Facile synthesis of magnetite iron oxide

nanoparticles via precipitation method

at different reaction temperatures
M. F. Tai, C. W. Lai, S. B. A. Hamid*, D. D. Suppiah, K. S. Lau,
W. A. Yehya, N. M. Julkapli, W. H. Lee and Y. S. Lim
The nano-scale magnetite iron oxide particles have been synthesised by a facile precipitation
method. Magnetite iron oxide nanoparticles were synthesised in a bath with electrolytes
composed of 0·10 M of iron (II) chloride with 0·45 M of sodium hydroxide at different reaction
temperatures under oxidising environment. In the present study, the influence of reaction
temperatures (30, 45 and 80°C) on the morphology, particle size and crystallinity of the iron
oxide particles were investigated in detail. Based on the Malvern Zetasizer analysis, the iron
oxide particles with variable size from ∼250 to ∼70 nm could be achieved when increasing the
reaction temperature up to 80°C. The magnetite phase of iron oxide particles was determined by
using X-ray diffraction analysis. In addition, field emission scanning electron microscopy
micrographs were further affirmed that our synthesised iron oxide particles were in nano-scale
with a spherical shape. It was found that the high reaction temperature is helpful in controlling
the formation of uniform magnetite iron oxide nanoparticles.
Keywords: Magnetite, Iron oxide particles, Precipitation, Particle size, Reaction temperature

Introduction presence of different iron oxide phases such as magnetite

Today, development and design of nano-scale materials
have gained a lot of attention because mechanical, chemi-
cal, electrical, optical, magnetic, electro-optical and
magneto-optical properties of these materials are differ-
ent from their bulk properties and depend on the particle
size.1 In this manner, magnetite iron oxide has exhibited
great potential for their applications as catalytic
materials,2,3 wastewater treatment adsorbents,4,5 pig-
ments,6 flocculants, coatings,7 gas sensors, magnetic
recording devices, magnetic data storage devices,8 mag-
netic resonance imaging9 and medicine applications.10
Iron oxide nanoparticles have been comprehensively
studied because of their non-toxicity, biocompatibility,11
superparamagnetism, high coercivity and low Curie
temperature properties. Several synthesis procedures
have been developed for preparing magnetite nanoparti-
cles, such as chemical co-precipitation,12 sol–gel13 and
hydrothermal.
The precipitation technique is the simplest and most
efficient chemical route to obtain iron oxide particles.
However, it has difficulty in the control of particle size,
size distribution and sometimes simultaneous the
Nanotechnology & Catalysis Research Centre (NANOCAT), 3rd Floor,
Block A, Institute of Postgraduate Studies (IPS), University of Malaya,
50603 Kuala Lumpur, Malaysia
*Corresponding author, email sharifahbee@um.edu.my
and maghemite.14,15 A wide variety of experimental
factors such as pH, temperature, Fe2+/Fe3+ molar ratio
and stirring velocity affect the synthesis of iron oxide
nanoparticles and their properties. In this study, a
simple and efficient one-step precipitation method is
reported to study the influence of reaction temperatures
(30, 45 and 80°C) on the morphology, particle size and
crystallinity of the iron oxide particles synthesised.
Experimental procedure
Ferrous chloride tetrahydrate (FeCl2·4H2O, Sigma
≥99%) and sodium hydroxide (NaOH, Sigma ≥97·0%)
were used for the synthesis of iron oxide nanoparticles.
All chemicals used were of reagent grade and without
further purification. The aqueous solution was prepared
by dissolving 2·00 wt-% of FeCl2 in 100 mL deionised
water. Subsequently, 0·45 M of NaOH solution was
added at a speed of 1·0 mL min−1 into the solution
under vigorous stirring to reach a final pH 12. These reac-
tions were carried in air medium for three different temp-
eratures, i.e. 30, 45, and 80°C. It was observed that the
solution became black because of the formation of
Fe3O4 particles. The resultant black precipitate was iso-
lated by centrifugation at 7000 rev min−1 and then
removed by decantation. The precipitate was rinsed
three times with deionised water and then dried in an
oven at 50°C for 12 hours. Microstructure properties of

© W. S. Maney & Son Ltd 2014

S6-470 DOI 10.1179/1432891714Z.0000000001000 Materials Research Innovations 2014 VOL 18 SUPPL 6
 Tai et al. Facile synthesis of magnetite iron oxide nanoparticles

nanoparticles were observed using a field emission scan-

ning electron microscope (FESEM). Particles sizes of
the magnetite Fe3O4 were measured by the dynamic
light-scattering method (DLS) by a Malvern Zetasizer
Nano-ZS. The crystalline phase of magnetite Fe3O4
nanoparticles was studied by X-ray diffraction (XRD)
using CuKα radiation (λ = 1·5406 Å, FK60-40 X-ray dif-
fractometer). The samples were also characterised by
Fourier transform infrared spectroscopy (FTIR, Perkin
Elmer-1600 Series).

