Methodologies for operando ATR-IR spectroscopy of magnesium battery electrolytes

Rudra N. Samajdar; Scott A. Brown; Shravan K. Kairy; Stuart D. Robertson; Andrew J. Wain

doi:10.1021/acs.analchem.2c02843

Methodologies for operando ATR-IR spectroscopy of magnesium battery electrolytes

Rudra N. Samajdar, Scott A. Brown, Shravan K. Kairy, Stuart D. Robertson, Andrew J. Wain

Pure And Applied Chemistry

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Abstract

We explore the suitability of operando attenuated total reflection infrared (ATR-IR) spectroscopy methodologies for the study of organoaluminate electrolytes for Mg battery applications. The "all-phenyl complex" in tetrahydrofuran (THF), with the molecular structure [Mg Cl ·6THF] [AlPh ] , is used as an exemplar electrolyte to compare two different spectroelectrochemical cell configurations. In one case, a Pt gauze is used as a working electrode, while in the second case, a thin (∼10 nm) Pt film working electrode is deposited directly on the surface of the ATR crystal. Spectroscopic measurements indicate substantial differences in the ATR-IR response for the two configurations, reflecting the different spatial arrangements of the working electrode with respect to the ATR sampling volume. The relative merits and potential pitfalls associated with the two approaches are discussed.

Original language	English
Pages (from-to)	14985-14993
Number of pages	9
Journal	Analytical Chemistry
Volume	94
Issue number	43
Early online date	19 Oct 2022
DOIs	https://doi.org/10.1021/acs.analchem.2c02843
Publication status	Published - 1 Nov 2022

Keywords

analytical chemistry
spectroscopy
electric batteries

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10.1021/acs.analchem.2c02843

Samajdar-etal-AC-2022-Methodologies-for-operando-ATR-IR-spectroscopyAccepted author manuscript, 1 MBLicence: Strath_1

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title = "Methodologies for operando ATR-IR spectroscopy of magnesium battery electrolytes",

abstract = "We explore the suitability of operando attenuated total reflection infrared (ATR-IR) spectroscopy methodologies for the study of organoaluminate electrolytes for Mg battery applications. The {"}all-phenyl complex{"} in tetrahydrofuran (THF), with the molecular structure [Mg Cl ·6THF] [AlPh ] , is used as an exemplar electrolyte to compare two different spectroelectrochemical cell configurations. In one case, a Pt gauze is used as a working electrode, while in the second case, a thin (∼10 nm) Pt film working electrode is deposited directly on the surface of the ATR crystal. Spectroscopic measurements indicate substantial differences in the ATR-IR response for the two configurations, reflecting the different spatial arrangements of the working electrode with respect to the ATR sampling volume. The relative merits and potential pitfalls associated with the two approaches are discussed.",

keywords = "analytical chemistry, spectroscopy, electric batteries",

author = "Samajdar, {Rudra N.} and Brown, {Scott A.} and Kairy, {Shravan K.} and Robertson, {Stuart D.} and Wain, {Andrew J.}",

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doi = "10.1021/acs.analchem.2c02843",

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T1 - Methodologies for operando ATR-IR spectroscopy of magnesium battery electrolytes

AU - Samajdar, Rudra N.

AU - Brown, Scott A.

AU - Kairy, Shravan K.

AU - Robertson, Stuart D.

AU - Wain, Andrew J.

PY - 2022/11/1

Y1 - 2022/11/1

N2 - We explore the suitability of operando attenuated total reflection infrared (ATR-IR) spectroscopy methodologies for the study of organoaluminate electrolytes for Mg battery applications. The "all-phenyl complex" in tetrahydrofuran (THF), with the molecular structure [Mg Cl ·6THF] [AlPh ] , is used as an exemplar electrolyte to compare two different spectroelectrochemical cell configurations. In one case, a Pt gauze is used as a working electrode, while in the second case, a thin (∼10 nm) Pt film working electrode is deposited directly on the surface of the ATR crystal. Spectroscopic measurements indicate substantial differences in the ATR-IR response for the two configurations, reflecting the different spatial arrangements of the working electrode with respect to the ATR sampling volume. The relative merits and potential pitfalls associated with the two approaches are discussed.

AB - We explore the suitability of operando attenuated total reflection infrared (ATR-IR) spectroscopy methodologies for the study of organoaluminate electrolytes for Mg battery applications. The "all-phenyl complex" in tetrahydrofuran (THF), with the molecular structure [Mg Cl ·6THF] [AlPh ] , is used as an exemplar electrolyte to compare two different spectroelectrochemical cell configurations. In one case, a Pt gauze is used as a working electrode, while in the second case, a thin (∼10 nm) Pt film working electrode is deposited directly on the surface of the ATR crystal. Spectroscopic measurements indicate substantial differences in the ATR-IR response for the two configurations, reflecting the different spatial arrangements of the working electrode with respect to the ATR sampling volume. The relative merits and potential pitfalls associated with the two approaches are discussed.

KW - analytical chemistry

KW - spectroscopy

KW - electric batteries

U2 - 10.1021/acs.analchem.2c02843

DO - 10.1021/acs.analchem.2c02843

M3 - Article

SN - 0003-2700

VL - 94

SP - 14985

EP - 14993

JO - Analytical Chemistry

JF - Analytical Chemistry

IS - 43

ER -

Methodologies for operando ATR-IR spectroscopy of magnesium battery electrolytes

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