2018 Facilities Days Open House – Speaker Abstracts

8:30 AM                

Overview—Jerry Hunter—Location: Varsity II

This presentation will quickly cover the range of techniques available in the CoE shared facilities and discuss learning objectives for the day.  A broad outline of how the various techniques fit together to provide a comprehensive characterization solution will also be discussed.


9:00 AM

Scanning Electron Microscopy & EDS—Chris Santeufemio—Location: Varsity II

The scanning electron microscope (SEM) is a type of microscope that produces images of a sample by scanning the surface with a focused beam of electrons. The electrons interact with atoms in the sample, producing various signals that contain information about the sample’s surface topography and composition. The electron beam is scanned in a raster scan pattern, and the beam’s position is combined with the detected signal to produce an image. SEM can achieve resolution better than 1 nanometer. Specimens can be observed in high vacuum in conventional SEM, or in low vacuum or wet conditions in variable pressure or environmental SEM, and at a wide range of cryogenic or elevated temperatures with specialized instruments. Characteristic X-rays that are produced by the interaction of electrons with the sample may also be detected in an SEM equipped for energy-dispersive X-ray spectroscopy or wavelength dispersive X-ray spectroscopy. Analysis of the x-ray signals can be used to map the distribution and estimate the abundance of elements in the sample.

User Applications—Location: Varsity II

Eric Kwon—Strain Sensor for Intraocular Applications

UW-Madison Graduate Student in the Electrical and Computer Engineering Department

Advisor: Professor Hongrui Jiang

Katy Jinkins—Scanning Electron Microscopy for Characterization of Carbon Nanotube Films

UW-Madison Graduate Student in the Materials Science Department

Advisor: Professor Michael Arnold


9:00 AM                

Optical Spectroscopy—Dr. Sergey Mamedov—Location: Northwoods Room

The tutorial will address fundamentals of the techniques (Raman, FT-IR, Fluorescence and UV-VIS), advantages and limitation of these techniques. Instrumentation and typical applications will be discussed during tutorial and the examples of applications will be shown.

User Applications—Location: Northwoods Room

Hongseung Yeon—Hydrophobic Hydration Behavior Near Positively-Charged Surfactants

UW-Madison Graduate Student in the Chemical and Biological Engineering Department

Advisor: Professor Nicholas Abbott

10:30 AM

Transmission Electron Microscopy—Paul Voyles—Location: Varsity II

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 measure atomic structure, defects, and electronic states in a variety of materials and in various sample environments.

Cryoelectron Microscopy—Desirée Benefield—Location: Varsity II

Multiple advances in microscope technology and image acquisition (dubbed the ‘resolution revolution’) have transformed cryo-electron microscopy (cryo-EM) into an incredibly powerful technique to visualize and study especially sensitive samples. The 2017 Nobel prize in Chemistry was awarded to three researchers involved in the development of the technique that has redefined how structural questions are asked. In this tutorial session I will explain how cryo-EM came to be, how far it has advanced, and where it may be headed in the future. A review/reality check of the feasibility of starting a cryo-EM based project will be discussed as well as a brief introduction to a typical project work-flow. This session will also highlight the resources on campus now available to you for a cryo-EM project of your very own.

User Applications—Location: Varsity II

Hong Zhan—Structural Analysis Of RNA Virus Genome Replication Complexes By Cryo Electron Tomography

UW-Madison Postdoctoral Research Fellow in the Institute of Molecular Virology

Advisor: Dr. Paul Ahlquist

Chenyu Zhang—Application of 4D-STEM to Study Material Structure

UW-Madison Graduate Student in the Department of Materials Science and Engineering

Advisor: Professor Paul Voyles

10:30 AM

Surface Analysis—Jerry Hunter, Dr. Scott Bryan—Location: Northwoods Room

This presentation will cover several surface analytical techniques (XPS, Auger and Backscattering), with a focus on X-ray Photoelectron Spectroscopy (XPS).  The fundamentals of the techniques, typical data, instrumentation and how these techniques fit into the larger analytical space will be discussed.

The seminar will focus on recent applications of XPS and Auger to the development and understanding of materials.  Examples will be given where XPS and Auger provide unique chemical information on the near-surface region of materials that is critical to understanding their properties. Combining this chemical information with structural information from AFM and electron microscopy provides a more complete understanding of the material under study. A brief introduction to the applications of TOF-SIMS, which is not yet available to UW Madison, will be discussed and the complimentary information it provides to the electron spectroscopy techniques will be summarized.

