Electron Microscopy for Materials Characterization

National Laboratory: 
Pacific Northwest National Laboratory
Characterization Class: 
Extreme Environment Testing
Microscopy
Description: 

The materials science and characterization facilities at Pacific Northwest National Laboratory are home to a suite of high-resolution analytical microscopes that support characterization of base metal, welds, phase analyses, HAZ composites, grain boundaries, and fracture surfaces. Specific to lightweight alloy development, these capabilities align well in the areas of carbide and precipitate analyses. Instrumentation can be used for low-level radioactive, as well as non-radioactive sample analysis. The microscopy suite includes a recently purchased probe-corrected JEOL ARM200-CF, fully equipped with the latest in analytical detectors, including a high-collection-angle Centurio silicon drift detector for x-ray spectroscopy, a Gatan Quantum 965 GIF, and a high-angle dark field detector. The Cs probe correction produces probes less than 0.1 nm in diameter with high beam currents, enabling atomic-level analysis from both a structural and chemical standpoint. A JEOL 7600F field emission scanning electron microscope, an FEI Quanta 3D focused ion beam (FIB) scanning electron microscope, and a JEOL microprobe also are available for characterization work. These instruments enable energy dispersive x-ray spectroscopy, wavelength dispersive x-ray spectroscopy, and electron backscatter diffraction at the nanometer scale. A Cameca LEAP 4000XHR 3D atom probe tomography instrument is available for interrogation of the microchemistries present at grain boundaries, phase boundaries, and crack tips, as well as radiation-induced effects in grain interiors.

Capability Bounds: 

Physical dimensions of scanning electron microscopy specimens are limited by the type of analysis needed. Up to 2.5-in. diameter specimens can be accommodated for imaging and compositional evaluation. PNNL Electron Backscatter Diffraction specimens are restricted to 0.75 in. × 0.5 in. × 0.5 in. Transmission electron microscopy specimens are thinned to electron transparency.

Unique Aspects: 

The entire suite of analytical instrumentation can be used can be used for low-level and non-radioactive sample analyses.

Availability: 

To assess and use the Rad Annex FIB and microprobe, work proposals must be submitted and approved by the Environmental Molecular Sciences Laboratory.

Single Point of Contact: 

Name: Nicole R. Overman
Email: Nicole.Overman@pnnl.gov
Phone: 509- 375-1913

References: 
  1. Yan, Pengfei; et.al. Probing the Degradation Mechanism of Li2MnO3 Cathode for Li-Ion Batteries. Chem. Mater. 2015 DOI: 10.1021/cm504257m
  2. Yan, Pengfei; et.al. Atomic Resolution Visualization of Distinctive Chemical Mixing Behavior of Ni, Co, and Mn with Li in Layered Lithium Transition Metal Oxide Cathode Materials. Chem. Mater. 2015 DOI: 10.1021/acs.chemmater.5b02016
  3. Perea DE et. al. "Determining the Location and Nearest Neighbors of Aluminum in Zeolites with Atom Probe Tomography."Nature Communications” 2015. doi:10.1038/ncomms8589
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