Deve I opment of next-enerat i on e I ectron tomography for 3D mesa-ea I e structural analysisDeve I opment of next-enerat i on e I ectron tomography for 3D mesa-ea I e structural analysisDeve I opment of next-enerat i on e I ectron tomography for 3D mesa-ea I e structural analysis

• Project/Area Number: 21241030
• Research Category: Grant-in-Aid for Scientific Research (A)
• Allocation Type: Single-year Grants
• Section: 一般
• Research Field: Nanomaterials/Nanobioscience
• Research Institution: Kyushu University (2010-2011); Kyoto Institute of Technology (2009)
• Principal Investigator: JINNAI Hiroshi 九州大学, 先導物質化学研究所, 特任教授 (20303935)
• Project Period (FY): 2009 – 2011
• Project Status: Completed (Fiscal Year 2011)
• Budget Amount: ¥48,100,000 (Direct Cost: ¥37,000,000、Indirect Cost: ¥11,100,000); Fiscal Year 2011: ¥2,210,000 (Direct Cost: ¥1,700,000、Indirect Cost: ¥510,000); Fiscal Year 2010: ¥17,940,000 (Direct Cost: ¥13,800,000、Indirect Cost: ¥4,140,000); Fiscal Year 2009: ¥27,950,000 (Direct Cost: ¥21,500,000、Indirect Cost: ¥6,450,000)
• Keywords: 電子線トモグラフィー法 / 走査型光学系 / 被写界深度 / ナノ材料解析 / 評価

Research Abstract

透過型電子顕微鏡法(TEM)と計算機トモグラフィ(CT)を組み合わせ、材料の内部構造をナノメートル(nm)スケールで3次元可視化できる電子線トモグラフィー法(Transmission Electron Microtomography, TEMT)に注目が集まっている。本研究の目的は、メゾスケール(nmとμmの間のスケール)の3次元観察が可能な"被写界深度が深い"光学系を備えた次世代のTEMTを開発することである。通常、TEMTでは試料(板状試料)を70°程度まで傾斜させ多数の透過像を撮影する。試料の傾斜に伴い、入射電子線に対する"実効的な"試料厚みは増加し、従って、本申請のように数μmの試料の3次元観察を可能とするためには、被写界深度の深い長焦点光学系を実現することが必須となる。本申請の全ての検討・開発項目は、いかにして被写界深度の深い明るい光学系を実現するか、という一点に集約されていると書いても過言ではない。
3年の研究期間を通して、長焦点光学系を実現するための高コントラスト走査型ポールピースと高感度検出器などの開発を行い、これらを実際に電子顕微鏡に組み込んだ。また、試料内での電子の多重散乱による(=色収差による)像のボケを低減するために「磁場制御型Ωフィルター」も電子顕微鏡に組み込んだ。この新型電子顕微鏡において、被写界深度の実測(実測で数μmを実現)、長焦点光学系による走査電子ビームの収束角度の実測、走査系の動作プログラムの開発、明るい光学系の実現のためのレンズパラメーターの最適化、検出器の高感度化など様々な装置開発・改良を行い、上に述べた「被写界深度の深い明るい光学系」を実現した。さらに、この新型顕微鏡を用いて厚み数百nm～数μmの複数の高分子試料の3次元観察を行ったところ、3次元画像の分解能は試料の厚みとともに劣化するものの、2μm程度の厚みの高分子試料の観察は可能であること、数nm程度の分解能を保った状態での3次元観察は0.5μm程度が限界であること、などの上重要な知見を得ることができた。

Research Products

• [Journal Article] Morphological Transition of Triblock Copolymer Cylindrical Micelles Responding to Solvent Change (2012)
  • Author(s): D.Han, et al
  • Journal Title: Soft Matter Volume: 8 Issue: 7 Pages: 2144-2151
  • DOI: 10.1039/c2sm07020k
  • Peer Reviewed
• [Journal Article] Creating Suprapolymer Assemblies : Nanowires, Nanorings, and Nanospheres Prepared from Symmetric Block-Copolymers Confined in Spherical Particles (2012)
  • Author(s): H.Yabu, et al
  • Journal Title: J.Mater.Chem. Volume: 22 Issue: 16 Pages: 7672-7675
  • DOI: 10.1039/c2jm30236e
  • Peer Reviewed
• [Journal Article] Tilt-angle measurement of a sample stage using a capacitive liquid-based inclinometer (2012)
  • Author(s): M.Matoba, et al
  • Journal Title: J.Electron.Microsc. Volume: 61(3) Pages: 193-198
  • DOI: 10.1093/jmicro/dfs034
  • Peer Reviewed
• [Journal Article] Tilt-angle measurement of a sample stage using a capacitive liquid-based inclinometer (2012)
  • Author(s): K. Matoba, J. Takagi, T. Yasunaga, H. Jinnai, K. Iwasaki
