Microanalysis of Materials

Materials MicroÅnalysis 

The MMÅ group seeks to understand materials’ structure, chemistry, and function through the development and application of analytical microscopy, atom probe tomography, in situ S/TEM and cryo-EM techniques.

• Atom Probe Tomography (Cameca LEAP 4000X HR)   

  • A local electrode atom probe (LEAP) with a UV, 250 kHz laser, a 200 kHz high-voltage pulse generator, reflectron energy compensating lens, and a single atom cross delay line position-sensitive detector. The instrument is used for the atomic level 3-dimensional compositional characterization (capable of sub-nm resolution and <10 ppm chemical sensitivity) of a wide range of materials, including metallic conductors, semi-conductors, oxides, insulators, and nanostructured materials.
    
    VIDEO - Atom Probe Facilities CNMS 

• FIB-preparation of atom probe needles (FEI Nova200)

  • The FIB is dedicated to the fabrication of site-selective needle shaped specimens required for APT. It is equipped with an annular STEM detector for site-specific FIB-milling, a Kleindiek nano-manipulator, and EDS.

• 300kV Aberration-corrected S/TEM-EELS (FEI Titan)

  • 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 and 300 kV). Instrument is equipped with high-angle annular dark field (HAADF), annular dark field (ADF), and bright field (BF) STEM detectors for sub-Å imaging. The FEI Titan-S aberration-corrected TEM/STEM is also equipped with a large active area (60mm²) EDAX silicon drift detector (SDD) for high-collection-efficiency energy dispersive X-ray spectroscopy (EDS) and specialized in-situ TEM holders: Protochips Atmosphere gas environmental cell holder for conducting in-situ gas reactions at pressures up to 1 atm and temperatures up to 1000°C,  Protochips Poseiden electrochemistry/liquid-flow holder for in-situ electrochemistry, Protochips Aduro electrical biasing and heating holder, Nanofactory in-situ AFM/STM electrical biasing holder, Fischione 3D electron tomography holder, and a Gatan LN₂ double-tilt cooling holder. The Titan is also equipped with a Gatan OneView CMOS camera with in-situ option for high-frame-rate image/video capture and a Gatan STEMx detector for 4D-STEM experiments.

• 30-200kV Aberration-corrected S/TEM-EELS (JEOL NeoARM)

  • Microscope is equipped with a cold-field emitter and JEOL ASCOR aberration corrector; microscope operates at 30 kV, 60 kV, 80kV, or 200 kV and under low-dose conditions. The microscope can be operated in TEM, STEM, and Lorentz modes and can acquire high-angle annular dark-field (HAADF), annular bright-field (ABF), bright-field (BF), secondary electron (SE), and backscatter electron (BSE) STEM images. The NEOARM is equipped with a pixelated detector, which is ideal for 4D-STEM experiments (e.g., differential phase contrast imaging, strain mapping, and ptychography). This instrument can also simultaneously acquire energy dispersive X-ray spectroscopy (EDS) using dual 100 mm² EDS detectors and electron energy-loss spectroscopy (EELS) data using a Gatan Quantum GIF. The NeoARM is also equipped with specialized holders: Hummingbird tomography and double-tilt Cryo-EM holders.

• 300kV Cryo-S/TEM (FEI Titan Krios G4) (Note: Coming Soon)

  • The dedicated Cryo-S/TEM uses a high brightness ‘extreme Schottky’ field emission gun (X-FEG) and operates at 300kV. It is equipped with an autoloader, phase plate, bright-field (BF) and annular dark-field (ADF) STEM detectors, automated TEM and STEM tomography data acquisition software, a Falcon 3EC direct electron camera for low-dose imaging, and a Gatan Continuum S electron energy-loss spectrometer for analytical characterization. Specialized Cryo-EM specimen preparation is also available. 

• 120kV Cryo-TEM (FEI Talos L120C) (Note: Coming Soon)

  • The dedicated high-throughput Cryo-TEM operates at 120kV.

• TEM Specimen Preparation (FIB, microtome, ion mill, etc.)

  • Leica EM UC7 Ultramicrotome
    The ultramicrotome is used to section materials with a diamond knife to electron transparency. Note: also equipped with a Leica EM FC7 for cryo-preparation of materials

  • ThermoFisher Scientific Vitrobot
    Automated vitrification system for the preparation of cryo-EM specimens.

  • Leica EM ICE
    High-pressure freezing instrument to prepare samples to liquid nitrogen temperature for Cryo-EM.

  • Fischione Instruments Model 1010 Ion Mill
    After mechanically thinning and polishing TEM samples, this instrument uses an argon ion beam to perform final ion-beam milling of the specimen to electron transparency. The stage can be cooled with liquid nitrogen for milling beam-sensitive materials.

  • Fischione Model 1040 Nanomill
    Ultra-low energy argon ion beam milling system for thinning TEM samples. Removes amorphous surface damage and Ga+ implantation from FIB-prepared TEM specimens and surface damage on conventionally prepared specimens.

  • Gatan Ilion Precision Cross-Section Milling System
    Broad beam argon ion milling system for preparing ultra-smooth surfaces for SEM and EBSD.