TRANSMISSION ELECTRON

MICROSCOPY
Danqi Wang

Swagelok Center for Surface Analysis of Materials (SCSAM)

Case Western Reserve University

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OUTLINE
SCSAM TEM Instrument
Introduction
Scanning TEM
Imaging
XEDS
EELS
TEM
Bright-field/Dark-field Imaging
High-resolution Imaging
Diffraction
Energy-filtered TEM
Transmission Kikuchi Diffraction/ASTAR system
Sample Preparation Nanomill
SCSAM TEM Instruments
FEI Tecnai F30 (300 kV)
Zeiss Libra 200EF (200 kV)

TEM Sample Preparation

Focused Ion Beam
NanoMill Model 1040
Precision Ion Polishing System
Twin Jet Electropolishing System
 FEI TECNAI F30

Operating at 300 kV

Resolution Limit 0.17 nm

High-resolution imaging

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ZEISS LIBRA 200EF

Operating at 80, 120, and 200 kV

Energy Resolution < 0.5 eV

Analytical chemical analysis

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OUTLINE
INTRODUCTION
Resolving Power of Microscopes

Transmission Electron Microscope

 Useful Signals Generated from
ElectronMatter Interaction

Major Contrast
Mechanisms
for imaging
Mass thickness contrast,
Diffraction contrast,
Phase contrast (HRTEM).

It is essential that specimens for TEM be extremely thin, i.e, a few tens of nms
or less, so as for the energetic electron beam to penetrate and generate useful
signals.
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Modes of Imaging
Scanning Microscopy Full Frame Imaging
Scanning electron microscopy Transmission electron microscopy
Scanning transmission electron Regular light microscopy
microscopy X-ray imaging
Focused Ion Beam Visible light photography

Source Source

Object imaged Object imaged

Detector Image forming lens
image pixel by pixel
Recording 2D media
CCD, negative
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 What do can we learn?
Structure Information Composition
Elastic scattering Inelastic scattering/XEDS
Morphology and microstructure. Elemental composition
Crystallographic structure Bonding state

High Resolution Electron Energy Loss Spectroscopy (EELS)

Transmission Electron Microscopy

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Scheu et. al., Phil Mag A, 78(2) 1998, 439.
XEDS Elemental Mapping
Solid Oxide Fuel Cell

Purple Zr; Yellow LSM;

Green Mn.
OUTLINE
SCANNING
TRANSMISSION ELECTRON
MICROSCOPY (STEM)
Imaging
EDS

EELS
 Gold on Carbon film
STEM DF

BF

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Atomic Resolution
STEM

20 nm

Carburized Ferrite in 17-7 PH

Stainless Steel
1 nm
XEDS Elemental Mapping
Solid Oxide Fuel Cell

Purple Zr; Yellow LSM;

Green Mn.
XEDS Line Scan in STEM
Cu-Al2O3 Composite
Si

Ca

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ELECTRON ENERGY-LOSS SPECTROSCOPY
 EELS Analysis- Valence State
Grain-1

Grain-2

O-K edge results show the presence of precipitates in 2 valence states

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Electron Spectroscopy Imaging (ESI) Elemental Mapping

Ti 452 eV

N 398 eV

Oxygen map Ti map Color Mix: Red:Ti, Green:O

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High Temperature MEMS Device
 Life Science Applications
Dark-field STEM Image of Fe Deposit in a
Erythroid Precursor Cell

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XEDS Spectrum of Fe Deposit

Grid

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EELS Spectrum of Fe in Different Oxidation States

Fe2+
FeCO3 (Siderite)

Fe2+ + Fe3+
Fe3O4 (Magnetite)
707 eV
OUTLINE
TEM
Bright-field/Dark-field Imaging
Diffraction

High-resolution Imaging

Energy-filtered TEM
Diffraction Imaging
Full Frame Imaging

TEM imaging system can be

operated in two modes:
diffraction mode (left),
imaging mode (right).
Shown here are simplified ray
diagrams of both modes.

