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Characterization of a Laser-Based Heating System Coupled With In Operando Raman Spectroscopy for Studying Solar Thermochemical Redox Cycles.

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Title: Characterization of a Laser-Based Heating System Coupled With In Operando Raman Spectroscopy for Studying Solar Thermochemical Redox Cycles.
Authors: Kangjae Lee1, Scheffe, Jonathan R.1 jscheffe@ufl.edu
Source: Journal of Solar Energy Engineering. Apr2019, Vol. 141 Issue 2, p1-7. 7p.
Subjects: Laser heating, Raman spectroscopy, Thermochemistry
Abstract: A 200 W CO2 laser-based heating system coupled with in operando Raman spectroscopy has been developed. The system delivers highly concentrated radiation capable of driving thermochemical reactions and simulates heat fluxes expected by 3D solar concentrating systems. 10 mol% Gd-doped and pure ceria pellets were prepared and used to characterize the system because of their well-established thermodynamic and kinetic properties, as well as their strong Raman peak due to F2g symmetrical mode at 460 cm-1. Reduction in an H2 atmosphere has been carried out to investigate the behavior of the full width at half maximum (FWHM) of the F2g Raman peak resulting from changes in temperature and oxidation state. For both samples, an increase in temperature during heating in air (i.e., fully oxidized) resulted in a peak shift toward low wavenumber and an increase of FWHM. The FWHM versus temperature curves were then measured for controlled reduction extents ranging between sample averaged nonstoichiometries of δ = 0-0.209 as a function of temperature. At a fixed temperature, Gd-doped ceria exhibited an increase in FWHM with increasing reduction extent until δ = 0.056. At greater reduction extents, the FWHM decreased with increasing reduction extents. We attribute this to changes in the lattice parameter caused by the eventual formation of intermediate cubic Ce2O3 at the radiated surface. This study demonstrates the promise of utilizing Raman spectroscopy to probe thermochemical reactions in operando. Going forward, we expect that this will be an especially promising tool for characterizing emerging thermochemical materials with complex phase equilibria, especially for nonequilibrium processes. [ABSTRACT FROM AUTHOR]
Copyright of Journal of Solar Energy Engineering is the property of American Society of Mechanical Engineers and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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DbLabel: Engineering Source
An: 136140358
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  Label: Title
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  Data: Characterization of a Laser-Based Heating System Coupled With In Operando Raman Spectroscopy for Studying Solar Thermochemical Redox Cycles.
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  Data: <searchLink fieldCode="AR" term="%22Kangjae+Lee%22">Kangjae Lee</searchLink><relatesTo>1</relatesTo><br /><searchLink fieldCode="AR" term="%22Scheffe%2C+Jonathan+R%2E%22">Scheffe, Jonathan R.</searchLink><relatesTo>1</relatesTo><i> jscheffe@ufl.edu</i>
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  Data: <searchLink fieldCode="JN" term="%22Journal+of+Solar+Energy+Engineering%22">Journal of Solar Energy Engineering</searchLink>. Apr2019, Vol. 141 Issue 2, p1-7. 7p.
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  Data: <searchLink fieldCode="DE" term="%22Laser+heating%22">Laser heating</searchLink><br /><searchLink fieldCode="DE" term="%22Raman+spectroscopy%22">Raman spectroscopy</searchLink><br /><searchLink fieldCode="DE" term="%22Thermochemistry%22">Thermochemistry</searchLink>
– Name: Abstract
  Label: Abstract
  Group: Ab
  Data: A 200 W CO2 laser-based heating system coupled with in operando Raman spectroscopy has been developed. The system delivers highly concentrated radiation capable of driving thermochemical reactions and simulates heat fluxes expected by 3D solar concentrating systems. 10 mol% Gd-doped and pure ceria pellets were prepared and used to characterize the system because of their well-established thermodynamic and kinetic properties, as well as their strong Raman peak due to F2g symmetrical mode at 460 cm-1. Reduction in an H2 atmosphere has been carried out to investigate the behavior of the full width at half maximum (FWHM) of the F2g Raman peak resulting from changes in temperature and oxidation state. For both samples, an increase in temperature during heating in air (i.e., fully oxidized) resulted in a peak shift toward low wavenumber and an increase of FWHM. The FWHM versus temperature curves were then measured for controlled reduction extents ranging between sample averaged nonstoichiometries of δ = 0-0.209 as a function of temperature. At a fixed temperature, Gd-doped ceria exhibited an increase in FWHM with increasing reduction extent until δ = 0.056. At greater reduction extents, the FWHM decreased with increasing reduction extents. We attribute this to changes in the lattice parameter caused by the eventual formation of intermediate cubic Ce2O3 at the radiated surface. This study demonstrates the promise of utilizing Raman spectroscopy to probe thermochemical reactions in operando. Going forward, we expect that this will be an especially promising tool for characterizing emerging thermochemical materials with complex phase equilibria, especially for nonequilibrium processes. [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Journal of Solar Energy Engineering is the property of American Society of Mechanical Engineers and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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    Identifiers:
      – Type: doi
        Value: 10.1115/1.4042229
    Languages:
      – Code: eng
        Text: English
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      Pagination:
        PageCount: 7
        StartPage: 1
    Subjects:
      – SubjectFull: Laser heating
        Type: general
      – SubjectFull: Raman spectroscopy
        Type: general
      – SubjectFull: Thermochemistry
        Type: general
    Titles:
      – TitleFull: Characterization of a Laser-Based Heating System Coupled With In Operando Raman Spectroscopy for Studying Solar Thermochemical Redox Cycles.
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            NameFull: Kangjae Lee
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            NameFull: Scheffe, Jonathan R.
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            – D: 01
              M: 04
              Text: Apr2019
              Type: published
              Y: 2019
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            – Type: volume
              Value: 141
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              Value: 2
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            – TitleFull: Journal of Solar Energy Engineering
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