Rapid assessment of automotive epoxy primers by electrochemical techniques

Soluble, redox-active, organic materials hold promise as charge-storage species for flow batteries; however, their stability during extended operation remains a key challenge. While a number of spectroscopic and electrochemical techniques are currently used to probe these complex and often ill-defined decay pathways, each technique has limitations, including accessibility and direct evaluation of practical electrolytes without preparatory steps. Here, we use microelectrode voltammetry to directly observe nonaqueous flow battery electrolytes, simultaneously identifying the rate of charged materials decay (reversible material loss) and total material decay (irreversible material loss). We validate this technique using ferrocene as a stable model redox couple, examine and address sources of error, and finally, demonstrate its capability by assessing the decay of a well-studied and moderately-stable substituted dialkoxybenzene [2,5-di-tert-butyl-1,4-bis(2-methoxyethoxy)benzene]. These results suggest that microelectrodes may have utility for rapid assessment of redox electrolyte state-of-charge and state-of-health, both in-operando and post-mortem.

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A Method for Evaluating Soluble Redox Couple Stability using Microelectrode Voltammetry

10.26434/chemrxiv.12331655 ◽

2020 ◽

Author(s):

Jeffrey Kowalski ◽

Alexis Fenton Jr ◽

Bertrand Neyhouse ◽

Fikile Brushett

Keyword(s):

Electrochemical Techniques ◽

Rapid Assessment ◽

Redox Couple ◽

Stable Model ◽

Material Loss ◽

Direct Evaluation ◽

Redox Electrolyte ◽

Redox Active ◽

Extended Operation ◽

In Operando

Soluble, redox-active, organic materials hold promise as charge-storage species for flow batteries; however, their stability during extended operation remains a key challenge. While a number of spectroscopic and electrochemical techniques are currently used to probe these complex and often ill-defined decay pathways, each technique has limitations, including accessibility and direct evaluation of practical electrolytes without preparatory steps. Here, we use microelectrode voltammetry to directly observe nonaqueous flow battery electrolytes, simultaneously identifying the rate of charged materials decay (reversible material loss) and total material decay (irreversible material loss). We validate this technique using ferrocene as a stable model redox couple, examine and address sources of error, and finally, demonstrate its capability by assessing the decay of a well-studied and moderately-stable substituted dialkoxybenzene [2,5-di-tert-butyl-1,4-bis(2-methoxyethoxy)benzene]. These results suggest that microelectrodes may have utility for rapid assessment of redox electrolyte state-of-charge and state-of-health, both in-operando and post-mortem.

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Zone-axis ALCHEMI for the rapid assessment of site occupancies in garnets

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100144905 ◽

1986 ◽

Vol 44 ◽

pp. 706-707

Author(s):

M.T. Otten ◽

P.R. Buseck

Keyword(s):

Single Crystals ◽

Rapid Assessment ◽

Site Occupancy ◽

Zone Axis ◽

Synthetic Compounds ◽

X Ray ◽

Large Group ◽

Crystallographic Planes

ALCHEMI (Atom Location by CHannelling-Enhanced Microanalysis) is a TEM technique for determining site occupancies in single crystals. The method uses the channelling of incident electrons along specific crystallographic planes. This channelling results in enhanced x-ray emission from the atoms on those planes, thereby providing the required site-occupancy information. ALCHEMI has been applied with success to spinel, olivine and feldspar. For the garnets, which form a large group of important minerals and synthetic compounds, the channelling effect is weaker, and significant results are more difficult to obtain. It was found, however, that the channelling effect is pronounced for low-index zone-axis orientations, yielding a method for assessing site occupancies that is rapid and easy to perform.

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