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Nanostructural and magnetic studies of virtually monodispersed NiFe2O4

nanocrystals synthesized by a liquid–solid-solution assisted hydrothermal
route

Article  in  Journal of Nanoparticle Research · March 2012

DOI: 10.1007/s11051-012-0751-6

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J Nanopart Res (2012) 14:751
DOI 10.1007/s11051-012-0751-6
RESEARCH PAPER
Nanostructural and magnetic studies of virtually
monodispersed NiFe2O4 nanocrystals synthesized
by a liquid–solid-solution assisted hydrothermal route
Xinghua Li • Guoguo Tan • Wei Chen •
Baofan Zhou • Desheng Xue • Yong Peng •
Fashen Li • Nigel J. Mellors
Received: 29 August 2011 / Accepted: 18 January 2012
Ó Springer Science+Business Media B.V. 2012
Abstract This study presents a comprehensively
and systematically structural, chemical and magnetic
characterization of *9.5 nm virtually monodispersed
nickel ferrite (NiFe2O4) nanoparticles prepared using
a modified liquid–solid-solution (LSS) assisted hydro-
thermal method. Lattice-resolution scanning transmis-
sion electron microscope (STEM) and converged
beam electron diffraction pattern (CBED) techniques
are adapted to characterize the detailed spatial mor-
phology and crystal structure of individual NiFe2O4
particles at nano scale for the first time. It is found that
each NiFe2O4 nanoparticle is single crystal with an fcc
structure. The morphology investigation reveals that
the prepared NiFe2O4 nanoparticles of which the
surfaces are decorated by oleic acid are dispersed
Electronic supplementary material The online version of
this article (doi:10.1007/s11051-012-0751-6) contains
supplementary material, which is available to authorized users.
X. Li  G. Tan  W. Chen  B. Zhou  D. Xue 
Y. Peng (&)  F. Li (&)
Key Laboratory of Magnetism and Magnetic Materials
of Ministry of Education, Lanzhou University,
Lanzhou 730000, China
e-mail: pengy@lzu.edu.cn
F. Li
e-mail: lifs@lzu.edu.cn
N. J. Mellors
Nano Materials Group, School of Computing,
Science and Engineering, University of Salford,
Greater Manchester M5 4WT, UK
individually in hexane. The chemical composition of
nickel ferrite nanoparticles is measured to be 1:2
atomic ratio of Ni:Fe, indicating a pure NiFe2O4
composition. Magnetic measurements reveal that the
as-synthesized nanocrystals displayed superparamag-
netic behavior at room temperature and were ferro-
magnetic at 10 K. The nanoscale characterization and
magnetic investigation of monodispersed NiFe2O4
nanoparticles should be significant for its potential
applications in the field of biomedicine and magnetic
fluid using them as magnetic materials.
Keywords Nickel ferrite  Nanoparticles 
Liquid–solid-solution assisted hydrothermal method 
CBED  Magnetic properties
Introduction
Nanoscale spinel ferrites MFe2O4 (M = Fe, Co, Ni,
Mn, Mg etc.) have attracted much attention in recent
years due to their unique magnetic, electrical proper-
ties and chemical stabilities (Deng et al. 2005; Laurent
et al. 2008). These properties are significant not only
from a fundamental point of view, for example,
blocking behavior, nanoscale confinement and nano-
magnetism (Sandweg et al. 2011; Zhou et al. 2006;
Kodama et al. 1996), but also for their potential
applications, such as high-density data storage
(Frey et al. 2009), ferrofluids (Jacintho et al. 2009),
ferroelectromagnet (Zheng et al. 2004), magnetic
123
Page 2 of 9
resonance imaging (Lee et al. 2007; Jun et al. 2008a;
Tromsdorf et al. 2007) and magnetically guided drug
delivery systems (Laurent et al. 2008; Latham and
Williams 2008). Nickel ferrite (NiFe2O4) is one of the
ferrite family with significant qualities such as low
coercivity, high electrical resistivity, low eddy current
loss, chemical and thermal stabilities (Jacob and
Khadar 2010; Ebrahimi and Azadmanjiri 2007; Wang
2006). Its crystal structure is an inverse spinel with
oxide anions arranged in a cubic close-packed lattice
and cations Ni2? and Fe3? occupying some or all of
the octahedral and tetrahedral sites in the lattice
structure. As one of the most important soft magnetic
materials, the magnetization of ferromagnetic
NiFe2O4 derives from anti-paralleled alignments of
spins between Fe3? ions at tetrahedral sites and Ni2?
ions at octahedral sites (Kinemuchi et al. 2002).
