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Observation of nano -crystal on carbon nanohorns and analysis of Y-shaped molecules

Observation of nano -crystal on carbon nanohorns and analysis of Y-shaped molecules. Ｍａｒ . 13, 2010. Nano-Structural Characterization Group: (collaboration w/ K. Suenaga) Koshino, Masanori Niimi, Yoshiko Suzuki, Hironori . Contents. Observation of nano -crystals

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Observation of nano -crystal on carbon nanohorns and analysis of Y-shaped molecules

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  1. Observation of nano-crystal on carbon nanohornsand analysis of Y-shaped molecules Ｍａｒ. 13, 2010 Nano-Structural Characterization Group: (collaboration w/ K. Suenaga) Koshino, Masanori Niimi, Yoshiko Suzuki, Hironori

  2. Contents • Observation of nano-crystals • Analysis of nano-crystals A control experiment 1,3,5-tris(P-bromophenyl)benzene

  3. 1-1. Observation of nano-crystals A control experiment The purpose • To confirm whether it is possible to crystallize on amino-NH without Y-molecule modification. Sample information preparation by T. Homma 1. THO-10-012was dispersed in MeOH……(a) 2. A droplet of (a) was put onto a TEM grid with molybdenum mesh pre-coated by lacy carbon films…….(b) 3. We observed (b) the same condition as last time.

  4. 1-2. Observation of nano-crystals helloA helloG helloC helloF helloJ helloR helloN helloO helloS helloW helloT helloX 2nm There were not a material like a crystal. We made “movies” about the images including the molybdenum contrast.

  5. Movie 1-3. Observation of nano-crystals Step 2, width 2 Reconstruction 0.5s helloC helloF helloG helloT helloW helloX 2nm We confirmed the contrast of bromine, but they not piled up in each other. table1.The ratio of contents. Crystal Materials (string-like, others ) No material THO-10-012 90% (15%, 75%) 10% 0% /1728 horns THO-10-002 75% (66%, 9%) 24% 1% /3780 horns

  6. 2-1. Observation of nano-crystals • The purpose • To make clear the process of crystallization of a nano-material. 1,3,5-tris(P-bromophenyl)benzene A crystal Sample information by Mr. Homma, THO-10-002,003 The crystal information _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_gt 0.0354 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 1/2-x,-y,1/2+z 4 1/2+x,1/2-y,-z _cell_length_a 14.4165(3) _cell_length_b 18.9655(4) _cell_length_c 21.9088(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Br 1.21 preparation by T. Homma Sample preparation at AIST 1. Y-shaped molecule(THO-10-002,003)on NH was dispersed in MeOH……(a) 2. A droplet of (a) was put onto a TEM grid with molybdenum mesh pre-coated by lacy carbon films.

  7. 2-2.Analysis of nano-crystals The area of crystals THO-10-002 helloI-22 helloK-7 helloR-5 helloS-9 helloJ-10 100225-11-7C 1nm helloQ-0 helloG02-7 helloA-17 helloF-0506 helloN-2 helloF3-14 helloD-12 helloF2-14 helloG1-19 helloC0-0 100211-11-6B helloJ-00 helloB0-02 helloA-0304 helloC-1314 The real shape of that measured are not an accurate rectangle. These show the rough shape of an area. We measured the area of regular shapes that molybdenum molecules are lined on outside.

  8. THO-10-003 003_100225-11-7B 2-3.Analysis of nano-crystals 0014 0013 0016 0005 100nm 200nm 100nm 200nm It shows the crystal is not simply put on NH but integrated. 0001 0008 0012 0009 100nm 200nm 100nm 10μm 0003 004 0017 0002 10μm 10μm 10μm 10μm We measured about only 17 micro-crystals with clear boundaries.

  9. THO-10-002 2-4.Analysis of nano-crystals [nm2] THO-10-003 [µm2] Fig1,The histogram of nano-crystals Fig2,The histogram of micro-crystals Population Population [µm2] [nm2] Area Area

  10. 2-5.Analysis of nano-crystals 「110」 「101」 「011」 nano-crystals Population micro-crystals 10.3nm2 13.8nm2 14.3nm2 [×106 nm2] Area Fig3,The histogram of all crystals Population [011] [110] [101] The comparison of sizes of models and real TEM images. 0.77nm2 1.18nm2 1.57nm2 [×106 nm2] Area Fig4,The histogram of nano-crystals and the models

  11. THO-10-002 2-6.Analysis of nano-crystals 100225-11-7C_movie (A) (C) (B) helloA FFT an Image Inversed FFT(B) FFT applied a mask Image16 helloS Image 28 1nm helloI Image 21 There are some lines at the crystal area in the images (C). 2nm That shows that the crystals have some of regularity.

  12. 2-7.Analysis of nano-crystals THO-10-002 100225-11-7C_movie helloK helloG02 2nm 100202-11-6B 100218-11-7A-helloA 100202-11-6B_helloF2 Image 11 100202-11-6B_helloD Image4 A nano-crystal changes to the crystal structure only in a short time. There are a membrane structureoutside of crystal structure in some TEM images( I&K,F).

  13. Summary • The crystals do not grow up on amino-base. The Y-shaped molecule-base is needed to grow up and to be a crystal. • A nano-crystal changes to the crystal structure only in a short time. It is not stable structure or stable sizes? • From the histograms, a lot of nano-clystalsare about three molecules sizes. There is a factor that block the growth? There are a membrane structureoutside of crystal structure in some TEM images( 2-6_I & 2-7_K,F2).

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