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The scanning electron microscope and the archaeologist

Article  in  Physics Education · March 2004

DOI: 10.1088/0031-9120/39/2/004

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SPECIAL FEATURE: ARCHAEOLOGY
www.iop.org/journals/physed

The scanning electron microscope

and the archaeologist
Matthew Ponting
English Heritage, Centre for Archaeology, Fort Cumberland, Fort Cumberland Road,
Eastney, Portsmouth PO4 9LD, UK
E-mail: Matthew.Ponting@english-heritage.org.uk

Abstract
Images from scanning electron microscopy are now quite common and they
can be of great value in archaeology. Techniques such as secondary electron
imaging, backscattered electron imaging and energy-dispersive x-ray
analysis can reveal information such as the presence of weevils in grain in
Roman Britain, the composition of Roman coins and the burial of an Iron
Age warrior on a sheep’s fleece that has long since rotted away.

How it works of surface atoms. Secondary electrons are of

The scanning electron microscope (SEM) is
essentially a powerful microscope that creates
an image using electrons instead of light energy
(figure 1). It produces a greyscale image
with particularly good depth of field at high
magnification. To create the image, a very
narrow beam of electrons is produced by an
‘electron gun’ arrangement. This beam is focused
by electromagnetic coils, usually referred to as
‘lenses’, and is then scanned very quickly back and
forth across the sample. The scanning is controlled
by other coils. The whole path of the beam is
kept under vacuum so that electrons do not interact
with air molecules. Samples have to be conducting
and well earthed to avoid the build-up of charge.
Organic samples are often coated with a thin layer
of gold.
As the electron beam hits the sample there are
three main types of interaction, which produce:
• backscattered electrons
• secondary electrons
• x-rays
Backscattered electrons have been deflected
(high energy elastic scattering) by the nuclei
lower energy and result from inelastic collisions
between the electron beam and the atoms
of the target material. These are electrons
ejected from conduction or valence bands of the
atoms. Both types of electrons provide imaging
information, and most modern SEMs allow
switching between secondary electron images
(SEI) and backscattered electron (BSE) images.
When a secondary electron is ejected, an
electron from a higher orbit then takes the vacant
space and this process causes an x-ray photon
to be generated. The emitted x-rays have a
characteristic energy and wavelength specific to
each element and each shell. Two techniques
commonly used to identify x-rays are energy-
dispersive x-ray analysis (EDX) and wavelength-
dispersive x-ray analysis (WDX).
Secondary electron imaging
The usual imaging mode for the SEM is the
secondary electron image. The image appears
as a greyscale picture with good definition and
depth of field. This mode is usually used
for the study of microstructures and textures

166 PHYSICS EDUCATION 39 (2) 0031-9120/04/020166+05$30.00 © 2004 IOP Publishing Ltd

 The scanning electron microscope and the archaeologist

Optical microscope Scanning electron microscope

OM SEM

light source electron soucre

(lamp) (electron gun)

condenser lens
condenser lens
specimen
objective lens
objective
lens scanning objective lens aperture
coil
scanning
circuit

specimen
detector

secondary electrons image

amplifier
eyepiece

deflection coil
naked eye CRT

Figure 1. Comparison of the optical microscope with the scanning electron microscope. In the transmitted light
optical microscope (on the left) light passes through a sufficiently thin sample and is magnified by glass lenses;
with reflected light microscopy the light would be reflected back off the sample. In the scanning electron
microscope, an electron beam is scanned over a sample and the brightness on the CRT is modulated by the
signal obtained.

(microtopography) of material retrieved from and early detection is difficult because of the larvae
archaeological excavations. being inside the grain. They are usually found in
Microscopic study of organic remains can tell grain storage or processing installations and today
us about the environment in the past and the way
people lived. Figure 2 shows a secondary electron
image of a burnt wheat grain that was recovered
from the excavation of a Roman corn drying oven
found at Grateley in Hampshire. The wheat grain
dates from between the third and fourth centuries
AD and its shape tells us that it is of the variety
called spelt (Triticum spelta L.). Spelt wheat was
the most important type of wheat grown in much
of Britain during the Roman period. Scanning
electron microscopy also reveals a hole in the grain
that was made by the granary weevil (Sitophilus
granarius). The female weevil bores a hole in the
grain, in which it lays a single egg. The weevil
larva then gradually eats its way out of the grain Figure 2. SEI of a burnt wheat grain from a Roman
from the inside, leaving the tell-tale exit hole. grain drying oven showing the exit hole left by the
Granary weevils can be a serious pest, even today, departing weevil larva.

