W18O49 Nanowhiskers Decorating SiO2 Nanofibers: Lessons from in situ SEM/TEM growth to large scale synthesis and fundamental structural understanding

Vojtech Kundrat, Kristyna Bukvisova, Libor Novak, Lukas Prucha, Lothar Houben, Jakub Zalesak, Antonio Vukusic, David Holec, Reshef Tenne, Jiri Pinkas

Publikation: Beitrag in FachzeitschriftArtikelForschungBegutachtung


Tungsten suboxide W 18O 49 nanowhiskers are a material of great interest due to their potential high-end applications in electronics, near-infrared light shielding, catalysis, and gas sensing. The present study introduces three main approaches for the fundamental understanding of W 18O 49 nanowhisker growth and structure. First, W 18O 49 nanowhiskers were grown from γ-WO 3/a-SiO 2 nanofibers in situ in a scanning electron microscope (SEM) utilizing a specially designed microreactor (μReactor). It was found that irradiation by the electron beam slows the growth kinetics of the W 18O 49 nanowhisker, markedly. Following this, an in situ TEM study led to some new fundamental understanding of the growth mode of the crystal shear planes in the W 18O 49 nanowhisker and the formation of a domain (bundle) structure. High-resolution scanning transmission electron microscopy analysis of a cross-sectioned W 18O 49 nanowhisker revealed the well-documented pentagonal Magnéli columns and hexagonal channel characteristics for this phase. Furthermore, a highly crystalline and oriented domain structure and previously unreported mixed structural arrangement of tungsten oxide polyhedrons were analyzed. The tungsten oxide phases found in the cross section of the W 18O 49 nanowhisker were analyzed by nanodiffraction and electron energy loss spectroscopy (EELS), which were discussed and compared in light of theoretical calculations based on the density functional theory method. Finally, the knowledge gained from the in situ SEM and TEM experiments was valorized in developing a multigram synthesis of W 18O 49/a-SiO 2 urchin-like nanofibers in a flow reactor.

Seiten (von - bis)378-390
FachzeitschriftCrystal growth & design
PublikationsstatusElektronische Veröffentlichung vor Drucklegung. - 5 Dez. 2023

Bibliographische Notiz

Funding Information:
We acknowledge Cryo-Electron Microscopy and Tomography Core Facility of CIISB, Instruct-CZ Centre, supported by MEYS CR (LM2018127). CzechNanoLab project LM2018110 funded by MEYS CR is gratefully acknowledged for the financial support of the measurements/sample fabrication at CEITEC Nano Research Infrastructure. We thank Matěj Boček for through discussions of the work. This work was supported by the project Quantum materials for applications in sustainable technologies (QM4ST), funded as project No. CZ.02.01.01/00/22_008/0004572 by Programme Johannes Amos Commenius, call Excellent Research. We acknowledge CB2-WIS-Rehovot group for consultations. This research has been financially supported by the Horizon 2020 Research and Innovation Programme under the grant agreement No. 810626 (SINNCE). RT acknowledges the support of The Estate of Manfred Hecht and the Estate of Diane Recanati. We are also grateful to the Perlman Family Foundation, the Kimmel Center for Nanoscale Science.

Publisher Copyright:
© 2023 The Authors. Published by American Chemical Society

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