  • Journal Title: J. Electron. Microsc Volume: (未定)
• [Journal Article] Creating Suprapolymer Assemblies : Nanowires, Nanorings, and Nanospheres Prepared from Symmetric BlockCopolymers Confined in Spherical Particles (2012)
  • Author(s): H. Yabu, S. Sateo, T. Higuchi, H. Jinnai, M. Shimomura
  • Journal Title: J. Mater. Chem Volume: 22 Pages: 7672-7675
• [Journal Article] Threedimensional observation of confined phaseseparated structures in block copolymer nanoparticles (2012)
  • Author(s): T. Higuchi, K. Motoyoshi, H. Sugimori, H. Jinnai, H. Yabu*, M. Shimomura
  • Journal Title: Soft Matter Volume: 8 Pages: 3791-3797
• [Journal Article] Single chain distribution analysis near a substrate using a combined method of three-dimensional imaging and SCF simulation (2011)
  • Author(s): H.Morita, et al
  • Journal Title: Eur.Polymer J. Volume: 47 Pages: 685-691
  • Peer Reviewed
• [Journal Article] Structural characterization of the Fddd phase in a diblock copolymer thin film by electron microtomography (2011)
  • Author(s): J.Jung, et al
  • Journal Title: Soft Matter Volume: 7 Pages: 10424-10428
  • Peer Reviewed
• [Journal Article] Three-dimensional observation of confined phase-separated structures in block copolymer nanoparticles (2011)
  • Author(s): T.Higuchi, et al
  • Journal Title: Soft Matter Volume: 8 Issue: 14 Pages: 3791-3797
  • DOI: 10.1039/c2sm07139h
  • Peer Reviewed
• [Journal Article] Single chain distribution analysis near a substrate using a combined method of threedimensional imaging and SCF simulation (2011)
  • Author(s): H. Maritaa, H. Sugimori, M. Doli, H. Jinnai
  • Journal Title: Eur. Polymer J Volume: 47 Pages: 685-691
• [Journal Article] Solvent-Driven Evolution of Block Copolymer Morphology under 3D Confinement (2010)
  • Author(s): L. Li, K. Matsunaga, J. Zhu, T. Higuchi, H. Yabu, M. Shimomura, H. Jinnai, R. C. Hayward*, T. P. Russell
  • Journal Title: Macromolecules Volume: 43(18) Pages: 7807-7812
• [Journal Article] Dependence of beam broadening on detection angle in scanning transmission electron microtomography (2010)
  • Author(s): S. Motoki, T. Kaneko, Y. Aoyama, H. Nishioka, Y. Okura, Y. Kondo, H. Jinnai
  • Journal Title: J. Electron. Microsc Volume: 59
• [Journal Article] Transmission Electron Microtomography and Polymer Nanostructures (2010)
  • Author(s): H. Jinnai*, R. J. Spontak, T. Nishi
  • Journal Title: Macromolecules Volume: 43(4) Pages: 1675-1688
• [Journal Article] Dependence of beam broadening on detection angle in scanning transmission electron microtomography (2010)
  • Author(s): S.Motoki, et al.
  • Journal Title: J.Electron.Microsc. Volume: 59
  • Peer Reviewed
• [Journal Article] Single chain distribution analysis near a substrate using a combined method of three-dimensional imaging and SCF simulation (2010)
  • Author(s): H.Morita, et al.
  • Journal Title: Eur.Polymer J. Volume: 47 Pages: 685-691
  • Peer Reviewed
• [Journal Article] Transmission Electron Microtomography and Polymer Nanostructures (2010)
  • Author(s): H.Jinnai, et al.
