510
O. Aksimentyeva et al.
known compounds for the purpose of phase identification, refinement of the parameters of elementary cells was performed using a software package STOE WinXPOW
3.03 [27] ta PowderCell 2.4 [28]. The calculation of the microstructural parameters
was carried out in an isotropic approximation by the methods of the integral width of
the diffraction peaks using a software package WinPLOTR [29] according to [30].
Structural studies of the morphology and content of the synthesized composites were performed by scanning electron microscopy (SEM) and energy-dispersive
spectroscopy (EDAX) on a microscope microanalyzer, PMMA-102-02. Samples
for study were prepared by applying polyaniline or a composite from solution of
N-methylpyrrolidone on a polished platinum plate. The distance from the electron
source to the sample surface was 300 mm. The electron energy was scanned in the
range of 0–10 kV. Statistical processing of the results was performed by software
MAGELLAN v1.2.
For investigation by atomic force microscopy, atom-force microscope Nanoscope
IIIa Dimension 3000TM Digital instruments were used. Polymer–metal composite
was dissolved in N-methylpyrrolidone and sonicated for 15 min. Then a drop of
the solution was taken with a micro-syringe and deposited on a silvered glass, after
which the solvent was dried in vacuum.
Molecular spectra of PAn and its composites were obtained by FT-IR spectroscopy
on an IFS 66 spectrometer. For this, the sample PAn or composite was triturated in an
agate mortar with pre-dried and crushed KBr and formed into a tablet under pressure.
The electrical conductivity of the samples was measured by the van der Pauw
method [30]. Samples were formed in tablets with a diameter of 2×10
−2 m using
a mold, acting at a constant pressure of 100 kg/cm
2 for 5 min. They were placed
between four paired silver contacts. To measure the temperature dependence of the
resistivity, the sample was placed in a special quartz cell between the nickel flat
contacts and the soldered thermocouple. The change in temperature at a constant
speed in the range 273–333 K was controlled and kept of 5 K/min. During measurements, constant load of 10 N/cm
2 acted at the sample. The resistance of the tablet
was recorded with a digital ohmmeter W-306-1. The specific volumetric resistance
was calculated according to the formula:
R =
ρ · l
S
,
where S—cross-sectional area of cylindrical sample (m), l—height (m), R—
measured resistance value (Ohms). The relative error of determination for the parallel
measurement series did not exceed 5%.
3 Results and Discussion
The use of precious metals as components to create polymer–metal composites is due
to their high performance, the relative stability of their nanoparticles compared to
O. Aksimentyeva et al.
known compounds for the purpose of phase identification, refinement of the parameters of elementary cells was performed using a software package STOE WinXPOW
3.03 [27] ta PowderCell 2.4 [28]. The calculation of the microstructural parameters
was carried out in an isotropic approximation by the methods of the integral width of
the diffraction peaks using a software package WinPLOTR [29] according to [30].
Structural studies of the morphology and content of the synthesized composites were performed by scanning electron microscopy (SEM) and energy-dispersive
spectroscopy (EDAX) on a microscope microanalyzer, PMMA-102-02. Samples
for study were prepared by applying polyaniline or a composite from solution of
N-methylpyrrolidone on a polished platinum plate. The distance from the electron
source to the sample surface was 300 mm. The electron energy was scanned in the
range of 0–10 kV. Statistical processing of the results was performed by software
MAGELLAN v1.2.
For investigation by atomic force microscopy, atom-force microscope Nanoscope
IIIa Dimension 3000TM Digital instruments were used. Polymer–metal composite
was dissolved in N-methylpyrrolidone and sonicated for 15 min. Then a drop of
the solution was taken with a micro-syringe and deposited on a silvered glass, after
which the solvent was dried in vacuum.
Molecular spectra of PAn and its composites were obtained by FT-IR spectroscopy
on an IFS 66 spectrometer. For this, the sample PAn or composite was triturated in an
agate mortar with pre-dried and crushed KBr and formed into a tablet under pressure.
The electrical conductivity of the samples was measured by the van der Pauw
method [30]. Samples were formed in tablets with a diameter of 2×10
−2 m using
a mold, acting at a constant pressure of 100 kg/cm
2 for 5 min. They were placed
between four paired silver contacts. To measure the temperature dependence of the
resistivity, the sample was placed in a special quartz cell between the nickel flat
contacts and the soldered thermocouple. The change in temperature at a constant
speed in the range 273–333 K was controlled and kept of 5 K/min. During measurements, constant load of 10 N/cm
2 acted at the sample. The resistance of the tablet
was recorded with a digital ohmmeter W-306-1. The specific volumetric resistance
was calculated according to the formula:
R =
ρ · l
S
,
where S—cross-sectional area of cylindrical sample (m), l—height (m), R—
measured resistance value (Ohms). The relative error of determination for the parallel
measurement series did not exceed 5%.
3 Results and Discussion
The use of precious metals as components to create polymer–metal composites is due
to their high performance, the relative stability of their nanoparticles compared to