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Current Nanoscience, 2014, 10, 869-876 869
Correlation Between Size of CoFe
2
O
4
Nanoparticles Determined from
Experimental and Calculated Data by Different Mathematical Models
Danut Gabriel Cozma
a
, Daniel Gherca
a
, Ionut Mihalcea
b,c
, Constantin Virlan
a
, Nicoleta Cornei
a
and
Aurel Pui*
a
a
Faculty of Chemistry, “Alexandru Ioan Cuza” from Iasi, University, Carol I Bvd. No. 11, Iasi 700506, Romania;
b
Unité de Catalyse et Chimie du Solide (UCCS) – UMR CNRS 8181, Université de Lille Nord de France, USTL-ENSCL,
Bat C7, BP 90108, 59652 Villeneuve d’Ascq, France;
c
Institut für Nanotechnologie, Karlsruhe Institute of Technology,
Postfach 3840, D-76021 Karlsruhe, Germany
Abstract: This study reports the synthesis of CoFe
2
O
4
nanoparticles by coprecipitation method in the presence of Linseed
Oil as surfactant. The capping agent was used to stabilize the particles and prevent their agglomeration. The characteriza-
tion studies were conducted by in situ X-ray diffraction, transmission electron microscopy, thermal analysis (TG-DTA)
and FTIR spectroscopy. The average particle sizes obtained by XRD data were used to obtain a correlation with size of
CoFe
2
O
4
nanoparticles determined, using mathematical equations based on different models. The statistical studies show
that the cubic model gives a good correlation within the whole temperature range (100 – 850 °C). The result of these in-
vestigations was very useful for establishing the optimal calcination temperature. FT-IR spectroscopy and thermogra-
vimetric analysis (TG) showed that the core-shell structure type of CoFe
2
O
4
nanoparticles is stable below this annealing
temperature. TEM analysis indicates that the CoFe
2
O
4
samples during the calcinations treatment were spherical in shape
and uniform in morphology and particles size.
Keywords: Infrared spectroscopy, mathematical models, nanoparticles size, powder X-ray diffraction patterns.
INTRODUCTION
Cobalt ferrite, with a well-known cubic spinel ferrite
crystal structure, is considered to be a competitive candidate
for a wide area of applications in various fields of catalysis
[1], hyperthermia treatment [2], recording device and sensors
[3], microwave devices and magnetic ferrofluids technology,
magnetic resonance imaging, drug delivery, antitumor and
protein separation [4-6]. Among these applications it is well
know that synthesis protocols, reaction conditions and post-
synthesis processes strongly influence the properties of co-
balt ferrite magnetic materials, which have further impact on
their different practical uses.
Several synthetic methods have been developed for co-
balt nanoferrites and these include hydrothermal synthesis
[7], emulsion [8], sol-gel template approach [9], coprecipita-
tion route [10, 11], combustion [12] and organic thermal
decomposition process [13]. Among them, the coprecipita-
tion synthetic process is one of the most inexpensive meth-
ods to prepare in high-yield cobalt ferrite nanoparticles. Dur-
ing this process, the precipitates are produced simultaneously
and uniformly dispersed in the solution. The annealed fer-
rites at high temperature might have some inconveniences,
including agglomeration of the particles, chemical heteroge-
neity and uncontrolled growth of particle size. In order to
prevent such disadvantages, previous studies have concluded
*Address correspondence to this author at the Faculty of Chemistry, Univer-
sity “Alexandru Ioan Cuza” from Iasi, Carol I Bvd. No. 11, Iasi 700506,
Romania; Tel/Fax: +40 232 2013 13; E-mail: aurel@uaic.ro
that surfactant molecules can be employed in a whole syn-
thetic process [6, 14-21]. Other studies show that the synthe-
sis temperature and subsequent calcinations processes play
an important role in controlling the size of the cobalt ferrite,
which significantly influence the physical properties of the
product [22, 23].
A wide variety of regression models have been devel-
oped to evaluate different situations. The regression model
consists of a systematic component and a residual compo-
nent. The systematic component contains information about
the underlying dependencies between a set of predictor vari-
ables and a response. The aim of statistical regression analy-
sis is to model the mechanisms that produce the systematic
component [24]. Statistics models show the degree of corre-
lations between the experimental results and the predicted
values, which validates the accuracy of the mathematical
model [25].
The influence of the calcination temperature on the de-
gree of crystallinity, morphology, microstructure and phase
purity can be investigated by different techniques, e.g., pow-
der X-ray diffraction pattern (PXRD), transmission electron
microscopy (TEM), and Fourier transform infrared spectros-
copy (FT-IR), respectively [26]. From the literature survey
we conclude that there are no studies to correlate the
NP’s dimensions with temperature, based on mathematical
models.
The aim of this study is finding a mathematical model
that could best correlate the nanoparticles sizes and to deter-
mine the optimal calcination temperature for maintaining the
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