| 高分子 Vol.63 No.9 |
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特集 最新の可視化技術で高分子を探るPart2 電子顕微鏡特集
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| チュートリアル Tutorial |
| 透過電子顕微鏡法（TEM）の基礎と応用―高分子試料の観察を意識して― Basics and Applications of Transmission Electron Microscopy: In Viewpoint of Observation of Polymer Samples |
田中 信夫 Nobuo TANAKA |
| ＜要旨＞The basics of transmission electron microscopy are explained in viewpoints of the imaging mechanism, the resolution, image contrast, and appication to observation of polymer samples. Transmission elecron microscopy (TEM) enables us to see single atoms and atomic columns in a crystal, whose separation is less than 0.2 nm, by naked eyes. First, we review the basics of electron diffraction in a crystal and the image formation by a convex lens, whcih is mathematically described by two-dimensional Fourier transform. Next, we see the mechanism of contrast formation in the image in TEM, which is in two kinds of mechanisms by scattering (diffraction) absorption contrast and phase contrast. The former is strongly dependent on the size of objective aperture, and the later is depend on the deforcus of the objective lens. Finally, several methods to observe polymer samples are described as some typical images are presented. Keywords: Transmission Electron Microscopy (TEM) / Polymer Samples / Resolution of Microscopes / Image Contrast / Lattice Image / Single Atom Images |
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| 先進走査電子顕微法（SEM）の基礎と応用 Basics and Applications of Advanced Scanning Electron Microscopy |
板倉 賢 Masaru ITAKURA |
| ＜要旨＞ 最近の走査電子顕微鏡（SEM）は、とくに低加速電圧領域での実効的な空間分解能が著しく向上し、さらに複数の検出器を用いることで、従来のSEMでは得られなかったさまざまな微細構造情報を比較的容易に得ることが可能になっている。本稿では、最近のSEM装置の構造と特徴を概説し、これを用いた観察事例を紹介する。 Keywords: Scanning Electron Microscopy / Low-Voltage SEM / Image Contrasts / Channeling Contrast / Semiconductor Materials |
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| トピックス COVER STORY: Topics and Products |
| STEM-EDX/EELS による高分子界面の解析 Characterization of Polymer/Metal Interfaces by STEM-EDX/EELS |
堀内 伸 Shin HORIUCHI |
| ＜要旨＞ Scanning transmission electron microscopy (STEM) is a powerful technique, which enables us to perform high contrast imaging with annular dark field detectors and chemical analysis in ultra small regions of polymer materials. EDX/EELS simultaneous analysis was performed to measure the profiles of chemical structures using a scanning electron beam across a polymer/metal interface. EDX allows us to identify the elemental compositions while EELS provides us information on the valence structures of the elements of interest. It was found that CuO is reduced to Cu2O at the Cu/PPS (polyphenylene sulfide) interface, suggesting a chemical interaction between polymer and copper oxide. Keywords: STEM / EDX / EELS / Interface / Polymer / Metal |
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| 原子分解能STEM を用いた最先端材料研究 Atom- Resolved STEM Characterization for Advanced Materials |
幾原 雄一 Yuichi IKUHARA |
| ＜要旨＞ Recently developed Cs corrected HAADF and ABF STEM are applied to visualize a single atom in a crystal and to directly observe the light elements in a crystal. These results are quantitatively analyzed and interpreted by combining first principles calculations. It is demonstrated that HAADF-STEM enables us to directly observe single dopant in a crystal and the dopant distribution in Ce doped cubic boron nitride (CBN). It is also shown that ABF-STEM is very powerful to directly observe the light elements such as lithium and hydrogen atomic columns in the respective crystals. Keywords: Cs-corrector / STEM / HAADF / ABF / Dopant / Light Element / Lithium / Hydrogen |
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| TEM、SEM観察による高分子材料の形態と物性 Morphology-Properties of Polymer materials on the basis of TEM(SEM) Observation |
佐野 博成 Hironari SANO |
| ＜要旨＞Observation of polymer materials by SEM and TEM is an important sample preparation technology. It can follow the progress of the sample preparation technique, and reveal the structure and properties of the polymeric material as is shown with the example of cellulose nano-fiber composites in this report. Keywords: TEM Staining / Nano-Composite / Cellulose-Nano-Fiber |
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| フィラー充填加硫ゴムの脱亜鉛処理 Original Pretreatment for Removing Rubber-Soluble Zn Compounds from Rubber Vulcanizates |
加藤 淳 Atsushi KATO |
