World Journal of Nano Science and Engineering, 2016, 6, 20-28

Published Online March 2016 in SciRes. http://www.scirp.org/journal/wjnse

http://dx.doi.org/10.4236/wjnse.2016.61002

Fe3O4 and Fe Nanoparticles by Chemical

Reduction of Fe(acac)3 by Ascorbic Acid:
Role of Water
Ajinkya G. Nene1*, Makoto Takahashi1, Prakash R. Somani2
1
Department of Applied Chemistry, Chubu University, Kasugai, Japan
2
Applied Science Innovations Pvt. Ltd., Pune, India

Received 3 December 2015; accepted 28 February 2016; published 3 March 2016

Copyright © 2016 by authors and Scientific Research Publishing Inc.

This work is licensed under the Creative Commons Attribution International License (CC BY).
http://creativecommons.org/licenses/by/4.0/

Abstract
Nanoparticles of Fe3O4 and Fe are chemically synthesized by reduction of Fe(acac)3 using ascorbic
acid in controlled condition. It was observed that addition of water during the chemical synthesis
process yields Fe3O4 nanoparticles, whereas if the reaction is carried out in absence of water
yields Fe nanoparticles—which get oxidized upon exposure to air atmosphere. Fe3O4 (15 ± 5 nm)
and Fe/iron oxide nanoparticles (7 ± 1 nm) were successfully synthesized in the comparative
study reported herewith. Mechanism for formation/synthesis of Fe3O4 and Fe/iron oxide nano-
particles is proposed herewith in which added water acts as an oxygen supplier. Physico-chemical
characterization done by SEM, TEM, EDAX, and XPS supports the proposed mechanism.

Keywords
Fe3O4 Nanoparticles, Fe-Nanoparticles, Iron Oxide, Chemical Reduction Method

1. Introduction
Material properties change dramatically in their nano-form as compared to their bulk form [1]. In recent years,
magnetic nanoparticles have attracted much attention because of their unique properties and various applications
such as in the field of magnetic recording media (e.g. data storage devices, audio and videotape, recording discs,
magnetic fluid) [2], various in vivo and in vitro applications in biomedical science such as cancer hyperthermia,
targeted drug delivery, NMR imaging, bioseparation [3]-[5]. Magnetic nanoparticles have applications in cataly-
sis and other industrial usages [4]. Also, magnetic nanoparticles are also used to fabricate nanoscale electronic
*
Corresponding author.

How to cite this paper: Nene, A.G., Takahashi, M. and Somani, P.R. (2016) Fe3O4 and Fe Nanoparticles by Chemical Reduc-
tion of Fe(acac)3 by Ascorbic Acid: Role of Water. World Journal of Nano Science and Engineering, 6, 20-28.
http://dx.doi.org/10.4236/wjnse.2016.61002
 A. G. Nene et al.

devices [5].
Magnetite (Fe3O4) crystal has an inverse spinel structure with alternating octahedral and tetrahedral sites and
shows interesting electrical properties because electrons are transferred between Fe2+ and Fe3+ ions present in
octahedral sites [6]. Main requirement for application of Fe3O4 nanoparticles in biomedical science is size less
than 20 nm [7]—for their easy penetration and motion inside the human body. In general, as size of Fe3O4 na-
noparticles decreases the Curie temperature (Tc) also decreases. This puts an additional restriction that Fe3O4
nanoparticles should be used below Tc to utilize their magnetic properties. Thus, it is important to select correct
size of nanoparticles. At the same time, synthesis method should be highly reproducible, scalable, and economi-
cal.
Different polymers and surfactants such as polyvinylalcohol (PVA) [8], poly(vinylpyrolidone) (PVP) [9], po-
lyethylene glycol (PEG) [10], oleic acid [11], polyacrylic acid (PAA) [12] are used for coating of Fe3O4 nano-
particles or as capping agent (for controlling the size of the nanoparticles during synthesis and suppressing the
aggregration). This results in improved morphology, prevention of agglomeration and aggregation of nanopar-
ticles, but may affect the properties of nanoparticles. Also, polymers and surfactants are expensive and difficult
to (naturally) decompose. Thus, their use restricts the applications of Fe3O4 nanoparticles in biomedical science
and also can cause environmental problems. Fe3O4 nanoparticles are prepared by co-precipitation and polyol-
methods. There are reports on successful synthesis of Fe3O4 nanoparticles by hydrothermal method [13], co-
precipitation method [14] [15]. Some of the drawbacks/limitations associated with reported co-precipitation
synthesis processes are: slow process and high temperature, size not suitable for in vivo biomedical applications
(63 ± 25 nm) and wide size distribution [14]. When the magnetite particles (Fe3O4) which have a particular
stoichiometric composition are made by co-precipitation method, the pH adjustment or pH control is very im-
portant and a tedious task. In the coprecipitation method, magnetite nanoparticles are made by the hydrolysis of
Fe2+ ion and Fe3+ ion (mole ratio: 1:2) by a base (usually NaOH or NH4OH). In this case, overall composition of
the precipitate is same as that of the reaction system. But, as the hydrolysis rate of Fe3+ ion is greatly different
from that of Fe2+ ion, the composition of the nanoparticle may not be same. For pH > 11, re-dissolutions of
Fe(OH)3 and Fe(OH)2 happen.

