Page 59 - Introduction to Colloid and Surface Chemistry

Optical properties 49

and show little contrast against the background support, whereas
materials containing heavy metal atoms make ideal specimens.
To enhance contrast and obtain three-dimensional effects, the
technique of shadow-casting is generally employed. A heavy metal,
such as gold, is evaporated in vacuum and at a known angle on to the
specimen, which gives a side illumination effect (see Figure 3.2).
From the angle of shadowing and the length of the shadows, a three-
dimensional picture of the specimen can be built up. An even better
picture can be obtained by lightly shadowing the sample in two
directions at right angles.
A most useful technique for examining surface structure is that of
replication. One method is to deposit the sample on a freshly cleaved
mica surface on to which carbon (and, if desired, a heavy metal) is
vacuum-evaporated. The resulting thin film, with the specimen
particles still embedded, is floated off the mica on to a water surface.
The particles are dissolved out with a suitable solvent and the
resulting replica is mounted on a copper grid.

The scanning electron microscope
In the scanning electron microscope a fine beam of medium-energy
electrons scans across the sample in a series of parallel tracks. These
interact with the sample to produce various signals, including
secondary electron emission (SEE), back-scattered electrons (BSE),
cathodoluminescence and X-rays, each of which (with their varying
characteristics) can be detected, displayed on a fluorescent screen
and photographed. In the SEE mode the particles appear to be
diffusely illuminated, particle size can be measured and aggregation
behaviour can be studied, but there is little indication of height. In
the BSE mode the particles appear to be illuminated from a point
source and the resulting shadows lead to a good impression of height.
The magnification achieved in a scanning electron microscope
(resolution limit of c. 5 nm) is, in general, less than that in a
transmission electron microscope, but the major advantage of the
technique (which is a consequence of the low numerical aperture) is
the great depth of focus which can be achieved. At magnifications in
the range of optical microscopy the scanning electron microscope can
give a depth of focus several hundred times greater than that of the
optical microscope. In colloid and surface science this large depth of