Instrumentation of the Mossbauer

Spectrometer

Components of spectrometer
A transmission Mossbauer spectrometer consists of the following four basic parts:
source, Mossbauer drive, collimator and detector, as schematically shown in fig.1
Mossbauer spectrometers are extremely sensitive to vibrations from external sources
and therefore all basic components should be rigidly fixed to a heavy base. Due to
the ionizing nature of γ-rays, an additional part, i.e. a safety shutter based on a servo
mechanism that can be controlled externally to avoid radiation exposure during
sample changing, becomes an integrated part of the spectrometer.

Fig,1: Schematic of a transmission Mossbauer spectrometer.

Sources
The source was 57Co incorporated into a ∼7 µm metal rhodium foil with an initial
activity of 56.5 mCi. Other relevant properties are given in table 1. The source,

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whose surface is sealed/covered with a 40 µm aluminium foil, was purchased from
Cyclotron Co., Ltd., Russia. Aluminium foils are important for two reasons, 1. to
act as a filter to attenuate the 6.4 keV X-rays, which are more intense than 14.4 ke
Mossbauer transition, thereby increasing the efficiency of the detector, and 2. to
avoid the of radiation exposure.

Mossbauer drive
The radioactive source emits the 14.4 KeV γ-rays as shown in fig. 1 The Mossbauer
transition is monochromatic (energy is fixed) and in order to cover all the resonance
lines that lie around 14.4 KeV, the energy has to be tuned. Typically for iron
compounds the resonance line(s) can be somewhere ±500 neV around the 14.4 KeV
transition. The modulation of the γ-rays can be achieved by fixing the source to a
Mossbauer drive, which moves the source back and forth with respect to the sample,
i.e. making use of the Doppler effect. The velocity of the Mossbauer drive is scanned
from −v to +v and then goes back to −v, completing a backward scan, hence, in
one scan period, a computer will record two spectra, which are mirror images of each
other (+ means the source moving towards the sample). Therefore these two spectra
should be added (before adding one of them is inverted in the channel scale) and
the folding point, i.e. the point that separates the two spectra is determined by the
least-squares method such that the relative shift between the spectra is minimum.
The Mossbauer drive is an electromechanical device similar to a loudspeaker
system. It consists of rigidly connected driving and pickup coils moving in a
homogeneous magnetic field. These two coils are connected in series with the
reference signal. The current passing through the driving coil in a permanent magnet,
which is attached to the Mossbauer drive, forms the driving force. A drive unit with
an electronically controlled voltage (reference signal) is fed to the driving coil.

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Collimator
Another important part is the collimator, which should be designed carefully to avoid
cosine smearing, which causes line shifting and line broadening. Cosine smearing is
due to the solid angle between source and detector. The recorded γ-rays may be
emitted from the source under a finite angle relative to the direction of source
velocity. This may also give rise to a nonsymmetrical line shape if the resonance is
markedly shifted from zero velocity. To avoid all these problems, a lead circular
block was used as a collimator. The Mossbauer drive is not screwed rigidly
to the base so that the handling and transportation of the source is easier. But this
will cause serious line broadening problems and in order to circumvent this issue a
heavy collimator (lead block) of ∼6.5 kg is used. The collimator was made by a
casting process, i.e. melting lead in an electric oven and pouring it into a mould. For
improving the strength and hardness, ∼4% by weight of antimony powder was added
during the melting. Finally, the surface is cleaned by machining and a hole of
diameter 5 mm for the γ-ray passage was drilled. The collimator reduces the line
broadening by 44% on comparing the outer line widths of the spectrum obtained
from an α-Fe foil (with 0.1 kg collimator: 0.36 mm s−1, with 6.5 kg collimator: 0.25
mm s−1).

Counting system and count rate

The gamma counting system consists of a gas proportional counter (filled with
Xe-CO2, maximum voltage: 3 kV), preamplifier, single channel analyzer (SCA),

amplifier, discriminator and multichannel analyzer (MCA). All these components

are commercially available. For the spectrometer built in the frame of this thesis,

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a special data acquisition module was used—CMCA-550, manufactured from
Wessel GmbH, Germany.

Fig. 2. PHS of 57Co source and the experimental count rate for the 14.4 KeV
peak is 2502 counts s−1 (=area/time). The peak’s lower and upper limit
which is indicated as vertical bars corresponds to 125–220 mV.

Safety aspects
The source with Mossbauer drive is completely shielded with several lead sheets
each 3 mm thick to avoid radiation leakage to the outside. For a typical Mossbauer

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source some millimeters of lead are sufficient to decrease the radiation exposure by
a factor of about 100.

Application of Mossbauer spectrometer

 Corrosion of studies
 Magnetic Tape
 Glass manufacturing
 Nitrification of steel
 Martensitic phase transformation in gold alloys
 Mossbauer spectroscopy has been applied to analyse the iron compounds
present in car exhausts
 Mossbauer spectroscopy is used to characterize phase transformations in
iron catalysts, e.g., those used for Fischer–Tropsch synthesis.
 Mossbauer spectroscopy has been widely applied to bioinorganic chemistry,
especially for the study of iron-containing proteins and enzymes.
 Mossbauer spectroscopy has also been used to determine the relative
concentration change in the oxidation state of antimony (Sb) during the
selective oxidation of olefins.

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