Overview and What’s New at the WCNT
Tuesday, October 6th
12:00 – 1:30 p.m. Central Time
Presented by Jerry Hunter, WCNT Director, UW–Madison
This presentation introduces the Wisconsin Centers for Nanoscale Technology and then covers the range of techniques available and discusses learning objectives for the webinar series. A broad outline of how the various techniques fit together to provide a comprehensive characterization and fabrication solution is also given. Additionally, recent capability enhancements at the WCNT are presented.
Introduction to SEM
Thursday, October 8th
12:00 – 1:30 p.m. Central Time
Presented by Lisa Chan, Zeiss
The Field-Emission Scanning Electron Microscope (FESEM) imaging and analysis capabilities are explored. FESEMs are used when application analysis requires single-nanometer resolution for surface examination.
The discussion starts with a basic FESEM overview, reviewing the major physical scanning microscope components, such as the electron column, specimen chamber, workstation and detectors (including x-ray spectroscopy). This overview includes diagrams of the major vacuum components in the electron beam column and the specimen chamber. Next, the various detectors, chamber cameras, sample stage specifications and sample mounting techniques are discussed. Additionally, applications for both materials science (metals, composites and polymers) and life science (animal and plant) are examined.
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Project Highlights
Epitaxial growth of III-V semiconductors and Heusler alloys on graphene-terminated substrates
Presented by Sebastian Manzo, UW–Madison, Materials Science and Engineering
Epitaxial growth on graphene-terminated substrates has attracted great interest due to the absence of strict lattice matching requirements associated with conventional semiconductor epitaxy. Yet, the microscopic mechanisms that allow for the epitaxial growth of single crystalline films on monolayer graphene remain mysterious. Our group is studying these mechanisms through the molecular beam epitaxial growth of Heusler alloys and III-V semiconductors on patterned, epitaxial and transferred graphene supported on a variety of substrates. Our aim is to investigate the diffusion and nucleation of adatoms on graphene and the effect of the graphene-substrate interface on the growth. We have successfully demonstrated the epitaxial growth of cubic and hexagonal Heusler compounds on graphene-terminated Al2O3. Additionally, we have synthesized single-crystalline films of GaSb on graphene-terminated GaSb (001) substrates. Despite the presence of the graphene interlayer, these films have epitaxial registry to the underlying substrate, as revealed by x-ray diffraction, reflection high energy electron diffraction, transmission electron microscopy and scanning electron microscopy.
Experimental Characterization of Stainless-steel Engine Valves Exposed to High-Temperature CO2 Environment
Presented by Iman Abdallah, UW–Madison, Engineering Physics
In the framework of a project in collaboration between University of Florida (UF), University of Wisconsin (UW) Federal-Mogul Powertrain (division of Tenneco), and Idaho National Lab (INL), corrosion modeling and experimental campaigns on two selected high chromium austenitic SS alloys used in engine valves are being carried out to predict materials lifetime. The overall objective of the project is to develop a mechanistic modeling tool to predict corrosion of Stainless-Steel (SS) engine valve at high temperature in prototypical environments. A new experimental setup has been installed at UW including a gold mirror transparent furnace equipped with a state-of-the-art control evaporation mixer used for well-controlled mixed carbon dioxide and water vapor corrosion experiments.
Direct Electron Detectors for Materials Science Applications
Tuesday, October 13th
12:00 – 1:30 p.m. Central Time
Presented by Barnaby Levin, Applications Scientist, Direct Electron
Project Highlights presented by:
- Chenyu Zhang, UW–Madison, Materials Science and Engineering
- Carter Francis, UW–Madison, Materials Science and Engineering
Introduction to Focused Ion Beam
Thursday, October 15th
12:00 – 1:30 p.m. Central Time
Presented by Rick Passey, Thermo-Fisher Scientific
The Focused Ion Beam/Scanning Electron Microscopy technique has been widely adopted by the materials science and biological communities because it offers both high-resolution imaging and the ability to deposit and remove material from nanometer-sized areas. This presentation will introduce the FIB-SEM technique and cover some of the most popular applications that use the technique.
Rick Passey is an SEM/DualBeam applications expert who has been with Thermo Fisher Scientific (formerly FEI) for 12 years. His experience covers a wide range of microscopes and techniques, from environmental SEMs to the plasma FIB. Prior to working with FEI, Rick spent 13 years as a Process Engineer with Hewlett Packard, leading an SEM/FIB laboratory, supporting materials characterization and failure analysis of inkjet and related technologies.
