Materials Chemistry and Physics 129 (2011) 433–438
Contents lists available at ScienceDirect
Materials Chemistry and Physics
j ourna l ho me pag e: www.elsevier.com/locate/matchemphys
Studies on crystal growth and physical properties of 2-amino-5-chloropyridine
single crystal
T. Suthan
a
, N.P. Rajesh
a,∗
, C.K. Mahadevan
b
, G. Bhagavannarayana
c
a
Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110, India
b
Physics Research Centre, S.T. Hindu College, Nagercoil 629 002, India
c
C.G.C. Section, National Physical Laboratory, New Delhi 110 012, India
a r t i c l e i n f o
Article history:
Received 10 June 2010
Received in revised form 8 April 2011
Accepted 11 April 2011
PACS:
61.66.Hq
81.10.
74.25.Gz
81.70.Pg
77.22.Gm
Keywords:
A. Organic compounds
B. Crystal growth
C. Differential thermal analysis (DTA)
D. Dielectric properties
a b s t r a c t
Organic 2-amino-5-chloropyridine single crystals have been grown by slow evaporation technique suc-
cessfully. The grown crystal was confirmed by single and powder X-ray diffraction studies. The presence
of functional groups was identified by Fourier transform infrared (FTIR) study. High resolution X-ray
diffraction (HRXRD) analysis indicates the crystalline perfection of the grown crystal. UV–Vis–NIR anal-
ysis was performed to examine the optical property of the grown crystal. The thermal property of the
grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA).
The dielectric measurements were carried out and the results indicate an increase in dielectric and con-
ductivity parameters with the increase of temperature at all frequencies. The Vicker’s hardness study
reveals that the grown crystal is in soft nature.
© 2011 Elsevier B.V. All rights reserved.
1. Introduction
Researchers are giving an appreciable attention to grow organic
single crystals for technological applications. Microelectronics
industry needs replacement of dielectric materials in multilevel
interconnect structures with new low dielectric constant (ε
r
) mate-
rials, as an interlayer dielectric (ILD) which surrounds and insulates
interconnect wiring. Lowering the ε
r
values of the ILD decreases
the RC delay, lowers power consumption and reduces ‘crosstalk’
between nearby interconnects [1]. Silica has the ε
r
value ≈ 4.0, in
part as a result of Si–O bonds. Although several innovative devel-
opments have been made for the development of new low ε
r
value
materials to replace silica, there is still a need for new ε
r
value
dielectric materials. Porosity is an unwanted problem encountered
with the polycrystalline and thin film materials [1]. In this context,
materials in the single crystal form would be very much interesting.
The 2-hydroxy-4-methoxybenzophenone [2], KDP added with urea
[3] and l-arginine [4], l-arginine acetate [5] and l-arginine oxalate
[5] are the reported low dielectric constant materials. In this series,
∗
Corresponding author. Tel.: +91 044 27474844; fax: +91 044 27474844.
E-mail addresses: rajeshnp@hotmail.com, rajeshnp@ssn.edu.in (N.P. Rajesh).
the 2-amino-5-chloropyridine crystal is expected to be a candidate
for the low dielectric constant material. There are several meth-
ods for crystal growth. Solution methods, namely slow cooling or
slow evaporation of solutions, are commonly used for the growth of
organic molecular crystals. The 2-amino-5-chloropyridine is a non-
hygroscopic simple organic material and its molecular formula is
C
5
H
5
ClN
2
. Single crystal of this material cannot be grown using
the Bridgman technique because weight loss occurs before melting
point. In this reason, slow evaporation method is adopted to grow
this crystal. In this present study 2-amino-5-chloropyridine single
crystal was successfully grown by the slow evaporation method and
the grown crystal was analyzed by single crystal X-ray diffraction
study, powder XRD, FTIR, HRXRD, UV–Vis–NIR, TG/DTA, dielectric
and microhardness measurements.
2. Experimental
The 2-amino-5-chloropyridine was commercially purchased from sigma Aldrich
with 98% purity; it has a molecular weight of 128.56. The solubility study reveals
that 2-amino-5-chloropyridne was not soluble in water and dissolved in organic
solvent. In this study so we chose acetone as the solvent. The solubility curve of
2-amino-5-chloropyridine obtained by the gravimetric method is shown in Fig. 1
and it shows that solubility increases with temperature. The purity of the mate-
rial was further improved by successive recrystallization process. The recrystallized
salt was used for the preparation of saturated solution at room temperature.
0254-0584/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.matchemphys.2011.04.038