Volume 1, Issue 2 • Fall 2010
Open House and Short Courses at UCF’s Materials Characterization Facility MCF held its annual Open House on September 10, 2010. There were two sessions to showcase the 10,000 sq. ft. facility and inform UCF students, UCF faculty, and scientists/engineers from local industry of MCF’s capabilities and resources. Our three research engineers, Kirk Scammon, Dr. Qi Zhang and Mikhail Klimov, provided lectures and demonstrations of select instruments to more than 20 participants.
February 11, 2011 – Scanning Electron Microscopy (Kirk Scammon) March 18, 2011 – Focused Ion Beam (Mikhail Klimov) April 22, 2011 (Dr. Qi Zhang)
MCF also plans on offering short courses on SEM, FIB and TEM in February, March and April of 2011. These short courses are offered every year, and include both theoretical lectures and short hands-on training sessions. Tentative schedule for these courses are:
Image from a Small World In This Issue JEM-1011 Transmission Electron Microscope
Useful Tips from MCF 2 Profile: NanoSpective
Profile: Dr. Jianhua Liu of NSTC 3 MCF’s Instruments 4 MCF Contact Information
UCF’s MCF is operated by Advanced Materials Processing and Analysis Center (AMPAC). Sudipta Seal, Ph.D. is Director of AMPAC and NSTC.
Advanced Materials Processing & Analysis Center
NanoScience Technology Center
MCFâ€™s JEM-1011 Transmission Electron Microscope The JEM-1011 microscope is a simple, compatible and highperformance transmission electron microscope (TEM) at the Materials Characterization Facility (MCF). This TEM can be operated at different accelerating voltages from 40 kV to 100 kV. Its high contrast objective lens provides the highest possible contrast and brightness with 0.2 nm lattice resolution and 0.4 nm point resolution. The patented cool beam gun allows high-brightness and high coherence illumination conditions. JEM-1011 TEM is highly user friendly, which makes it relatively easy to obtain mass-thickness contrast images, diffraction contrast images and selected area electron diffraction patterns. The advanced features and functions of this TEM ensure that the users realize the morphological structure; understand crystal structure; obtain grain and nanoparticle size and observe planar defects inside the grains and/or at grain boundaries. The sample cooling stage, equipped with this TEM, brings the sample to liquid nitrogen temperature so that the structure evolution is observed in-situ. The high performance CCD camera acquires digital images quickly and conveniently with high resolution and large acquisition area. The digital imaging software can also help with further imaging analysis, i.e., determining particles sizes and diameters and measuring the d- spacings of electron dif-
fraction patterns. The digital imaging software is also compatible with other imaging processors to obtain statistical data easily and quickly. Since it was installed, this high performing and versatile microscope has been used to analyze various samples including soft materials from biological sciences. The figures below show some examples from JEM-1011. Figure (a) is a fuel cell sample from the Florida Solar Energy Center, showing the interface of polymer electrolyte and catalyst. Figure (b) shows the structure of nano device for failure analysis from an industrial company. The performance of this microscope is also demonstrated by the high quality image in Figure (c), the few nanometers size Pt particles. Figure (d) is the sample of a mouse heart from Sanford-Burnham Medical Research Institute. It was obtained at 80 kV accelerating voltage, showing the mitochondrial and muscle for mechanism understanding of heart disease.
Useful Tips from MCF: How to make TEM samples from nanoparticles, nanotubes and nanowires For nanoparticles, nanotubes and nanowires, lacey carbon film Cu grid or holey carbon film Cu grid is strongly recommended. Lacey carbon or holey carbon film is a carbon film with either net-like holes of different sizes and shapes or round holes of various sizes. Both lacey carbon grid and holey carbon Cu grid provide support for nanomaterials without any interference of image quality, especially for those with light elements. The procedure of making TEM samples for nanomaterials is summarized below: 1. Put the nanomaterials in solution: Ethanol, IPA, water, etc. 2. Use ultrasonic or centrifugal to disperse materials in solution. 3. Drop the droplets on either holey carbon film Cu grid or lacey carbon film Cu grid by pipette or syringe. 4. Wait until the solution is dry and clean sample at plasma cleaner for 10 seconds if needed before loading the sample to TEM column.
The TEM image shown is an example showing how TEM high images could be obtained when using correct TEM grids. The image was taken using the JEM-1011 TEM at MCF. This was a nanoparticles sample in which big particles were surrounded by smaller particles 1-2 nm in size. The TEM grid was lacey carbon film Cu grid. The amorphous area of the background is the carbon film. In the area of the holes without the TEM carbon film background, we see the 1-2 nm nanoparticles clearly at the edge of big particles or even on the top/bottom of the big particles. Without the interference of the TEM grid background, high quality TEM images can be obtained and interpreted.
Materials Characterization Facility Newsletter
Faces Around Materials Characterization Facility
was formed in November of 2002, incorporated in January of 2003 and joined the UCF Technology Incubator in April of 2003. The company was originally formed with four principals (above, left to right), CTO Brian Kempshall, CFO Jennifer McKinley, CEO Brenda Prenitzer and COO Stephen Schwarz. Brian (B.S. and Ph.D), Jennifer (B.S. and M.S.), Brenda (B.S. and Ph.D.) and Stephen (Ph.D.) received their degrees from UCF, and are accredited with impressive post-doctoral and professional experience from Lucent Technologies and UCF. NanoSpective has clientele worldwide. The availability of state-of-the-art equipment at the MCF is a key component facilitating NanoSpectiveâ€™s success. The company has been an industrial affiliate of the MCF since November 2002.
