Low-Temperature Nitridation of Fe<sub>3</sub>O<sub>4</sub> by Reaction with NaNH<sub>2</sub>
نویسندگان
چکیده
Low-temperature soft chemical synthesis routes to transition-metal nitrides are of interest as an alternative conventional high-temperature ammonolysis reactions involving large volumes chemotoxic NH3 gas. One such method is the reaction between metal oxides and NaNH2 at ca. 200 °C yield counterpart nitrides; however, there remains uncertainty regarding mechanism product phase assemblage (in particular, noncrystalline components). Here, we extend tool box mechanistic understanding reactions, demonstrating nitridation Fe3O4 by with 170–190 °C, via a pseudomorphic reaction. The more reduced precursor enabled nitride formation lower temperatures than previously reported equivalent Fe2O3. assemblage, characterized X-ray diffraction, thermogravimetric analysis, 57Fe Mössbauer spectroscopy, comprised 49–59 mol % ε-Fe2+xN, accompanied 29–39 FeO1–xNx 8–14 γ″-FeN. oxynitride was apparently in recovered but could be crystallized heating 180 °C. Although achieved oxide NaNH2, it evident from this investigation that may complex, which prove limitation if objective produce single-phase well-defined electrical, magnetic, or other physical properties for applications. However, significant identified study opens possibility metastable phases high yield, substrate either careful control H2O concentration system postsynthetic hydrolysis crystallization.
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ژورنال
عنوان ژورنال: Inorganic Chemistry
سال: 2021
ISSN: ['0020-1669', '1520-510X']
DOI: https://doi.org/10.1021/acs.inorgchem.0c03452