User Applications—Location: Northwoods Room

Vivek Saraswat—Nitrogen residuals on Carbon Nanotube Transistors

UW-Madison Graduate Student in the Department of Materials Science and Engineering

Advisor: Professor Michael Arnold


GD-OES—Philippe Hunault—Location: Northwoods Room

GD-OES (Glow Discharge – Optical Emission Spectometry) is a fast technique to characterize conductive and non conductive layers and coatings from nm to 100+ microns thickness. Depth resolution can be as low as 1nm. Concentration range is from ppm to 100%. The depth profile of the elemental composition vs depth will be obtained in minutes. Almost all elements detectable by OES can be analyzed, and more specifically O, N, H, Cl, F, Li, C, S, Na, K… After reviewing the theory and the instrument configuration, most of this presentation will be focused on a large variety of applications, among: Li Ion Batteries, Energy Storage, Photovoltaic, PVD &CVD Coating, Plating, Galvanization, ion Implantation, Nitriding, Carburizing, Glass, Wafer, Hard Disk and other Media, Organic Coatings, Thin and Thick Oxides, Failure Analysis.

12:15 PM              

Lunch Break (Feedback Survey)

1:15 PM                

Focused Ion Beam—Brandon Van Leer—Location: Varsity II

The DualBeam FIB-SEM microscope has gained widespread use in materials science and materials characterization over the last few decades because it offers both high-resolution imaging and flexible micromachining in a single instrument.  The FIB portion of a DualBeam is similar to a SEM, except that the beam that is rastered over the sample is an ion beam rather than an electron beam. Secondary electrons or secondary ions are generated by the interaction of the ion beam with the sample surface and can be used to obtain high-spatial-resolution images or be used to sputter material away to reveal buried features. In most commercially available systems, Ga ions are used though recent advances have allowed for inert gas species such as Xe ions to be used.  The ions’ sputtering action enables precise milling of samples.  Additive processes are also available in a DualBeam with the addition of chemical precursors for ion (IBID) or electron (EBID) beam induced deposition. During the last 35 years, DualBeam FIB-SEM microscopes have become an important technology for a wide array of materials science applications including tomography, circuit edit and S/TEM sample preparation. Benefits of attendance include fundamentals of the technique (how the technique works, sputtering, ion solid interactions, etc.), advantages or limitations of the technique, and the application space: how the instrumentation is used and how FIB fits into the broader analytical characterization space.

User Applications—Location: Varsity II

Kaila Bertsch—Using Plasma FIB Machining to Scale Up Preparation of TEM Thin Foils

UW-Madison Postdoctoral Researcher in the Materials Science and Engineering Department

Advisor: Dr. Dan Thoma

Ed Leonard—Focused Ion Beam for Multilayer Microfabricated Circuit Failure Analysis

UW-Madison Graduate Student in the Physics Department

Advisor: Professor Robert McDermott

1:15 PM                

X-ray Analysis Methods—Don Savage—Location: Northwoods Room

The tutorial will cover the basics of x-ray diffraction (XRD) and x-ray scattering. For XRD from polycrystalline materials, I will focus on phase identification, texture, and grain size determination highlighting the use of the Bruker d8 discover x-ray diffractometer. For single crystals, I will discuss high-resolution XRD to determine epitaxial film thickness and strain using the Panalytical Empyrean x-ray diffractometer. For x-ray scattering in reflection (XRR), thin-film thickness and interface roughness can be determined even from amorphous or polycrystalline layers. When used in transmission, the technique is called small-angle x-ray scattering (SAX), where ordering of domains on the 10’s of nanometer scale can be analyzed. As the talk proceeds I will focus on the best technique needed to approach a specific materials characterization problem as well as its strengths and limitations.


                                User Applications—Location: Northwoods Room

Yajin Chen—Nucleation and Growth Kinetics of Amorphous SrTiO3 Studied by Grazing-incidence X-ray Diffraction

UW-Madison Research Assistant in the Materials Science and Engineering Department

Advisor: Professor Paul G. Evans

Gabriel Jaffe—X-ray Reflectivity Measurements of III-V Superlattices

UW-Madison Graduate Student in the Physics Department

Advisor: Professor Mark Eriksson

2:15 PM                

Atom Probe Tomography—Rob Ulfig and Sue Babcock—Location: Varsity II

The improvements in the capability of 3D nanoscale atom probe tomography (APT) have been remarkable. Analysis volumes have increased dramatically, and the introduction of UV laser mode has enabled analysis of material systems far beyond traditional bulk metals.  In addition to traditional electrochemical polishing of samples, the maturation of FIB-based specimen preparation methods and the use of tEBSD has made site-specific analyses truly routine. This presentation will provide an overview of the recent advances in applications of the technique in metallurgical systems, semiconductors and dielectrics.

