Transmission Electron Microscopy

Transmission Electron Microscopy A Textbook for Materials Science David B Williams and C. Barry Carter

Electron Microscopy of Thin Crystals P.B. Hirsch, A. Howie, R.B. Nicholson, D.W. Pashley and M.J. Whelan
Practical Electron Microscopy in Materials Science J.W. Edington

Feb. 24, 2011 Instrument Modes of Operation, Scattering (Elastic and Inelastic) Mar 1, 2011 Mar 3, 2011 Mar 8, 2011 Instrument (contd) Diffraction (Introduction), Bragg, Laue Approach, Reciprocal Space Reciprocal Space (contd) - Examples

Mar 10, 2011 Diffraction from Crystals, Thin Foil Effect, Indexing patterns, Kikuchi Lines Mar 3 2011 Diffraction (continued), Convergent Beam Electron Diffraction Mar 8, 2011 Solving diffraction patterns - Examples

Mar 10, 2011 Diffracted Beams, Howie-Whelan Equations, Bloch waves Mar 15, 2011 II Test Mar 17, 2011 Imaging (introduction), Thickness and Bending Effects Mar 22, 2011 Thickness Fringes, Bend Contours and Planar Defects Mar 24, 2011 Strain Fields, Weak Beam Dark Field Imaging Mar 29, 2011 Phase Contrast Imaging, HR images Mar 31, 2011 Apr 5, 2011 Apr 7, 2011 Apr 12, 2011 HR images (continued) Other Special Techniques (Holography, Lorentz..), Analysis (Intro), XEDS, EELS EDS and EELS Specimen Preparation, Miscellaneous

Apr 14, 2011 Case studies

HVEM JEOL (1.25 MV)

UHV TEM (Hitachi)

AEM Philips (200 kV)

VG STEM (100 kV)

TEM is a great instrument capable of Imaging Diffraction Chemical Analysis Spectroscopy

from the same area on the specimen

However, beware . Artifacts due to projection

Interpretation not straight forward (like SEM) Poor Sampling Possibility of Radiation-induced damage

JEM- 2010 Configuration

Cross-section of a TEM!

Types of Diffraction Patterns

Amorphous Crystalline

Fine-grained

CBED

Mass-Thickness Contrast

Pb particles in Al matrix

Z-contrast

Pt nanoparticles on Al2O3 (Z-contrast)

High Angle Annular Dark Field Imaging (HAADF)

Diffraction Contrast Bright Field

BF

Dark Field
DF

S=0

S>0

S>>0

Weak Beam Dark Field

Phase Contrast Images

Moire Fringes due to overlapping crystals

Phase Contrast Images (continued) High Resolution Images

Ge GB

Si3N4 GB

Interpretation not straight forward. Image simulation needed Simulated Images Different defocus

Carbon Nanotubes

Chemical Analysis

XEDS from Stainless Steel

Electron Energy Loss Spectroscopy

EELS from TiC and TiN precipitates in SS

Ray Diagrams for Imaging and Diffraction

Parallel Beam Operation

C1 forms a demagnified image of the gun crossover C2 needs to form an underfocused image of the C1 crossover (for parallel illumination)

Alternately, C2 is focused to produce an image at the front focal plane of the upper objective lens (why do we get a parallel illumination here?)
For parallel beam mode, C1 kept at a constant setting. Only C2 needs to be manipulated

Use of C2 aperture reduces the beam current but increases the coherence of the beam (due to reduced convergence angle)

Convergent Beam Mode

Converged beam can be used as a probe (remember SEM) STEM mode and AEM Use a combination of lens settings and apertures to get this

With FEG, a fine probe can be obtained with C1 and C2. Otherwise, we require a C3 (condenser-objective lens)

Switch off C2 and use C3. Why does it give a finer probe than C2?

Effect of C1 lens strength on Probe Size

Condenser-Objective Lens System

Shifting and Tilting the Beam

Shifting to position probe on a region of interest (or centre)

Tilting for Centered Dark Field Imaging

C2 Aperture Alignment

Convergence Angle

Spot Size

Two Basic Operations of the TEM

DIFFRACTION

IMAGING

Selected Area Diffraction in TEM

Selected Area Diffraction in TEM We cannot inset an aperture in the specimen plane because the specimen is already there!! Inserting an aperture in the image plane is like inserting a virtual aperture in the specimen plane restricts the area from which we get the diffraction pattern Smallest aperture ~ 10 mm Demagnification typically around 25 => Selected area ~ 0.4 mm

Bright Field and Dark Field Images

Bright Field

Dark Field

STEM Mode

Scanning in STEM (remember SEM)

Bright Field and Dark Field in STEM Mode

We can collect BF signal and also annular dark field signal in STEM mode. This is not possible in conventional TEM. Why?

(well talk about it later)