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Bright-field and Dark-field Imaging in TEM
BF DF DF

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Bright-field vs Dark-field Imaging

To identify grain size

and distribution in the
microstructure

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Nanocrystalline Al. Scale markers are 500 nm.
Bright-field vs Dark-field Imaging

To identify a second
phase in the
microstructure

Nitrided ferrite in
17-7 PH Stainless
Steel
 High-resolution TEM (HRTEM)

A HRTEM image of an
interface between a Cu
particle and alumina
grain.

Grain
Boundary

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Electron Diffraction
Analyze the Lattice
Spacing and Orientation

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 3.620 3.622
Convergent-
beam electron
diffraction
(CBED)
ZA [323] ZA [221]
HOLZ lines used for
lattice parameter 3.620 3.624
determination
Austenitic stainless
steel

ZA [111] ZA [536]
MEASURED SAMPLE THICKNESS
FROM AUSTENITIC STAINLESS STEEL

Simulated Simulated

Experimental
ENERGY-FILTERED TEM (EFTEM) IMAGING
 Zero-loss EFTEM images:
Dislocations in 316 Stainless Steel after Low-temperature Gas-phase Carburization.
Specimen prepared by electropolishing

Un-Filtered Zero-loss Image

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 EFTEM Images from Co-Polymer
Polystyrene and PVDF
Zero loss Image 20 eV Loss Image*

With F

Without F

* Energy of plasmon excitation for Fluorine

OUTLINE

TRANSMISSION KIKUCHI DIFFRACTION

(TKD): STEM IN A SEM
 EBSD VS TKD
Bulk material Thin TEM foil
Surface Can resolve 3-5 nm
information -20 - 0 tilt
Tilted to 70 Exiting surface
Interaction volume structure
30-50 nm

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Tim Maitland and Scott Sitzman

Scanning Microscopy for Nanotechnology, Springer Ren de Kloe - EDAX
 WHY USE TKD?

Improved spatial resolution compared to EBSD: 30-50 nm

3-5 nm. Actual resolution will depend on sample
composition and preparation.

Users that have a FIB system together with EDS/EBSD,

can carry out this analysis at practically no extra cost.
Carburized Low-alloy Steel (15 nm/step)
XEDS
OUTLINE

ASTAR SYSTEM
PRECESSION ELECTRON DIFFRACTION (PED)
ADVANTAGES OF ASTAR
TEM diffraction patterns easier to interpret
Less sensitive to sample thickness variations
More diffraction spots higher precision
measurements
Automated analysis becomes possible
INDEXING TEM DIFFRACTION PATTERNS
Stereographic projection
Pre-calculated templates Acquired pattern
(cubic ) 111

Angular step size ~1

~ 3000 templates

001

1-11

Correlation index
 ASTAR ORIENTATION MAPPING
Similar results to SEM-EBSD but with much higher spatial
resolution. Down to 1 nm with FEG!

SEM image EBSD map TEM map

Deformed Ta6V (20-100 nm step size) (1-30 nm step size)
Al (9 nm) TiN (1 nm)
multilayer system

Al

Phase Map

Orientation Map

ASTAR system could both identify the phases

and orientations.

Note that the Al layers are finely twinned.

ASTAR ORIENTATION MAPPING

Quality Map Orientation Map

40 nm

Gold nanoparticles
OUTLINE

TEM SAMPLE PREPARATION

FISHIONE NANOMILL MODEL 1040
ADVANTAGES OF NANOMILL

Low energy ion source (up to 2kV Ar)

Removes amorphous and implanted layers
AS-FIBBED TEM FOIL

High-resolution TEM image of Si showing the effect of Ga

implantation and surface amorphization on phase contrast imaging
AFTER NANOMILLING

Same specimen after Ga implantation and

amorphization removal by the NanoMilling process
SUMMARY

TEM can provide information regarding to

Structure

Defects (dislocations, twins, etc.)

Morphology

Composition

Valence state

Orientation
THANK YOU!