Direct Observation of Tungsten Oxidation Studied by In Situ Environmental TEM

Togaru, Maanas; Sainju, Rajat; Zhang, Lichun; Jiang, Weilin; Zhu, Yuanyuan

doi:10.1016/j.matchar.2021.111016

Direct Observation of Tungsten Oxidation Studied by In Situ Environmental TEM

Journal Article · 01 April 2021 · Materials Characterization

DOI:https://doi.org/10.1016/j.matchar.2021.111016· OSTI ID:1783684

Togaru, Maanas ^[1]; Sainju, Rajat ^[1]; Zhang, Lichun ^[1]; ^[2]; Zhu, Yuanyuan ^[1]

University of Connecticut
BATTELLE (PACIFIC NW LAB)

In this study, in situ environmental transmission electron microscopy (ETEM) was applied, for the first time, to investigate the thermal oxidation of a pristine and a self-ion irradiated polycrystalline tungsten, using a MEMS-based gas cell at 500 oC to 900 oC in a 1 bar 2%O2/N2 gas mixture. By tracking the dynamic evolution of the tungsten oxide scale as it initiates, grows, and sublimates during a consecutive thermal oxidation experiment, we observed two distinctive tungsten oxide microstructure – one nanocrystalline o-WO3 scale grown on W{27-1 } and W{1-1 8} and another o-WO3 scale exhibits a novel highly textured nanostructure. While the two oxide microstructures shared a similar thickness of ~200 nm after 40-minute early-stage oxidation, the nanocrystalline scale on the W{27-1 } grew much more rapidly at 800 oC than the highly textured oxide at a higher temperature of 900 oC. This suggests both the microstructure of these tungsten oxide scales as well as their oxidation kinetics are highly sensitive to the tungsten surface orientation, and such correlations also change dynamically in the course of oxidation. We also discuss the tungsten oxidation mechanism, the effects of the TEM foil thickness, and the focused ion beam (FIB) Ga+ damage on in situ ETEM oxidation.

Research Organization:: Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

Sponsoring Organization:: USDOE

DOE Contract Number:: AC05-76RL01830

OSTI ID:: 1783684

Report Number(s):: PNNL-SA-158613

Journal Information:: Materials Characterization, Vol. 174

Country of Publication:: United States

Language:: English

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