SYNTHESIS OF IRON OXIDE NANO PARTICLES IN BATCH

REACTOR, SEMIBATCH REACTOR AND MICROREACTOR: A

COMPARATIVE STUDY
1

MAHENDRA L. BARI, PRASHANT SURYWANSHI, SATYENDRA MISHRA,

4
SHIRISH H. SONAWANE
1,2,3

University Institute of Chemical Technology, North Maharashtra University, Jalgaon.

3
National Institute of Technology, Warangal

Abstract- The novel material driven demand for sustained growth of industry focused research in the field of
nanotechnology. Nano particles exhibit unusual physical and chemical properties which are size and shape dependant. Iron
nanoparticles have found numerous applications in drug delivery, pharmaceutical industry, medical diagnosis and waste
water treatment. Conventionally batch and semibatch methodology was used for synthesis of the nano particles which results
in large size with wide size distribution of nanoparticles due to lack of precise control on nano particle formation process.
The microreactor is a new concept which is very small-scale system capable of continuous synthesis of narrow size of nano
particles. Objective of the investigation was to study the effect of reactor type and precursor concentration on nanoparticles
size. Particles size distribution, Zeta Potential and FESEM analysis was carried out to understand the effect of variables.
Keywords- Nanoparticles, semibatch reactor, microreactor, narrow size distribution

I. INTRODUCTION

synthesis of nano particles in semibatch and

continuous process. Microreactor is used
for
synthesis of monodispersed nano particles.
Microreactors provide small reaction volumes that are
more homogeneous with respect to concentration,
temperature, and mass transport, leading to a better
control of the reaction steps that govern particle size
distribution, i.e., nucleation and growth.[26].

Researchers focus on nano systems because of the

excellent properties of nana particles as compared to
bulk counterparts. The unique properties of these
nano material explore extensive
industrial
applications in the field of catalysis, electronics,
sensors, medical diagnosis water treatment [1-3] and
polymer [4-8]. Nanoparticles are providing bridge
between bulk materials and molecular structures.

In the present work, we carried out the synthesis of

iron oxide nano particles in batch, semibatch and
microreactor with
variation of
precursor
concentration to study the effect of reactor type and
precursor concentration on nanoparticles size.

The synthesis of magnetic nanoparticles with sizes

ranging from 2 to 20 nm, is of significant importance,
because of their applications in magnetic storage
devices, ferrofluids, magnetic fluid, magnetic carriers
for drug targeting [9].

Material
Ferric Chloride (99% pure, Himedia Laboratories,
Mumbai), Sodium BoroHydride (99% pure, Merck
PVT. LTD., Mumbai), SDS (99% pure, SD Fine
Chem LTD., Mumbai), were used as received.
Deionized and distilled water was used in the
experiments.

The synthesis of nanoparticles is carried out either by

top-down or bottom-up approaches [10]. Wetchemical synthesis was carried out either by
precipitation or chemical reduction methods further
which can be carried out either in batch techniques
[11-14] or continuous processes [15]. Metal salt
reduction assisted by reverse micelles, thermal
decomposition of organometallic precursor, solgel
and coprecipitation methods are adopted for synthesis
of metal oxide nano particles in liquid phase process.
[16-20] The key parameters that determine the size
of the nanoparticles and its size distribution in
chemical synthesis are the type of surfactant precursor
concentration, , ratio of surfactant to the precursor
salt, and control of reaction kinetics through rapid
nucleation followed by growth [21-25].

II. METHODOLOGY OF NANOPARTICLE

SYNTHESIS IN MICROREACTOR:
Synthesis of iron oxide nanoparticle in batch reactor:
In typical batch experiment, 0.001 M of FeCl3 and
1.4 M sodium borohydride each containing SDS
(2.336 gm/lit) were prepared in separate flask.
Then the solutions were added in batch reactor and
reaction was carried out under continuous magnetic
stirrering at room temperature for 120 min. The
process was repeated for 0.002 M to 0.005 M of
FeCl3 concentration.

The batch technique produces the nano particles with

broad size distribution so there is need to explore the
th

th

Proceedings of 12 IRF International Conference, 29 June-2014, Pune, India, ISBN: 978-93-84209-31-5

Synthesis of Iron Oxide Nano Particles In Batch Reactor, Semibatch Reactor And Microreactor: A Comparative Study

III. PROCESS FOR SYNTHESIS OF IRON

OXIDE NANOPARTICLES IN SEMIBATCH
REACTOR:
250 ml aqueous solution of FeCl3 (0.001 M) and 250
ml NaBH4 (0.004 M) was prepared separately and
SDS was added to both solutions at CMC value
((2.336 gm/lit)). Drop by drop addition of NaBH4
solution to FeCl3 solution was done under continuous
magnetic stirring. The process was repeated for 0.002
M to 0.005 M of FeCl3 with stichometric ratio of
FeCl3 to NaBH4 1:4.