| ＜要旨＞A 3D-TEM image slice of the silica-filled natural rubber (NR) before removing the Zn compounds has very low contrast, making it difficult to construct a clear 3D-image. The elements causing the electron beam to scatter are presumably contained in the NR vulcanizate and are heavier than sulfur, silica, carbon and hydrogen from which the rubber is made. Considering the recipes of the sulfur-cured rubber compounds used in this study, a very likely candidate of a compound containing such elements is ZnO. Rubber-soluble Zn compounds may include Zn (II) stearate and Zn complexes with accelerator fragments. We have succeeded in removing Zn compounds from NR vulcanizates by using an original pretreatment method. A 3D-TEM image slice of a silica-filled NR vulcanizate from which Zn compounds were removed has much higher contrast than that of the sample before removing the Zn compounds. The results indicate that some Zn compounds were solubilized in the NR vulcanizate and disturbed the 3D-TEM observation of nanofiller aggregates. Keywords: 3D-TEM / Electron Tomography / Natural Rubber Vulcanizate / Rubber-Soluble Zn Compounds / Removal of Zn Componds / Pretreatment |
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| ナノスーツ The NanoSuit® |
針山 孝彦 Takahiko HARIYAMA |
| ＜要旨＞ Scanning electron microscopy (SEM) has made remarkable progress, and has become an essential tool for observing biological materials at the microscopic level. However, various complex procedures have precluded observation of living organisms to date. Here, a new method is presented by which living organisms can be observed by field emission scanning electron microscope. Using this method, active movements of living animals were observed in vacuo (10-5-10-7 Pa) by protecting them with a coating of thin polymer membrane, the NanoSuit®, and it was found that the surface fine structure of living organisms is very different from that of traditionally fixed samples. After observation of mosquito larvae, despite the high vacuum it was possible to rear them subsequently in normal culture conditions. This method will be useful for numerous applications, particularly for electron microscopic observations in the life sciences. Keywords: NanoSuit® / Electron microscope / Life Science / Living Organism / High Vacuum / Surface Shield Effect |
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| イオン液体のSEM/TEM応用 Application of Ionic liquid for SEM/TEM Observation |
中澤 英子 Eiko NAKAZAWA |
| ＜要旨＞ Ionic liquid (IL) is widely utilized in various fields as functional materials such as reactants, catalysts, solvents due to its nature of lower evaporation pressure and higher ratio of ions. We’ve applied the ILs to the preparation of the sample for SEM/TEM. Some biological specimens were treated with the IL diluted with water, in which structures of samples could be preserved and definitely observed ultra-structure without dehydration and metal coating for SEM and fine structures of specimens. The ILs mounted directly on the microgrid was utilized for the supporting of samples in TEM. Some ILs was used as a solvent of liposomes and supporting films of nano-materials for TEM and could obtain its high resolution images and tomograms. Keywords: Ionic liquid / SEM / TEM / Yeast / Minute Crastaceae / Liposome / Nano Particles |
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| 金属ナノ構造のプラズモンを見る To See Surface Plasmons in Metal Nano-Structures |
山本 直紀 Naoki YAMAMOTO |
| ＜要旨＞ Surface plasmon (SP) is collective oscillation of surface charge on a metal surface, and is classified into two types, localized surface plasmon (LSP) and surface plasmon polariton (SPP). The author has developed a cathodoluminescence (CL) detection system combined with a scanning transmission electron microscope (STEM), and has applied this system to the study of SPs in metal nanostructures. The use of this system has an advantage for selectively examining a localized region using a converged electron beam with a probe size of 1 nm, and also observing emission intensity distribution as a monochromatic photon map. Mie and gap modes of LSP in spherical metal particles were investigated, and the size dependences of the resonant energies of the modes were found. Dispersion patterns of SPP in 1D and 2D plasmonic crystals were obtained from the angle-resolved spectral patterns, and the SPP modes were identified from the photon maps, which mimicked standing SPP waves in a real space. Keywords: Surface Plasmons / Cathodoluminescence / Electron Microscopy / Nanoparticles / Plasmonics |
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| 電子顕微鏡によるソフトマター観察 Electron Microscopy of Soft Materials |
末永 和知 Kazu SUENAGA |