Fe ( OH )3 → Fe ( OH )4 Fe ( OH )2 → Fe ( OH )3
− −

There are some other disadvantages of co-precipitation method such as broad nanoparticle size distribution,
poor crystallization and irregular crystal shape [16]. Polyol methods need long time (7 - 8 hours) and very high
temperature [16]. Exact mechanism leading to formation of Fe3O4 and origin of oxygen element in Fe3O4 is still
unclear in polyol method. Many other methods are reported such as green synthesis methods using plant extracts
and bacteria [17] [18], thermal decomposition/pyrolysis of organo-metallic precursors [19]-[22], ultrasound ir-
radiation [23], gamma radiolysis [24], and sol-gel method [25] [26]. Each of these methods has some disadvan-
tages and limitations. Most of these methods yield polydisperse nanoparticles, surface capped nanoparticles,
nanoparticles with impurities, in addition to poor reproducibility.
Various methods have been reported for the synthesis of Fe nanoparticles in aqueous medium, but synthesis
of Fe nanoparticles by reducing Fe(acac)3 using ascorbic acid is not yet reported. Iron has the highest room
temperature saturation magnetization and most importantly its Curie temperature (Tc) is high enough for various
possible applications [27]. Fe nanoparticles have various electrical, catalytic, and biomedical applications [27].
In addition, iron is a soft magnetic material with high magnetic moment density [27] [28].
Therefore, it is necessary to develop a simple, cost-effective, reproducible method to synthesize Fe3O4 and Fe
nanoparticles. In the present study, nanoparticles of Fe3O4 and Fe are chemically synthesized by reduction of
Fe(acac)3 using ascorbic acid in controlled condition. It was observed that addition of water during the chemical
synthesis process yields Fe3O4 nanoparticles, whereas if the reaction is carried out in absence of water yields Fe
nanoparticles—which were observed to get oxidized upon exposure to air atmosphere while handling (leading to
Fe/iron oxide particles). Fe3O4 (15 ± 5 nm) and Fe/iron oxide nanoparticles (7 ± 1 nm) were successfully syn-
thesized in the comparative study reported herewith. Mechanism for formation/synthesis of Fe3O4 and Fe nano-
particles is proposed based on water as an oxygen supplier [28] [29]. Physico-chemical characterization done by
SEM, TEM, EDAX, and XPS supports the proposed mechanism and gives us information about size and shape,
polydispersibility, crystallinity and crystal structure, and purity of the material.

21
A. G. Nene et al.

2. Experimental
2.1. Chemicals
Chemicals used in this work are: Fe(acac)3 (purity 99%, Strem chemicals, Japan), ascorbic acid (purity 99.6%,
Wako Pure Chemicals Industries, Ltd., Japan), dehydrated ethanol (prepared and used when required in our la-
boratory), diphenyl-ether (purity 99%, Wako Pure Chemicals Industries, Ltd., Japan), and Ultrapure deionized
(DI) water. All the chemicals were of analytical grade.

2.2. Instruments
Nanoparticulate powder samples were characterized by X-ray powder diffraction (XRD) using a Rigaku
RINT-2100 X-ray diffractometer (Japan) with CuKα radiation (λ = 1.5406 nm). Transmission electron micro-
scopy (TEM) images were obtained from JEOL JEM-2100F (USA) microscope. X-ray photoelectron spectros-
copy (XPS) was done using UlVac Phi Versa Probe CU (Japan).

