Abstract
Forming a stable solid electrolyte interphase (SEI) is critical for rechargeable batteries' performance and lifetime. Understanding its formation requires analytical techniques that provide molecular-level insight. Here, dynamic nuclear polarization (DNP) is utilized for the first time to enhance the sensitivity of solid-state NMR (ssNMR) spectroscopy to the SEI. The approach is demonstrated on reduced graphene oxide (rGO) cycled in Li-ion cells in natural abundance and 13C-enriched electrolyte solvents. Our results indicate that DNP enhances the signal of outer SEI layers, enabling detection of natural abundance 13C spectra from this component of the SEI on reasonable time frames. Furthermore, 13C-enriched electrolyte measurements at 100 K provide ample sensitivity without DNP due to the vast amount of SEI filling the rGO pores, thereby allowing differentiation of the inner and outer SEI layer composition. Developing this approach further will benefit the study of many electrode materials, equipping ssNMR with the necessary sensitivity to probe the SEI efficiently.
Highlights
Just Accepted “Just Accepted” manuscripts have been peer-reviewed and accepted for publication
Our results indicate that dynamic nuclear polarization (DNP) enhances the signal of outer solid electrolyte interphase (SEI) layers, enabling detection of natural abundance
We demonstrate one approach to overcome these issues by using low temperature and dynamic nuclear polarization (DNP), the latter being a technique in which the large polarization of unpaired electrons is transferred to surrounding coupled nuclear spins by microwave (MW) irradiation
Summary
Just Accepted “Just Accepted” manuscripts have been peer-reviewed and accepted for publication. They are posted online prior to technical editing, formatting for publication and author proofing. “Just Accepted” manuscripts appear in full in PDF format accompanied by an HTML abstract. “Just Accepted” manuscripts have been fully peer reviewed, but should not be considered the official version of record. They are accessible to all readers and citable by the Digital Object Identifier (DOI®). The “Just Accepted” Web site may not include all articles that will be published in the journal. After a manuscript is technically edited and formatted, it will be removed from the “Just. No copyright claim is made to original U.S Government works, or works produced by employees of any Commonwealth realm Crown government in the course of their duties
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