| ＜要旨＞ Here we show how a high-resolution transmission electron microscopy can be applied to characterize soft matters. Direct imaging of the hexagonal network of carbon nanostructures enables us to identify individual molecular structures and atomic structures; fullerene molecules (C80) have been successfully identified with this method on a single-molecular basis. Visualizing and identification of individual carbon atoms has been achieved by a newly developed low-accelerating voltage TEM/STEM with sophisticated aberration correctors, showing the different natures of radical carbon atoms at the graphene edge. Keywords: TEM / STEM / EELS / Graphene / Nanocarbon |
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| FIB 加工による超薄切片の作製およびTEMT 観察 TEMT Observation of Ultra Thin Section Prepared by FIB Processing |
山本 祥正・福原 吏奈・石井 宏幸 Yoshimasa YAMAMOTO, Lina FUKUHARA, Hiroyuki ISHII |
| ＜要旨＞ The state-of-the-art processing with focused ion beam (FIB) was applied to prepare ultra-thin sections for the transmission electron microtomography (TEMT) technique in order to perform 3D observation of the nanomatrix structure of natural rubber (NR) grafted with polystyrene (PS). The nanomatrix structure was found to be the complexly hierarchical structure comprising of the NR micro-particles and the nanomatrix of PS nano-particles and NR. The distance between the PS nano-particles was about 5 nm in the nanomatrix, as is evident from the 3D image of ultra-thin section prepared by FIB-processing. In contrast, damage of the nanomatrix was found for the ultra-thin section prepared with the cryo-microtome, suggesting a destruction of the morphology. Consequently, the FIB-processing was proved to be indispensable for the TEMT observation of the nano-strucutre, i.e. the nanomatrix structure of natural rubber grafted with polystyrene. Keywords: Focused Ion Beam-Scanning Electron Microscopy / Transmission Electron Microtomography / Ultra Thin Section / Morphology / Natural Rubber / Polystyrene |
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| プロジェクトP Project P |
| 電子顕微鏡開発逸話（ナノからピコへの挑戦！） Anecdotal Story of Development of Electron Microscope in the Company |
岩槻 正志 Masashi IWATSUKI |
| ＜要旨＞ Electron Microscope (EM) has become the state-of-Art technology due to contribution of many of scientists. Since joining the company, I had many opportunities to develop variety of instruments. In order to develop the high-end instrument, engineer should seeks the absolute value of the instrument rather than the difference of the competing instrument. Also, project manager should hear customer's voice and field problems to apply the future instrument at all times. Keywords: EM |
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| SEM 高性能化の歩み History of Technologies in High Resolution SEM |
佐藤 貢 Mitsugu SATO |
| ＜要旨＞ 筆者は入社以来約30年にわたり、一貫して走査電子顕微鏡（SEM）の高性能化にかかわってきた。本稿では、筆者がかかわったSEM高性能化の歩みを中心に、高分解能SEMの創生期の技術開発にも触れながら、分解能向上、コントラスト向上、操作性向上について、技術の生まれた背景とその内容を紹介する。 Keywords: SEM / Field Emission / Inlens / Semi-Inlens / E Cross B |
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| グローイングポリマー Polymer Science and I: A Personal Account |
| ふんどし “FUNDOSHI” : The Japanese Traditional Underwear |
酒井 崇匡 Takamasa SAKAI |
| ＜要旨＞ “FUNDOSHI” is the Japanese traditional underwear for males. Japanese often retightens “Fundoshi” before an impoartant event, in order to get a sense of tension. Thus, “FUNDOSHI” is used in a figurative sence. In this essay, I would like to remark the difference between my “Fundoshi” and others “Fundoshi”. |
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| 高分子科学最近の進歩 Front-Line Polymer Science |
| 有機金属触媒反応による重合反応 Recent Development of Organometallic-Catalyzed Polymerization |
岡本 専太郎 Sentaro OKAMOTO |
| ＜要旨＞ The article reviews recent developments of organometalic-catalyzed polymerization reactions which involve follows: 1） palladium phosphine-sulfonate complex- and double Decker-type nickel complex-catalyzed coordination-insertion co-polymerizations of ethylene and α-olefins bearing a polar or olefinic functional group, 2） sandwich structured nickel complex-catalyzed highly linear-selective polymerization of α-olefins via a chain-walking process, 3） rhodium complex-catalyzed polymerization of a cyclopropene derivative with intramolecular metal 1,4-migration, 4） nickel-catalyzed decarboxylative cycloaddition polymerization producing polyquinolone, 5） and cobalt-catalyzed chain-growth cycloaddition polymerization of yne-diyne monomers. Design of organometalic complexes as an effective and/or selective catalyst and searching suitable conditions serves novel efficient polymerization generating unique polymer structures. Keywords: Catalytic Polymerizaition / Organometallics / Coordination-Insertion / Chain-Walking / Cycloaddition Polymerization |
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