Electron Microscopy for Material Characterization

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Outline
Introduction to Electron Microscopy Why Electron Microscopy came in existence? Physical Principle Involved Components of Electron Microscope Comparison of LM, TEM and SEM Scanning Electron Microscope -Overview Transmission Electron Microscope Overview Disadvantages

Introduction to Electron Microscopy

For imaging of nanoscale objects Electron microscopes uses electrons instead of photons Electrons have a much shorter wavelength than photons Observe matter with atomic resolution Two general types of electron microscopes: 1.Scanning Electron Microscope (SEM) 2.Transmission Electron Microscope (TEM)

Magnifications achievable by the different microscopes

Variation in magnifications achieved by optical, scanning and transmission electron microscope

Comparison of Transmission and Scanning Electron Microscopic images

The electron range increases with beam energy. Fig.e.g.. The internal structure of the Au deposits examined at high electron beam energies in SEM and TEM.

Incident high KeV electron beam

Bremstrahlung

Secondary & Backscattered Electrons for SEM

Visible Light

Auger Electrons

Direct Beam for TEM

Characteristic X-Rays

SEM Electron beam is focused and scanned over the sample surface Secondary electrons or back scattered electrons and characteristic x-rays from each point of interaction is collected by the detector 2-D image of spatial distribution of these signals are mapped. TEM Transmitted electron beam (through sample) forms an enlarged image.

Instrumentation of Electron Microscope

Source Condenser lens Objective lens Projector lens (TEM) Suitably prepared specimen
Metallic coating for SEM - conducting Thin section for TEM - transmission

Electron Source
Thermionic gun: triode or self-biasing gun, W, LaB6, CeB6 Field Emission Gun: Single crystal W

Condenser Lens
Collects light to direct it at the small area of the object. It makes the object brighter (better contrast). Enables to control the angle at which the illumination reaches the object. Converge the light beam on object or can illuminate it with parallel rays. Condenser aperture: controls the area of specimen to be illuminated.

Comparison of LM, TEM and SEM

The Scanning Electron Microscope

Produces a 3-dimensional image of specimens surface features
The interactions of the electrons with surface are registered, and electrons reflected from surface create image.

Electron beam is scanned back and forth over the specimen, imaging only one point at a time. PE energy is kept relatively low (1-30 keV) to limit the interaction volume in the specimen so high sensitivity to surface composition (cannot penetrate far into the sample). Can be used for thicker specimens

Electron Beam Interaction

Primary electrons generate low energy secondary electrons, emphasize the topographic nature of the specimen Primary electrons backscattered produces images with a high degree of atomic number (Z) contrast Ionized atoms can relax by electron shell-toshell transitions, which lead to either X-ray emission or Auger electron ejection. The X-rays emitted are characteristic of the elements in the top few m of the sample.

Scanning Electron Microscopy (SEM) & Energy-dispersive X-ray Microanalysis (EDAX)

Impinging electrons interact with the samples molecular composition. The energy of the impinging electrons is in proportion to the type of electron interaction generated from the sample. A series of measurable electron energies produced are analyzed -creates a spectrum of the unique elements .

SEM

Fig. Schematic presentation of SEM

Range of Applications of SEM

Classification of materials Failure and defect analysis Examination of surface morphology (including stereo imaging) Analysis and identification of surface and airborne contamination Powder morphology, particle size and analysis Cleaning problems and chemical etching Welding and joining technology Paints and coating failures Identification and elimination of corrosion and oxidization problems.

Applications of SEM

Fig.Fracture section through a pellet of tungsten powder sintered and then sputter coated with an alloy of osmium and ruthenium.

Fig. The image is of the surface of a metal stamper.

EDAX analysis

Fig.Intermetallic particles from an aluminium alloy and EDAX analysis of an Al-rich intermetallic phase.

The Transmission Electron Microscope

Characterization of materials crystal structure and microstructure simultaneously by diffraction and imaging techniques. Electrons scatter when they pass through thin sections of a specimen Denser regions in specimen, scatter more electrons and appear darker Transmitted electrons (those that do not scatter) are used to produce image

TEM

Fig. Transmission Electron Microscope

Common Modes of Operation of TEM

Bright Field (BF) Microscopy Selected Area Diffraction Dark Field (DF) Weak Beam (Special case of DF)

Bright field & Dark field Image

Select Direct Beam Select Scattered Electrons

Resultant Image

Resultant Image

Bright-Field Image

Dark-Field Image

TEM Images

Fig. Bright Field & Dark field images of a grain in TEM

TEM Sample Preparation

Bulk ceramics
Mechanical grinding, Polishing, Focused ion thinning

Metals
Mechanical Grinding, Polishing,Electrolytic thinning

Organic Materials
Freeze drying, Ultramicrotomy (cryo)

Diffraction Pattern In TEM

Electrons through specimen are diffracted according to Bragg's law, n = 2d sin , forming a diffraction pattern. Diffraction pattern is Fourier transform of the periodic crystal lattice. Information on the periodicities in the lattice, and hence the atomic positions.

Diffraction pattern in TEM

Diffraction pattern :
The planar section of the reciprocal lattice perpendicular to beam direction. Also the zone of planes appearing as spots in the pattern.

Different types:
1. Kikuchi Patterns 2.Convergent-Beam Electron Diffraction (CBED) 3. Ring Patterns 4.Spot Patterns

Diffraction Pattern in TEM

Ring Pattern

Kikuchi Pattern

Spot Pattern

CBED Pattern

Imaging in TEM

Disadvantages of EM
Larger ,expensive and destructive technique. Some materials are sensitive to electron beam radiation, resulting in a loss of crystallinity and mass (TEM). Sample may be damaged by the electron beam, particularly in the case of biological materials. Field of view is relatively small- the region analysed may not be characteristic of the whole sample. Sample preparation is very time consuming, sample dimension small .