Latest Advances in Microscopy & Analytical Techniques

Wednesday, February 8, 2017

Symposium presented by JEOL, Gatan, and Oxford

Topics and Agenda

8:30AM - 9:30AM  Registration

9:30-10:30 Recent Advances in SEM Ultralow kV Imaging and Microanalysis;Some Amazing Data (Doing the Almost Impossible) and Some Words of Caution

10:45-11:30    Managing (High) Tension: Atomic Resolution (S)TEM from 30 kV to 300 kV 

11:30-12:15 Fast EDS Mapping under conditions not previously considered suitable for analysis in the SEM 

12:15 to 1:30 Lunch with facility tours from 1:00 to 1:30

1:30-2:30 Advantages of Direct Detection and Electron Counting for Electron Energy Loss Spectroscopy Data Acquisition

2:30-3:15 Electron Microscopy and Tomography: moving into the realm of three dimensions in both Life Sciences and Materials Science

3:15 til 4:00 Lab Tours: Scanning-Local Probe Facility, Quanttrone Nanofabrication Facility, Nanoscale Characterization Facility

Topics

Recent Advances in SEM Ultralow kV Imaging and Microanalysis; Some Amazing Data (Doing the Almost Impossible) and Some Words of Caution -Vern Robertson, JEOL

In just the last few years there has been a quantum leap in the ability of the scanning electron microscopes (SEM and EPMA) to observe and chemically analyze a wide variety of materials form various fields of interest and have drastically increased analysts capabilities. Field Emission (FEG) SEMs provide the capability to create a very small probe diameter (high resolution imaging) at very low accelerating voltage (high resolution microanalysis) with high beam currents required for analysis and with exceptional surface detail and reduced beam specimen interaction in a bulk sample with previously unattainable nanometer scale resolution at landing voltages as low as 10V allowing the examination of nonconductive materials both for imaging and analysis. In years past these samples would have required the application of a conductive coating lengthening the sample prep process and possibly obscuring surface sensitive information. However, these extremely low voltages come with some clearly defined sample preparation and handling procedures. Low vacuum (variable pressure) is another way of handling nonconductive samples and added to the FEG SEMs it increases their flexibility for handling any type of samples especially at higher kVs and beam currents. Advances in X-ray spectroscopy, both in Energy Dispersive Spectroscopy (EDS) and a new novel Wavelength Dispersive Spectrometer (WDS) have also pushed the boundaries to higher mag, lower voltage and lower X-ray energy (soft X-ray) analysis opening up new avenues for specimen observation and analysis. More & more we are seeing other accessories like EBSD, TKD, CL, etc. being integrated into the everyday operation of the electron microscopes.

These new state-of-the-art microscopes, detectors and spectrometers today allows one to overcome many of the historical limitations associated with low kV imaging and microanalysis. HOWEVER, there are some considerations that may not have been thought about in the past. Some case studies and examples of the good things (and some of the bad) that can result from ultralow kV imaging and analysis will be presented.

As you will see from the images and analyses, ultralow kV and or ultra-high spatial resolution is a VERY POWERFUL tool, and as with all powerful tools, it needs to be used with caution (or at least with keeping an eye out for the non-intuitive). Applications examples of previously “impossible tasks” will highlight how these new generations of microscopes & spectrometers have pushed the boundaries of electron microscopy for basic research and failure analysis.

Fast EDS Mapping under conditions not previously considered suitable for analysis in the SEM -Warren MoberlyChan, Oxford Instruments

Today there is no limitation on the types of materials that are being investigated in the Electron Microscope. New improvements in microscope technology, such as low-vacuum mode, have made it common to investigate beam sensitive and non-conductive materials. Fortunately detector technology for EDS (Energy Dispersive Spectrometry X-Ray analysis), and computer software/hardware have kept pace with advances in the SEM.  This now allows the acquisition of meaningful analytical data under conditions not previously considered suitable for analysis.Review and discuss: New analytical hardware that allows EDS acquisition to run 100x faster than a decade ago - as well as enabling improved precision• New software options that allow ~Data processing while still acquiring~Deconvolution of peak overlaps even while mapping~Better, standardless quantitation at low kV~Benefits of Large Area Mapping.