March 2004 PHYSICS EDUCATION 167

M Ponting
Figure 3. SEI of mineral preserved fibres showing the
detail that allows the precise identification of the fibres
as wool.
are controlled by superheating or supercooling the
grain, which kills off all stages of these weevils.
Heating to 54 ◦ C for half an hour is enough to
kill granary weevils, and we may surmise that the
discovery of weevil-infested grain inside a corn-
drying oven is no coincidence.
Apart from allowing the accurate identifica-
tion of minute plant and animal remains in archae-
ological deposits, secondary electron imaging can
also be used to identify traces of organic materials
that have long since rotted away. In particular, the
corrosion products of metal objects will sometimes
preserve organic material that was in contact with
them as negative impressions on the surface of the
metal. Figure 3 shows a secondary electron image
of the impressions left by fibres on the surface of
an Iron Age iron sword from a 2000 year-old burial
on the Isles of Scilly. The large depth of field of the
electron image allows detailed examination of the
impressions at high resolution. Here, the fibres are
clearly seen, measuring about 25 µm in diameter.
Their surfaces had overlapping scales and the pat-
tern seen allows the identification of these fibres
as sheep’s wool. Furthermore, the fibres were ran-
domly orientated and so are unlikely to be from a
woven fabric. It is more likely that they are from
a fleece on which the dead warrior was lain.
Backscattered electron imaging
The BSE signal is proportional to the atomic
number of the sample and can be used to create
images reflecting the composition of the object
under investigation that complement the SEI. A
BSE image shows the distribution of areas of
168 PHYSICS EDUCATION
Figure 4. SEI image (left) and BSE image (right) of a
section through a Roman crucible. See text for details.
different composition within the sample where the
contrast between the atomic number is sufficiently
high. Obviously the contrast between elements
that are adjacent in the periodic table is going to
be slight, such as between copper and zinc in a
brass since copper has an atomic number of 29 and
zinc an atomic number of 30. However, where the
difference is greater, as in the case of copper and
silver (atomic numbers 29 and 47 respectively),
there is good atomic number contrast. This
technique is particularly useful for the study of
ancient inorganic materials such as metals, pottery,
glass and wastes from their production, as it will
show the location of chemical phases of different
composition. The identification of these can
provide crucial evidence for the reconstruction of
past technologies and production processes.
Figure 4 shows two images of part of a
section through a bronze-melting crucible from the
Roman fort of Housesteads, on Hadrian’s Wall.
The sections were polished and so little surface
detail is visible, unlike the previous images. The
extra information provided by the atomic number
contrast of the phases in the BSE image can be
clearly seen. The white spots in the BSE image
are trapped metal droplets that stand out because of
their relatively high atomic number. The vitrified
surface of the crucible (to the right) appears as a
lighter area compared to that of the crucible body
(to the left) as it has a slightly higher mean atomic
number due to dissolved metal. The different
mineral phases of the crucible fabric can also be
seen, with the grains of silica appearing as darker
grey areas. The black areas are voids.
March 2004