  • Journal Title: Macromolecules 43 Pages: 1675-1688
  • Peer Reviewed
• [Journal Article] 3-Dimensional Characterization of Membrane with Nanoporous Structure Using TEM Tomography and Image Analysis (2010)
  • Author(s): F.H.She, et al.
  • Journal Title: Desalination 250 Pages: 757-761
  • Peer Reviewed
• [Journal Article] Grating-Assisted Spectrally-Narrowed Emissions from an Organic Slab Crystal Excited with a Mercury Lamp (2010)
  • Author(s): S.Hotta, et al.
  • Journal Title: Journal of Nanosci. Nanotechnol 10 Pages: 440-447
  • Peer Reviewed
• [Journal Article] Self-Assembled ABC Triblock Copolymer Double and Triple Helices (2009)
  • Author(s): J. Dupont, G. Lin*, K. Niihara, R. Kimoto, H. Jinnai
  • Journal Title: Angew. Chem Volume: 48(33) Pages: 6144-6147
• [Journal Article] Small-Molecule-Directed Nanoparticle Assembly Toward Stimuliresponsive Nanocomposites (2009)
  • Author(s): Y. Zhao, K. Thorkelsson, A. J. Mastroianni, T. Schilling, J. M. Luther, B. J. Rancatore, K. Matsunaga, H. Jinnai, Y. We, D. Poulsen, J. M. J. Frechet, A. P. Alivisatos, T. Xu*
  • Journal Title: Nat. Mater Volume: 8(12) Pages: 979-985
• [Journal Article] Cylindrically Confined Diblock Copolymers (2009)
  • Author(s): P.Dobriyal, et al.
  • Journal Title: Macromolecules 42 Pages: 9082-9088
  • Peer Reviewed
• [Journal Article] Small Molecule Directed Nanoparticle Assembly Toward Stimuli-responsive Nanocomposites (2009)
  • Author(s): Y.Zhao, et al.
  • Journal Title: Nature Materials 8 Pages: 979-985
  • Peer Reviewed
• [Journal Article] Polymer nanotechnology applied to polymeric nano-soft-materials (2009)
  • Author(s): T.Nishi, et al.
  • Journal Title: J.Phys.Conf.Ser. 184 Pages: 12-30
  • Peer Reviewed
• [Journal Article] The interface dynamics of bicontinuous phase separating structure in apolymer blend (2009)
  • Author(s): Saito, et al.
  • Journal Title: J.Phys.Conf.Ser. 184 Pages: 12-29
  • Peer Reviewed
• [Journal Article] Self-Assembled ABC Triblock Copolymer Double and Triple Helices (2009)
  • Author(s): J.Dupont, et al.
  • Journal Title: Angew.Chem.Int.Ed. 48 Pages: 6144-6147
  • Peer Reviewed
• [Presentation] Recent Development of Electron Tomography for Polymeric Nano and MesoStructures (2010)
  • Author(s): H. Jinnai
  • Organizer: International Microscopy Congress 17(IMC17)
  • Place of Presentation: Windsor Barra Convention Center, Rio de Janeiro, Brazil
  • Year and Date: 2010-09-24
• [Presentation] Recent Development of Electron Tomography for Polymeric Nano-and Meso-Structures (2010)
  • Author(s): H.Jinnai
  • Organizer: International Microscopy Congress 17(IMC17)
  • Place of Presentation: Windsor Barra Convention Center, Rio de Janeiro, Brazil(招待講演)
  • Year and Date: 2010-09-24
• [Presentation] Electron Tomography of Soft Polymeric Materials (2010)
  • Author(s): H. Jinnai
  • Organizer: SofTEAM Workshop
  • Place of Presentation: Berkeley, CA, U SA
  • Year and Date: 2010-03-08
• [Presentation] Electron Tomography of Soft Polymeric Materials (2010)
  • Author(s): 陣内浩司
  • Organizer: SofrEAM Workshop
  • Place of Presentation: Berkeley, CA, USA
