Formation of Fully Stoichiometric, Oxidation-State Pure Neptunium and Plutonium Dioxides from Molecular Precursors

Peterson, Appie; Kelly, Sheridon N.; Arino, Trevor; Gunther, S. Olivia; Ouellette, Erik T.; Wacker, Jennifer N.; Woods, Joshua J.; Teat, Simon J.; Lukens, Wayne W.; Arnold, John; Abergel, Rebecca J.; Minasian, Stefan G.

doi:10.1021/acs.inorgchem.4c02099

Formation of Fully Stoichiometric, Oxidation-State Pure Neptunium and Plutonium Dioxides from Molecular Precursors

Journal Article · Mon Sep 16 00:00:00 EDT 2024 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.4c02099· OSTI ID:2449670

Peterson, Appie ^[1]; Kelly, Sheridon N. ^[2]; Arino, Trevor ^[2]; Gunther, S. Olivia ^[1]; ^[2]; Wacker, Jennifer N. ^[1]; ^[1]; Teat, Simon J. ^[3]; ^[1]; ^[2]; ^[2]; ^[1]

Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States); University of California, Berkeley, CA (United States)
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)

Amidate-based ligands (N-(tert-butyl)isobutyramide, ITA) bind κ² to form homoleptic, 8-coordinate complexes with tetravalent ²³⁷Np (Np(ITA)₄, 1-Np) and ²⁴²Pu (Pu(ITA)₄, 1-Pu). These compounds complete an isostructural series from Th, U–Pu and allow for the direct comparison between many of the early actinides with stable tetravalent oxidation states by nuclear magnetic resonance (NMR) spectroscopy and single crystal X-ray diffraction (SCXRD). The molecular precursors are subjected to controlled thermolysis under mild conditions with the exclusion of exogenous air and moisture, facilitating the removal of the volatile organic ligands and ligand byproducts. The preformed metal–oxygen bond in the precursor, as well as the metal oxidation state, are maintained through the decomposition, forming fully stoichiometric, oxidation-state pure NpO₂ and PuO₂. Powder X-ray diffraction (PXRD), scanning transmission electron microscopy (STEM), and energy dispersive X-ray spectroscopy (EDS) elemental mapping supported the evaluation of these high-purity materials. This chemistry is applicable to a wide range of metals, including actinides, with accessible tetravalent oxidation states, and provides a consistent route to analytical standards of importance to the field of nuclear nonproliferation, forensics, and fundamental studies.

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Research Organization:: Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)

Sponsoring Organization:: USDOE National Nuclear Security Administration (NNSA), Office of Defense Nuclear Nonproliferation; USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 2449670

Alternate ID(s):: OSTI ID: 2477939

Journal Information:: Inorganic Chemistry, Journal Name: Inorganic Chemistry Journal Issue: 39 Vol. 63; ISSN 0020-1669

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
actinides
ligands
materials
organic polymers
organic reactions

Formation of Fully Stoichiometric, Oxidation-State Pure Neptunium and Plutonium Dioxides from Molecular Precursors

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