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Title: Hydrothermal synthesis and characterization under dynamic conditions of cobalt oxide nanoparticles supported over magnesium oxide nano-plates

Abstract

Here, a nano-catalyst comprised of oxidized Co NPs supported on MgO nano-plates was synthesized via a hydrothermal co-precipitation strategy and calcination in O 2 and subsequently in H 2 at 250 °C. Spectro-microscopy characterization was performed by scanning transmission electron microscopy, electron energy loss spectroscopy and scanning X-ray transmission microscopy. Surface measurements under H 2 and H 2 + CO atmospheres were obtained by ambient pressure X-ray photoelectron spectroscopy and in situ X-ray absorption spectroscopy in the 225–480 °C range. These measurements at the atomic and microscopic levels demonstrated that the oxidized Co nanoparticles uniformly decorated the MgO nano-plates. The surfaces are enriched with Co, and with a mixture of Co(OH) 2 and CoO under H 2 and H 2 + CO atmospheres. Under a H 2 atmosphere, the outermost surfaces were composed of (lattice) O 2-, CO 3 2- and OH -. No inorganic carbonates were observed in the bulk. Chemisorbed CO, likely on the oxidized Co surfaces, was observed at the expense of O 2- under 300 mTorr H 2 + CO (2:1) at 225 °C. Gas phase CO 2 was detected under 32 Torr H 2 + CO (2:1) at 225 °C upon prolonged reaction time, andmore » was attributed to a surface chemical reaction between O 2- and chemisorbed CO. Furthermore, sp 3 like carbon species were detected on the otherwise carbon free surface in H 2 + CO, which remained on the surface under the subsequent reaction conditions. The formation of sp 3 like hydrocarbons was ascribed to a surface catalytic reaction between the chemisorbed CO and OH - as the apparent hydrogen source.« less

Authors:
 [1];  [1];  [1]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Chemical Sciences, Geosciences & Biosciences Division
OSTI Identifier:
1464133
Grant/Contract Number:  
AC02-05CH11231
Resource Type:
Accepted Manuscript
Journal Name:
Dalton Transactions
Additional Journal Information:
Journal Volume: 45; Journal Issue: 24; Related Information: © 2016 The Royal Society of Chemistry.; Journal ID: ISSN 1477-9226
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 36 MATERIALS SCIENCE; 77 NANOSCIENCE AND NANOTECHNOLOGY

Citation Formats

Alayoglu, Selim, Rosenberg, Daniel J., and Ahmed, Musahid. Hydrothermal synthesis and characterization under dynamic conditions of cobalt oxide nanoparticles supported over magnesium oxide nano-plates. United States: N. p., 2016. Web. doi:10.1039/c6dt00204h.
Alayoglu, Selim, Rosenberg, Daniel J., & Ahmed, Musahid. Hydrothermal synthesis and characterization under dynamic conditions of cobalt oxide nanoparticles supported over magnesium oxide nano-plates. United States. doi:10.1039/c6dt00204h.
Alayoglu, Selim, Rosenberg, Daniel J., and Ahmed, Musahid. Mon . "Hydrothermal synthesis and characterization under dynamic conditions of cobalt oxide nanoparticles supported over magnesium oxide nano-plates". United States. doi:10.1039/c6dt00204h. https://www.osti.gov/servlets/purl/1464133.
@article{osti_1464133,
title = {Hydrothermal synthesis and characterization under dynamic conditions of cobalt oxide nanoparticles supported over magnesium oxide nano-plates},
author = {Alayoglu, Selim and Rosenberg, Daniel J. and Ahmed, Musahid},
abstractNote = {Here, a nano-catalyst comprised of oxidized Co NPs supported on MgO nano-plates was synthesized via a hydrothermal co-precipitation strategy and calcination in O2 and subsequently in H2 at 250 °C. Spectro-microscopy characterization was performed by scanning transmission electron microscopy, electron energy loss spectroscopy and scanning X-ray transmission microscopy. Surface measurements under H2 and H2 + CO atmospheres were obtained by ambient pressure X-ray photoelectron spectroscopy and in situ X-ray absorption spectroscopy in the 225–480 °C range. These measurements at the atomic and microscopic levels demonstrated that the oxidized Co nanoparticles uniformly decorated the MgO nano-plates. The surfaces are enriched with Co, and with a mixture of Co(OH)2 and CoO under H2 and H2 + CO atmospheres. Under a H2 atmosphere, the outermost surfaces were composed of (lattice) O2-, CO32- and OH-. No inorganic carbonates were observed in the bulk. Chemisorbed CO, likely on the oxidized Co surfaces, was observed at the expense of O2- under 300 mTorr H2 + CO (2:1) at 225 °C. Gas phase CO2 was detected under 32 Torr H2 + CO (2:1) at 225 °C upon prolonged reaction time, and was attributed to a surface chemical reaction between O2- and chemisorbed CO. Furthermore, sp3 like carbon species were detected on the otherwise carbon free surface in H2 + CO, which remained on the surface under the subsequent reaction conditions. The formation of sp3 like hydrocarbons was ascribed to a surface catalytic reaction between the chemisorbed CO and OH- as the apparent hydrogen source.},
doi = {10.1039/c6dt00204h},
journal = {Dalton Transactions},
number = 24,
volume = 45,
place = {United States},
year = {2016},
month = {3}
}

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