Results and discussion

In this part of the experimental study, the effect of reac-
tion temperatures on the morphology of magnetite
Fe3O4 is discussed. The surface morphology of prepared
nanoparticles at 30, 45 and 80°C was determined by
FESEM (Fig. 1). From Fig. 1, it is shown that increasing
reaction temperatures during precipitation could modify
the particles size and morphology significantly.16
Referring to Tao et al.14 the process of Ostwald ripening
would accelerate with the increase in reaction tempera-
tures, which means smaller nanoparticles would decrease
in their size more easily and bigger particles would keep
growing further, therefore leading to the widening of the
size distributions. In contrast, the resultant particle size
of magnetite Fe3O4 became more uniform as reaction
temperature slowly rose to 80°C.
As shown in these FESEM micrographs, the particle
size of Fe3O4 was dependent on the reaction tempera-
tures. It could be noted that the Fe3O4 particles syn-
thesised at 30 and 45°C were spherical in shape with an
average diameter of 180 and 80 nm as exhibited in
Fig. 1a and b, respectively. Interestingly, smaller Fe3O4
particles with an average diameter of 60 nm were
obtained when the reaction temperature slowly rose to
80°C. The reason might be attributed to the activation
energy of the nucleus formation, which was inversely pro-
portional to the square of temperature. The nucleation
rate and number of nucleus would increase with the
increasing temperature and, therefore, nanoparticles
would reduce in their size slightly. According to the
FESEM images, there was agglomeration of Fe3O4 par-
ticles occurred in the samples. The agglomeration hap-
pened because of van der Waals force between Fe3O4
particles.
The volume-based particle size of the sample obtained
by DLS measurement is shown in Table 1. The particles
size of magnetite synthesised was decreased as tempera-
ture elevated. Karaagac et al. 16 and Babes et al.17
reported that synthesis temperature exhibited insignifi-
cant influence on the Fe3O4 particles size, while Liu
et al. 18 reported that Fe3O4 particles size increased with 1 Field emission scanning electron microscope images of
increasing temperature. However, our results showed magnetite Fe3O4 synthesised at reaction temperatures of
that the particle size of magnetite Fe3O4 was decreased a 30°C, b 45°C and c 80°C
significantly when increasing the reaction temperatures.
It was found that the magnetite Fe3O4 synthesised at
30°C was approximately 257·20 nm while the particle
size dropped down to 93·82 and 67·57 nm for the magne- Table 1 Particles size for magnetite Fe3O4 synthesised at
tite Fe3O4 synthesised at 45 and 80°C, respectively. At different reaction temperatures
higher temperature, the reaction condition set to be com- Sample Reaction temperatures (°C) Particles size (d.nm)
pleted, and samples with reduced crystal defects and
smaller particle size were produced.19 Nevertheless, the A 30 257·20
particles size obtained by DLS was larger as compared B 45 93·82
C 80 67·57
to the average diameter measured by FESEM. This

Materials Research Innovations 2014 VOL 18 SUPPL 6 S6-471

Tai et al. Facile synthesis of magnetite iron oxide nanoparticles
2 X-ray diffraction patterns of magnetite Fe3O4 synthesised
at reaction temperatures of a 30°C, b 45°C and c 80°C
phenomenon may be attributed to the aggregation of
Fe3O4 nanoparticles.20
As shown in Fig. 2, all of the resultant samples have a
face-centred cubic spinel structure, which indicates a rela-
tive phase purity of Fe3O4. It has the characteristic (220),
(311), (400), (511) and (440) peaks of magnetite at around
2θ ≈ 30, 35, 43, 57 and 63°, respectively. However, the
maghemite phase also has the same crystal as the magne-
tite phase. Figure 3 shows that the intensity of peaks
increased from Sample A, B to Sample C. Karaagac
et al. 16 reported that Fe3O4 synthesised at higher temp-
erature showed intensified peaks, which indicated that
the crystallinity of Fe3O4 became stronger. It was
observed that the peaks of Sample C at 35° 2θ (311)
were broadened because of the smaller particle size.21
The average crystallite size was calculated from the full-
width at half-maximum (FWHM) of the Fe3O4 (311) dif-
fraction peak at 2θ = 35·5° using Scherrer’s equation.
From this equation, crystallite size of samples synthesised
at 30, 45 and 80°C was determined 23·60, 17·70 and
3 Fourier transform infrared spectroscopy spectra of
magnetite Fe3O4 synthesised at reaction temperatures of
a 30°C, b 45°C and c 80°C
S6-472 Materials Research Innovations 2014 VOL 18
14·10 nm, respectively. Based on the result, it could be
assumed that some of the samples might contain maghe-
mite as impurity but no other non-magnetic impurities.
The black colour of the samples inferred that these
maghemite impurities were low in content since maghe-
mite Fe3O4 was brown in colour.22
The FTIR spectra of magnetite Fe3O4 synthesised at
30, 45 and 80°C are presented in Fig. 3a–c, respectively.
In the present study, FTIR analysis was performed to
identify the structure of the samples within the
500–1500 cm−1 region. Based on the results obtained,
all three samples have a transmittance peak at 584 cm−1
which is corresponding to δ(Fe–O) stretching vibration
in the tetrahedral site.23 This finding was confirmed that
the presence of magnetite Fe3O4 within the sample. In
addition, another obvious peak could be observed at
around 631 cm−1 from the FTIR spectra. The resultant
peak indicated the existence of maghemite Fe3O4.24
This analysis shows the destructive influence of the
atmospheric oxygen on the structural stability of magne-
tite nanoparticles.
Conclusion
In summary, reaction temperature during the precipi-
tation played a critical role in controlling the particles
size and crystallinity of magnetite Fe3O4 nanoparticles.
Based on our results, it can be concluded that higher reac-
tion temperature of 80°C resulted in higher crystallinity of
the magnetite phase with uniform nano-scale particles
size (∼70 nm in diameter). The main reasons might be
attributed to the loss of surface defect, nucleation rate
and number of nucleus increased with temperature
increased.
Acknowledgements
The authors would like to thank University of Malaya for
funding this research work under National
Nanotechnology Directorate (NND-53-02-03-1090) and
High Impact Research (H21001-F0032).
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