Nanoscale ferromagnetic NiFe2O4 materials have
various potential applications in magnetic fluids
(Sousa et al. 2001; Gomes et al. 2008), electrodes
(Vidal-Abarca et al. 2010), catalysis (Rashad and
Fouad 2005), core material for power transformer
in electronics and telecommunication applications
(Ebrahimi and Azadmanjiri 2007), sorbent (Deraz
et al. 2010), gas sensor (Satyanarayana et al. 2003),
thermal therapy (Kobayashi et al. 2010), and biomed-
icine (Jun et al. 2008b).
However, the magnetic behaviors of nanoscale
nickel ferrites are extremely sensitive to their size,
purity, and magnetic stability (Li et al. 2010b). There
is already significant interest in synthesizing high
quality NiFe2O4 nanoparticles for achieving optimal
magnetic properties, including co-precipitation (Maaz
et al. 2009; Salavati-Niasari et al. 2009), solid state
reaction (Ceylan et al. 2008), sol–gel method (Vidal-
Abarca et al. 2010; Srivastava et al. 2009; Chen and He
2001), reverse microemulsion process (Fang et al.
2003), sonochemical synthesis (Shafi et al. 1997),
combustion reaction (Costa et al. 2006; Vivekanand-
han et al. 2004), high-energy-milling (Šepelák et al.
2003), and pulsed wire discharge (Kinemuchi et al.
2002; Lee et al. 2006). The preferred method of
hydrothermal synthesis (Wang 2006; Baykal et al.
2008; Liu et al. 2009; Wang et al. 2009; Bućko and
Haberko 2007; Wang et al. 2010; Chen et al. 2003; Li
et al. 2010a, b) has been widely adopted to prepare
ferrite nanomaterials. This method has a relatively low
reaction temperature, low cost, environmental safety
123
J Nanopart Res (2012) 14:751
and high degree of compositional control (Baykal
et al. 2008; Ma et al. 2010) and can produce tailored
size and shape ferrite nanocrystals.
A common problem in the preparation of magnetic
ferrite nanoparticles is agglomeration, which derives
from the magnetic attractive forces between nanopar-
ticles. In addition, experimental conditions, such as pH
value and solution concentration, can cause a variety
of physical and chemical properties of ferrite nano-
particles. Li and co-workers (Wang et al. 2005; Wang
and Li 2007) have made a significant contribution by
developing a facile hydrothermal strategy based on a
general liquid–solid-solution (LSS) phase transfer and
separation mechanism for synthesizing a large variety
of ferrite nanoparticles. So far, virtually monodi-
spersed hematite, goethite, magnetite and magnetite
doped with various metal elements (Mg, Zn, Co, Mn,
Gd, Sm, Nd, Y and Lu) nanoparticles have been
prepared (Liang et al. 2006). We have recently
contributed an improvement to this LSS-assisted
hydrothermal method for the preparation of monodi-
spersed CoFe2O4 nanoparticles (Li et al. 2010b).
In this article, we describe a modified LSS-assisted
hydrothermal method to prepare virtually monodi-
spersed NiFe2O4 nanoparticles, which reduces the
synthetic costs and simplify the preparation proce-
dures. We also contribute a nanoscale characterization
of individual NiFe2O4 nanoparticles for the first time.
The morphology, structure, chemical, and magnetic
characterization of the NiFe2O4 nanoparticles have
been systemically investigated.