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Project Highlights
Efficient Preparation of TEM Lamellae from Heavy-Ion-Irradiated High-Entropy Alloys Using Focused-Ion Beams
Presented by Calvin Parkin, UW–Madison, Engineering Physics
Inside the core of a nuclear reactor, structural components are subjected to an array of harmful conditions. High temp and often pressure, corrosive coolants more exotic than steam, and a damaging radiation field where energetic particles born from fission displace atoms from the lattice site that then diffuse around to form extended defects. The speaker’s process for practice and preparation of TEM lamellae from irradiated specimens using both the Thermo/FEI Helios pFIB and Zeiss Auriga FIB is described. The high milling currents available on the Helios allow for long liftouts that can be thinned in two sections, while the Auriga allows for more precise and reliable final thinning. An example of a final product thin enough for TEM/STEM is shown.
Radiation-induced Segregation in SiC
Presented by Hongliang Zhang, UW–Madison, Engineering Physics
SiC has many great properties for nuclear application. Radiation-induced segregation (RIS) is one of the most dramatic changes in the materials under irradiation. It can cause changes in the structure and chemical of GBs, and significantly degrade the materials’ properties. Understanding RIS in SiC provides the necessary foundation to explain and predict the radiation effects on multiple material properties. The most important challenges in the RIS study include: 1.To find the clean, edge-on GBs. 2. To measure the misorientation and exact crystal index of the grains. With the help of FIB, EBSD and t-EBSD, these problems can be solved.
Atomic Force Microscopy – Overview and Recent Developments
Tuesday, October 20th
12:00 – 1:30 p.m. Central Time
Presented by John Thornton, Senior Applications Engineer, Bruker Nano Surfaces
The field of Atomic Force Microscopy (AFM) encompasses a variety of techniques that provide the ability to visualize and measure surfaces at high resolution in three dimensions in air and fluid environments. A common application of AFM is the study of surface morphology and dimensional measurements of heights, widths, and roughness, down to sub-nanometer resolution in some cases. However, AFMs are also frequently used to measure mechanical properties, such as modulus and adhesion, as well as electrical properties, such as current or work function of materials. The combination of these abilities produces a wide range of measurements and properties that can be studied with a single AFM. Furthermore, the ability of the AFM to make measurements in a fluid environment at the nanoscale makes it unique, and is often used for biological and electrochemical studies. This presentation will concentrate on providing an overview of the AFM techniques and applications, with an emphasis on the capabilities of the AFM instruments at UW-Madison.
John Thornton is a Senior Applications Engineer at Bruker Nano Surfaces with 25+ years of experience in the field of Atomic Force Microscopy (AFM). He learned AFM at North Carolina State University in the 1990s, and then joined Digital Instruments, a pioneering company in early AFM development, and continued with the company through acquisitions by Veeco Instruments, and then Bruker. John has co-authored many scientific publications and developed scanning probe microscopy training courses. Currently, John spends a significant amount of time running AFMs and educating others on techniques. Contact email: John.Thornton@bruker.com
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Project Highlight
AFM Characterization of 3D Thin Films Crystallized by Solid Phase Epitaxy
Presented by Rui Lui, Graduate Student, Materials Science and Engineering, UW–Madison
At present, the synthesis of crystalline oxide materials in the form of nanostructures and thin films largely employs epitaxial growth techniques that are highly developed and widely used, but which are limited in planner geometry because of the rapid surface diffusion in conventional epitaxial growth techniques. These limitations can be alleviated by crystallization of amorphous complex oxides via solid phase epitaxy (SPE), in which diffusive processes during crystallization are largely suppressed. SPE enables a wide range of opportunities in the formation of oxide materials in new geometries like 3D thin films. Study of the surface morphology using AFM at different stages of SPE help us understand the crystallization process from amorphous form, kinetics of nucleation and crystal growth. We will also briefly discuss how AFM can contribute to the characterization of lateral crystallization, which is critical in forming 3D nano structures via SPE.
Measuring Nanoscale Mechanical Properties: Nanoindentation and AFM Indentation Techniques
Thursday, October 22nd
12:00 – 1:30 p.m. Central Time
Presented by Julie Morasch, AMIC Director and WCNT Instrument Manager
Measuring the mechanical properties of materials at the nanoscale allows determination of local mechanical properties as well as mechanical properties of small samples and thin films. This presentation will discuss the basics of both nanoindentation and AFM indentation and discuss the advantages and disadvantages of each technique.
