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Ultrafast X-ray diffraction with an XFEL: Probing transient structures of nanoparticles

Niozu, Akinobu 京都大学 DOI:10.14989/doctor.k22990

2021.03.23

概要

物質の性質を理解する上で、物質を形作る原子や分子の配列に関する情報は最も基本的な性質であり、20 世紀初頭以降、X 線を用いた構造解析法は物質の原子スケールの構造情報を得るための手法として広く利用されてきた。近年、X 線自由電子レーザー（XFEL）と呼ばれる新規な X 線光源の開発により、高強度、高コヒーレンスかつ短パルス（～千兆分の 1 秒程度）という特長を有する X 線パルスが利用可能となり、 X 線イメージングを用いた単粒子構造解析や、X 線非線形光学などの新しい研究領域が開拓されつつある。特に、XFEL の短パルス性を利用することで、これまで観測が困難であった状態変化の途上にある物質の過渡的な構造の観測が期待される。単一パルスにより X 線回折像を得られる XFEL 実験では、XFEL のコヒーレンスに起因する干渉(スペックル)パターンから従来の手法を超えた詳細な構造情報が得られると期待される一方で、アンサンブル平均・時間平均を経ない回折像データの取り扱いに関しては XFEL の特長を活かす解析手法の開発が重要な課題となっている。本研究では、国内の XFEL 施設である SACLA において、ナノ粒子の超高速 X 線回折実験を実施し、XFEL の短パルス性を活かした、過渡的な構造の観測手法の確立を目指した。

申請者は上記の背景および動機に基づき、キセノン(Xe)ナノ粒子を試料とした実験を行い、①結晶化直後におけるナノ粒子の構造とその起源、②強力なレーザー照射に伴うナノ粒子のプラズマ化に伴う構造変化の２つのテーマについて研究を行った。

1つ目のテーマでは、Xe ナノ粒子が結晶化する際の構造変化ダイナミクスの観測を、XFEL を用いる超高速 X 線回折によって行った。真空中へ Xe ガスを噴出すると、断熱膨張による冷却により試料ガスはごく短時間で過冷却状態に至り、そこからの結晶核生成を経てナノ粒子が生成してゆくと考えられる。ファンデルワールス力によって凝集するXe は、バルク固体では面心立方構造を取ることが知られているが、小さなナノ粒子の安定構造は面心立方構造とは異なることが知られており、粒子成長とともに面心立方構造へ至る経路は自明ではない。申請者は XFEL を用いる単粒子 X 線回折実験で得られた回折像の解析から、粒子生成後、数百マイクロ秒という早い時間におけるXe ナノ粒子において、安定な面心立方構造だけでなく、積層欠陥を多数含むランダム六方最密充填構造と呼ばれる準安定な構造が存在していることを明らかにするとともに、この構造が結晶成長の kinetics に基づくことを示した。

2つ目のテーマでは近赤外（NIR）レーザーと XFEL を用いる時分割の X 線回折実験を行い NIR レーザーパルス（波長 800nm、パルス幅～30 fs）照射後の Xe ナノ粒子中の結晶構造の変化を、SACLA から供給される硬 X 線パルス（10 keV、パルス幅～10 fs、強度～4×1017 W/cm2）を用いて観測した。NIR レーザーパルスの強度を系統的に変えることで、NIR レーザー照射によって生成するプラズマの状態を制御し、NIR レーザー照射後にXe ナノ粒子中の結晶構造が消失する時間スケールが生成したプラズマ状態を特徴づけるプラズマ音速で支配されることを明らかにした。

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