VI.

SYNTHESIS
OF
IRON
OXIDE
NANOPARTICLE IN SEMIBATCH REACTOR:
In semibatch production process of iron oxide nano
particles, the limiting reactant NaBH4 was added to
control the nucleation and growth of nano particles.
The molar ratio of FeCl3 to NaBH4 was kept 1:4 and
concentration of FeCl3 was varied from 0.001 M
to
1.5 M.

IV.

SYNTHESIS
OF
IRON
OXIDE
NANOPARTICLE IN MICROREACTOR:
The synthesis of iron oxide nano particles was carried
out in microreactor of 6 ml volume, model Amar-2
Mumbai, India. The aqueous FeCl3 and NaBH4
solution was prepared of required concentration and
SDS was added in both the solutions at CMC level.
The two peristaltic pumps were used to fed reactant
to Y junction of reactor, and the flow rate of both the
reactants was kept 6 ml/min. The product was
collected at outlet of the reactor.

V. RESULT AND DISCUSSION:

Synthesis of iron oxide nanoparticle in batch reactor:
The synthesis of iron oxide nano particles was carried
out in batch reactor with variation of FeCl3
concentration from 0.001 M to 0.005 M and SDS is
used as stabilizing agent. Addition of surfactant in
precursor solution creates micelles, these micelles act
as nano reactor for the synthesis of nano particles.
Ferric chloride was reduced by sodium borohydride
to form the metal ion for nano particles synthesis. In
batch process initially as the reaction starts, the metal
ions concentration starts to increase providing the
metal ions to reach to supersaturation value so that
nucleation process starts. Further the nuclei grow
with proceeding the reaction. The largest particle size
(256 nm) was obtained at 0.004 M FeCl3, while
smallest size (95 nm) was obtained at 0.002 M FeCl3
concentration. Figure 1 shows that in batch reactor no
consistent trend is observed for nano particle size
with concentration of metal precursor. Initially
particle size deceases with increase in concentration
and again increases with increase in concentration.

Fig.1 Effect of precursor concentration on size of nano

particles synthesized in batch reactor

Fig.2 Effect of precursor concentration on size of nano

particles synthesized in semibatch reactor

In semibatch production process the size of nano

particles increases with increase in concentration as
shown in figure 2. Drop by drop addition of NaBH4 at
small precursor concentration, limits the growth of
initially formed nuclei giving the small size of iron
oxide nano particles. At higher concentration of
precursor rate of reaction was fast and metal ion
formed were responsible for the growth of nuclei
resulting in larger size of nano particles. Figure 4
shows that the size distribution was wide at low
concentration of FeCl3 whereas narrow size
distribution was obtained at high concentration of
FeCl3.

Fig.3 FESEM images of nano particles synthesized in

semibatch reactor

concentration. It was found that the small size nano particles were obtained at low concentration in semibatch reactor and microreactor whereas the

The 2-4 nm particles with narrow size distribution were obtained in microreactor at 0.002 M FeCl3 solution; and narrow size distribution of nano part

sodium borohydrate
Fig.4 Size distribution of nano particles synthesized in
semibatch reactor at 0.001 M FeCl3 and
0.005 M FeCl3

VII.

SYNTHESIS
OF
IRON
OXIDE
NANOPARTICLE IN MICROREACTOR:
The reduction route was adopted for synthesis of iron
oxide nano particles in microreactor. The molar ratio
of FeCl3 to NaBH4 was kept 1:4 with variation of
FeCl3 concentration from 0.001 M to 0.003 M. The
smallest size of nano particle was obtained at 0.002
M FeCl3 whereas largest size of nano particle was
obtained at 0.003 M FeCl 3. The zeta potential analysis
shows iron oxide nano particles produced at 0.001 M
FeCl3 were stable and the particles obtained at higher
concentration were not stable, hence the aggregation
was observed at higher concentration of FeCl3. Figure
5 shows that narrow particle size distribution was
obtained at 0.002 M FeCl3.
Table 1 Avg. particle size and zeta potential of nano
particles synthesized in microreactor
NaBH4
FeCl3
Avg.
Sr. No
Concentrati
Concentrati
Partic
.
on
on
le
(M)
(M)
Size
(nm)
1
0.001
0.004
6.98
2
0.002
0.008
1.6
3
0.003
0.012
283.8

Fig.5 Size distribution of nano particles synthesized in

microreactor at .0.002 M FeCl3

CONCLUSION:
Synthesis of iron oxide nanoparticles in batch
reactor, semibatch reactor and microreactor was
carried out by reduction of ferric chloride with

with variation of precursor

particles were
microreactor.

obtained

in

semibatch

and

ACKNOWLEDGMENT:
One of the author is thankful to TEQIP II
MHRD, New Delhi, Government of India,North
Maharashtra University authorities for providing
financial assitance, Akash for his assistanceship
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