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Low-Temperature Synthesis of Titanium Oxynitride Nanoparticles.

ABSTRACT: The synthesis of transition metal oxynitrides is complicated by extreme reaction conditions such as high temperatures and/or high pressures. Here, we show an unprecedented solution-based synthesis of narrowly dispersed titanium oxynitride nanoparticles of cubic shape and average size of 65 nm. Their synthesis is performed by using titanium tetrafluoride and lithium nitride as precursors alongside trioctylphosphine oxide (TOPO) and cetrimonium bromide (CTAB) as stabilizers at temperatures as low as 250 °C. The obtained nanoparticles are characterized in terms of their shape and optical properties, as well as their crystalline rock-salt structure, as confirmed by XRD and HRTEM analysis. We also determine the composition and nitrogen content of the synthesized particles using XPS and EELS. Finally, we investigate the applicability of our titanium oxynitride nanoparticles by compounding them into carbon fiber electrodes to showcase their applicability in energy storage devices. Electrodes with titanium oxynitride nanoparticles exhibit increased capacity compared to the pure carbon material.

SUBMITTER: Jansen F

PROVIDER: S-EPMC8065472 | biostudies-literature | 2021 Mar

REPOSITORIES: biostudies-literature

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Low-Temperature Synthesis of Titanium Oxynitride Nanoparticles.

Jansen Felicitas F Hoffmann Andreas A Henkel Johanna J Rahimi Khosrow K Caumanns Tobias T Kuehne Alexander J C AJC

Nanomaterials (Basel, Switzerland) 20210326 4

The synthesis of transition metal oxynitrides is complicated by extreme reaction conditions such as high temperatures and/or high pressures. Here, we show an unprecedented solution-based synthesis of narrowly dispersed titanium oxynitride nanoparticles of cubic shape and average size of 65 nm. Their synthesis is performed by using titanium tetrafluoride and lithium nitride as precursors alongside trioctylphosphine oxide (TOPO) and cetrimonium bromide (CTAB) as stabilizers at temperatures as low ...[more]

PMID: 33810321

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Project description:In the present work, we report on a synergistic relationship between platinum nanoparticles and a titanium oxynitride support (TiOxNy/C) in the context of oxygen reduction reaction (ORR) catalysis. As demonstrated herein, this composite configuration results in significantly improved electrocatalytic activity toward the ORR relative to platinum dispersed on carbon support (Pt/C) at high overpotentials. Specifically, the ORR performance was assessed under an elevated mass transport regime using the modified floating electrode configuration, which enabled us to pursue the reaction closer to PEMFC-relevant current densities. A comprehensive investigation attributes the ORR performance increase to a strong interaction between platinum and the TiOxNy/C support. In particular, according to the generated strain maps obtained via scanning transmission electron microscopy (STEM), the Pt-TiOxNy/C analogue exhibits a more localized strain in Pt nanoparticles in comparison to that in the Pt/C sample. The altered Pt structure could explain the measured ORR activity trend via the d-band theory, which lowers the platinum surface coverage with ORR intermediates. In terms of the Pt particle size effect, our observation presents an anomaly as the Pt-TiOxNy/C analogue, despite having almost two times smaller nanoparticles (2.9 nm) compared to the Pt/C benchmark (4.8 nm), manifests higher specific activity. This provides a promising strategy to further lower the Pt loading and increase the ECSA without sacrificing the catalytic activity under fuel cell-relevant potentials. Apart from the ORR, the platinum-TiOxNy/C interaction is of a sufficient magnitude not to follow the typical particle size effect also in the context of other reactions such as CO stripping, hydrogen oxidation reaction, and water discharge. The trend for the latter is ascribed to the lower oxophilicity of Pt-based on electrochemical surface coverage analysis. Namely, a lower surface coverage with oxygenated species is found for the Pt-TiOxNy/C analogue. Further insights were provided by performing a detailed STEM characterization via the identical location mode (IL-STEM) in particular, via 4DSTEM acquisition. This disclosed that Pt particles are partially encapsulated within a thin layer of TiOxNy origin.

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Low-Temperature Synthesis of Titanium Oxynitride Nanoparticles.

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Low-Temperature Synthesis of Titanium Oxynitride Nanoparticles.

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