  • Year and Date: 2010-03-08
• [Presentation] Electron tomography for thick polymeric s amples of the order of micrometer (2010)
  • Author(s): H. Jinnai
  • Organizer: 10-th International Symposium on Biomimeti c Materials Processing(BMMP-10)
  • Place of Presentation: Nagoya, Japan
  • Year and Date: 2010-01-28
• [Presentation] Electron tomography for thick polymeric samples of the order of micrometer (2010)
  • Author(s): 陣内浩司
  • Organizer: 10-th International Symposium on Biomimetic Materials Processing (BMMP-10)
  • Place of Presentation: Nagoya, Japan
  • Year and Date: 2010-01-28
• [Presentation] 高分子材料の3次元構造解析一最新の技術と可能性一 (2010)
  • Author(s): 陣内浩司
  • Organizer: 日本接着学会粘着研究会1.月度例会
  • Place of Presentation: 大阪市立工業研究所
  • Year and Date: 2010-01-22
• [Presentation] 高分子材料の3次元構造解析-最新の技術と可能性- (2010)
  • Author(s): 陣内浩司
  • Organizer: 日本接着学会粘着研究会1月度例会
  • Place of Presentation: 大阪市立工業研究所
  • Year and Date: 2010-01-22
• [Presentation] ポリマー材料の定量的3D解析 (2010)
  • Author(s): 陣内浩司
  • Organizer: 階層的3D4Dフォーラム
  • Place of Presentation: 九州大学伊都キャンパス鉄鋼リサーチセンター
  • Year and Date: 2010-01-12
• [Presentation] ポリマー材料の定量的3D解析 (2010)
  • Author(s): 陣内浩司
  • Organizer: 階層的3D4Dフオーラム
  • Place of Presentation: 九州大学伊都キャンパス鉄鋼リサーチセンター
  • Year and Date: 2010-01-12
• [Presentation] 3D Elemental Mapping of Soft Materials using Transmission Electron Microtomography (2009)
  • Author(s): H. Jinnai
  • Organizer: 7th International Symposium on Atomic Level Characterizations for New Mate rials and Devices' 09(ALC' 09)
  • Place of Presentation: The Westin Maui Reso rt & Spa, Maui, Hawaii, USA
  • Year and Date: 2009-12-10
• [Presentation] 3D Elemental Mapping of Soft Materials using Transmission Electron Microtomography (2009)
  • Author(s): 陣内浩司
  • Organizer: 7th International Symposium on Atomic Level Characterizations for New Materials and Devices '09 (ALC'09)
  • Place of Presentation: The Westin Maui Resort & Spa, Maui, Hawaii, USA
  • Year and Date: 2009-12-10
• [Presentation] ソフトマテリアル機能材料の3次元構造観察と解析 (2009)
  • Author(s): 陣内浩司
  • Organizer: 第29回水素エネルギー協会大会
  • Place of Presentation: タワーホール船堀5階小ホール
  • Year and Date: 2009-12-03
• [Presentation] トモグラフィから何が測れるか?(3次元測定の種類と阻害要因) (2009)
  • Author(s): 陣内浩司
  • Organizer: 日本顕微鏡学会3次元電子線トモグラフィ法のマテリアルへの展開研究部会講演会
  • Place of Presentation: 工学院大学
  • Year and Date: 2009-11-28
• [Presentation] トモグラフィから何が測れるか? (3次元測定の種類と阻害要因) (2009)
  • Author(s): 陣内浩司
  • Organizer: 日本顕微鏡学会 3次元電子線トモグラフィ法のマテリアルへの展開研究部会講演会
  • Place of Presentation: 工学院大学
  • Year and Date: 2009-11-28
• [Presentation] 電子線トモグラフィー法による観察・評価の現状と今後 (2009)
  • Author(s): 陣内浩司
  • Organizer: 半導体計測・評価技術ネットワーク」ワークショップ
  • Place of Presentation: 茨城県つくば市国際会議場
  • Year and Date: 2009-11-24
• [Presentation] 電子線トモグラフィー法による観察・評価の現状と今後 (2009)
  • Author(s): 陣内浩司
  • Organizer: 「半導体計測・評価技術ネットワーク」ワークショップ
  • Place of Presentation: 茨城県つくば市国際会議場
  • Year and Date: 2009-11-24
• [Presentation] 電子線トモグラフィー法のソフトマテリアルへの応用 (2009)
  • Author(s): 陣内浩司
  • Organizer: 日本顕微鏡学会第53回シンポジウム
  • Place of Presentation: 東京工業大学大岡山キャンパス
  • Year and Date: 2009-10-31
• [Presentation] 電子線トモグラフィー法のソフトマテリアルへの応用 (2009)
  • Author(s): 陣内浩司
