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<p>This study investigates the steam oxidation resistance of a TiN/TiAlN bilayer coating deposited on Zircaloy-4 (Zr-4) using cylindrical magnetron sputtering. The coated samples were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Raman Spectroscopy, X-ray Photon Spectroscopy (XPS), and weight gain measurements before and after exposure to a steam environment at 400&#xa0;°C and 10&#xa0;MPa for 72&#xa0;h. Post oxidation, the TiN/TiAlN bilayer developed a surface layer of anatase TiO<sub>2</sub>, while maintaining the structural integrity of the underlying coating. Cross-sectional SEM analysis confirmed the formation of a thin and compact TiO<sub>2</sub> layer (~ 250&#xa0;nm) on the TiN/TiAlN coating surface. XPS results revealed surface hydroxylation and the presence of sub-stoichiometric TiO<sub>x</sub> on the outer layer. Notable, nitrogen depletion was also observed, evidenced by the absence of N 1s peak, and the Ti 2p envelopes were dominated by Ti–O bonds. Wettability tests revealed a significant difference between the uncoated and coated samples. Post oxidation, the uncoated Zr-4 exhibited a hydrophilic response for, whereas the TiN/TiAlN bilayer retained its hydrophobicity. Weight gain measurements after steam oxidation at 400&#xa0;°C, 10&#xa0;MPa, 72&#xa0;h showed a nearly four-fold reduction for coated samples (~ 5.3&#xa0;mg·dm<sup>− 2</sup>) compared to the uncoated Zr-4 (~ 19.5&#xa0;mg·dm<sup>− 2</sup>). Further, high temperature steam oxidation behavior of coated samples was evaluated at 600&#xa0;°C and 700&#xa0;°C to assess its suitability for accident tolerant fuel (ATF) application. Superior oxidation resistance of TiN/TiAlN bilayer showcased enhanced protection, supporting its suitability under high temperature steam (up to 600&#xa0;°C) for Zr-4 fuel cladding tubes.</p>

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Steam oxidation kinetics of TiN/TiAlN bilayer deposited on plasma etched Zircaloy-4 substrates using cylindrical magnetron sputtering

  • 期刊论文

  • 发表日期：

    2026年5月20日

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  • Kunal Trivedi,
  • Ramkrishna Rane,
  • Kiran K. Mandapaka,
  • Alphonsa Joseph,
  • Supratik Roychowdhury,
  • Amit Arora

摘要

This study investigates the steam oxidation resistance of a TiN/TiAlN bilayer coating deposited on Zircaloy-4 (Zr-4) using cylindrical magnetron sputtering. The coated samples were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Raman Spectroscopy, X-ray Photon Spectroscopy (XPS), and weight gain measurements before and after exposure to a steam environment at 400 °C and 10 MPa for 72 h. Post oxidation, the TiN/TiAlN bilayer developed a surface layer of anatase TiO2, while maintaining the structural integrity of the underlying coating. Cross-sectional SEM analysis confirmed the formation of a thin and compact TiO2 layer (~ 250 nm) on the TiN/TiAlN coating surface. XPS results revealed surface hydroxylation and the presence of sub-stoichiometric TiOx on the outer layer. Notable, nitrogen depletion was also observed, evidenced by the absence of N 1s peak, and the Ti 2p envelopes were dominated by Ti–O bonds. Wettability tests revealed a significant difference between the uncoated and coated samples. Post oxidation, the uncoated Zr-4 exhibited a hydrophilic response for, whereas the TiN/TiAlN bilayer retained its hydrophobicity. Weight gain measurements after steam oxidation at 400 °C, 10 MPa, 72 h showed a nearly four-fold reduction for coated samples (~ 5.3 mg·dm− 2) compared to the uncoated Zr-4 (~ 19.5 mg·dm− 2). Further, high temperature steam oxidation behavior of coated samples was evaluated at 600 °C and 700 °C to assess its suitability for accident tolerant fuel (ATF) application. Superior oxidation resistance of TiN/TiAlN bilayer showcased enhanced protection, supporting its suitability under high temperature steam (up to 600 °C) for Zr-4 fuel cladding tubes.