Electron Microscopy and Tomography: moving into the realm of three dimensions in both Life Sciences and Materials Science -  Dr. Jaap Brink, JEOL USA

Electron microscopy has for the past decade steadily moved into the realm of three dimensions in both Life Sciences and Materials Science. The application of tomography on thicker, unique specimens using image modalities like TEM, STEM and EDS have given scientists unprecedented opportunities to probe structures. The application of imaging on samples consisting of identical copies of one species in random orientation has evolved fro being heavily favored to viruses (because of their icosahedral symmetry and larger objects like ribosomes) to increasingly smaller molecules, currently as small as around 100 kDa. Simultaneously, the attained resolution has increased to an unprecedented 1.8 Å, which rivals that achievable by more traditional methods like NMR and x-ray crystallography. Concurrently, a technique borrowing much from x-rtay crystallography, microED, has enabled scientists to use the electron microscope on small crystals of small proteins to routinely break the 2-Å barrier. My talk will highlight each of these endeavors and discuss future directions.

Advantages of Direct Detection and Electron Counting for Electron Energy Loss Spectroscopy Data Acquisition - Dr. Paolo Longo, Gatan, Inc.

Transmission electron microscopes primarily employ indirect cameras (IDC) for electron detection in imaging, diffraction and EELS modes. Such cameras convert incident elec-trons to photons which, through a fiber optic network or lens, are coupled to a light sensitive camera. This indirect detection method typically has a negative impact on the point spread function (PSF) and detective quantum efficiency (DQE) of the camera. Over the last decade, radiation tolerant CMOS active pixel sensors, which directly detect high-energy incident electrons and have the speed to count individual electrons events, have been developed. These detectors result in greatly improved PSF and DQE in comparison to conventional IDCs. Such direct detection cameras (DDCs) have revolutionized the cryo-TEM field as well as have strong advantages for in-situ TEM in both imaging and diffraction applications. EELS applications can benefit from the improved PSF and the ability to count electrons. The improved PSF allows spectra to be acquired over larger energy ranges while maintaining sharp features and greatly reduced spectral tails. The ability to count electrons nearly eliminates the noise associated with detector readout and greatly reduces the proportional noise associated with detector gain variations. This effectively leaves the shot noise as the limiting noise source present. The implication for EELS acquisition is that fine structure analysis becomes more straightforward for typical conditions and even possible for the case of low signal levels.In this presentation, we will review the current state of electrons counting detectors for electron microscopy with an emphasis on system for EELS measurements.

Managing (High) Tension: Atomic Resolution (S)TEM from 30 kV to 300 kV - Dr. Thomas Isabell, JEOL USA 

Choosing the correct microscope high tension, or accelerating voltage, is an important experimental consideration for TEM imaging and microanalysis.    Higher accelerating voltages naturally lead to better spatial resolution for imaging, but will also lead to accelerated specimen damage.   For microanalysis, lower accelerating voltages mean more beam spreading and worse spatial resolution, but also enhanced microanalysis cross sections for EDS and EELS.   A new generation of aberration corrected microscopes gives the user the flexibility to operate over a wide range of high tension with unprecedented imaging and chemical spatial resolution.  This means that on the same instrument, the voltage can be dialed in for a given experiment and readily changed as different experimental needs arise.  The addition of a cold field emission gun, advanced aberration correctors and advanced detectors only enhances operation at both high and low voltages, further adding to instrument flexibility.

 

Speakers

Vern Robertson has been with JEOL USA for 30 years and was appointed EPMA/Surface Analysis Product Manager and will continue as SEM Technical Sales Manager post 2010, providing in-house and in the field, technical product support and customer applications support. Vern served as the senior SEM Applications Specialist at JEOL beginning in 1986.  He was appointed National Laboratory Manager in 2004, and FEG SEM Product Manager in 2005. Vern received his B.Sc. in Geology from the University of New Hampshire. His prior industrial experience included eight years of consulting in an independent testing lab specializing in industrial and environmental problem solving, with responsibilities including polarized light optical microscopy, and atomic emission and absorption spectroscopy SEM with EDS/ WDS and x-Ray diffraction. Vern is a current member of the MAS (Microanalysis Society) Council.

