Journal of Electrostatics, 21 (1988) 145-149 145
Elsevier Science Publishers B.V., Amsterdam -- Printed in The Netherlands
A NOVEL SAMPLE-PREPARATION TECHNIQUE FOR
INFRARED AND FAR-INFRARED SPECTROSCOPY
F. KREMER
Max-Planck-Institut fgtr Polymerforschung, Postfach 3148, 6500 Mainz (F.R.G.)
A. MASON
University of Bath, School of Physics, Bath BAZ 7A9 (Great Britain)
and D. B(~HME
Max-Planck-Institut fiir Festk6rperforschung, Heisenbergstrasse 1, 7000 Stuttgart 80 (F.R.G.)
(Received January 18, 1988; accepted April 14, 1988)
Summary
A novel technique of preparing thin ( < 10 #m) homogeneous samples for infrared (IR) and far-
infrared (FIR) spectroscopic studies is presented. In contrast to conventional methods (e.g. cast-
ing a film from solution, pressing a pellet of a mixture of KBr with the sample), the material to
be studied is dissolved in a suitable solvent and made into an aerosol by use of an ultrasonic
vaporizer. The sample material is then freeze dried on a substrate mounted on a temperature-
controlled (100 K to 300 K) cold finger of a cryostat placed in a glass chamber. By this method,
especially highly crystalline materials obtained in powder form can easily be prepared as thin solid
films with a diameter of about 20 mm.
Introduction
Infrared (IR) but especially far-infrared (FIR) spectroscopy requires sam-
ples that are homogeneous in thickness over a diameter of about 20 mm be-
cause otherwise scattering may spoil the measurements. This causes serious
problems for crystalline materials which are often obtained in a powder form
(e.g. biological samples like lysozyme, alcohol dehydrogenase (ADH), sugars ).
For these materials [1,2] the usual preparation method of casting a film from
solution on a suitable window-substrate is hardly applicable because crystal-
lization results in the formation of small crystals of a few millimeters in di-
ameter. An alternative approach would be to prepare a mixture of the material
under study with an inert matrix such as KBr. By pressing a pellet from this
mixture a disc-shaped sample is obtained. The major disadvantage with this
method is that the influence of matrix material on vibrational modes of the
sample molecules cannot easily be calculated, especially at FIR-frequencies. It
0304-3886/88/$03.50 © 1988 Elsevier Science Publishers B.V.