成工程は、電極温度が300℃以下で行うことを特徴とする(1)に記載のナノ構造炭素材料の製造方法。
(6)(1)から(5)の何れか1項に記載の製造方法により形成されたことを特徴とするナノ構造炭素材料。
(7)(6)に記載のナノ構造炭素材料が、カーボンナノチューブであることを特徴とするナノ構造炭素材料。
(8)(7)に記載のナノ構造炭素材料を表面に有することを特徴とする基板。
第2図は大気圧プラズマ放電処理装置のガス導入部及び電極部の他の例を示す断面図である。
第3図は大気圧プラズマ放電処理装置の他の例を示す図である。
第4図は大気圧プラズマ放電処理装置の更に他の例を示す図である。
第5図は実施例の金属微粒子付着工程に用いた装置構成を示すモデル図である。
第6図は実施例のナノ構造炭素材料形成工程に用いた装置構成を示すモデル図である。
これらの樹脂基板、複合基板を板型、もしくはフィルム状として用いる。
この例では移動ステージ27が対向する一方の電極を構成し、電源11に接続した2本の電極21a、21bが移動ステージ電極27に各々平行になるように併設されている。電極21a、21b、27は各々、少なくとも一方を誘電体22で被覆されており、その電極21、27間で形成された空間23に電極11により高周波電圧が印加される様になっている。なお、電極21、27の内部は中空構造24を有し、放電中は水、オイルなどによって放電により発生する熱の廃熱を行い、かつ安定な温度に保つための熱交換ができるようになっている。
21a、21bは、金属母材の表面を誘電体22で被覆した誘電体被覆電極である。内部は中空構造24を有し、放電中は、その内部を冷却水、もしくはオイル等を流通させることにより、電極表面温度を一定に制御することができる構成となっている。
印加電源記号 メーカー 周波数 製品名
A1 神鋼電機 3kHz SPG3−4500
A2 神鋼電機 5kHz SPG5−4500
A3 春日電機 15kHz AGI−023
A4 神鋼電機 50kHz SPG50−4500
A5 ハイデン研究所 100kHz* PHF−6k
A6 パール工業 200kHz CF−2000−200k
A7 パール工業 400kHz CF−2000−400k
等の市販のものを挙げることが出来、何れも使用することが出来る。
印加電源記号 メーカー 周波数 製品名
B1 パール工業 800kHz CF−2000−800k
B2 パール工業 2MHz CF−2000−2M
B3 パール工業 13.56MHz CF−5000−13M
B4 パール工業 27MHz CF−2000−27M
B5 パール工業 150MHz CF−2000−150M
等の市販のものを挙げることが出来、何れも好ましく使用出来る。
V1≧IV>V2
または V1>IV≧V2を満たし、前記第2の高周波電界の出力密度が、1W/cm2以上であることが好ましい。
高周波とは、少なくとも0.5kHzの周波数を有するものを言う。
重畳する高周波電界が、ともにサイン波である場合、第1の高周波電界の周波数ω1と該周波数ω1より高い第2の高周波電界の周波数ω2とを重ね合わせた成分となり、その波形は周波数ω1のサイン波上に、それより高い周波数ω2のサイン波が重なった鋸歯状の波形となる。
本発明においては、ナノ構造炭素材料の形成を容易にするために、予め基板上に金属微粒子を付着させる金属微粒子付着工程を経て、該金属微粒子が付着した基板上にナノ構造炭素材料を形成することが好ましい。
本発明の方法においては、ナノ構造炭素材料の形成の際高温にする必要が無いことから、例えば一般的なソーダガラス、低ソーダガラス(無アルカリガラスを含む)やプラスチックといった素材の基板も用いることが可能となる。従って、例えば、今後量産の要請があるフィールドエミッションディスプレイ(FED)用の電子放出源を製造する様な場合、ガラス基板、プラスチック基板にナノ構造炭素材料を形成し得る好適な方法となる。なおフィールドエミッションはディスプレイのほかにも電子線源や微小真空管などのさまざまな応用が期待されている。
(金属微粒子付着工程)
第5図に示す装置構成で基板上に金属微粒子を付着させた。
電極21a、21bとしては、20×20mmで長さ120mmの純Feターゲットを用いた。このターゲットには、保温冷却用シリコンオイルが流れるように穴を貫通させ、角をR3に加工した部材を2本用いた。
