Introduction to Electron, Atom Probe and Scanned Probe

be able to select a technique for a particular materials problem.

Microscopy

explain the origin of magnification in different imaging modes.

Dr Sarah Haigh sarah.haigh@manchester.ac.uk

Estimate or derive spatial resolution limits for the techniques

described, and to explain the difference between resolution and

Lecture 1

magnification.

1. Introduction

resolution and how it might be interpreted.

This course is concerned with some of the more common experimental

methods used for the physical examination and analysis of materials and
biological structures. Methods used for characterizing crystal structures,
biological structures and materials microstructure fall into two classes: (i)

Resources
There are many books on microscopy, and it is worth browsing the
library. The course synopsis also lists many books. Much of the course

Those which give information averaged over a relatively large volume of

discusses transmission electron microscopy and scanning electron

the specimen. Examples include the X-ray diffraction techniques you

microscopy. A useful introduction to these subjects can be found in:

encountered in the first-year. (ii) Imaging methods, which examine local

microstructural features directly. The latter are the subject of this course.

Electron Microscopy and Analysis by Goodhew and Humphreys (a

compact and gentle coverage of both TEM and SEM).

There exist a very large number of such techniques, and we cannot hope

Microscopy is a fast developing field and there are also excellent on-line

to cover them all. Our main emphasis will be on gaining an

resources for the subject such as

understanding of the principles of some of the main microscopy

techniques used in most materials science laboratories so that other

http://www.doitpoms.ac.uk/tlplib/index.php (good sections on TEM,

AFM, Diffraction and Imaging, Optical Microscopy)

techniques can build of this knowledge.

The official synopsis for this course is given on Blackboard but you might

http://www.matter.org.uk/tem

http://www.scribd.com/doc/27761327/Microscopy-With-Light-andElectrons

find it helpful to know that by the end of the course I would expect you to
be able to:

explain how analytical information may be measured at high spatial

Use words and sketch diagrams to explain the principle behind all
the microscopy techniques outlined in this course including optical
microscopy, transmission electron microscopy, scanning
electron microscopy, scanning probe microscopy, atom probe,

These lecture notes are largely based on the course developed over
many years by Prof M L Jenkins and Prof Peter Nellist (University of
Oxford) and I am extremely grateful to them for making these available to
me. Many additional sources have been used to compile these notes and
I would like to thank colleagues including Dr Rik Brydson, Dr. Andrew
Scott and Dr Peter Evennett (University of Leeds) from whom I have
received data.

and x-ray spectroscopy.

Methods of generating magnification:

2. Background
The introduction of the microscope as a tool for the biologist brought

Fig. 1.1. Generating magnification.

about a complete reappraisal of the micro-anatomy of biological tissues,

organisms and cells. In the early days of its application to biological
materials, it was the tool of anatomists and histologists, and many
previously unimagined structures in cells were revealed. More recent
developments in biological specimen preparation have come from
biochemists and physicists who have used the microscope to examine
cells and tissue in many different ways.
In a similar way the field of Materials Science has been largely driven by
the development of techniques to characterize the microstructure of
materials (for example observations of dislocations by Hirsch and coworkers).
What microstructural or biological features might we want to

examine?

Types of signal we can detect:

Fig. 1.2. Types of signals.

3. Types of microscopy
In microscopy, we need to generate magnification so that we can see the
microstructure, and we need to detect a particular type of signal.

By the end of this course you should be able to assign all the

Estimate the magnification of the FIM:

microscopes you will have learnt about to one of these methods of

magnification and all the methods of imaging to one of the types of
signals (annotate 1.1 and 1.2).

4. Examples of projection microscopes

a)

The field-ion microscope (FIM)

Fig. 1.3. Field ion microscope.

The FIM allows imaging of the structure of individual atoms on a surface.

A typical result is shown in Fig. 1.4a, which is of a (100) oriented Pt17%Rh catalyst, imaged in Ne gas, with an applied voltage of 10kV and
a specimen temperature of 80 K. Each of the bright dots is an image of
an individual atom on the specimen surface. Fig 1.4b shows a ball model
of the specimen apex, constructed form a number of spheres arranged in
a cubic lattice. The prominent sites, representing kink atom sites on the
surface of the specimen, are coloured white. These form a series of
concentric rings similar to those seen in the FIM image.

Fig. 1.4. (a) FIM of Pt-Rh catalyst. (b) model structure

The principles of operating of the field ion microscope are:

The specimen is held at a high positive voltage.

The specimen is surrounded by a suitable gas at low pressure.

Ions produced in the high field near the specimen tip are accelerated
towards the screen and imaged.

Higher fields, and therefore more ions, will be produced near

irregularities, such as atoms at the edge of planes.

arrival on the position sensitive detector allows us to determine the mass

There are some limitations to FIM:

the Time Of Flight of the ions: the time between the pulse and the

The stresses in the tip produced by the field may affect it (rearrange

over charge ratio and hence the composition.

defects or cause fracture).

It is intrinsically a surface technique and the results may not be

position and the order of arrival of the ions on the position sensitive

characteristic of the bulk of the specimen.

detector allows us to gain spatial information and therefore to reconstruct

It can tell you where atoms are but not what they are.

the original position of the atoms on the tip.

the (X,Y) position of the ion impact on the detector: the X-Y

By repeating this sequence, the atoms are progressively removed from

b)

the tip, and a 3D image of the material can be reconstructed at the

Atom probe microscopy

atomic scale. Much of the development work of atom probe microscopy

has been in the UK. By including spatial information from the position
Fig. 1.5. Schematic of position sensitive atom probe.

sensitive detector
The atom probe (also referred to as position sensitive atom probe or
PoSAP) can position single atoms and has ~60% detection efficiency.
The resolution of the technique is sub-nanometre laterally and single
atom layer in depth. A typical specimen is needle shaped with a radius of
50nm. The volume analyzed is typically 20 nm by 20 nm by 50 nm (Fig
1.6).
The main limitation of the technique is the requirement for a very sharp
needle sample (preferably conducting). It has the advantage of being
able to detect even low mass elements including hydrides.

The atom probe microscope uses the same projection principle as the
FIM but can provide three dimensional information of the sample
structure and composition as shown in Fig. 1.5. A voltage pulse (or laser)
is used to stimulate atoms being emitted from the surface, i.e. deliberate
use is made of field-evaporation. The detector allows us to
simultaneously measure:

Fig. 1.6. Three separate samples showing mapping of Co

concentration at different stages of ageing at 723K in a solution
treated Cu-1at%Co alloy. All types of atom are detected but only Co
atoms are shown for display purposes.

More details in :
Setna, Hyde, Cerezo, Smith and Chrisholm. Position sensitive atom probe study of the decomposition
of a Cu 2.6at% C alloy. Applied surface science 67 (1993) 368-379
http://www.sciencedirect.com/science/article/pii/016943329390340H
Cerezo et al. Materials Characterisation 25 :143 -156 (1990)
http://www.sciencedirect.com/science/article/pii/104458039090026G
For prospects of using this techniques for biomaterials see the book Nanosystem characterization
tools in the life sciences By Challa S. S. R. Kumar