Julie Morasch is an Instrument Manager in the Nanoscale Imaging and Analysis Center, providing support for the nanoindenter, the atomic force microscope (AFM) and the confocal and light microscopes. She received her B.S in Electrical Engineering from UW–Madison and her Ph.D. in Materials Science from the University of Minnesota. She has over 25 years of experience in AFM and has been with the WCNT for 9 years.
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Project Highlights
Crystal Misorientation Correlates with Hardness in Tooth Enamels
Presented by Cayla Stifler, UW–Madison, Physics
Polarization-dependent contrast (PIC) maps reveal that adjacent crystals in tooth enamel from mice, humans, sheep, and parrotfish are slightly misoriented. Within the 2-8° range, the mean misorientation between adjacent crystals is positively correlated with the hardness and elastic modulus demonstrating and important structure-function relationship.
Characterization of Disease-Inspired Tissue Engineered Aortic Valves via AFM
Presented by Lysmarie Figueroa Rios, UW–Madison, Biomedical Engineering
Calcific Aortic Valve Disease is one of the most prevalent valvular diseases affecting mostly the aging population in developed countries. Currently, there is not available treatment other than surgical valve replacement to eradicate or stop progression of CAVD. This is due in part to limitations in our understanding of the cellular and molecular underpinnings of the disease. In our lab, we focus on developing disease-inspired aortic valve tissue engineered systems that allow us to closely study cellular responses to ECM composition and mechanical changes characteristic of hallmarks present during disease progression. Understanding how cells respond to changes in their ECM can help us identify key features that can one day be targeted to find better treatments for this disease.
Introduction to Electron Backscattered Diffraction and Energy Dispersive X-ray Microanalysis
Tuesday, October 27th
12:00 – 1:30 p.m. Central Time
Presented by Chris Stephens, Thermo-Fisher Scientific
Project Highlights presented by:
- Mohamed Elbakhshwan, Assistant Scientist in Engineering Physics
- Dongzheng Chen, Graduate Student in Materials Science
Introduction to Transmission Electron Microscopy
Thursday, October 29th
12:00 – 1:30 p.m. Central Time
Presented by Paul Voyles, Wisconsin MRSEC Director and Professor of Materials Science and Engineering, UW–Madison
What if we could know everything there was to know about the structure of a piece of material? Complete knowledge would constitute something like a list of all the 3D positions of all atoms, with the element of each atom specified, and measurement of all the electronic states at high resolution in real and momentum space. Modern electron microscopy cannot provide quite all of that information, but it can get surprisingly close. This talk will review the basics of TEM and STEM, including imaging, diffraction, and spectroscopy, then provide examples of cutting-edge applications that measure atomic structure, defects, and electronic states in a variety of materials and in various sample environments.
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Project Highlight
Microstructure and Microchemistry Study of Irradiation-Induced Precipitates in Proton Irradiated ZrNb Alloys
Presented by Zefeng Yu, Graduate Student in Engineering Physics
Proton irradiation induced Nb redistribution in Zr-xNb alloys has been investigated using scanning transmission electron microscopy/energy dispersive X-ray spectroscopy (STEM/EDS). ZrxNb alloys are mainly composed of Zr matrix, native ZreNbeFe phases, and b-Nb precipitates. After 2 MeV proton irradiation at 350 C, a decrease of Nb content in native precipitates, as well as irradiation induced precipitation of Nb-rich platelets (135 ± 69 nm long and 27 ± 12 nm wide) were found. Nb-rich platelets and Zr matrix form the Burgers orientation relationship, [111]//[2110] and (011)//(0002). The platelets were found to be mostly coherent with the matrix with a few dislocations near the ends of the precipitate. The coherent strain field has been measured in the matrix and platelets by the 4D-STEM technique. The growth of Nb-rich platelets is mainly driven by coherency and dislocation-induced strain fields. Irradiation may both enhance the diffusion and induce segregation of interstitial Nb to the ends of the irradiation induced platelets, further facilitating their growth.
Introduction to Raman Spectroscopy and Imaging
Tuesday, November 3rd
12:00 – 1:30 p.m. Central Time
Presented by David Tuschel, Raman Applications Scientist, HORIBA Scientific
This tutorial will teach introductory Raman spectroscopy and imaging. The chemical bond origins of Raman scattering along with the instrumentation used to acquire Raman spectra and images will be explained. In particular, we will discuss the selection of laser excitation wavelength, lateral and axial spatial resolution, detection limits, and laser polarization in micro-Raman sampling. We will also discuss the importance of spectral resolution and how to apply it when rendering a Raman image. Regarding applications, we will show examples of how Raman spectroscopy provides insight into the energetics of molecular interactions in the liquid and vapor phases, and that it can be used to distinguish crystalline polymorphs and differentiate single crystal, polycrystalline and amorphous materials in the solid state. The effects of chemical bonding, strain and crystallite size on Raman spectra will be addressed and we will show you how to image these characteristics. In addition, we will discuss how combined spectral imaging by laser excited photoluminescence and Raman scattering can be used to reveal the spatially varying solid-state structure of materials.
