W18O49 Nanowhiskers Decorating SiO2 Nanofibers: Lessons from in situ SEM/TEM growth to large scale synthesis and fundamental structural understanding
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In: Crystal growth & design, Vol. 24.2024, No. 1, 05.12.2023, p. 378-390.
Research output: Contribution to journal › Article › Research › peer-review
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TY - JOUR
T1 - W18O49 Nanowhiskers Decorating SiO2 Nanofibers
T2 - Lessons from in situ SEM/TEM growth to large scale synthesis and fundamental structural understanding
AU - Kundrat, Vojtech
AU - Bukvisova, Kristyna
AU - Novak, Libor
AU - Prucha, Lukas
AU - Houben, Lothar
AU - Zalesak, Jakub
AU - Vukusic, Antonio
AU - Holec, David
AU - Tenne, Reshef
AU - Pinkas, Jiri
N1 - Publisher Copyright: © 2023 The Authors. Published by American Chemical Society
PY - 2023/12/5
Y1 - 2023/12/5
N2 - 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.
AB - 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.
UR - http://www.scopus.com/inward/record.url?scp=85180075677&partnerID=8YFLogxK
U2 - 10.1021/acs.cgd.3c01094
DO - 10.1021/acs.cgd.3c01094
M3 - Article
VL - 24.2024
SP - 378
EP - 390
JO - Crystal growth & design
JF - Crystal growth & design
SN - 1528-7483
IS - 1
ER -