Characterization and Fabrication Techniques for Nanoscience and Nanotechnology Research Electron Microscopy at Columbia Nano Initiative The Webinar will Dr. Nava Ariel-Sternberg Begin at 1 PM Director , Columbia Nano Initiative Labs eastern time Dr. Amir Zangiabadi Director , Electron Microscopy Labs
Webinar Objectives u Overview of CNI Shared Labs, research capabilities, and fields of research u Overview of Electron Microscopy and sample preparation u Examples from recent research projects at CNI using Electron Microscopy
Dr. Nava Ariel- Sternberg Director , Dr. Amir Columbia Nano Zangiabadi Robert Ehrmann Initiative Labs Director , Managing Director , Electron NACK Network Microscopy Labs
Webinar Objectives u Overview of CNI Shared Labs, research capabilities, and fields of research u Overview of Electron Microscopy and sample preparation u Examples from recent research projects at CNI using Electron Microscopy
The Fu Foundation The Faculty of Arts School of Columbia Nano and Sciences Engineering and Initiative Applied Science Founded in 2014 Columbia Nano Initiative Shared Labs Columbia Nano Initiative Administrative Office Supply research services to approximately 100 research groups on campus, external academic institutes and some industrial companies! 5
Research at CNI 2D Materials and Devices Silicon Photonics Bioelectronics Grating Emitter Non conventional Photonics Design and flexible and Architecture electronics Waveguides Superatoms 6 6
NOVEL RESEARCH AREAS ENABLED BY SILICON PHOTONICS Fluidics Quantum Optics Prof. Michal Lipson Neuroscience syntheti Silicon Photonics ω pump ω signal ω idler ω pump 3 µ m Nonlinear Optics Mechanics http://lipson.ee.columbia.edu/ 7
Bioelectronics for Neuroscience applications: 1024-channel prototype In vivo 1k-channel 1,024 channels per layer. 10 layers. NeuroProbe Prof. Kenneth Shepard https://bioeeweb.ee.columbia.edu/wordpress/research/ Kenneth Shepard, BioelectronicSystems Laboratory, Columbia University, New York, NY 8
CNI Shared Facilities Electron Microscopy Clean Room Materials Characterization Over 400 users from approximately 100 research groups. External users are welcome! 9
Meet the staff – CNI Shared Facilities Dr. Nava Ariel- James Vichiconti Dr. Dan Paley Dr. Amir Nirit Porecki- Dr. Jaeeun Melody Gonzalez Sternberg Zangiabadi Shamay (Jen) Yu Director of Director of Clean Director of Director of EM Senior Clean Clean room Research Shared Facilities Room SMCL lab room Engineer Engineer Operation Assistant 10
CNI Clean Room An environmentally controlled lab – tight limits for temperature and humidity , air u exchange Particle filtering, class 1000 to 10,000 u Clean room apparel u *T erra Universal Inc. 11
Clean Room Utilities and Supporting system Non Contact Cooling Water system to cool u equipment DI water supply for processing u N2 and compressed dry supply u AHUs, dehumidifier and Clean Steam Generator u for tight temperature and humidity control Exhaust for chemicals fumes and air exchanges u Lab monitoring system u Safety systems - Toxic Gas monitoring System u (TGMS) 12
Patterning: Photolithography and Etch • SUSS Mask aligner for UV exposure Oxford Reactive Ion Etching • down to 248nm (sub-micron resolution) 13
Deposition and thin film growth Angstrom e-beam evaporation AJA magnetron sputtering Expertech LPCVD furnace 14
Back End: Connecting the device to the outside world Westbond Wirebonders Disco DAD 3220 Dicing CMP: Poli-400L saw 15
Materials Characterization Lab Particle size, Molecular Crystallographic structure Surface Analysis and weight distribution, and Z- and orientation surface area potential Optical and Magnetic Molecular structure and Thermal Properties Properties bonding information 2D materials device fabrication and characterization 16
Surface Analysis and bonding BET analyzer: Surface area by measuring nitrogen adsorption isotherms for porous materials at 77 Bruker AFM K. XPS: For surface elements survey and depth profiles 17 Renishaw Micro-Raman: 405, 532, 633 or 785 nm lasers with spectral resolution of ~ 1
Crystallographic structure, phase, orientation Information Agilent SuperNova SCXRD: Mo/Cu dual micro-focus PANalytical PXRD: For powder crystallographic source of 50W. analysis. Temp. measurements in the -173-400°C range 18
Particle size, Molecular size distribution, and Z-Potential GPC: gel permeation chromatography Dynamic Light Scattering (DLS) and Z-potential to analysis of polymers at different solvents and measure: particle size, molecular weight, and zeta temperatures. potential for organic and aqueous colloids, nanoparticles, and proteins. 19
Optical and Magnetic Characterization Spectrophotometer: measuring absorbance Woollam Ellipsometer: thin film thickness in the 190-1100 nm range. Temp and refractive index measurements measurements in the -20-110°C. SQUID: DC and AC measurements of magnetic susceptibility. Sample temperature between 1.8 20 and 300 K.
