MICROSCOPY, NEUTRON AND X-RAY SCATTERING CAPABILITIES

Advanced Scanning Electron Microscopy (SEM) and Spectroscopy

  • Zeiss Merlin VP SEM
    This SEM features variable-pressure capability to optimize studies of nonconductive samples or samples with low vapor pressures. Equipped with BF-STEM detector, surface profile backscatter imaging, and EDS spectroscopy.
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Advanced Transmission Electron Microscopy (TEM), Scanning Transmission Electron Microscopy (STEM), Electron Energy Loss Spectroscopy (EELS), and Energy Dispersive Spectroscopy (EDS)

  • Soft Matter TEM (Zeiss Libra 120 TEM)
    This TEM features variable voltage (60 to 120 kV) and offers enhanced capabilities for studies of soft nanomaterials while maintaining precision needed for work in catalysts and other “hard” nanomaterials. The instrument is equipped with in-line EELS, providing real-time energy filtered imaging, high angular resolution nano-diffraction, and has cryogenic specimen-loading capabilities. Coupled with user access to higher-voltage and aberration-corrected instruments through the SHaRE user proposal appendix, this new low-voltage TEM offers CNMS users direct access to a very broad range of TEM capabilities.
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  • Hitachi HF3300 high-resolution TEM-STEM
    Instrument combines high-resolution TEM structure imaging (<1.2Å) with high-resolution STEM (HAADF and BF) detectors and a secondary electron (SE) detector for SEM imaging. Primary operation is conducted at 300 kV. Microscope features a Gatan Quantum EELS/GIF and a Bruker silicon drift detector (SDD) for EDS spectrum imaging. Specialized in-situ holders are available for heating (up to 1200°C Protochips Aduro), cryo-transfer (Gatan CT3500), Hitachi 360° rotation micropillar tomography, nanoindenter (Hysitron), and liquid flow cell (Hummingbird).
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  • Nion UltraSTEM 100 (U100) dedicated aberration-corrected STEM Instrument features a 3rd-generation C3/C5 aberration corrector, 0.5 nA current in atomic-size probe, ~1.0-1.1Å HAADF-STEM imaging resolution at 60 kV and 100 kV operating voltages. The Nion U100 features a Gatan Enfina EELS and a cold FEG for energy resolutions <350 meV at 100kV. This instrument has an unparalleled combination of atomic-resolution imaging and spectroscopy at mid- and low-voltages, and is especially valuable for the characterization of 2-dimensional materials (graphene, BN, transition metal dichalcogenides, etc.), catalysts, and other beam-sensitive materials.
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  • FEI Titan S aberration-corrected TEM-STEM
    Probe-corrected microscope features a Gatan Quantum EELS and Gatan Imaging Filter (GIF), with dual-EELS and fast spectrum imaging capabilities, an ‘extreme Schottky’ high-brightness field emission gun (X-FEG), and variable operating voltages (60, 120, and 300 kV). Instrument is equipped with high-angle annular dark field (HAADF), annual dark field (ADF), and bright field (BF) STEM detectors for sub-Å imaging.  Specialized in-situ holders are available for experiments requiring heating (up to 1200°C – Protochips Aduro), biasing (Protochips PE), Nanofactory AFM/STM, liquid cell electrochemistry (Protochips Poseidon 500), electron tomography (both high-tilt and 360° rotation), and LN2-cooling.
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Instruments for Atom Probe Tomography (APT)

  • Cameca Instruments Local Electrode Atom Probe (LEAP) 4000X HR
    Advanced LEAP features a 1 MHz laser and 200 kHz high-voltage pulse generator, reflectron energy compensating lens, and a crossed delay line, single atom, position-sensitive detector. Instrument is used for the atomic level 3-dimensional compositional characterization of a wide range of materials, including metallic conductors, semi-conductors, oxides, and nanostructured materials.
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  • FEI Nova 200 dual beam focused ion beam (FIB)-SEM
    The FIB is dedicated to precision preparation and annular milling of needles required for APT, and is equipped with an annual STEM detector for site-specific FIB-milling, a Kleindiek nano-manipulator, and EDS.
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Helium-ion Microscopy

  • Zeiss Orion NanoFab
    The Zeiss Orion Nanofab helium-ion microscope (HIM) features three primary capabilities: imaging, detailed ion-milling/patterning using He-ions, and high-rate milling using heavier Neon ions. It is located in the CNMS cleanroom to facilitate clean transfer of samples.

    This instrument has the ability to image, in the manner of an SEM, at unprecedented resolution and with high surface sensitivity; and the ability to pattern through direct ion-milling and exposure of lithographic resists, down to feature sizes of about 5 nm. The instrument is complementary to a Focused Ion Beam (FIB), but capable of feature sizes 10-20 times smaller. Scientifically, the instrument allows users to explore entirely new types of devices and engineered nanostructures that cannot be fabricated with other techniques.
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X-ray Diffraction

  • 2-circle X-ray diffraction
    0-20 X-ray powder diffraction with temperature-controlled sample environment. 77K to 1200K at 1 Bar, 273K to 1200K up to 10 Bar. Reactive gasses such as H2, CO for varying chemical composition in sample environment.
  • • 4-circle X-ray diffraction
    4-circle plus translation stage, high temperature, in-plane thin film diffraction. Also texture, reflectivity, microdiffraction, reciprocal space mapping.
  • • Small-angle X-ray scattering, SAXS
    Anton Paar SAXSess instrument for small-angle scattering to obtain nanoscale structural information. Also equipped for grazing-incidence measurements on nanomaterial films.
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Neutron Scattering

  • CNMS users are encouraged to take advantage of the world-class neutron scattering facilities that are available at ORNL’s High-Flux Isotope Reactor (HFIR) and the Spallation Neutron Source (SNS). Beamlines of particular relevance to CNMS Scientific Themes include the small-angle scattering and diffractometry instruments on the HFIR cold source, HFIR thermal neutron diffraction and spectroscopy capabilities, and instruments at the SNS including the backscattering spectrometer and the liquids and magnetism reflectometers. Please visit the ORNL Neutron Sciences website for more information about these neutron scattering facilities.

    CNMS users who would like to incorporate neutron scattering as a supporting component in their user proposals may request neutron beamtime by checking the appropriate box on the CNMS proposal form and attaching the 2-page Neutron Scattering appendix to provide details of their beamtime request. However, if the primary thrust of the proposal is to obtain access to neutron scattering, prospective users must submit the proposal directly to the neutron scattering user program.

Capabilities provided by other CNMS groups