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