3. Synthesis of Fe3O4 Nanoparticles

In a typical synthesis procedure, 50 mL of 30 mM Fe(acac)3 diphenyl-ether solution was made (by dissolving
Fe(acac)3 in diphenyl-ether) and the solution was kept under stirring in N2 gas atmosphere. Subsequently, tem-
perature was increased up to 70˚C. A reducing acid solution made up of 0.025 M ascorbic acid, 12 M ultrapure
water and dehydrated ethanol were then added at a dropping rate of 2 mL/min after the solution temperature
reached at 70˚C. After the addition of reducing acid solution, the solution was heated to 190˚C again and ref-
luxed for 1 hour. Finally, it was cooled down to room temperature naturally. Product was separated by filtration
and washed 4 - 5 times by chloroform to remove any impurities, followed by dried in vacuum. Dry powder ob-
tained is subsequently used for physico-chemical characterization.

4. Synthesis of Fe Nanoparticles
In another experiment, same procedure (as that for synthesis of Fe3O4 nanoparticles) was followed but reducing
acid solution made up of dissolving 0.025 M ascorbic acid into dehydrated ethanol (without using ultrapure wa-
ter) was added at 70˚C with a dropping rate of 2 mL/min.

5. Estimation of Decomposition Efficiency of Fe(acac)3

Same experiment of synthesis reaction was carried out and after the addition of ascorbic acid solution containing
dehydrated ethanol, ultrapure water, and ascorbic acid, ultraviolet-visible (UV-VIS) spectrum of 1 mL sample
taken at different time interval from reaction and diluted to 50 mL using diphenyl ether was measured to deter-
mine the concentration of precursor at that time. The concentration of precursor present in each sample was cal-
culated from absorbance by using Beer-Lamberts law. The decomposition efficiency was calculated by the fol-
lowing equation:
Initial concentration − Unreacted
=
Decomposition Efficiency × 100
Initial concentration

6. Results and Discussions

Figure 1(a) represents XRD patterns of samples prepared using ultrapure water and without ultrapure water.
Figure 1(a) shows a typical XRD spectrum of Fe3O4 nanoparticles and all peaks can be indexed as pure Fe3O4
phase with inverse spinel structure and matched well with the reported data (JCPDS:65-3107). No impurities
were detected. The crystallite size calculated by Scherrer equation and full-width-at-half-maximum (FWHM) of
the strongest peak (3 1 1) is 15 nm. Figure 1(b) shows a comparative study on decomposition efficiency at 70˚C
at different ultrapure water concentrations. It can be observable that the change in ultrapure water concentration
has no effect on decomposition efficiency. Figure 1(a) and Figure 1(c) show XRD pattern of samples prepared
without using ultrapure water. Peaks at 2θ of 30.22˚, 35.4˚, 43.12˚, 57˚ and 62.84˚ having d values as 2.9558,
2.5338, 2.0966, 1.6145, 1.4776 respectively corresponds to iron oxide. This was expected. This is due to the fact
that although sample was prepared in oxygen free condition (in presence of nitrogen); however, sample was

22
 A. G. Nene et al.

Without ultrapure water

311 With ultrapure water

220 400 440

511
111 222
422
2

10 20 30 40 50 60 70
2θ
(a)

1.2 M ultrapure water

100 2.4 M ultrapure water
Decomposition Efficiency (%)

12 M ultrapure water
80

60

40

20

0
10 15 20 25 20 30 40 50 60 70 80
Time (Minutes) 2θ
(b) (c)

Figure 1. (a) XRD pattern of sample prepared using ultrapure water and without ultrapure water; (b) Decomposition effi-
ciency of Fe(acac)3 at 70˚C at different ultrapure water concentration; (c) XRD pattern of sample prepared without ultrapure
water.

