appreciating the very little things: status and future ...•count 1500 full fps –3.7x the frame...
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Appreciating the very little things: Status and future prospects of TEM at NUANCE
Dr. Roberto dos Reis
11/28/2018
Nature 542, pages75–79 (2017)
TEM Facility Manager:Dr. Xiaobing Hu
Resources
- Microscopes and techniques available
• 75kV 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 ProtochipsPoseidon 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
Hitachi H-8100
Resources Available
• 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 900oC
Hitachi HD-2300 Dual EDS Cryo-STEM
Resources Available
Hitachi HT-7700 Biological TEM
• Resolution 0.20nm lattice
• 40 to 120kV at 100V increments
• Magnification of 50-1000x, with 200x - 600,000x zoom
• Image rotation +/- 90˚ in 15˚ steps
• STEM unit at 1 nm resolution
• Bruker EDS system for elementary analysis
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
Resources Available
Si [112] Zone Axis
Upper row: simultaneously acquired high angle annular dark‐field (HAADF) and annular bright‐field (ABF) STEM images of SrTiO3
Lower row: EDS maps of Sr, Tiand O from the same sample
• 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 60-200kV• Gatan OneView CMOS camera
JEOL JEM-ARM200CF S/TEM
Resources Available
• 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 Torrto 1 atm), with local specimen heating
Tomography TEM holder ‐accommodates TEM grids, FIB, and atom probe samples.
Nanofactory nano‐manipulation and electric biasing holder
Ref: L. Luo, J. Wu, et al. ACS Nano, 8, 11560 (2014).
JEOL JEM-ARM300CF S/TEM
Resources Available
Nature 563, 462-464 (2018)
Nature 559, 343–349 (2018)
Phys. Rev. Lett. 102, 096101 (2009)
Instrument comparison: Reconstructed phase images of Au [110]
Credit C. Kisielowski, LBNL
Spot size and shape limited by aberrations
Aberration Correction
Aberration Correction
Adv. Struct Chem Imag (2016) 2:15
Aberration Correction
Fast-pixelated direct electron detectors
Direct Electron Detectors
• 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)
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 ratioIn-situ studies•Full- or sub-area sampling at rates up to 1600 fps
Fast‐pixelated direct electron detectors: Enabling new imaging modalities
V. B. Ozdol et al. Appl. Phys. Lett. (2015).
Strain Mapping
O. Panova et al. Micron 88, 30 (2016).
Orientation Mapping in Polymers
C. Ophus, Nat. Comm 7, 1 (2016).
Hybrid Materials– MIDI-STEM Local Symmetry/Composition - PACBED
C. Ophus, J. Ciston et al APL. (2017).
R. dos Reis, APL (2018).
Ptychography
Low dose – structural biology
Yuxi Liu et al, PNAS 2017
D. Zhang et al, Science 2018
Low dose – COF/MOF
2D real x 2D reciprocal space = 4D-STEM
NUANCE Seminar – April 26th, 2018
Courtesy of C. Ophus(NCEM,MF, LBNL)
Experimental K2 IS dataset, 256x256 probe positions, 1920x1792 CBED image sizes.
225 billion pixels (420 gigabytes) in ≈3 minutes.
Data manipulation / analysis is our biggest challenge by far!
NUANCE Seminar – April 26th, 2018
2D real x 2D reciprocal space = 4D-STEM
Courtesy of C. Ophus(NCEM,MF, LBNL)
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
3) Data storage demands
Acquisition of large datasets is possible..how to analyze/transport/share..etc?
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
4D STEM Experiments
1.
PACBED: matching experimental diffraction patterns to
simulations
STO STO-LMO mix STO STO-LMO mix STO
Thickness/Composition
APL. 110, 063102 (2017);
APL. 110, 063102 (2017);
Thickness/Composition
APL. 110, 063102 (2017);
S.Cheema, R. dos Reis et al, (under review)APL 98, 052904 (2011).
Local Symmetry
TEM Facility Manager:Dr. Xiaobing Hu