Micro-Notes from NMCF

Solvothermal synthesis procedures to obtain films of NU-901 and NU-100 with parallel orientation and perpendicular orientation (Verma et al. 2020)

Out of hundreds of papers, Prince K. Verma, a doctoral student in UVa's Department of Chemical Engineering, had his publication selected as one of the Top-Ten scientific peer-reviewed articles submitted for the Malvern Panalytical Scientific Award 2022. Verma's publication, "Controlling Polymorphism and Orientation of NU-901/NU-1000 Metal-Organic Framework Thin Films," was published in Chemistry of Materials in December 2020 (Chem. Mater. 202, 32, 24, 10556-10565). In this work, Verma's team investigates NU-1000, a zirconium (Zr)-based metal-organics frameswork (MOF), that is a promising candidate for heterogeneous catalysis, gas storage, electrocatalysis, and drug-delivery applications due to its large pore size and mesoporous structure.

For this research, the team utilized several of the NMCF instruments available to UVa students and researchers, including our Malvern Panalytical Empyrean X-ray Diffractometer for out-of-plane powder X-ray diffraction measurement; the FEI Quanta 650 Field-Emission Secondary Electron Microscope for imaging of the NU-901 & NU-1000 thin films, Au-Pd coated to improve conductivity with the Gatan 682 Precision Etching and Polishing System; and the PHI Versaprobe X-ray Photoelectron Specctrometer for surface concentration analysis.

NMCF's electron microscopy principal scientist, Helge Heinrich, co-authored this work.

Congratulations to Prince, Helge, and their co-authors!

UVa Environmental Science Students in Prof. Steve Macko's Geochemistry Class ( EVGE 7850 ) tour the X-ray Diffraction and X-ray Photoelectron Spectroscopy laboratories, where NMCF Scientists, DIane Dickie and Helge Heinrich, describe instrumentation and methods.

Last Friday, Oct. 28, 2022, graduate and undgraduate students in Prof. Steve Macko's Geochemistry (EVE 7850) took a short field trip from the Environmental Science department to the NMCF, where our staff (Diane Dickie and Helge Heinrich) demonstrated X-ray instrumentation. Dr. Dickie ran samples of table salt on the Empyrean X-ray Diffractometer (XRD) to determine the mineral composition, while Dr. Heinrich showed the students around the X-ray Photoelectron Spectrometer (XPS). Students learned what information can be learned from each instrument's spectra, as well as the types of samples appropriate for each analytical method.

NMCF Director Jim Howe has trained hundreds of students to utilize transmission electron microscopy (TEM) and high-resolution scanning-TEM at the University of Virginia. He is shown here with Ph.D. student Niquana Smith.

With his retirement from UVa, Professor Jim Howe has stepped down as Director of the UVa's Nanoscale Materials Characterization Facility (NMCF), a position he has held for more than 18 years. During his tenure, the NMCF has grown significantly in both instrumentation and personnel. The facility is now host to two state-of-the-art scanning transmission electron microscopes (STEMs) for atomic-resolution imaging and X-ray and energy-loss analysis at the atomic level, two scanning electron microscopes (SEMs) for high-resolution imaging and compositional characterization, a combined focused ion beam (FIB)-SEM for preparation of TEM samples and cross-sectional analysis, three X-ray diffractometers (XRDs) for identification and characterization of crystal structures, a mapping X-ray photoelectron spectrometer (XPS) for determination of material surface composition and chemistry, a combined confocal Raman spectrometer/atomic force microscope (AFM) to provide chemical analysis in combination of surface structure, an X-ray fluorescence spectrometer (XRF) for sensitive measurement of bulk composition, a Fourier-transform infrared spectrometer (FT-IR) for chemical bond analysis, and a complete suite of optical instruments and metallographic preparation facilities for determining the microstructure of materials. At the same time, NMCF staff has risen from a single member to a team of five professionals with varied characterization and analytical expertise.  Jim organized facility operation during the renovation of Jesser Hall and oversaw the development of remote training modules for instrumentation during the COVID shutdown. His strong advocacy, positive outlook, and scientific leadership within the NMCF will be missed. A replacement Director has not yet been named.

UVa's Nanoscale Materials Characterization Facility (NMCF) featured during SEAS annual public open house.

Saturday, April 23rd, 2022, our laboratory spaces were opened to the public.

Demonstrations by NMCF scientists and students were given during UVa's School of Engineering and Applied Science (SEAS) Open House, which included engineering school building tours and program visits.

This year's tours featured NMCF's new FEI Themis High-Resolution Scanning Transmission Electron Microscope (HR-STEM), the Helios Focused Ion Beam and Scanning Electron Microscope (FIB-SEM), the X-ray Diffraction Laboratory with both powder and single-crystal diffractometers (XRD) on display, as well the Versaprobe III Imaging X-ray Photoelectron Spectroscopic (XPS) Microscope.

Expert student users and scientists spent time describing each sophisticated instrument and materials characterization methodology, providing real-world examples to participants, as well as demonstrating the type of data acquired and answering questions.

Masks and COVID vaccinations are now optional at UVa and within the NMCF, including during for-credit laboratory classes.

If you have had close contact with someone who has recently tested positive for COVID, please wear a mask in the NMCF facilities per UVa policy.

If you have significant health concerns where universal masking is advised, please reach out to the appropriate NMCF instrument scientist or class instructor.

Details concerning UVa's COVID policy for staff & visitors can be found here.

Heads up if you use AZTtec software for your SEM/TEM analysis.

AztecTimed is no longer free to download, and has been updated.

AZtecTimed is now AZtecFlex and for students the licence is discounted, from ($1,399.00) to ($139.00). For more information on how to access this discount as a student, click here.

AZtecFlex is a 12-month personal subscription licence for installation on your desktop or laptop, designed to let you use AZtec anywhere and without needing to access shared facilities. 

AZtecFlex includes advanced data processing features, for example, particle analysis and EBSD data processing, allowing you to access them even if they aren’t enabled on the system used to acquire the data.  Your licence will also provide access to the latest AZtec release as soon as it is available.

Tutorials and Demos can be found here.

3D Reconstruction Software is now available on the NMCF Phenom Scanning Electron Microscope (SEM).

3D Reconstruction Software can generate three-dimensional images and provide submicrometer roughness measurements over areas and lines. Calculation of Rz, Rz, and Sa, as well as topographical surface scans and line scans can be acquired. Scans can be displayed as heat maps (image below) or as profiles. Data can be exported to be displayed in user software.

Details can be found here: https://www.thermofisher.com/us/en/home/electron-microscopy/products/software-em-3d-vis/3d-reconstruction-software.html

A brief User Guide is available on Sharepoint, and additional information can be found in the Phenom Manual.

Note that NMCF has a temporary license (expiration: 1 November 2021), so get your measurements in now!

Would this software would be a useful permanent addition to the SEM toolkit? Let NMCF know! (email: rrw3q@virginia.edu)