exposed to air atmosphere during filtration, drying, and XRD measurement process—leading to formation of
iron oxide (Fe/iron oxide nanoparticle). Broad peaks are indicating the amorphous nature of nanoparticles. Fig-
ure 2 represents the EDAX spectra of sample prepared using ultrapure water (a) and without using ultrapure
water (b). When ultrapure water was used in reaction then magnetite is formed and EDAX spectrum shows the
iron content of 62.16 at% and oxygen of 22.23 at%. Large amount of oxygen is observable in this sample which
corresponds to the lattice oxygen (supported by XRD). But when ultrapure water was not used (Figure 2(b))
sample shows high content of iron (85.06 at%) and very small amount of oxygen (3.89 at%). We believe that
this small amount of oxygen is actually an adsorbed oxygen on the surface of iron nanoparticles when they are
exposed to air atmosphere while handling (which is also supported by XRD results). In both the samples, carbon
was detected (which is approximately of same amount suggesting our conclusion about oxygen to be true) which
arises from carbon tape used for mounting the sample. EDAX measurements were performed at three different
locations of each sample and similar results were observed (oxygen of about 3 - 6 at% for the sample prepared
without using water, as against 20 - 30 at% for the sample prepared with water).
Figure 3 represents the TEM images of Fe3O4 nanoparticles and Fe/iron oxide nanoparticles, respectively.
Figure 3(a) represents sample prepared with addition of ascorbic acid solution at 70˚C. The mean particle di-
ameter is observed to be 15 ± 4 nm. Fe3O4 nanoparticles with size less than 25 nm were successfully synthesized
by fine tuning of the reaction parameters such as addition temperature, reflux temperature, dropping rate, and
reflux time. In Figure 3(b), the size of Fe/iron oxide nanoparticles is observed to be 7 ± 1 nm. Although synthe-

23
A. G. Nene et al.

(a)

(b)

Figure 2. EDAX spectra of sample prepared using ultrapure water (a) and without using ultrapure water (b).

(a) (b)

(c) (d)

Figure 3. (a) (b) HRTEM images of Fe3O4 nanoparticles; (c) (d) Fe/iron oxide nanoparticles.

24
 A. G. Nene et al.

sis parameters were same for preparation of both the samples (i.e. with and without water); because of the ab-
sence of oxygen (coming from water), smaller size Fe/iron oxide nanoparticles have been obtained.
Figure 4 represents XPS spectra of Fe3O4 nanoparticles. Sample prepared by using ultrapure water (Figure
4(a)) shows Fe2p region which is deconvoluted into 5 peaks. XPS peak at binding energy of 724.70 eV corres-
ponds to 2p1/2 of Fe3+ species, while the peak at binding energy of 722.90 eV can be assigned to 2p1/2 of Fe2+
species (in accordance with the earlier reported results) [30]. The peaks at 710.29 eV and 711 eV can be as-
signed to 2p3/2 of Fe2+ and Fe3+ species, respectively [29]. The peak at 719.06 eV is a satellite peak for above
four peaks. This shows the formation of Fe3O4 nanoparticles.
Fe2p region of sample prepared without ultrapure water (Figure 4(b)) is deconvoluted into five peaks. Peak at
707.94 eV correspond to 2p3/2 of zero-valent iron (Fe0) confirms the presence of metallic iron [31]-[33]. The
peak at 711.21 eV can be assigned to 2p3/2 of Fe3+ species. Photoelectron peaks at 722.93 eV and 724.46 eV can
be assigned to 2p1/2 Fe2+ and 2p1/2 Fe3+ species. Peak at 719.02 eV is a satellite peak for all above peaks.
Figure 4(c) and Figure 4(d) display the photoelectron spectra of O1s for the sample without using ultrapure
water and with ultrapure water, respectively. Both of these spectra show a single broad peak centered around
531 eV and 532 eV, respectively.
No appreciable difference is observable through the XPS analysis between the samples prepared with and
without using ultrapure water. This might be due to two reasons: 1) XPS is a surface sensitive technique with
very small penetration depth (about 5 nm), and 2) sample prepared without using ultrapure water gets oxidized
when exposed to air atmosphere while handling. This was expected due to high reactivity of iron in nanoparti-
culate form and its affinity and high reactivity towards oxygen. Formation of iron oxide on the surface of iron
nanoparticles is also reported earlier by other researchers [29]-[33].

4000 7000
6500
3500
6000
Intensity (a.u.)

Intensity (a.u.)

3000 5500
5000
2500 4500
4000
2000
3500
1500 3000
2500
1000
705 710 715 720 725 730 735 705 710 715 720 725 730 735

Binding Energy (eV) Binding Energy (eV)

(a) (b)
12000
6000
10000
5000
Intensity (a.u.)

Intensity (a.u.)

8000
4000

3000 6000

2000 4000

1000 2000

0 0
520 525 530 535 540 545 524 526 528 530 532 534 536 538 540
Binding energy (eV) Binding energy (eV)
(c) (d)

Figure 4. (a) XPS Fe2p spectrum of sample prepared using ultrapure water and (b) without using ultrapure water; (c) O1s
spectrum of sample prepared using ultrapure water; (d) O1s spectrum of sample prepared without using ultrapure water.