Experimental
Materials
All chemicals were of analytical grade and used as
received without further purification. FeCl36H2O
(AR 99.0%) was purchased from Tianjin Guangfu
Chemical Company (Tianjin, China). NiCl26H2O
(AR 98.0%) was bought from Tianjin Kaitong Chem-
ical Company (Tianjin, China). C18H33NaO2 (CP) was
purchased from Guoyao Chemical Company (Shang-
hai, China). Ethanol was purchased from Rionlon
BoHua Pharmaceutical and Chemical Limited Com-
pany (Tianjin, China). Deionized water was used
through the experiment (18.25 MX cm resistance).
J Nanopart Res (2012) 14:751
Preparation of NiFe2O4 nanoparticles
Virtually monodispersed nanocrystalline nickel ferrite
was synthesized by using our modified LSS-assisted
hydrothermal method. The advantage of this modified
method compared with the traditional LSS-assisted
hydrothermal method is that sodium hydroxide was
not used to precipitate metal ions, which avoids the
influence of solution pH value on the phases and
properties of specimens, in addition to reducing the
synthetic costs and simplifying the preparation proce-
dures. The detailed preparation method has been
detailed in our previous report (Li et al. 2010b). The
reaction solution was prepared as follows: An 80-mL
aqueous solution composed of 1.622 g ferric chloride
hexahydrate and 0.713 g nickel chloride hexahydrate
were mixed with a solution of 7.307 g sodium oleate
dissolved in 40 mL ethanol. 7 mL of oleic acid were
added into the above solution as surfactant, which was
continuously agitated throughout for 2 h at room
temperature by a magnetic stirrer. The prepared
solution was then sealed in a 150 mL Teflon-lined
stainless autoclave and hydrothermally treated at
180 °C for 12 h. Then the autoclave was allowed to
cool to room temperature naturally, and the specimens
were collected by using hexane. Ethanol was added to
the sample-containing hexane solution and nanocrys-
tals formed. The powder was then obtained by
centrifugation. The hexane-dispersed and ethanol-
precipitated processes were repeated several times for
a further purifying of the nickel ferrite nanocrystals.
Characterizations
The morphology, structure, and chemistry of the
nickel ferrite nanoparticles were analysed using a
number of methods, including high-resolution trans-
TM
mission electron microscope (TEM) (Tecnai G2 F30,
FEI) embedded with energy-dispersive X-Ray analy-
sis (EDX, Oxford Instrument), high angle annular dark
field (HAADF) and scanning transmission electron
microscopy (STEM), X-ray diffraction (XRD) instru-
ment using Cu Ka radiation (k = 1.5418 Å) (X’pert
powder, Philips), Fourier transform infrared (FTIR)
spectrometer (170SX, Nicolet) and inductively cou-
pled plasma emission spectrometer (ICP-ES) (IRIS
Intrepid ER/S, Thermo Elemental). The magnetic
properties of NiFe2O4 nanoparticles were measured by
a vibrating sample magnetometer (VSM) (Lake Shore
Page 3 of 9
7,304) at room temperature and superconducting
quantum interference device (SQUID) (MPMS-XL,
Quantum Design) magnetometer in the temperature
range from 10 to 300 K with an applied field of 100
Oe. Nanoparticles dispersed in hexane were dispersed
on holey carbon film coated Cu grids for TEM, SAED,
CBED and EDX analysis.
Results and discussion
Figure 1a shows a representative bright-field TEM
image of the NiFexOy nanoparticles dispersed on
holey carbon film coated Cu grids. A monodispersed
distribution of NiFexOy nanoparticles with spherical
shape can be seen, revealing non-agglomeration
between NiFexOy particles. The inset of Fig. 1a
indicates that the NiFexOy nanoparticles have a
uniform diameter, which was confirmed by all spec-
imens in this study. Figure 1c shows a histogram of
diameter distribution of 400 NiFexOy nanoparticles,
showing that their average diameter is approximately
9.5 nm with a 10% standard deviation. The histogram
can be fitted with a Gaussian distribution, indicating
that the NiFexOy nanoparticles are individually dis-
persed in the hexane solution.
