Optik 124 (2013) 4614–4617
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Optik
j o ur nal hom epage: www.elsevier.de/ijleo
Investigation on sodium potassium bitartrate crystals grown in silica gel and its
characterization
V. Mathivanan
a,b
, M. Haris
a,∗
a
Department of Physics, Karunya University, Karunya Nagar, Coimbatore 641 114, Tamil Nadu, India
b
Department of Physics, United Institute of Technology, Coimbatore 641 020, India
a r t i c l e i n f o
Article history:
Received 11 September 2012
Accepted 20 January 2013
Keywords:
Gel technique
Sodium potassium bitartrate
FTIR
Powder XRD
Magnetic moment and thermal properties
a b s t r a c t
The single-crystal growth of sodium potassium bitartrate by controlled diffusion in silica gel is reported.
The influence of growth parameters, e.g. reactant concentrations, gel pH, gel aging on the size and nuclea-
tion density of crystals has been studied. Operative mechanisms of crystallization, results of growth
kinetics and morphology of crystals are discussed. The energy dispersive X-ray analysis (EDAX), Fourier
transform infra red (FTIR) spectroscopy, powder X-ray diffraction (XRD), magnetic properties and Ther-
mal analysis (TGA/DTA) have been made to find the stoichiometric composition of the crystals and its
structure.
© 2013 Elsevier GmbH. All rights reserved.
1. Introduction
Crystal growth in gels has made remarkable progress in the
recent years. With the advent of extensive work by Henisch and
co-workers [1,2], gel growth research has made rapid strides in the
field of crystal growth in general, and the growth of materials in
gel in particular. The importance of gel growth can be visualized by
the fact that a number of researchers have started to develop crys-
tals of technological potential by this method [3–8]. Another factor
arousing interest in this type of growth is that crystals of various
sorts of ionic, organic and even metallic can be grown at ambient
temperatures. Growth kinetics which is so vital in understanding
the growth mechanisms in this type of growth has also been dealt
with extensively [1,9–16].
It is pertinent to point out here essentially no work has been
reported so far on the gel growth of sodium potassium bitartrate
crystals. We report here the growth of sodium potassium bitartrate
in gel medium. The growth mechanism and characterization of the
grown crystals are described and discussed.
2. Experimental procedures
The crystallization apparatus for the growth of sodium potas-
sium bitartrate consist of glass tube of length 20 cm and diameter
2.5 cm placed vertically on plastic stand. Silica gel was prepared by
∗
Corresponding author. Tel.: +91 9841848926; fax: +91 422 24615615.
E-mail address: harismuthiah@karunya.edu (M. Haris).
acidifying pure sodium meta silicate (Na
2
SiO
3
) of specific gravity
1.05 g/cm
3
, with tartaric acid of a concentration in accordance with
the requirements of a particular pH value. The tartaric acid solution
was added slowly to sodium metasilicate solution with continuous
stirring to avoid any local ion concentration which would otherwise
cause premature local gelling and make the final solution inho-
mogeneous. Here, tartaric acid acted as a lower reactant. A fixed
amount of gel solution with the desired value of pH was then trans-
ferred to several test tubes. The test tubes were sealed with cotton
to prevent fast evaporation and contamination of the exposed sur-
face of the gel. The gel solution was allowed to set. The setting of gel
is strongly dependent on pH. High pH value gel takes lower time to
set than the low pH value. After confirming the gel setting, an aque-
ous solution of NaCl and KCl of required concentration was poured
slowly along the sides of the test tube, to prevent the breaking up of
gel surface. Slow diffusion of the upper reactants ions through the
narrow pores of the silica gel leads to the reaction between these
ions and the ions present in the gel as lower reactant. The following
reaction was expected inside the gel
xNaCl + (1 - x)KCl + C
4
H
6
O
6
→ Na
x
K
(1-x)
HC
4
H
4
O
6
+ HCl (x = 0.7, 0.6, 0.5, 0.4, 0.3)
The grown crystals of sodium potassium bitartrate are shown in
Fig. 1. The details of experiments for the growth of sodium potas-
sium bitartrate are shown in Table 1.
With appropriate boundary conditions Fick’s law, in the case of
one-dimensional diffusion, gives the rate of growth of the crystal in
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http://dx.doi.org/10.1016/j.ijleo.2013.01.101