第6図に示す装置構成で上記金属微粒子が付着した基板26´上にナノ構造炭素材料を形成させた。
得られた試料について、ラマン散乱スペクトルを測定したところ、共にカーボンナノチューブに特徴的なスペクトル、すなわち、Gバンド(Graphite band;1590cm−1)、Dバンド(Disorder band;1360cm−1)に大きなピークを示すという分析結果が得られた。
(導電性膜を有する基板を用いた実施例)
基板を表面に導電性を持つ薄膜を有するものに変えた以外は、金属微粒子付着工程、ナノ炭素構造体材料形成工程を実施例1同様に逐次実施した。この結果においても、前記実施例とほぼ同様のカーボンナノチューブ構造の炭素材料ができた。なお、基材上への導電性薄膜形成は以下のように行った。
また、アルミニウムアセチルアセトナートは、容器内を230℃に保ちつつ所定の窒素によりバブリングさせて導入した。
なお、ここではAl膜を用いたが、導電性をもつものであれば何でもよい。
第4図に示す装置構成で実施例1と同様に金属微粒子を付着させた基板上にナノ構造炭素材料を形成させた。
酢酸モリブデン(II)(関東化学社製)と酢酸コバルト(II)四水和物(関東化学社製)をエタノールに溶解し、各0.05質量%の混合溶液を調製した。この溶液に、100mm×100mm×0.5mmの低ソーダガラス(コーニング社製)を浸し、1cm/分の速度で引き上げてディップ塗布を行った。
Claims (8)
- 基板上に、有機金属化合物を含む溶液を塗布した後、当該有機金属化合物の有機成分を分解除去して金属微粒子を付着させる金属微粒子付着工程と、
大気圧又は大気圧近傍の圧力下で、対向する電極間に少なくとも放電ガスとしてN2ガス、Arガスから選ばれるガスを導入し、前記電極間に高周波電圧を印加することにより放電プラズマを発生させ、ナノ構造炭素材料を形成する原料ガスを前記放電プラズマと共存させて活性化した原料ガスとし、前記金属微粒子が付着した基板を前記活性化した原料ガスに晒すことで、前記基板上にナノ構造炭素材料を形成するナノ構造炭素材料形成工程と、を有し、
前記ナノ構造炭素材料形成工程は、電極温度が400℃以下で行うことを特徴とするナノ構造炭素材料の製造方法。 - 電極間に印加する電圧が周波数0.5kHz〜100MHzであることを特徴とする請求項1に記載のナノ構造炭素材料の製造方法。
- 少なくとも一方の電極が誘電体で被覆されていることを特徴とする請求項1に記載のナノ構造炭素材料の製造方法。
- 前記電極間に導入するガスの50体積%以上がArガス及び/又はN2ガスであることを特徴とする請求項1に記載のナノ構造炭素材料の製造方法。
- 前記ナノ構造炭素材料形成工程は、電極温度が300℃以下で行うことを特徴とする請求項1に記載のナノ構造炭素材料の製造方法。
- 請求項1から5の何れか1項に記載の製造方法により形成されたことを特徴とするナノ構造炭素材料。
- 請求項6に記載のナノ構造炭素材料が、カーボンナノチューブであることを特徴とするナノ構造炭素材料。
- 請求項7に記載のナノ構造炭素材料を表面に有することを特徴とする基板。
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JP2005515470A JP5002960B2 (ja) | 2003-11-17 | 2004-11-08 | ナノ構造炭素材料の製造方法、前記製造方法により形成されたナノ構造炭素材料および前記ナノ構造炭素材料を有する基板 |
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KR20060133975A (ko) | 2006-12-27 |
EP1686092A4 (en) | 2012-03-07 |
JP2010222248A (ja) | 2010-10-07 |
US7485348B2 (en) | 2009-02-03 |
EP1686092A1 (en) | 2006-08-02 |
WO2005047180A1 (ja) | 2005-05-26 |
US20050106094A1 (en) | 2005-05-19 |
KR101158590B1 (ko) | 2012-06-22 |
JPWO2005047180A1 (ja) | 2007-05-31 |
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