  • Organizer: 日本顕微鏡学会 第53回シンポジウム
  • Place of Presentation: 東京工業大学 大岡山キャンパス
  • Year and Date: 2009-10-31
• [Presentation] Self-assembled polymer nanostructures (2009)
  • Author(s): H. Jinnai
  • Organizer: International Conference on Supercrit ical Fluids(Supergreen2009)
  • Place of Presentation: Sendai, Japan
  • Year and Date: 2009-10-17
• [Presentation] Self-assembled polymer nano-structures (2009)
  • Author(s): 陣内浩司
  • Organizer: International Conference on Supercritical Fluids (Supergreen2009)
  • Place of Presentation: Sendai, Japan
  • Year and Date: 2009-10-17
• [Presentation] Helical structures formed from an amorph ous, achiral ABC triblock terpolymer (2009)
  • Author(s): H. Jinn
  • Organizer: International Symposium on Nano S tructured Polymeric Materials : Synthesis, Cha racterization and Application
  • Place of Presentation: Gwangju, Korea
  • Year and Date: 2009-10-07
• [Presentation] Helical structures formed from an amorphous, achiral ABC triblock terpolymer (2009)
  • Author(s): 陣内浩司, et al.
  • Organizer: International Symposium on Nano Structured Polymeric Materials : Synthesis, Characterization and Application
  • Place of Presentation: Gwangju, Korea
  • Year and Date: 2009-10-07
• [Presentation] 高分子ブロック共重合体の自己秩序化するメソスケール構造 (2009)
  • Author(s): 陣内浩司
  • Organizer: 日本化学会第3回関東支部大会
  • Place of Presentation: 早稲田大学理工キャンパス
  • Year and Date: 2009-09-05
• [Presentation] ACA(American Crystallographic Associati on) (2009)
  • Author(s): H. Jinnai
  • Organizer: Meeting
  • Place of Presentation: Toronto, Canada
  • Year and Date: 2009-07-29
• [Presentation] Microphase-separated structure in a cylinder-forming block copolymer thin film studied by neutron reflectivity aided by transmission electron microtomography (2009)
  • Author(s): 陣内浩司, et al.
  • Organizer: Structure of Nanophase Materials (SAS) in 2009 ACA (American Crystallographic Association) Meeting
  • Place of Presentation: Toronto, Canada
  • Year and Date: 2009-07-29
• [Presentation] 電子線トモグラフィー法とエックス線CTによる高分子材料の三次元観察・解析 (2009)
  • Author(s): 陣内浩司
  • Place of Presentation: 東京大学先端科学技術センター
  • Year and Date: 2009-05-15
• [Presentation] Science for Future Molecul ar Systems (2009)
  • Author(s): 陣内浩司
  • Organizer: ブロック共重合体の自己秩序化に関する最近の進展,陣内浩司
  • Place of Presentation: 九州大学伊都キャンパス
  • Year and Date: 2009-04-30
• [Presentation] ブロック共重合体の自己秩序化に関する最近の進展 (2009)
  • Author(s): 陣内浩司
  • Organizer: Kyushu University Global COE "Science for Future Molecular Systems" Global COE Seminar No. 77
  • Place of Presentation: 九州大学伊都キャンパス
  • Year and Date: 2009-04-30
• [Presentation] Microphaseseparated structure in a cylind erforming block copolymer thin film studied by neutron reflectivity aided by transmission electron microtomography (2009)
  • Author(s): H. Jinnai et al
  • Organizer: St ructure of Nanophase Materials
  • Place of Presentation: SAS
• [Remarks]
  • URL: http://muse.ifoc.kyushu-u.ac.jp/TLAB/TINNAI_LABORATORY/Welcome.html
• [Remarks]
  • URL: http://muse.ifoc.kyushu-.ac.jp/JLAB/JINNAILABORATORY/Welcome.html
• [Remarks]
  • URL: http://www.cis.kit.ac.jp/?mechanic/jinnai/research.html