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Bi2O2CO3 Growth at Room Temperature: In Situ X-ray Diffraction Monitoring and Thermal Behavior


Moré, René; Olah, Michael; Balaghi, S Esmael; Jäker, Philipp; Siol, Sebastian; Zhou, Ying; Patzke, Greta R (2017). Bi2O2CO3 Growth at Room Temperature: In Situ X-ray Diffraction Monitoring and Thermal Behavior. ACS Omega, 2(11):8213-8221.

Abstract

The room-temperature formation of bismuth oxycarbonate (Bi2O2CO3) from Bi2O3 in sodium carbonate buffer was investigated with in situ powder X-ray diffraction (PXRD) in combination with electron microscopy and vibrational spectroscopy. Time-resolved PXRD measurements indicate a pronounced and rather complex pH dependence of the reaction mechanism. Bi2O2CO3 formation proceeds within a narrow window between pH 8 and 10 via different mechanisms. Although a zero-dimensional nucleation model prevails around pH 8, higher pH values induce a change toward a diffusion-controlled model, followed by a transition to regular nucleation kinetics. Ex situ synthetic and spectroscopic studies confirm these trends and demonstrate that in situ monitoring affords vital parameter information for the controlled fabrication of Bi2O2CO3 materials. Furthermore, the β → α bismuth oxide transformation temperatures of Bi2O2CO3 precursors obtained from different synthetic routes differ notably (by min 50 °C) from commercially available bismuth oxide. Parameter studies suggest a stabilizing role of surface carbonate ions in the as-synthesized bismuth oxide sources. Our results reveal the crucial role of multiple preparative history parameters, especially of pH value and source materials, for the controlled access to bismuth oxide-based catalysts and related functional compounds.

Abstract

The room-temperature formation of bismuth oxycarbonate (Bi2O2CO3) from Bi2O3 in sodium carbonate buffer was investigated with in situ powder X-ray diffraction (PXRD) in combination with electron microscopy and vibrational spectroscopy. Time-resolved PXRD measurements indicate a pronounced and rather complex pH dependence of the reaction mechanism. Bi2O2CO3 formation proceeds within a narrow window between pH 8 and 10 via different mechanisms. Although a zero-dimensional nucleation model prevails around pH 8, higher pH values induce a change toward a diffusion-controlled model, followed by a transition to regular nucleation kinetics. Ex situ synthetic and spectroscopic studies confirm these trends and demonstrate that in situ monitoring affords vital parameter information for the controlled fabrication of Bi2O2CO3 materials. Furthermore, the β → α bismuth oxide transformation temperatures of Bi2O2CO3 precursors obtained from different synthetic routes differ notably (by min 50 °C) from commercially available bismuth oxide. Parameter studies suggest a stabilizing role of surface carbonate ions in the as-synthesized bismuth oxide sources. Our results reveal the crucial role of multiple preparative history parameters, especially of pH value and source materials, for the controlled access to bismuth oxide-based catalysts and related functional compounds.

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Additional indexing

Item Type:Journal Article, refereed, original work
Communities & Collections:07 Faculty of Science > Department of Chemistry
08 University Research Priority Programs > Solar Light to Chemical Energy Conversion
Dewey Decimal Classification:540 Chemistry
Language:English
Date:2017
Deposited On:09 Feb 2018 08:06
Last Modified:18 Apr 2018 11:49
Publisher:American Chemical Society (ACS)
ISSN:2470-1343
Funders:SNF (Sinergia Grant No. CRSII2_160801/1), National Natural Science Foundation of China (U1232119), COST Project IZCNZ0-174856 C16.0075
OA Status:Closed
Publisher DOI:https://doi.org/10.1021/acsomega.7b01359
Project Information:
  • : FunderSNSF
  • : Grant ID
  • : Project TitleSNF (Sinergia Grant No. CRSII2_160801/1)
  • : Funder
  • : Grant ID
  • : Project TitleNational Natural Science Foundation of China (U1232119)
  • : Funder
  • : Grant ID
  • : Project TitleCOST Project IZCNZ0-174856 C16.0075

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