Observing the Surface Termination of LaScO3 Perovskite Using Solid-State Nuclear Magnetic Resonance

Zhao, Tommy Yunpu; Greenstein, Emily P.; Peczak, Ian L.; Poeppelmeier, Kenneth R.; Perras, Frédéric A.

doi:10.1021/jacs.4c07055

Observing the Surface Termination of LaScO₃ Perovskite Using Solid-State Nuclear Magnetic Resonance

Journal Article · Wed Aug 07 00:00:00 EDT 2024 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.4c07055· OSTI ID:2434273

^[1]; ^[2]; Peczak, Ian L. ^[2]; ^[2]; ^[3]

Ames Laboratory (AMES), Ames, IA (United States)
Northwestern University, Evanston, IL (United States)
Ames Laboratory (AMES), Ames, IA (United States); Iowa State University, Ames, IA (United States)

Materials with well-defined surfaces are drawing increased attention for the design of bespoke catalysts and nanomaterials. Gaining a detailed understanding of the surfaces of these materials is an important challenge, which is often complicated by surface polymorphism and dynamic restructuring. We introduce the use of surface-enhanced NMR spectroscopy for the observation of such surfaces, focusing on LaScO₃ as an example. Here, we show that double-resonance NMR experiments correlating surface oxygen and probe molecules to the ¹³⁹La and ⁴⁵Sc nuclei at the surface reveal the material to be terminated by a ScO_x monolayer. Surface-selective ¹⁷O and ⁴⁵Sc NMR experiments further showed the material to be hydroxyl terminated and that the surface may be prone to dynamic restructuring as a result of moisture exposure. Perhaps most interestingly, surface-selective ¹³⁹La NMR experiments revealed the existence of previously undetected surface lanthanum defects, suggesting that surface-enhanced NMR may be useful as a guide in the synthesis of defect-free surfaces in the design of various nanomaterials.

View Accepted Manuscript (DOE)

Research Organization:: Ames Laboratory (AMES), Ames, IA (United States); Northwestern University, Evanston, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-07CH11358; FG02-03ER15457

OSTI ID:: 2434273

Alternate ID(s):: OSTI ID: 2480926

Report Number(s):: IS-J--11,401

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 33 Vol. 146; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Observing the Surface Termination of LaScO3 Perovskite Using Solid-State Nuclear Magnetic Resonance

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Observing the Surface Termination of LaScO₃ Perovskite Using Solid-State Nuclear Magnetic Resonance