HAADF-STEM has a much better spatial resolu-
tion than HRTEM because of an enhanced depth of
field, which is very useful to observe the spatial shape
of nanomaterials. Figure 1b shows a representative
HAADF-STEM image of the NiFexOy nanoparticles.
It is clear that the NiFexOy nanoparticles are virtually
monodispersed. Particle 1 shows distinct spinel
geometry, revealing a clear crystalline structure. A
number of NiFexOy nanoparticles show various
shapes, which is believed to derive from damage
due to the centrifugation process. Their diameters are
almost uniform. A statistical analysis of particle
diameters imaged by STEM was found to be in
agreement with the HRTEM statistical results of
approximately 9.5 nm. The contrast of incoherent
high-resolution HAADF-STEM images depends
directly on the atomic number, Z, and in the
nanoparticle images each NiFe2O4 nanoparticle shows
the expected uniform contrast, revealing a single
crystal structure.
The chemical composition of the NiFexOy nano-
particles was analyzed by energy-dispersive X-ray
spectroscopy (EDX) and inductively coupled plasma
123
Page 4 of 9
(a)
10 nm
(c)
Fig. 1 a A representative TEM bright-field image of NiFexOy
nanoparticles dispersed on a holy carbon film coated Cu
grids. b HAADF-STEM image of monodispersed NiFexOy
atomic emission spectroscopy (ICP-AES). Figure 1d
shows a representative EDX spectrum of the 9.5 nm
NiFexOy nanoparticles. EDX technique is not accurate
for analyzing oxygen element and the surfaces of
NiFexOy nanoparticles were covered by a thin layer of
organic surfactant of oleic acid which contains oxy-
gen, carbon, and hydrogen element, therefore, only the
atomic ratio of nickel and iron was simulated in this
spectrum to avoid error. Quantitative analysis of the
EDX spectra from the NiFexOy nanoparticles indicates
a 1:2 atomic ratio of Ni:Fe, inferring a NiFe2O4
composition for the nanoparticles prepared under
these experimental conditions. The Cu, Si, and C
peaks on the NiFe2O4 spectra came from carbon
coated copper grids and sample holder, which was
confirmed by EDX of an empty carbon coated copper
grid and sample holder.
123
J Nanopart Res (2012) 14:751
(b)
(d)
nanoparticles. c Histogram of the diameter distribution of 400
NiFexOy nanoparticles. d A typical EDX spectrum of the
NiFe2O4 nanoparticles
Further evidence for the bulk chemical composition
of NiFe2O4 nanoparticles is detected by ICP-AES
technique, displaying a 1:1.95 molar ratio of Ni and
Fe. This result is in full agreement with the earlier
nanoscale elemental analysis obtained by EDX. Both
results prove that this modified LSS-assisted hydro-
thermal method can be used to prepare a homogeneous
formation of NiFe2O4 phase.
Figure 2a shows an SAED pattern obtained from
numbers of NiFe2O4 nanoparticles as shown in the
top-right inset, revealing a face centered cubic (FCC)
structure. A further XRD spectrum of NiFe2O4
nanoparticles (Fig. 2b) confirms the above crystal
characterization. It shows that the 9.5 nm NiFe2O4
nanoparticles are an Fd3 m cubic spinel structure
(JCPDS 10-0325), of which peaks can be indexed by
(220), (311), (400), (422), (511), (440), (531), (620),
J Nanopart Res (2012) 14:751
(533) and (444) lattice planes. No diffraction peaks of
NiO or a-Fe2O3 are observed, revealing that the
sample is pure NiFe2O4. The broadening effect of each
peak reveals that the NiFe2O4 nanoparticles are small
crystalline structures. The average diameter of the
NiFe2O4 nanoparticles calculated using Scherrer’s
equation (Baykal et al. 2008) is in good agreement
with the above direct HRTEM observation, which
means that each particle is a single crystal.
The crystalline structure of individual NiFe2O4
nanoparticles was also characterised using high-reso-
lution TEM. High-resolution bright-field lattice imag-
ing of the individual NiFe2O4 nanoparticles is shown
in Fig. 2c, clearly indicating a single crystal. The
lattice distance corresponds to (220) serial planes.