The electronic structure of GaAs1-xBix solid solutions is highly sensitive to the Bi concentration and provides opportunities for development of optoelectronic devices with new capabilities. This sensitivity also demands the development of GaAs1-xBix thin-film materials with homogeneous Bi distribution down to the nanoscale that is stable against phase separation during post processing and application. This short talk will describe our use of laser-pulsed atom probe tomography to elucidate the Bi incorporation processes during chemical vapor deposition (CVD) growth of supersaturated epitaxial GaAs1-xBix thin films and also the Bi precipitation pathway in annealed samples. Atom probe tomography investigation of annealed materials reveal ~ 5 nm diameter phase-separated particles. Analysis of the distribution of the elements within these tiny particles suggests that the annealing-induced phase separation may be facilitated by the formation of mobile nanoscale liquid droplets in the GaAs1-xBix films.

Co-workers Weixin Chen, Adam W. Wood, Kamran Forghani, Honghyuk Kim, Yingxin Guan, Thomas F. Kuech and Luke J Mawst, all of the University of Wisconsin-Madison are gratefully acknowledged. This research primarily is supported by NSF through the University of Wisconsin Materials Research Science and Engineering Center (DMR-1121288).

2:15 PM                

Nanoindentation—Douglas Stauffer—Location: Northwoods Room

Materials behavior is often dominated by highly localized phenomena, and the ability to probe these local properties for engineering devices is critical. Often these devices are operating in environments with large differences in temperature and pressure: from the high vacuum and cold of space to the high temperature and high pressure inside a deep water oil well. Nanoindentation is a uniquely suited technique for the measurement of mechanical properties at small scales, with benefits of simple sample preparation, reliability, and ability to test on limited sample volumes being major advantages.

The basics of nanoindentation, how to prepare, test, and evaluate samples will presented.  This will be followed by application examples that increase in complexity, taking advantage of the Bruker / Hysitron technology opening up the testing regimes to low temperature, down to -120C, high temperatures, up to 800C, and looking at the mechanics in a statistical fashion with tests up to 6 indents/s. These technologies give the researcher information on the role of individual phases in a composite or precipitate steel, and improving statistics by generating very large datasets.

Finally, a study exploring incipient mechanical failure is presented. This leads to a phenomenological understanding of crack initiation at stress concentrators. Here, in situ fatigue is demonstrated using cyclic mechanical loading experiments at frequencies up to several hundred Hz. More than 106 cycles can be reached within one hour. Moreover, the nanometer-scale spatial resolution of the TEM allows the observation of “incipient” crack growth rates of <10-12 m·cycle-1 very near to the minimum threshold stress intensity factor. With Daniel C. Bufford, William M. Mook, S.A. Syed Asif, Brad L Boyce, and Khalid Hattar

User Applications—Location: Northwoods Room

Guebum Han—Poroelastic and Intrinsic Viscoelastic Dissipation in Cartilage

UW-Madison Graduate Student in the Mechanical Engineering Department

Advisor: Dr. Melih Eriten

Li He—Nanoindentation Measurement of Irradiation Induced Hardening in Advanced Nuclear Materials

UW-Madison Graduate Student in the Engineering Physics Department

Advisors: Professor Kumar Sridharan, Professor Todd Allen and Professor Adrien Couet

3:15 PM                

Scanned Probe Microscopy—Julie Last, John Thornton—Location: Varsity II

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 concentration on providing an overview of the AFM techniques and applications, with an emphasis on the capabilities of the AFM instruments at UW-Madison.

User Applications—Location: Varsity II

Chaiyapat Tangpatjaroen—Size Dependence of Nanoscale Wear of Silicon Carbide and Silicon

UW-Madison Graduate Student in the Materials Science and Engineering Department

Advisor: Professor Izabela Szlufarska

Le Pham—AFM Testing of Air Bubbles Extracted From Cement Paste

UW-Madison Graduate Student in the Civil Engineering Department

Advisor: Professor Steven Cramer

3:15 PM                

Electron Beam Lithography—Yong Sun—Location: Northwoods Room

Electron Beam Lithography – direct-writing of user-defined patterns with a beam of electrons, as a technique, has existed since the early 60s to 70s. In this presentation, I’ll walk you through some of the advanced ebeam lithography techniques by using Elionix ELS-G100 as a model system. The following are the main topics covered in this talk: (1) ebeam system configuration and its components; (2) the principle of operation for ebeam exposure; (3) limits of ebeam and its implication; (4) ebeam proximity effect; (5) post-exposure resist processing.

User Applications—Location: Northwoods Room

Jad Salman—Low-loss Metasurfaces Using Silicon

UW-Madison Graduate Student in the Electrical Engineering Department

Advisor: Professor Mikhail Kats

Evan McQuarrie—Electron Beam Lithography For Quantum Devices in Silicon

UW-Madison Postdoctoral Researcher in the Physics Department

Advisor: Professor Mark Eriksson

4:15 PM                 Wrap Up—Jerry Hunter—Location: Varsity II