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Argon Milling of Bulk and Post-FIB Specimens for Multi-Length Scale Analyses by EBSD, TEM, and APT under Controlled Environments

Journal Article · · Microscopy and Microanalysis
 [1];  [2];  [1];  [1];  [1]
  1. E.A. Fischione Instruments, Inc., Export, PA (United States)
  2. Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)
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Correlative investigations involve structural characterization by transmission electron microscopy (TEM) combined with compositional analysis by atom probe tomography (APT) using the same specimen. A critical component of successful correlative analyses is specimen preparation; probing individual atoms requires a surface and subsurface with minimal defects, beginning with the bulk material through to the prepared specimen for TEM or APT analysis. Our previous work showed that low-energy concentrated ion beam Ar ion milling improves TEM [1] and APT [2,3] specimen quality by removing surface oxides and Ga damage caused by focused ion beam (FIB) preparation. Further enhancement in specimen quality of APT specimens is achieved in the established workflow under controlled environments, as shown in [4]. In this work, we present specimen preparation using Ar ion milling techniques not only for the APT specimen, but also the bulk sample for subsequent multi-length scale analyses by electron backscatter diffraction (EBSD), TEM, and APT under controlled environments. The removal of surface damage and oxidation, which is crucial for probing atomic layer specimens by broad and concentrated Ar ion beam milling techniques under controlled environments, is highlighted.

Research Organization:
Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)
Sponsoring Organization:
USDOE
Grant/Contract Number:
AC05-76RL01830
OSTI ID:
1987545
Report Number(s):
PNNL-SA-176773
Journal Information:
Microscopy and Microanalysis, Journal Name: Microscopy and Microanalysis Journal Issue: S1 Vol. 28; ISSN 1431-9276
Publisher:
Microscopy Society of America (MSA)Copyright Statement
Country of Publication:
United States
Language:
English

References (3)

A Small Spot, Inert Gas, Ion Milling Process as a Complementary Technique to Focused Ion Beam Specimen Preparation journal June 2017
Post-FIB Specimen Preparation of Atom Probe Specimens under Controlled Environments for Correlative Microscopy journal August 2019
Optimal Specimen Preparation for Correlative Atom Probe Tomography and Electron Microscopy of Environmentally Sensitive Materials journal July 2021

Figures / Tables (2)

Figure 1(p. 2)figure Figure 1
Figure 2(p. 2)figure Figure 2

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Related Subjects

36 MATERIALS SCIENCE
chemistry
environmentally sensitive materials
materials science