25
A. G. Nene et al.

7. Mechanism for Formation of Fe3O4 Nanoparticles

In our synthesis process, ascorbic acid acts as reducing agent and ultrapure water acts as supplier of oxygen. The
role of dehydrated ethanol is a solvent in ascorbic acid solution. Fe(acac)3 in diphenyl-ether is reduced by ascor-
bic acid and hydrolyzed by ultrapure water [34].
6Fe ( III )( acac )3 + ascorbic acid ( act as reducer ) + 8H 2 O
→ 2Fe3 O 4 + dehydroascorbic acid + 18acac
Ascorbic acid reduces the Fe(acac)3 as follows:
Fe2+ is formed because of reduction of Fe3+(acac)3 by ascorbic acid, and because of ultrapure water Fe(OH)2 is
generated as follows:
Fe3+ ( acac )3 + 1 2 ( C6 H8 O6 ) → Fe2 +

2H 2 O ⇔ 2H + + 2 ( OH )
−

Fe 2 + + 2 ( OH ) → Fe ( OH )2
−

And 2Fe(OH)3 is formed as follows:

6H 2 O ⇔ 6H + + 6 ( OH )
−

2Fe ( acac )3 + 6 ( OH ) + 6H + → 2Fe ( OH )3

−

In general, Fe(acac)3 is reduced by ascorbic acid and Fe3(OH)8 is synthesized as follows:

2Fe3+ + Fe + + 8H 2 O → Fe32+ Fe 2+ ( OH )8
When reaction mixture is heated to reflux, it results in crystallization of Fe3O4 nanoparticles and hydrolysis.
The formation of Fe3O4 is as follows:
Fe3 ( OH )8 
reflux
→ Fe3 O 4 + 4H 2 O
The general reaction can be written as:
6Fe ( acac )3 + C6 H8 O8 + 8H 2 O → 2Fe3 O 4 + C6 H 6 O6 + 18 ( acac )
If ultrapure water is not used in reaction, then Fe(acac)3 is reduced by ascorbic acid; but due to lack of oxygen
source Fe3O4 is not formed, leading to formation of Fe nanoparticles. This also proves that ultrapure water is
oxygen supplier in our reaction. In reported polyol-methods, the exact mechanism leading to formation of Fe3O4
and origin of oxygen element in Fe3O4 is still unclear. Our mechanism proves the origin of oxygen and the role
of water during our synthesis process (Table 1).
Fe(acac)3 
reduction by ascorbic acid
( )
→ Fe ions Fe3+ , Fe 2 + → Fe nanoparticles
→ Iron oxide ( due to exp osure to air atmosphere )

8. Conclusion
We have successfully developed and demonstrated a new and simple approach to synthesize Fe3O4 and Fe na-
noparticles (without using any capping agent for size and shape control) in which Fe(acac)3 is reduced by ascor-
bic acid in a controlled atmosphere with respect to temperature and hydrolyzed by ultrapure water. Ultrapure

Table 1. Elemental composition of samples obtained with and without addition of water during the synthesis process.

Sample Fe (at%) O (at%) C (at%)

Fe3O4 (sample with water) 62.16 22.23 15.61

Fe/iron oxide (sample without water) 85.06 3.89 11.05

26
 A. G. Nene et al.

water acts as oxygen supplier. Fe3O4 nanoparticles are observed to form with addition of water; whereas Fe na-
noparticles are formed in absence of water. It was observed that such Fe nanoparticles get oxidized to form
Fe/iron oxide nanoparticles due to exposure to air atmosphere. Reproducible synthesis of Fe3O4 nanoparticles of
size 15 ± 5 nm and Fe/iron oxide nanoparticles of size 7 ± 1 nm were achieved. Mechanism for the synthesis of
Fe3O4 and Fe nanoparticles is proposed. Method presented herewith should prove to be very useful for synthesis
of Fe3O4 nanoparticles having surface available for further use such as uploading of drug molecules for bio-
medical applications. Further work for biomedical application of these nanoparticles is in progress.

Acknowledgements
One of the authors Ajinkya G. Nene acknowledges the financial support from Japanese Government through
Monbukagaksho fellowship. We acknowledge Chubu University, Japan for providing characterization facilities
for this study.

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