An operando surface enhanced Raman spectroscopy (SERS) study of carbon deposition on SOFC anodes

Li, Xiaxi; Liu, Mingfei; Lee, Jungpil; Ding, Dong; Bottomley, Lawrence A.; Park, Soo‐Jin; Liu, Meilin

doi:10.1039/c4cp05176a

Cited by 37 publications

(38 citation statements)

References 35 publications

(63 reference statements)

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“…Li et al have extended this technique by implementing in situ surface enhanced Raman spectroscopy to strengthen signals from carbon and hydrocarbon intermediates, spatially resolved with regard to the Ni/YSZ interface. Their Ni based SOFCs were operated with propane at 450 °C and under various biases [16]. As another example, Cumming et al have pioneered diffuse reflectance infrared Fourier transform spectroscopy for in situ measurements of electrochemical intermediates (including surface hydroxyls, carbonates, and bicarbonates) in SOEC applications [17].…”

Section: Introductionmentioning

confidence: 99%

In situ, simultaneous thermal imaging and infrared molecular emission studies of solid oxide fuel cell electrodes

Kirtley

Qadri

Steinhurst

et al. 2016

Journal of Power Sources

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Various in situ probes of solid oxide fuel cells (SOFCs) have advanced recently to provide detailed, real time data regarding materials and chemical processes that relate to device performance and degradation. These techniques offer insights into complex fuel chemistry at the anode in particular, especially in the context of model predications. However, cell-to-cell variations can hinder mechanistic interpretations of measurements from separate, independent techniques. The present study describes an in situ technique that for the first time simultaneously measures surface temperature changes using near infrared thermal imaging and gas species using Fourier-transform infrared emission spectra at the anodes of operating SOFCs. Electrolytesupported SOFCs with Ni-based anodes are operated at 700 °C with internal, dry-reformed methane at 75% maximum current and at open circuit voltage (OCV) while electrochemical and optical measurements are collected. At OCV, more cooling is observed coincident with more CO reforming products. Under load, CO is depleted while the anode cools less, especially near the current collectors. The extent of cooling is more sensitive to polarization for electrolytesupported cells because their anodes are thinner relative to anode-supported cells. This study exemplifies how this duplex technique can be a useful probe of electrochemical processes in SOFCs.

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Section: Introductionmentioning

confidence: 99%

In situ, simultaneous thermal imaging and infrared molecular emission studies of solid oxide fuel cell electrodes

Kirtley

Qadri

Steinhurst

et al. 2016

Journal of Power Sources

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“…This method is highly suitable for the detection of surface species and adsorbates and could show even greater potential when more stable and/or thinner coatings can be produced. 92,93 …”

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confidence: 99%

Surface- and Tip-Enhanced Raman Spectroscopy in Catalysis

Hartman

Wondergem

Kumar

et al. 2016

J. Phys. Chem. Lett.

158

145

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Surface- and tip-enhanced Raman spectroscopy (SERS and TERS) techniques exhibit highly localized chemical sensitivity, making them ideal for studying chemical reactions, including processes at catalytic surfaces. Catalyst structures, adsorbates, and reaction intermediates can be observed in low quantities at hot spots where electromagnetic fields are the strongest, providing ample opportunities to elucidate reaction mechanisms. Moreover, under ideal measurement conditions, it can even be used to trigger chemical reactions. However, factors such as substrate instability and insufficient signal enhancement still limit the applicability of SERS and TERS in the field of catalysis. By the use of sophisticated colloidal synthesis methods and advanced techniques, such as shell-isolated nanoparticle-enhanced Raman spectroscopy, these challenges could be overcome.

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“…Vibrational Raman spectroscopy has become increasingly attractive for high‐temperature applications when noninvasive, molecularly specific information is needed in real time and when alternatives such as X‐ray or electron beam‐based techniques are difficult or costly to implement. For example, in situ Raman spectroscopy has been used to investigate materials within high‐pressure/high‐temperature environments to understand phase changes and estimate local temperatures, solid oxide fuel cell studies under electrochemical control, and glass melts up to ~1,400 °C to determine that the technique is feasible as an online process sensor . The technique has also demonstrated success as a remote sensor for hazardous and explosive materials, as well as minerals …”

Section: Introductionmentioning

confidence: 99%

A comparison of pulsed and continuous lasers for high‐temperature Raman measurements of anhydrite

Kirtley

Leichner

Anderson

et al. 2018

J Raman Spectroscopy

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Oxygen carrier particles (OCPs) serve as fuel oxidant in emerging chemical looping combustion systems. However, chemical looping combustion process optimization is hindered by the lack of online sensors for measurements of OCP oxidation states at temperatures up to 1,000 °C and pressures up to 10 atm. We are investigating Raman spectroscopy as a potential solution, as this technique is known for its ability to provide noninvasive, molecularly specific information in real time in a wide variety of applications. As a case study, Raman spectra from high‐temperature (>1,000 °C) anhydrite, a potential OCP, are presented using pulsed and continuous wave excitation at 532 nm. When pulsed excitation is coupled with time‐gated detection, background signal from thermal radiation can be significantly reduced from single pulse spectra, outperforming results using an ungated detector. Also, laser heating of the sample is not observed but laser‐induced breakdown spectra increasingly appear with increasing temperature and pulse intensity. Compared with pulsed excitation, continuous wave excitation with longer acquisition time, offers higher signal to noise and avoids the risk for laser‐induced breakdown spectra but demonstrates minor sample heating. Finally, the data demonstrate practical utility by (a) providing a calibration of anhydrite's ν1 (1,017 cm−1) Raman temperature‐dependent band position and by (b) providing estimates of temperature using the ratios of the Stokes/anti‐Stokes ν1 integrated intensities. These results demonstrate the first high‐temperature, pulsed Raman spectra from anhydrite while evaluating challenges associated with high‐temperature, Raman measurements of OCP materials in general.

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An operando surface enhanced Raman spectroscopy (SERS) study of carbon deposition on SOFC anodes

Cited by 37 publications

References 35 publications

In situ, simultaneous thermal imaging and infrared molecular emission studies of solid oxide fuel cell electrodes

In situ, simultaneous thermal imaging and infrared molecular emission studies of solid oxide fuel cell electrodes

Surface- and Tip-Enhanced Raman Spectroscopy in Catalysis

A comparison of pulsed and continuous lasers for high‐temperature Raman measurements of anhydrite

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