NanoSpective serves markets ranging from intellectual property protection to failure analysis to quality control to support of research and development. NanoSpective is called upon for materials characterization applications involving a large variety of materials systems. Work that is commonly performed by NanoSpective includes using the FEI 200 TEM FIB to pinpoint features tens of nanometers in size and subsequently thin the region of interest to electron transparency (50-80nm) in preparation for TEM analysis using the Tecnai F30 TEM. The TEM is capable of imaging with sub-nanometer resolution. Equipped with two spectrometers, the TEM can provide elemental identification with nanometer scale lateral spatial resolution in concentrations at or below one atomic percent. In addition to elemental information, the EELS capability can also be used to discern chemical information.
Dr. Jianhua Liu from NSTC Jianhua Liu is a postdoctoral research associate in the NanoScience and Technology Center (NSTC), University of Central Florida. He received his BS (Applied Chemistry) and Ph.D. (Polymer Chemistry and Physics) from the University of Science and Technology of China (Hefei, P.R. China) in 2003 and 2008, respectively. At NSTC, he is conducting research in conjugated polymers, which are promising semiconductive materials for low-cost, large-scale, and flexible organic electronics such as thin film solar cells and field-effect transistors. He utilizes the TEM (JEOL 1101) to study the evolution of conjugated polymer nanowirelike crystals on their molecular weight. By this approach, he demonstrated the chain folding behavior (from extending to folding, as shown in Figure A) of poly(3-hexylthiophene) (P3HT) as well as other conjugated polymers when they form crystals. Such results are essential to understand the crystal-
lization mechanism and the structure-property relationship of conjugated polymers. In addition, he also observed the formation of hierarchical P3HT/carbon nanotube (CNT) supramolecular structures when using CNTs to induce the crystallization of P3HT. As shown in the TEM images (pictured at right), P3HT nanowires grow perpendicular from CNT surface to form centipede-like structures. This observation provides a general approach to build functional supramolecular structures that will lead to applications in nanoscale electronics.
Materials Characterization Facility Newsletter
MCF Instruments The Materials Characterization Facility (MCF) is home to a variety of state-of-the-art surface and materials characterization equipment. MCF is dedicated to helping researchers perform cutting edge research and training and educating students in the successful use of the available instruments. Currently, three engineers (Dr. Qi Zhang, Kirk Scammon and Mikhail Klimov) are employed full-time to assist students, faculty and members of the industrial community. Participation from other universities and industries is encouraged. This facility is located in the Central Florida Research Park, adjacent to the UCF main campus. • Molecular Imaging PicoSPM (Scanning Tunneling Microscopy, Atomic Force Microscopy)
• Cameca IMS-3F Secondary Ion Mass Spectrometer (Ion Microscope)
• FEI Tecnai F30 Transmission Electron Microscope
• PHI 560 ESCA (X-Ray Photoelectron Spectrometer/Auger Electron Spectrometer)
• JEOL 1011 Transmission Electron Microscope • FEI 200 TEM Focused Ion Beam • Zeiss Ultra-55 Scanning Electron Microscope • General IONIX 1.7 MV Tandetron Particle Accelerator • JEOL SuperProbe 733 Electron Probe X-Ray Microanalyser • Rigaku XRD (X-Ray Diffraction)
• PHI 5400 Electron Spectroscopy for Chemical Analysis (X-Ray Photoelectron Spectrometer) • PHI 600 Auger Electron Spectrometer/Scanning Auger Microscope • Hitachi S3500N Scanning Electron Microscope
Sample Preparation Equipment: • Critical Point Dryer • Gatan PECS (Coating System) • Ion Milling for TEM • Ultra Microtome (TEM/FTIR Sample Prep) • Sputter Coater (EMITECH) • Vacuum Evaporator (JEOL) Carbon Coater • Diamond Saw (Slow Speed)
• Diamond Band Saw • Electro Jet Polisher (TEM Prep) • Dimple Grinder (TEM) • Allied Polisher (TEM) • Metallurgical Polisher • Streuers Polisher • Plasma Cleaner
UCF Materials Characterization Facility Associate Director: Yongho Sohn, Ph.D., Professor (firstname.lastname@example.org, 407.882.1181) Staff Engineers: Kirk Scammon, M.S. (email@example.com, 407.882.1514) Mikhail Klimov, M.S. (firstname.lastname@example.org, 407.882.1509) Qi Zhang, Ph.D. (email@example.com, 407.882.1511)
Administration: Karen Glidewell (firstname.lastname@example.org, 407.882.1500) Kari Stiles (email@example.com, 407.882.1455) Materials Characterization Facility 12443 Research Parkway, Suite 304 Orlando FL 32826-2455 Phone: (407) 882-1500 • Fax: (407) 882-1502 www.ampac.ucf.edu/facilities/MCF.php
Advanced Materials Processing and Analysis Center Engineering Building 1, Suite 381 • Box 162455, 4000 Central Florida Boulevard, Orlando FL 32816-2455 Phone: (407) 882-1455 • Fax: (407) 882-1462 • www.ampac.ucf.edu NanoScience Technology Center 12424 Research Parkway, Suite 400, Orlando FL 32826-3252 • Phone: (407) 882-1578 • Fax: (407) 882-2819 www.nanoscience.ucf.edu