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

Dr. Roberto dos Reis

roberto.reis@northwestern.edu

11/28/2018

Nature 542, pages75–79 (2017)

TEM Facility Manager:Dr. Xiaobing Hu

xbhu@northwestern.edu

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

xbhu@northwestern.edu