Unraveling the molecular and growth mechanism of colloidal black In2O3−x

Author(s)Armstrong, Cameron
Author(s)Otero, Kayla
Author(s)Hernandez-Pagan, Emil A.
Date Accessioned2024-05-30T19:08:50Z
Date Available2024-05-30T19:08:50Z
Publication Date2024-04-19
DescriptionThis article was originally published in Nanoscale. The version of record is available at: https://doi.org/10.1039/D3NR05035A. This journal is © The Royal Society of Chemistry 2024
AbstractBlack metal oxides with varying concentrations of O-vacancies display enhanced optical and catalytic properties. However, direct solution syntheses of this class of materials have been limited despite being highly advantageous given the different synthetic handles that can be leveraged towards control of the targeted material. Herein, we present an alternate colloidal synthesis of black In2O3−x nanoparticles from the simple reaction between In(acac)3 and oleyl alcohol. Growth studies by PXRD, TEM, and STEM-EDS coupled to mechanistic insights from 1H, 13C NMR revealed the particles form via two paths, one of which involves In0. We also show that variations in the synthesis atmosphere, ligand environment, and indium precursor can inhibit formation of the black In2O3−x. The optical spectrum for the black nanoparticles displayed a significant redshift when compared to pristine In2O3, consistent with the presence of O-vacancies. Raman spectra and surface analysis also supported the presence of surface oxygen vacancies in the as-synthesized black In2O3−x.
SponsorThe authors thank Brandon Vance for his help in our collection of N2O chemisorption data, Dr Sviatoslav Baranets for his help with the thermal annealing, Danielle Gendler for aiding in the collection of FTIR and NMR data, Ashkan Yazdanshenas for aiding in NMR data collection. Financial support for this work was provided by University of Delaware start-up funds and a Delaware COBRE seed grant supported by the National Institute of General Medical Sciences (NIGMS 1 P20 GM104316-01A1). K. O. thanks the GEM Fellowship Program for support. XPS analysis was performed with the instrument sponsored by the National Science Foundation under grant no. CHE-1428149. Raman analysis was performed with the instrument sponsored by the National Science Foundation under grant no. CHE-1828325. NMR facilities are supported through NIH P20GM104316. HRTEM and STEM-EDS was conducted at the Vanderbilt Institute of Nanoscale Science and Engineering. We also thank the reviewers for their comments and suggested experiments.
CitationArmstrong, Cameron, Kayla Otero, and Emil A. Hernandez-Pagan. “Unraveling the Molecular and Growth Mechanism of Colloidal Black In 2 O 3− x .” Nanoscale 16, no. 20 (2024): 9875–86. https://doi.org/10.1039/D3NR05035A.
ISSN2040-3372
URLhttps://udspace.udel.edu/handle/19716/34434
Languageen_US
PublisherNanoscale
dc.rightsAttribution-NonCommercial 4.0 Internationalen
dc.rights.urihttp://creativecommons.org/licenses/by-nc/4.0/
TitleUnraveling the molecular and growth mechanism of colloidal black In2O3−x
TypeArticle
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