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

doi:10.1016/j.ultramic.2019.01.012

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

Materials Science and Engineering

Research output: Contribution to journal › Article › peer-review

3 Scopus citations

Abstract

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 language	English (US)
Pages (from-to)	6-11
Number of pages	6
Journal	Ultramicroscopy
Volume	200
DOIs	https://doi.org/10.1016/j.ultramic.2019.01.012
State	Published - May 2019

Funding

The authors gratefully acknowledge funding from the Office of Naval Research MURI on contract no. N00014-16-1-2280 and the National Science Foundation on grant no. CMMI-1400618 . Work at the Molecular Foundry was supported by the Office of Science , Office of Basic Energy Sciences , of the US Department of Energy under contract no. DE-AC02-05CH11231 . We thank John R. Scully ( University of Virginia ) for providing the samples used in this study and Frances Allen ( University of California, Berkeley ) for helpful discussions. The authors gratefully acknowledge funding from the Office of Naval Research MURI on contract no. N00014-16-1-2280 and the National Science Foundation on grant no. CMMI-1400618. Work at the Molecular Foundry was supported by the Office of Science, Office of Basic Energy Sciences, of the US Department of Energy under contract no. DE-AC02-05CH11231. We thank John R. Scully (University of Virginia) for providing the samples used in this study and Frances Allen (University of California, Berkeley) for helpful discussions.

Keywords

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

ASJC Scopus subject areas

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

Access to Document

10.1016/j.ultramic.2019.01.012

Cite this

@article{495646c45f404939bb6c4bb5f52a42a2,

title = "Early-stage NiCrMo oxidation revealed by cryo-transmission electron microscopy",

abstract = " 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.",

keywords = "Corrosion, Cryo-focused ion beam milling, Cryo-transmission electron microscopy, Hydroxide growth, Sample preparation",

author = "Lin, {Alex Y.W.} and Alexander M{\"u}ller and Yu, {Xiao xiang} and Minor, {Andrew M.} and Marks, {Laurence D.}",

note = "Publisher Copyright: {\textcopyright} 2019 Elsevier B.V.",

year = "2019",

month = may,

doi = "10.1016/j.ultramic.2019.01.012",

language = "English (US)",

volume = "200",

pages = "6--11",

journal = "Ultramicroscopy",

issn = "0304-3991",

publisher = "Elsevier",

}

TY - JOUR

T1 - Early-stage NiCrMo oxidation revealed by cryo-transmission electron microscopy

AU - Lin, Alex Y.W.

AU - Müller, Alexander

AU - Yu, Xiao xiang

AU - Minor, Andrew M.

AU - Marks, Laurence D.

PY - 2019/5

Y1 - 2019/5

N2 - 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.

AB - 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.

KW - Corrosion

KW - Cryo-focused ion beam milling

KW - Cryo-transmission electron microscopy

KW - Hydroxide growth

KW - Sample preparation

UR - http://www.scopus.com/inward/record.url?scp=85061664402&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=85061664402&partnerID=8YFLogxK

U2 - 10.1016/j.ultramic.2019.01.012

DO - 10.1016/j.ultramic.2019.01.012

M3 - Article

C2 - 30797183

AN - SCOPUS:85061664402

SN - 0304-3991

VL - 200

SP - 6

EP - 11

JO - Ultramicroscopy

JF - Ultramicroscopy

ER -

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

Abstract

Funding

Keywords

ASJC Scopus subject areas

Access to Document

Other files and links

Fingerprint

Cite this