Dr. Jacob “Jaap” Brink received his Ph.D. in 1988 from the Rijksuniversiteit Groningen, the Netherlands where he studied NADH:Co-­ enzyme-­Q oxidoreductase from bovine heart mitochondria by electron microscopy under prof.em. Ernst F.J. van Bruggen. During his graduate days he learnt low-­dose techniques and working with frozen-­hydrated specimens on two-­dimensional (2D) crystals. In 1988 Jaap and his family moved to Houston, Texas where he started his post-­doc with Dr. Wah Chiu at the Baylor College of Medicine. While there, he studied crotoxin complex, a thin 3D crystal by electron crystallography using a JEOL4000EX and pioneered electron diffraction tomography as well as spot-­scan imaging using a CCD camera. Starting in 1999 Jaap worked on several single–particle projects, notably human fatty acid synthase. In 2002 Jaap left academia and started working for JEOL USA, Inc. as an application manager. Following a promotion to product manager in 2007, he is involved with technical issues that come up in the sales process, as well as support and development issues with software used in electron microscopy. As such, he is the resident expert in JEOL USA on electron tomography, electron cryo-­microscopy and high-­throughput high resolution imaging. He is a lecturer at the Lehigh Microscopy School for Micro-­analysis as well as an invited speaker at the IMANI symposia at NCKU in Taiwan and travels the world supporting JEOL colleagues in Life Sciences.

Dr. Paolo Longo is the Business Development Manager – Analytical Products at Gatan, Inc. He received his 
PhD in 2008 from the University of Glasgow, UK, and Physics Post-doctoral training at the University of Glasgow. His positions and honors include: April 2016 to present: Business Development Manager – Analytical Products, Gatan Inc; May 2014 to present: Applications and Training Manager, Gatan Inc; March 2011 to May 2014: TEM Applications Scientist, Gatan Inc; Feb 2010 to Feb 2011: Technical & Sales Representative, Oil Gas & Chemicals division, SGS, Genoa, Italy; Jan 2008 – Feb 2010: Research Assistant, Department of Physics & Astronomy, University of Glasgow, UK.

Thomas C. Isabell, Ph.D. - Tom is Director of Product Management at JEOL USA, leading the TEM, SEM and Microprobe product divisions.  Since joining JEOL in 2003 as Assistant Product Manager, Tom has worked closely with the JEOL USA product groups, JEOL Ltd. in Japan and with JEOL customers to help keep the company at the forefront of technology in materials and life sciences research.  Prior to joining JEOL, Tom held positions in business development at EmiSpec in Tempe, Arizona and applications support at Fischione Instruments in Export, Pennsylvania.  Tom received a B.S. in Materials Science and Engineering from the University of Minnesota and a Ph.D. in Materials Science and Engineering from Northwestern University.

Dr. Warren J. MoberlyChan is a microscopist in the NanoAnalysis Applications Group at Oxford Instruments.  He received his PhD in Materials Science & Engineering from Stanford University, and ScB from Brown University.  He is a Past President (2009 &2010) of the New England Society for Microscopy and a Berks Award recipient of MAS.  He has recently worked at Lawrence Livermore National Laboratories in the Materials Sciences Division; and at Lawrence Berkeley National Laboratories in the Advanced Ceramics Group.  He has worked extensively in the Information Storage industry at ReadRite, Komag, Quantum, MPI, and SSL.  He has taught Materials Engineering courses at Stevens Institute of Technology, San Jose State, Stanford, & Harvard Universities.  His research interests are thin film interfaces and surfaces and the study of their chemical and mechanical properties through the application of microscopy, spectroscopy and FIB.  His accomplishments include cryolithography, deformation twinning both for intermetallic ductility and for femto-shock unloading, record toughening of SiC ceramic composites, crystallographic-growth-control of magnetic media, defect-growth-control of nanowires, and creating the first picostructures via ion-beam-stimulated self-assembly.

 

 

 

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