単層カーボンナノチューブ Single-Walled Carbon Nanotubes 電子顕微鏡観察と分光 Electron Microscopy & Spectroscopy
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1 Molecular Thermo-Fluid Engineering 1 単層カーボンナノチューブ Single-Walled Carbon Nanotubes 電子顕微鏡観察と分光 Electron Microscopy & Spectroscopy Diameter (nm) units) Intensity (arb Raman Shift (cm 1 ) Raman Shift (cm 1 ) 5 nm 丸山茂夫 Shigeo Maruyama 東京大学大学院工学系研究科機械工学専攻 TEM 1keV SEM 1keV Al K eV C 1s 84.5eV Length, Wavelength and Energy Scale HeNe 633nm Ar YAG 488nm 164nm ArF 193nm G 159cm 1 Raman Ar 1.67x1 1 J RBM cm 1 H H 3.18meV C C.4meV BS 1GHz Microw ave.45ghz Docomo 8MHz K sun Planck 6K kev 1 6 Absorb. (7,5) SWNT PLE XPS absorb. ev mev UHF 13ch 473MHz TokyoFM 8MHz TV 1 1ch 93 19MHz Energy (J) Temperature (K) Energy (ev) NHK Radio 594KHz THz GHz Frequency (Hz) Wavenumber (cm 1 ) Å nm m mm m Length (m) 1
2 ArF 193nm HeNe 633nm Ar 488nm Length, Wavelength and Energy Scale YAG 164nm G 159cm 1 Raman RBM cm sun Planck 3K 6K 1 5 (7,5) PLE Absorb. ev Energy (J) Temperature (K) Energy (ev) Frequency y( (Hz) Wavenumber (cm 1 ) m Length (m) ArF 193nm Length, Wavelength and Energy Scale 3 Ar 488nm HeNe 633nm YAG 164nm G 159cm 1 Raman sun 6K Planck (7,5) PLE ev Absorb K Energy (J) Temperature (K) Energy (ev) Frequency y( (Hz) Wavenumber (cm 1 ) m Length (m)
3 Characterization of Carbon Nanotubes Electron Microscopy Transmission Electron Microscopy (TEM) Scanning Electron Microscopy (SEM) Scanning Transmission Electron Microscopy (STEM) Scanning Probe Microscopy Atomic Force Microscopy (AFM) Scanning Tunneling Microscopy (STM) Optical Spectroscopy Resonant Raman Scattering Absorption Spectroscopy (UV-Vis-NIR) Fluorescence Spectroscopy X-ray X-ray diffraction X-ray photoelectron spectroscopy (XPS, ESCA) Transmission Electron Spectroscopy 透過型電子顕微鏡 (TEM) 高分解能像 (Phase contrast) 電子線回折 (Electron diffraction) 電子線分光 (EELS, Electron energy loss spectroscopy) 末永和知, カーボンナノチューブの基礎と応用, 培風館 3
4 Transmission Electron Spectroscopy Phase Contrast Diffraction EELS 末永和知, カーボンナノチューブの基礎と応用, 培風館 TEM Images of Carbon Nanotubes S.Iijima, Nature, 354, pp (1991). 4
5 TEM Pictures of SWNT Ropes 5 nm By ACCVD About 1 SWNTs Individual tube diameter: 1.3 nm Spacing:.34 nm Misalignments and Terminations TEM from Smalley et al. at Rice University HRTEM images of DWNTs & TWNTs バンドルの DWNTs ( 直径分布は 1~nm) nm Bundles of DWNTs nm N. Shinohara s Powerpoint 5
6 Peapods Shinohara, 培風館 Peapod with 84 Suenaga et al., PRL 3 Scanning Electron Spectroscopy Hitachi S48, 日立ハイテク HP より 6
7 Images of As-Grown Sample Vertically Aligned SWNTs on Quartz Substrate Y. Murakami, S. Chiashi, Y. Miyauchi, M. Hu, M. Ogura, T. Okubo, S. Maruyama, Chem. Phys. Lett. 385 (4) 98 7
8 STEM Image of Vertically Aligned SWNTs Amorphous Carbon Support Substrate 15 nm Slice by FIB Scanning Probe Microscopy 中山喜萬, カーボンナノチューブの基礎と応用, 培風館 8
9 SWNTs Directly Generation on the AFM Stage isolated SWNT (not bundle) length : 1 15 nm diameter : 1.3. nm density : 1 m - Height (nm) Position (nm) AFM image of SWNTs directly grown on silicon. STM Image of Individual Atoms 9
![] Absorption Spectra c (a) On quartz As Grown Energ gy [ev] c1 E 11 v1 E Ab bsorbance (arb.](/docs-images/94/119474061/images/10-0.jpg "unit) (c) HiPco Isolated (b) On zeolite Isolated Energy Se paration (ev) 3 1 v DOS (d) HiPco Bundle 5")
