金属および合金
共通の課題
ナノ材料から建築構造物まで、多くの製品の重要な構成要素が金属と合金から作られています。個々の金属または合金の組成は、目的とする材料の強度、微細構造、耐腐食性を達成する上で非常に重要です。この特定の組成を実現するために、研究者たちは局所的な特徴や微細構造の特徴を研究して、原材料の合金組成と仕様純度への適合性の理解を深め、特定の部品の製造に使用する合金を選定し、部品の故障解析中には異物によるコンタミネーションの調査を行います。これらの属性をより深く理解するには、以下の情報が役立ちます。
- 分析に適した適切な試料作製技術の採用
- 試料の微細構造を識別する能力
- 焼結、再結晶、および相変化をリアルタイムで像取得
革新的な手法
金属および合金の特性を的確に評価し、理解するには、まず最初に、材料界面を解像できるように各試料が高品質であることと、必要に応じて環境刺激下で処理できるように各試料が適切に管理されていることが重要です。試料を作製したら、材料の性能を向上させるため、材料の複雑さと不具合をより深く理解するためにいくつかの手法を利用できます。
材料の成長、素子の超微細構造と不具合を理解するのに役立つ、権威ある賞を受賞した高分解能イメージングツール。
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原子分解能の化学および組成分析。
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ナノメートルレベルの分解能で像内の元素と化学物質を強調しマッピングを行い定量化するイメージング手法の1つ。
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EELSデータの空間分布を生成するための体系的な方法。
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成長過程、化学反応と酸化、照射効果、機械特性、磁気特性、強誘電特性をリアルタイムで観察。
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独自のSEM、TEM、またはSTEMアプリケーション用に試料を切削、エッチング、研磨、および凍結するための高性能ツール。
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試料の元素または化学特性を解明するのに役立つ。
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材料の結晶方位や組織を調べるのに役立つ。
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関連するアプリケーションの詳細については、「組成分析」または「化学分析」をご覧ください。
結果の活用
組成分析のための的確な試料作製
EBSD実験中、試料表面にダメージ層があると、結晶試料から取得される回析パターンが著しく変化する可能性があります。したがって、PECS II システムなどの電解研摩ツールを使用して、試料の表面が十分に滑らかで、回析パターンにぼやけを生成しないようにすることが重要です。次の画像は、PECS IIシステムにより高応力下のジルカロイ2合金試料をダメージの無いの状態に保ち、1 x 0.7 mm視野でIPFZマップの境界や粒界を高解像度で識別できることを示しています。結果は、オックスフォード大学の物質科、Angus Wilkinson教授およびHamidreza Abdolvand博士のご厚意によるものです。試料はPECS IIシステムによって作製。データはBruker Quantax EBSDシステムを搭載したZeiss Compact Merlinで取得。
微細な試料の詳細を識別
試料の動きやドリフト、照射による損傷は、影響を受けやすい試料を取り扱う場合や経時的な試料の活性を測定する場合に直面する共通の課題です。ライブドリフト補正を使用すると、隣接した画像間のドリフトを自動的に常時補正し、アーチファクトの発生や分解能の低下をほぼ防ぐことができます。次の画像は、OneView®カメラを使用して取得した4k x 4k解像度の電子線照射に敏感なゼオライト試料を示しています。
焼結、再結晶、および相変化に関する情報の取得
以下は、in-situ実験中の金ナノ粒子焼結を示しています。OneViewカメラを使用して最大解像度で個々の画像を記録することで、これらのビデオの全フレームが4k x 4kの高解像度画像になっていることがわかります。この方法を使用すると、個々の画像の抽出、取得後のドリフト補正の適用、全部または一部の画像からの動画の作成などの後処理が可能になります。これにより、非常に高い時間分解能と空間分解能で反応を捉えることができます。下の左の動画は、全視野(35 x 35 nm2)で5フレームをスキップした1k x 1kのもの、中央の動画は、関心領域(ROI)に合わせてトリミングし(ビニングx1)、3フレームをスキップしたもの、右の動画は、ROIに合わせてトリミングしたもの(ビニングx1)です。
左の画像は、800 ºCのin situで撮影した青銅試料の再結晶化を示すEBSDマップです。右の画像は、SEMの厳しい検出器レイアウトにおいても動的EBSDによる相変化を分析できることを示しています。
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Probing light atoms at sub-nanometer resolution: Realization of scanning transmission electron microscope holography
Cornell University Library2018Yasin, F. S.; Harvey, T. R.; Chess, J. J.; Pierce, J. S.; Ophus, C.; Ercius, P.; McMorran, B. J. -
Fast gas–solid reaction kinetics of nanoparticles unveiled by millisecond in situ electron diffraction at ambient pressure
Angewandte Chemie2018Yu, J.; Yuan, W.; Yang, H.; Xu, Q.; Wang, Y.; Zhang, Z. -
Electrostatic adsorption-microwave synthesis of palladium nanoparticles on graphene for improved cross-coupling activity
Applied Catalysis A: General2018S.E.Gilliland III, Tengco, J. M. M.; Yang, Y.; Regalbuto, J. R.; Castano, C. E.; Gupton, B. F. -
Stabilization of spherical nanoparticles of iron(III) hydroxides in aqueous solution by wormlike micelles
Journal of Colloid and Interface Science2018Destefani, T. A.; Onaga, G. L.; de Farias, M. A.; Percebom, A. M.; Sabadini, E. -
Atomic-resolution transmission electron microscopy of electron beam–sensitive crystalline materials
Science2018Zhang, D.; Zhu, Y.; Liu, L.; Ying, X.; Hsiung, C. -E.; Sougrat, R.; Li, K.; Han, Y. -
In situ nanobeam electron diffraction strain mapping of planar slip in stainless steel
Scripta Materialia2017Pekin, T. C.; Gammer, C.; Ciston, J.; Ophus, C.; Minor, A. M. -
In-situ study of the mechanisms of high temperature damage in elastic-plastic cyclic loading of nickel superalloy
Advanced Materials Research2014Petrenec, M.; Polák, J.; Šamořil, T.; Dluhoš, J.; Obrtlík, K.