Introduction to X-ray Diffraction based techniques
Thursday, November 5th
12:00 – 1:30 p.m. Central Time
Presented by Don Savage, WCNT, UW–Madison
The tutorial will cover the basics of x-ray diffraction (XRD) and x-ray scattering. For XRD from polycrystalline materials, the focus will be on phase identification, texture, and grain size determination highlighting the use of the Bruker d8 discover x-ray diffractometer. Methods to determine thin-film stress, by measuring strain anisotropy will also be discussed. For single crystals, high-resolution XRD to determine epitaxial film thickness and strain using the Panalytical Empyrean x-ray diffractometer will be discussed. For x-ray scattering in reflection (XRR), film density, thickness, and interface roughness can be determined even for amorphous or polycrystalline layers. When used in transmission, the technique is called small-angle x-ray scattering (SAX), where the size and ordering of domains in the 10’s of nanometer scale can be analyzed. As the talk proceeds, the focus will be on the best technique needed to approach a specific material’s characterization problem as well as its strengths and limitations.
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Project Highlights
Surface X-ray Scattering and Reflectivity Studies for Complex Oxide Solid Phase Epitaxy
Presented by Samuel Marks, Graduate Student, Materials Science & Engineering
X-ray Diffraction Study of Magnetic Half-Heusler Thin Films and Membranes
Presented by Dongxue Du, Graduate Student, Materials Science & Engineering
Introduction to XPS
Tuesday, November 10th
12:00 – 1:30 p.m. Central Time
Presented by Jerry Hunter, WCNT Director, UW–Madison
New Capabilities in Nanoscale in situ X-Ray Characterization
Thursday, November 12th
12:00 – 1:30 p.m. Central Time
Presented by Paul Evans, Professor of Materials Science and Engineering, UW-Madison
This talk will focus on new opportunities available through the development of instrumentation bringing nanoscale characterization to in situ materials synthesis and crystal growth processes.
Paul Evans is a professor of Materials Science and Engineering at UW-Madison and a participant in the UW’s Materials Research Science and Engineering Center (MRSEC). His research includes the development of novel approaches in x-ray scattering of materials, including the use of national facilities such as synchrotron light sources and free-electron lasers.
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Project Highlights
- Solving Puzzles in Oxide Crystallization
Presented by Rui Liu, Postdoctoral Research Associate, Materials Science & Engineering, UW-Madison - Structure and Properties of Vapor-Deposited Organic Molecular Thin Films
Presented by Ben Kasting, Graduate Student, Chemistry, UW-Madison
Fundamentals of Secondary Ion Mass Spectrometry
Tuesday, November 17th
12:00 – 1:30 p.m. Central Time
Presented by Jerry Hunter, WCNT Director, UW–Madison
Secondary Ion Mass Spectrometry offers analysis of inorganic and organic materials with ppm to ppb detection limits. Owing to its low detection limits and ability to obtain in-depth information, dynamic-SIMS has been used extensively by the semiconductor community for depth profiling of dopants in a variety of electronic materials. More recently static-SIMS has been applied to organic and biological material analysis. This presentation will introduce users to both the dynamic SIMS and static SIMS techniques, including how the techniques work, quantification, instrumentation, strengths and limitations of the technique, and applications.
Overview of the Dynacool Physical Property Measurement System
Thursday, November 19th
12:00 – 1:30 p.m. Central Time
Presented by Rick Hapanowicz, U.S.A. & Canada Sales Manager, Quantum Design
Quantum Design developed Physical Property Measurement System (PPMS) to provide experimentalists the ability to measure electrical, magnetic, thermal and optical properties of materials. The Cryogen Free DynaCool PPMS system can control the sample temperature from 1.8K to 400K with a maximum applied magnetic field of 12 Tesla. The DynaCool system in the Wisconsin Centers for Nanoscale Technology has the Electrical Resistance, Sample Rotator, Multi-function Probe and Helium-3 Options. This seminar will give an overview the DynaCool system operation and provide details on each experiment option.