10 ] Absorption Spectra c (a) On quartz As Grown Energ gy [ev] c1 E 11 v1 E Ab bsorbance (arb. unit) (c) HiPco Isolated (b) On zeolite Isolated Energy Se paration (ev) 3 1 v DOS (d) HiPco Bundle Wavelength (nm) Nanotube Diameter (nm) Resonance Raman Spectra of SWNTs A.M. Rao et al, Science 75 (1997) 187 RBM (Radial breathing Mode) 1-4cm -1 d -1 t G-Band, (Graphite) cm -1, Splitting d - t BWF (Breit-Wigner-Fano) peaks d -1 t cm -1, Metallic SWNT D-band, (Disorder) depends on d t cm -1, depends on E laser Diameter Selective BWF Electronic density of states 5 15 [cm -1 ] 1 1
11 ラマン分光装置 AFM/STM Micro and Macro Raman Raman Scattering (Excitation 488nm) 48 d nm) ( cm ( 1 ) Diameter (nm) G band (Tangential Mode) Radial Breathing Mode (RBM) Inte ensity (arb. units) Raman Shift (cm 1 ) CCVD 8 D band laser Raman Shift (cm 1 ) 11
12 Kataura Plot E / d M 11( dt ) 6acc t E / d S 11( d t ) acc t ) of States (states/1c atom/ev) Density 1 (5,5) E E 11 (1,1) (1,) (17,) Energy (ev) Energy Sepa aration (ev) 3.54 ±.1eV 1 E S 11 E S E M 11 =.9 ev, a cc =.144nm 1 Nanotube Diameter (nm) Raman Spectra aration (ev) Energy Sepa b.units) Intensity(arb Nanotube Diameter (nm) nm nm 633 nm (a) On quartz (b) On zeolite (c) HiPco (d) On quartz Raman Shift (cm 1 ) (e) On zeolite (f) HiPco (i) HiPco 488 nm nm 633 nm Inten nsity (arb.units) 488 nm (a) ACCVD on quartz (b) ACCVD on zeolite * * (g) On quartz (c) HiPco * * (h) On zeolite * * Raman Shift (cm 1 ) 1
13 Kataura Plot 市田正夫, 中村新男, カーボンナノチューブの基礎と応用, 培風館 Resonance Raman spectroscopy En nergy Separation (ev) 3 1 Tight Binding LDA empirical TB Nanotube Diameter (nm) Energy Separa ation (ev) RBM (7,5) (7,6) Observed RBM (1,3) Calculated RBM Raman shift (cm 1 ) d 3.5 /( 1.5) 13
14 Optical absorption and Raman RBM Absorbance (arb.units s) A (a) 85 C (b) 75 C (c) 65 C (d) HiPco Inte ensity (arb.units) Diameter (nm) by d = 48/ Diameter (nm) by d = 3.5/( 1.5) B (a) 85 C (b) 75 C (c) 65 C (d) HiPco Wavelength (nm) Absorption of Isolated SWNTs Raman Shift (cm 1 ) Raman RBM of as grown samples Band Gap Fluorescence Strong Sonication 6min DOS (1,5) DO 1.1g /cm3 SDS or NaDDBS c Energy [ev] c 1 fluorescence v 1 absorption 1.g / cm3 v Density of Electronic States (arb. units) Centrifugation,67g x 4h Centrifugation 18,g x 1h M. J. O Connell et al., Science 97 () 593 InGaAs Detector S. M. Bachilo et al., Science 98 ()
15 Comparison of ACCVD and HiPco (1,) (1,1) (9,4) (1,5) (11,3) (8,7) (8,6) (8,3) (8,6) (9,5) (7,5) (7,6) (6,5) (7,5) (7,6) (8,4) (1,3) (11,1) (a) ACCVD 85 (b) HiPco Photoluminescence from Individual Nanotube 45 5 m 9 rb. units) PL Intensity (ar 1..5 exp fit I PL p(θ) µ 135 µ:dipole moment p:light polarization θ :angle of light polarization and dipole Excitation Polarization (degrees) Strong polarized emission: ideal 1D electronic structure 18 Collaboration with K. Matsuda (KAST, Saeki Group) (4) 15
16 XPS 日東分析センタ HP より, Demonstration of Root Growth and Yield by XPS Root Side Co:.5 at%, Mo:.3 at% C: 91.3 at%, O: 8.69 at% C/M=114, (1,1) x 5 m =813,5 atoms C/M = 71 Metal of 1.3 nm = 3 atoms Removed & Left Co:.41 at%, Mo:.15 at% C: at%, O: 79.8 at% C/M=197,3 Co:.4 at%, Mo:.1 at% C: at%, O: 1.9 at% Tip Side Hatas s SuperGrowth.13Fe Supergrowth:5, wt% Acknowledgement to Shimazu for the use of KRATOS (AXIS-NOVA) 16
17 X-Ray Diffraction SWNTs 触媒金属 真庭豊, カーボンナノチューブの基礎と応用, 培風館 17
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