Figure 5. X-ray spectrum produced from the
characteristic x-rays emitted by a sample under an
electron beam.
Compositional information from x-ray
analysis
Energy-dispersive x-ray analysis (EDX) is the
most common method used, although modern
detectors require the detector to be immersed
in liquid nitrogen. The process is fully
automated with the emitted x-rays being collected
simultaneously as a series of pulses. The pulses
are amplified and sent to a multichannel analyser
(MCA). This allocates each pulse to one of about
1000 channels, each representing a particular x-ray
energy. In this way the MCA creates a histogram
of all the different energies of the x-rays detected.
The histogram is displayed on a computer screen
with each peak representing a different energy
(figure 5). The peak height indicates the number of
pulses (intensity) of that particular energy. Each
element produces a series of peaks in a unique
pattern and the analyst then decides which peak
of the series is going to be measured to quantify
the amount of that element present. The most
commonly used EDX detectors cannot measure
elements lighter than sodium, but newer types can
now detect elements down to oxygen.
It is possible to measure the emitted x-
rays from a small area of an object and to
carry out microanalysis. This technique gives
compositional information on different areas of
the same image and is very useful in the study
of archaeological material.
Burial in the ground usually results in the
corrosion of the surface layers of inorganic objects,
which can often penetrate the whole object. With
metal objects, the degree of corrosion is partly a
function of the chemical reactivity of the metals
from which the object was made. An iron object
will tend to corrode faster than a copper or bronze
object, and a silver object will corrode more slowly
than either. In the case of glass objects, the alkali
March 2004
The scanning electron microscope and the archaeologist
Figure 6. BSE image of a section cut through a bronze
sheet showing the characteristic angular cracks caused
by corrosion as it penetrates the metal structure. The
surface of the sheet is at the far right-hand side. See
text for details.
components of the glass will be leached out. Thus
the composition at the surface of an archaeological
object is unlikely to be representative of its original
composition. With the SEM, it is possible to
visually identify the areas that have been affected
by burial and select an area for chemical analysis
that is as representative of the original composition
as possible.
Sometimes it is necessary to take a sample
from an object in order to obtain a section but it
may be possible to just grind and polish the edge of
an object to see beneath the corrosion layers. An
example of this is the analysis of ancient copper-
alloy objects. Figure 6 shows a section cut through
a bronze sheet. The surface areas of the sheet
(right-hand third) are characterized by angular
cracks that penetrate inwards from the surface (far
right-hand side). This is where corrosion has crept
along the boundaries between the grains of metal,
and the more easily corroded metal in the alloy (the
copper) has been leached out. An analysis of this
area reveals an alloy with 20% tin, whereas the
correct analysis of the uncorroded interior metal
(to the left) has a tin content of only 10%.
However, the enrichment of the less reactive
component of an alloy is not always solely the
result of natural corrosion processes. In silver-
alloy coins, for example, the more reactive copper
component of the alloy was often leached out at
the surface of the coin in order to give it a more
silvery appearance. Figure 7 shows a section cut
through a Roman silver coin (denarius); the BSE
PHYSICS EDUCATION 169
 M Ponting
Figure 7. BSE of part of a section cut through a
Roman coin. The differences in the observed structure
correspond to differences in the chemical composition
that can be measured by EDS. The surface of the coin
is at the bottom of the picture. The original alloy in the
middle of the coin has a silver content of 48%. Where
some of the copper has been chemically leached out or
mineralized the silver content rises to around 63%, but
where this has been consolidated by striking the coin,
the surface has a silver content of over 95%.
image clearly shows a well segregated two-phase
structure, showing that this is an alloy of silver and
something else. The microanalysis capabilities of
the SEM mean that it is possible to analyse the
two different phases and confirm that the lighter-
coloured phase—the one with the higher atomic
number—is almost pure silver, and the other is
almost pure copper. Towards the surface of the
coin (the lower part of the image) there are some
structural changes showing that the copper has
been leached out of the surface layers. Analysis of
a small but representative area of the interior metal
shows that the alloy is a mixture of approximately
half silver and half copper, but analysis of the
surface layers shows that the leaching out of the
copper has resulted in a surface with a silver
content of over 90%!
Another valuable use of SEM microanalysis
is for the identification of coatings. Figure 8 shows
an SEI of a section of an Anglo-Saxon brooch
that has revealed a thin metal coating preserved
within the layers of corrosion products which,
when subjected to analysis, was shown to be gold.
170 PHYSICS EDUCATION
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Figure 8. SEI of a section through an Anglo-Saxon
brooch showing a layer of gilding on the original
surface within layers of corrosion.
A small trace of mercury in the gold indicates
that the coating was initially applied as a paste
of mercury and gold. This paste would have been
rubbed onto the copper-alloy brooch, which was
then heated to drive off the mercury as a vapour,
leaving the coating of gold behind. This type
of gilding is often called ‘fire gilding’ and was
common before electroplating was invented.
Conclusions
The scanning electron microscope is a very
versatile analytical tool that uses electrons and
their interactions with a sample to provide a
great deal of information about the sample.
Its application in archaeology provides many
different types of information, from the purely
structural to the purely chemical.
Most of the images shown here can be found along
with others on the English Heritage website at:
www.english-heritage.org.uk/default.asp?wci=
mainframe&URL1=default.asp%3FWCI%3D
Node%26W
Received 14 October 2003, in final form 3 December 2003
PII: S0031-9120(04)70291-9
DOI: 10.1088/0031-9120/39/2/004
March 2004