Transmission electron microscope project

Thermo-Fisher/FEI Spectra, 300 kV

The new S-TEM provides ultra-high resolution in characterizing both structure and energy, in addition to accurate quantitative chemical analysis down to sub-angstrom level
Utilizing this new S-TEM will benefit research in nuclear materials and behaviors (diffusion along phase boundaries, for example), bringing the highest resolution imaging and spectroscopic capabilities for nuclear science post-irradiation examination in the nation

Energy spread: 0.2 – 0.3 eV
Information limit: 60 pm
S-TEM resolution: 50 pm (125 pm @ 30 kV)

STEM 1.jpg?fit=scale&fm=pjpg&h=1024&ixlib=php 3.3 Thermo-Fisher/FEI Spectra, 300kV

Technical highlights:

  • Monochromated, probe- and image-corrected30 – 300 kV HT for various applications
  • Single electron sensitive S-TEM detection
  • Equipped with ultra-sensitive Panther S-TEM detection system - new detector geometry offers access to advanced S-TEM imaging capability combined with the sensitivity and detectability to measure single electronsSTEM 2.jpg?fit=scale&fm=pjpg&h=1024&ixlib=php 3.3 Thermo-Fisher/FEI Spectra, 300kV
  • Eight segmented BF and ADF detectors provide the possibility of combining detector segments in arbitrary ways
  • Integrated differential phase contrast (iDPC) imaging for the study of magnetic and electrical properties and for optimized Z-contrast imaging from hydrogen to uranium
  • Fully automated, single-click access to the highest-resolution S-TEM (<50 pm) and energy-resolution EELS (<30 meV), drift corrected frame integration (DCFI)
  • Field-free imaging in TEM Lorentz mode with 2 nm resolution for magnetic property studies
  • Super-X 4 detector EDS system (≤136 eV for Mn-Kα and 10 kcps (output)), Gatan Ultrafast EELS/DualEELS.
  • Electron microscope pixel array detector (EMPAD) – 4D-S-TEM
    Tilt range ±40 degrees for analytical double tilt holder, ±75 degrees for tomography holder
  • Electron Microscope Pixel Array Detector (EMPAD) records the full diffraction pattern in one scan. Once data is acquired, BF, DF and DPC can be extracted by applying mask.
  • Phase and defects can also be revealed by selecting the proper diffraction spots. EDS and 4D S-TEM mapping can be done simultaneously. Thickness can be obtained from analyzing CBED.

EDS & EELS

  • Super-X is composed of 4 highly sensitive detectors with a large collection solid angle. Absence of detector window allows the detection of all elements down to boron. In addition, no stage tilting is required. Much faster than the 1-detector EDS.
  • Gatan Continuum Ultrafast DualEELS can achieve the energy resolution between <0.025 eV and 1 eV. The detector can record two energy ranges at the same timeThe system can support simultaneous EDS and EELS data acquisition.

 

STEM 2 pic with Yaqiao.jpg?fit=scale&fm=pjpg&h=682&ixlib=php 3.3 Thermo-Fisher/FEI Spectra, 300kV

How CAES benefits
CAES was built to leverage the resources at the universities and national laboratory to help solve complex energy challenges and to help develop the next generation of energy workers. The TEM will support both these efforts. The need for a robust, skilled, and diverse workforce has never been higher as the nation's energy landscape shifts from carbon-based generation sources such as coal and natural gas to intermittent renewables. This shift has led to increased need for the research and development in energy storage and advanced nuclear reactors. The new TEM will help with the analysis and development of advanced materials that are critical to the nation's new energy landscape.

Initially, the TEM will be a part of the Microscopy and Characterization Suite (MaCS), a Nuclear Science User Facilities (NSUF) laboratory accessible to students and faculty at the CAES universities and to researchers all over the world. Private industry also has access to the lab's world-class microscopes and high-end imaging equipment. More than 1,000 visitors utilized the MaCS lab in FY19.

The ease of access of CAES not only applies to students, faculty and private industry; its proximity to INL's Energy Research Campus enables several INL mission areas to grow collaborative materials research programs with external partners, including the universities and industry. The S-TEM is INL's latest investment in CAES that is designed to create opportunities for collaborative materials research. CAES also is equipped with complementary materials analysis instrumentation (including a Focused Ion Bean and Local Electron Atom Probe) that will enable complete sample preparation and analysis in one location.

S TEM pics.jpg?fit=scale&fm=pjpg&h=682&ixlib=php 3.3 Thermo-Fisher/FEI Spectra, 300kV

Advanced Manufacturing focus area
The S-TEM is the centerpiece of a new Advanced Manufacturing Suite, and the TEM advances collaborative research, education, and innovation in several ways, including:

  • Its technological advances accelerate the timeline for nuclear innovation and modeling efforts needed to further the discovery and qualification of materials for nuclear applications, while allowing for the investigation of defects in functional energy materials found in batteries with atomic precision — a key step in improving battery performance.
  • It provides a new perspective on the dynamic effects of phenomena such as irradiation damage, diffusion mechanisms and kinetics, as well as plasticity, which all must be well understood to advance materials in extreme environments such as seen in a reactor core.
  • Its state-of-the-art atomic scale chemical imaging, paired with 3D tomography capability, enables new understanding of reacting interfaces of materials, providing immediate advances to collaborative CAES research currently under way in battery anodes, catalysis, and corrosion.