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TSD Current Spectroscopy of NCO Terminated Liquid

Crystalline Polyurethane

J.K. Quamara, Sohan Lal, S.K. Mahana and Pushkar Raj*

Department of physics
National institute of Technology, Kurukshetra-136119
*DRDO,Delhi
Email: jkquamara@yahoo.com

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INTRODUCTION was added followed by another stirring for 5 minutes.


In this solution small quantity of Di-Butyl Tin
The unique properties of liquid crystal polymers DiLaurate (DBTDL C32H6404Sn) was added as
i.e. pol ym ers exhi bi t i ng li qui d crys t al l i ne catalyst. This solution was stirred continuously for
s t at e have led to the increasing interest of two hours at room temperature in nitrogen
researchers. Though these polymers are still in the atmosphere then the temperature was raised to 50
research stage but some of them have found degree Celsius and again stirring was continued for
significant applications in science as well as in two hours, the viscous fluid so obtained was poured
technology. Thermotropic liquid crystalline on a Teflon mould to obtained the film once the
polyurethanes are an important class of polymers solvent got evaporated. The film so obtained was
owing to their widespread commercial applications in kept in desicator for a day to remove traces of
high-strength fibers, thermoplastics displays and solvent.
optical storage devices. In the present paper we are EXPERIMENTAL
reporting on the multiple dielectric relaxation
processes in side chain liquid crystalline The experimental arrangement for TSDC
polyurethane (LCPU) based on NCO- terminated measurements was the conventional one as described
polybutadiene and Bi-Phenol using thermally by the authors elsewhere. The samples were
stimulated depolarization current (TSDC) technique. polarized by subjecting them to the desired dc field
(Ep) at a constant temperature (Tp) for 1h. The
samples were then cooled to the room temperature
SYNTHESIS OF LIQUID within fixed time (1/2h) in the presence of Ep. The
depolarization currents were measured with the help
CRYSTALLINE of Keithley electrometer (610C) at a linear heating
POLYURETHANE 0
rate of 2 C/minute. Activation energies were
In order to synthesize liquid crystal calculated using Bucci- Plot method.
polyurethane 5 grams of NCO terminated
Polybutadine was taken in a 100 ml conical flask, to RESULTS AND DISCUSSION
this 25ml of tetrahydofuron (THF) was added, in The TSD current spectra of pristine LCPU
order to dissolve the NCO terminated Polybutadine in samples in the temperature range 300 to 2500C for
THF the solution was stirred continuously for 5
minutes. In the solution so obtained, 4-4 Bi-Phenol
various polarization conditions have been illustrated does not appreciably differ from the theoretical
in Figures 1 and 2 respectively. predicted value (~0.24eV) assigned to the dipolar
polarization. Emergence of this peak is also
Polarizing Field (Ep) Effect consistent with the glass transition temperature of this
The TSDC characteristics for LCPU samples PLC which is around 700C. The broad nature of this
polarized at different polarizing fields (Ep) ranging peak shows a distributed dipolar polarization
from 27.0 to 82.0 kV/cm for T p: 800C are shown in associated with β - relaxation owing to unidentical
Fig.1. These TSD spectra consist of a well defined environment around the different >C=O groups. The
peak around 800C denoted as β - peak. The peak LCPU has rigid liquid crystal (LC) groups (biphenyl
magnitude increases with Ep. In high temperature groups) connected together by either rigid or flexible
region we observe abnormal TSDC (i.e. same current non - LC spacers. The type and length of the spacers
direction as that of charging current). The can determine whether a nematic, cholesteric or
temperature at which the current reversal takes place smectic phase is formed. For these longitudinal
increases with increasing Ep. polymers the viscosity in the isotropic phase is higher
than in the nematic phase. At elevated temperature
and under the influence of field, reduction in the
length of the spacer results in the increase of rigidity
of molecules, thereby shifting Tg to higher
temperature, which explains the occurrence of β -
peak at higher temperature than the reported Tg value.
The peak (α - peak) appearing around 1600C
(Fig.2) has been associated to the space charge
trapping mechanism. In LCPU the charge trapping is
possible due to various mechanisms The flexible
segment but-2-ene in LCPU and the unsaturated
carbonyl groups may act to a significant extent as
traps for charge carriers contributing to their transport
and trapping. If the charges are in the form of ions,
their transport in the polymer takes place trough
FIGURE 1. The TSDC spectrum of pristine LCPU sample
hopping from one trap site to another while the
polarized at different field: ■50kV/cm, ▲60kV/cm and
electrons or holes remain immobile in the local traps.
× 75kV/cm.
Further the cold crystallization of biphenyl phase
may also be held responsible for α - relaxation.
Polarization Temperature
(Tp) Effect
The effect of polarizing temperature (Tp) on the
TSDC spectrum of LCPU samples polarized at Ep:
55.0 kV/cm has been shown in Fig.2. The β - peak is
very broad at low Tp and becomes sharp at high Tp. A
significant enhancement in peak magnitude occurs
with a shift towards higher temperature with
increasing Tp. The abnormal TSDC is also observed
in low Tp samples. Tp.
The dielectric relaxation processes in liquid
crystalline polymers are quite complex and results
from several different competitive mechanisms
involving various physical states associated with
crystalline and amorphous phase. The liquid
crystalline polyurethane structure contains large FIGURE 2. The TSDC spectrum of pristine LCPU sample
number of carbonyl [>C=O] groups, which provide polarized at different temperature: ▲800C, × 1500C,
polar nature to this polymer. The TSDC current peak ♦1800C
(β - peak) appearing around 800C has been assigned
to dipole orientation polarization. This observation is
confirmed by the fact that the average activation
energy (~0.31eV) corresponding to this relaxation
Acknowledgments References
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