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L. K. Matkovska et al.
11.2 Experimental
Materials and Synthesis The epoxy oligomer (diglycide aliphatic ester of polyethylene glycol, DEG-1), Macromer, Vladimir, Russia, and salt of lithium perchlorate
(LiClO 4 , Sigma-Aldrich, USA) were used for synthesis of ion-conductive epoxy
polymer composites. These components were previously pre-dried in vacuum at
80 ◦ C during 24 hours. After drying, the salt was dissolved in the DEG-1 oligomer.
Solutions of DEG-1-LiClO 4 were prepared with LiClO 4 content from 0 to 50
phr (parts per hundred) on 100% of polymer matrix. Ten percent of polyethylene
polyamine hardener (PEPA, Chimia, Kharkov, Ukraine) was used as a curing agent
for synthesis of the composites.
Methods The thermal characteristics were studied by differential scanning
calorimetry (DSC) using TA Instruments DSC Q2000 (TA Instruments, New Castle,
DE, USA) in the temperature range from −70 ◦ C to +150 ◦ C with the heating rate
of 10 ◦ C/min. Glass transition temperature (T g ) was determined from the DSC
curves at the second heating. The experimental error of determination of the glass
transition temperatures was ±1 ◦ C.
The electrical and dielectric characteristics of the synthesized composites were
investigated by broadband dielectric analyzer Novocontrol Alpha coupled with
Novocontrol Quatro Cryosystem (Novocontrol Technologies, Montabaur, Germany)
that was equipped with a two-electrode circuit, in the frequency range 10 −1 to
10 7 Hz and the temperature range from −60 ◦ C to +200 ◦ C. The voltage applied
to a sample was equal to 0.5 V. The test samples had diameter of 20 mm and a
thickness of 0.5 mm and were previously coated by aluminum under vacuum. The
obtained data was analyzed using Novocontrol WinDeta 3.8 software.
Structural organization and features of macromolecular ordering of the synthesized polymer systems were investigated by wide-angle X-ray spectra (WAXS)
using X-ray diffractometer DRON-4.07 (Burevestnik, Saint Petersburg, Russia).
X-ray optical scheme was performed by Debye-Scherrer method on passing the
primary beam through the polymer sample using Cu K α emission (λ = 1.54 Å) that
was made monochromatic using Ni filter. The X-ray tube BSV27Cu (U = 30 kV,
I = 30 mA) was used as a source of characteristic X-ray irradiation. The investigations were carried out by automatic step scanning in the range of scattering angles
(2θ ) from 2.6 ◦ to 40 ◦ ; the exposure time was 5 s.
Infrared (IR) spectroscopic studies have been performed using spectrometer
with Fourier transformation “Tensor 37” from Bruker Corp. in the range of wave
numbers (600–3800) ◦ cm −1 . According to the passport of the device, the relative
measurement error is <2%.
Morphological features of the synthesized composites were studied using transmission optical microscopy (TOM) with the microscope Carl Zeiss Primo Star
and reflective optical microscopy (ROM) with Unicorn NJF 120A polarization
microscope at polarization angles 0–90 ◦ . Microphotographs analysis was performed
using Carl Zeiss Imaging Solutions AxioVision V4.7.1 software.
L. K. Matkovska et al.
11.2 Experimental
Materials and Synthesis The epoxy oligomer (diglycide aliphatic ester of polyethylene glycol, DEG-1), Macromer, Vladimir, Russia, and salt of lithium perchlorate
(LiClO 4 , Sigma-Aldrich, USA) were used for synthesis of ion-conductive epoxy
polymer composites. These components were previously pre-dried in vacuum at
80 ◦ C during 24 hours. After drying, the salt was dissolved in the DEG-1 oligomer.
Solutions of DEG-1-LiClO 4 were prepared with LiClO 4 content from 0 to 50
phr (parts per hundred) on 100% of polymer matrix. Ten percent of polyethylene
polyamine hardener (PEPA, Chimia, Kharkov, Ukraine) was used as a curing agent
for synthesis of the composites.
Methods The thermal characteristics were studied by differential scanning
calorimetry (DSC) using TA Instruments DSC Q2000 (TA Instruments, New Castle,
DE, USA) in the temperature range from −70 ◦ C to +150 ◦ C with the heating rate
of 10 ◦ C/min. Glass transition temperature (T g ) was determined from the DSC
curves at the second heating. The experimental error of determination of the glass
transition temperatures was ±1 ◦ C.
The electrical and dielectric characteristics of the synthesized composites were
investigated by broadband dielectric analyzer Novocontrol Alpha coupled with
Novocontrol Quatro Cryosystem (Novocontrol Technologies, Montabaur, Germany)
that was equipped with a two-electrode circuit, in the frequency range 10 −1 to
10 7 Hz and the temperature range from −60 ◦ C to +200 ◦ C. The voltage applied
to a sample was equal to 0.5 V. The test samples had diameter of 20 mm and a
thickness of 0.5 mm and were previously coated by aluminum under vacuum. The
obtained data was analyzed using Novocontrol WinDeta 3.8 software.
Structural organization and features of macromolecular ordering of the synthesized polymer systems were investigated by wide-angle X-ray spectra (WAXS)
using X-ray diffractometer DRON-4.07 (Burevestnik, Saint Petersburg, Russia).
X-ray optical scheme was performed by Debye-Scherrer method on passing the
primary beam through the polymer sample using Cu K α emission (λ = 1.54 Å) that
was made monochromatic using Ni filter. The X-ray tube BSV27Cu (U = 30 kV,
I = 30 mA) was used as a source of characteristic X-ray irradiation. The investigations were carried out by automatic step scanning in the range of scattering angles
(2θ ) from 2.6 ◦ to 40 ◦ ; the exposure time was 5 s.
Infrared (IR) spectroscopic studies have been performed using spectrometer
with Fourier transformation “Tensor 37” from Bruker Corp. in the range of wave
numbers (600–3800) ◦ cm −1 . According to the passport of the device, the relative
measurement error is <2%.
Morphological features of the synthesized composites were studied using transmission optical microscopy (TOM) with the microscope Carl Zeiss Primo Star
and reflective optical microscopy (ROM) with Unicorn NJF 120A polarization
microscope at polarization angles 0–90 ◦ . Microphotographs analysis was performed
using Carl Zeiss Imaging Solutions AxioVision V4.7.1 software.