Early-stage NiCrMo oxidation revealed by cryo-transmission electron microscopy

Alex Y.W. Lin, Alexander Müller, Xiao xiang Yu, Andrew M. Minor, Laurence D. Marks*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

1 Scopus citations


Hydroxide formation at the surface of corroded alloys is critical for understanding early-stage oxidation of many corrosion-resistant alloys. Many hydroxides are unstable in an ambient environment and are electron-beam sensitive, limiting the use of conventionally-prepared specimens for transmission electron microscopy characterization of these alloy-water interfaces. In order to avoid sample dehydration, NiCrMo alloys corroded in a Cl -containing electrolyte solution were cryo-immobilized by plunge freezing. A cryo-focused ion beam microscope was used to thin the sample to electron transparency, while preserving the alloy-water interface, and the sample was then cryo-transferred to a transmission electron microscope for imaging and diffraction. The presence of rocksalt Ni 1-x Cr 2x/3 O and β-Ni 1-x Cr 2x/3 (OH) 2 phases and their orientational relationship to the underlying alloy were observed with electron diffraction, confirming the preservation of the surface structure through the fully-cryogenic sample preparation and analysis.

Original languageEnglish (US)
Pages (from-to)6-11
Number of pages6
StatePublished - May 2019


  • Corrosion
  • Cryo-focused ion beam milling
  • Cryo-transmission electron microscopy
  • Hydroxide growth
  • Sample preparation

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Atomic and Molecular Physics, and Optics
  • Instrumentation


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