Thermal Properties and 2D materials device fabrication and Characterization TGA: Thermal analysis 2D Material processing in protective environment: Autofinder temperatures between ambient (microscope with computer-controlled xyz axes and a remote- and 1000 °C. controlled micromanipulator, 0.5 µ precision) 21
Electron Microscopy and Imaging FEI Nova NanoSEM 450: • FEG with Through lense SED, Everhart Zigma VP Zeiss SEM: Thormley SED, Low Vacuum SED, Through FEG with Inlens, SE, BSED and • lens BSED detectors. FEI Talos F200X TEM/STEM: VPSE detectors • NPGS – Nabity system for e-beam writing • Max acc voltage of 200 kV, configured for Bruker EDS system • 80kV as well • Super X-EDS system; 4 Silicon drift detectors (SDD) • TEM point resolution (nm) 0.25 • Sample preparation suite 22
Types of Microscope Using electrons to “see” objects to atomic level q Similar to optical microscopy except with electrons rather than photons q Used to image samples with a resolution of 10 Å q Can image many different structural geometries q Mostly limited by radiation damage from the electron beam X-ray ϒ -ray http://nobelprize.org/educational_games/physics/microscopes/powerline/index.html 23
Types of Microscope Using electrons to “see” objects to atomic level q Similar to optical microscopy except with electrons rather than photons q Used to image samples with a resolution of 10 Å q Can image many different structural geometries q Mostly limited by radiation damage from the electron beam X-ray ϒ -ray http://nobelprize.org/educational_games/physics/microscopes/powerline/index.html 24
Electron Microscope Same principle, but in very different shapes Electromagnetic Glass lenses lenses Direct observation Video imaging https://www.hitachi-hightech.com/global/sinews/si_report/07046/ 25
Testing the Resolution in STEM May 2017 March 2015 (approved in Czech Republic) 26
Specimen Preparation - general techniques for materials sciences Direct lattice resolution in polydiacetylene single crystal showing 27 http://www.ph.qmw.ac.uk/images/molwires.jpg (010)lattice planes spaced at 1.2 nm.
Why Sample Preparation is so Important? • Bad sample prep, unclear observation, wrong analysis! Cross section, Ion Milling (>2kV) Cross section, Ion Milling (down to 100V) D. Laub, Interdisciplinary Centre for Electron Microscopy, EPFL 28
Sample Preparation Overview 29 Transmission Electron Microscopy, David B. Williams C. Barry Carter 2009
Mechanical à Tripod Method • Mechanical thinning, in a wedge configuration, down to electron transparency or to a thickness that requires very short ion milling time. • Polishing with diamond-impregnated lapping films; Finish with colloidal silica TiO 2 / Silicon, Optical microscope, reflected light 30
Dimple Grinding Thinning the central part of the sample to less than 20 µm before ion milling. Mechanical grinding + Polishing Dimple Grinding Ion milling 31
Focused Ion-Beam (FIB) – Collaboration with CUNY Using precise focused ion beam to select the sample. Then using manipulator to pickup the sample http://www.nature.com/nprot/journal/v6/n6/abs/nprot.2011.332.html 32
https://www.youtube.com/watch?v=vNOpzDViAhE
Focused Ion-Beam (FIB) 34
Biological Specimen Preparation bacteriophage 35 http://pressblog.uchicago.edu/2011/05/20/traffic-carl-zimmer-and-timothy-lu.html
Overview of Biological Specimen Preparation – Focusing on Sectioning Killing & Fixation - Death; Molecular stabilization Dehydration - Chemical removal of H 2 O Interference reflection angle from Sjöstrand (1967) Infiltration - Replace liquid phase with resin Embedding & Polymerization - Make solid, sectionable block Sectioning - Ultramicrotome, mount, stain 36
Examples from Research Studies at Columbia Nano Initiative Columbia University bacteriophage 37
Solar–Thermal Energy Absorber At 200 C, copper tends to diffuse outside of the particles J. Mandal et al, Adv. Mater. 2017, 29, 1702156 38 Courtesy of Prof. Y. Yang
Solar–Thermal Energy Absorber J. Mandal et al, Adv. Mater. 2017, 29, 1702156 Courtesy of Prof. Y. Yang 39
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