Appreciating the very little things: Status and future prospects of TEM at NUANCE

Transcription

1 Appreciating the very little things: Status and future prospects of TEM at NUANCE Dr. Roberto dos Reis 11/28/2018

2 Nature 542, pages75 79 (2017)

3 TEM Facility Manager: Dr. Xiaobing Hu

4 Resources - Microscopes and techniques available

5 Resources Available Hitachi H kV to 200kV thermionic emission (W hairpin filament) Large specimen tilt (+/- 45 degrees) pole piece In situ heating experiments with a heating stage (up to 900 degrees) A cryo-tem with a cryo-holder (down to -170 degrees) High quality Gatan TV rate CCD camera for imaging (down to 0.5 nm resolution) and diffraction (large tilting with a Gatan double tilt holder) Liquid flow/electrochemical process capabilities with Protochips Poseidon holder Operation at low kv (75 and 100 kv) for soft- and bio-materials and 200 kv for inorganic materials CBED, nanodiffraction capabilities Hollow-Cone Illumination

6 Resources Available Hitachi HD-2300 Dual EDS Cryo-STEM High brightness FEG operated at 80, 120 and 200 kv Ultra-sensitive dual-eds capability, compatible with cryogenic specimen holder and low kv (80,120) operation Gatan Enfina EELS system Secondary electron detector for SE imaging Multiple STEM imaging modalities (BF, ADF, HAADF), down to ~ 0.23 nm Gatan Cryo-TEM holder and transfer system Low-dose operation mode Gatan diffraction CCD for nano-diffraction with a full-space tilting rotation holder High voltage cryo-sem capability: secondary electron imaging is suitable for checking thick and frozen samples, like cells, tissues up to tens of micron Gatan heating stage, up to 900 o C

7 Hitachi HT-7700 Biological TEM Resources Available Resolution 0.20nm lattice 40 to 120kV at 100V increments Magnification of x, with 200x - 600,000x zoom Image rotation +/- 90 in 15 steps STEM unit at 1 nm resolution Bruker EDS system for elementary analysis

8 Resources Available JEOL JEM-2100 FasTEM High brightness Schottky FEG emitter operated at 200kV 0.1 nm lattice resolution in HRTEM mode 0.2 nm spatial resolution in STEM and analytical mode HAADF STEM detector, Oxford EDS system and Gatan GIF system for atomic resolution Z-contrast imaging, sub-nanoscale resolution EDS and EELS point analysis, and automated line scans and maps Gatan double-tilt heating stage (up to 1100 degrees) Low-Z(Be) double -tilt holder for analytical x-ray microanalysis Hummingbird tomography holder for 3D tomography

9 JEOL JEM-ARM200CF S/TEM Resources Available 200 kv Cold FEG Flash & Go Aberration corrected (probe) 0.08 nm STEM/0.23 nm TEM Resolution 0.35 ev energy resolution Dual SDD EDS detector (1.7sr!) Simultaneous HAADF/BF/ABF Gatan Quantum Dual EELS Atomic resolution at kV Gatan OneView CMOS camera Si [112] Zone Axis Upper row: simultaneously acquired high angle annular darkfield (HAADF) and annular brightfield (ABF) STEM images of SrTiO 3 Lower row: EDS maps of Sr, Ti and O from the same sample

10 Resources Available JEOL JEM-ARM300CF S/TEM 300 kv Cold FEG Flash & Go 0.19 nm STEM/0.22 nm TEM resolution Wide gap pole-piece for in situ expts. HAADF/BF/ABF & Diffractive STEM imaging SDD EDS detector Gatan OneView-IS camera for fast imaging (300 fps (1k x 1k) with automated drift correction) K3 beta site in 2019 Hummingbird gas holder & delivery system Compatible with other in situ holders (heating, fluidic, biasing, mechanical straining...) Gas flow TEM holder can deliver up to 8 pressure controlled gases (from 10 7 Torr to 1 atm), with local specimen heating Tomography TEM holder accommodates TEM grids, FIB, and atom probe samples. Nanofactory nanomanipulation and electric biasing holder Ref: L. Luo, J. Wu, et al. ACS Nano, 8, (2014).

11 Nature 559, (2018) Nature 563, (2018) Phys. Rev. Lett. 102, (2009)

12 Instrument comparison: Reconstructed phase images of Au [110] Credit C. Kisielowski, LBNL

13 Spot size and shape limited by aberrations

14 Aberration Correction

15 Aberration Correction

16 Aberration Correction Adv. Struct Chem Imag (2016) 2:15

17 Fast-pixelated direct electron detectors

18 Direct Electron Detectors Counting and in-situ studies 14.2 Megapixel direct detection sensor reads out at 400 fps with each frame delivering a usable image Highest DQE maximizes signal-to-noise ratio In-situ studies Full- or sub-area sampling at rates up to 1600 fps Count 1500 full fps 3.7x the frame rate of K2K3 IS model (1027) 24 megapixels (5,760 x 4,092) K3 Base IS model (1026) 14 megapixels (3,456 x 4,092)

19 Fast pixelated direct electron detectors: Enabling new imaging modalities Strain Mapping Low dose structural biology Orientation Mapping in Polymers Yuxi Liu et al, PNAS 2017 Low dose COF/MOF V. B. Ozdol et al. Appl. Phys. Lett. (2015). Hybrid Materials MIDI-STEM Ptychography C. Ophus, Nat. Comm 7, 1 (2016). D. Zhang et al, Science 2018 O. Panova et al. Micron 88, 30 (2016). Local Symmetry/Composition - PACBED C. Ophus, J. Ciston et al APL. (2017). R. dos Reis, APL (2018).

20 2D real x 2D reciprocal space = 4D-STEM Courtesy of C. Ophus (NCEM,MF, LBNL) NUANCE Seminar April 26 th, 2018

21 2D real x 2D reciprocal space = 4D-STEM Experimental K2 IS dataset, 256x256 probe positions, 1920x1792 CBED image sizes. 225 billion pixels (420 gigabytes) in 3 minutes. Courtesy of C. Ophus (NCEM,MF, LBNL) Data manipulation / analysis is our biggest challenge by far! NUANCE Seminar April 26 th, 2018

22 Managing Big Datasets from newly developed TEM-based experiments: 1) Limitations imposed by the detector acquisition speed data acquisition and storage have evolved to a point where it is now possible to capture and save high resolution multi dimensional data sets rapidly 2) Synthesis and visualization of the of the data to extract useful information: Basic assumptions about the image formation process preconditions the expectation of what information is available limiting the potential information that can be extracted New data analysis algorithms (or even translate the current ones to a larger audience) are needed to follow up with the current detector technology 3) Data storage demands Acquisition of large datasets is possible..how to analyze/transport/share..etc?

23 4D STEM Experiments 1. PACBED: matching experimental diffraction patterns to simulations

24 Thickness/Composition STO STO-LMO mix STO STO-LMO mix STO APL. 110, (2017);

25 Thickness/Composition APL. 110, (2017);

26 APL. 110, (2017);

27 Local Symmetry APL 98, (2011). S.Cheema, R. dos Reis et al, (under review)

28 TEM Facility Manager: Dr. Xiaobing Hu