Lattice-resolution HAADF-STEM image (Figure S1
(a)
(c)
d(220}=0.294 nm
Fig. 2 a SAED pattern obtained from numbers of NiFe2O4
nanoparticles. Inset is the selected NiFe2O4 nanoparticles for
this electron diffraction pattern. Scale bar is for 50 nm. b XRD
Page 5 of 9
in Supporting Information) double confirms that the
individual NiFe2O4 nanoparticles have a coherent
crystalline structure. The cloudy lattice-resolution
STEM image derives from a very quick carbon
accumulation (typically less than 5 s when using
STEM mode to scan the specimen). It is believed that
the carbon mainly decomposed from organics covered
on the surface of NiFe2O4 nanoparticles during the
electron beam scanning of the specimen. The carbon
accumulation is not as prominent when using STEM
on non-organic materials.
In order to analyze the crystal structure of a single
NiFe2O4 nanoparticle, CBED using a 0.5 nm spot size
configuration was adapted. The converged beam was
only incident on the analyzed particle. As an example,
Fig. 2d shows a CBED pattern of another single
(b)
(d)
131
202
131
spectrum of the NiFe2O4 nanoparticles. c HRTEM image of a
single particle. d CBED pattern of a single NiFe2O4 nanoparticle
123
Page 6 of 9
NiFe2O4 nanoparticle, revealing a single crystal spinel
structure with h101i orientation indexed by (131),
(202), ð131Þ; and so on.
NiFe2O4 nanoparticles can be individually dis-
persed in hexane to form a stabilized magnetic fluid.
Fourier transform infrared (FTIR) spectrum was
employed to investigate the intrinsic dispersion.
Figure 3 shows a typical FTIR spectrum of the
solution of NiFe2O4 nanoparticles dispersed in hex-
ane. The broad peak located at 3,402 cm-1 is associ-
ated with O–H vibrations. The sharp peaks at 2,920
and 2,850 cm-1 are attributed to the asymmetric and
symmetric stretching modes of the long CH2 chain of
oleic acid, respectively. The peaks at 1,535 and
1,406 cm-1 derived from the asymmetric and sym-
metric COO- chain separately. The 594 and 402 cm-1
peaks are associated with the stretching vibration of
metal–oxygen bonds in the tetrahedral and octahedral
sites individually. These peaks show that the surfac-
tant of oleic acid has been coated on the surface of
individual NiFe2O4 nanoparticles as expected, allow-
ing NiFe2O4 nanoparticles to be dispersed in non-polar
solvent without an agglomerating. This also accounts
for the carbon accumulation when the nanoparticles
were scanned by STEM as shown above.
The magnetic property of NiFe2O4 nanoparticles
were studied by VSM and SQUID. Figure 4 a shows
the magnetic hysteresis loops of the 9.5 nm NiFe2O4
nanoparticles measured at 10 and 300 K. There are no
coercivity and remanence observed in the NiFe2O4
nanoparticles at room temperature (300 K), reveal-
ing that the 9.5 nm NiFe2O4 nanoparticles are
Fig. 3 FTIR spectrum of the NiFe2O4 nanoparticles dispersed
in hexane
123
J Nanopart Res (2012) 14:751
superparamagnetic at room temperature. The satura-
tion magnetization (Ms) of the NiFe2O4 nanoparticles
was found to be 40 emu/g, which is smaller than that of
bulk nickel ferrite (55 emu/g) (Jiang and Yang 2007).
It is deduced that the decrease of Ms in 9.5 nm NiFe2O4
nanoparticles is mainly due to the spin-canting effect
on the surface of the small ferromagnetic particles
(Pankhurst and Pollard 1991) and the presence of a
magnetic dead or antiferromagnetic layer on the
surface caused by the reduced particle size (Bao et al.
2007). The coercivity of the NiFe2O4 nanoparticles is
84 Oe at 10 K as shown in the inset of Fig. 4a,
revealing that NiFe2O4 nanoparticles are ferromag-
netic at 10 K. The Ms of the 9.5 nm NiFe2O4
nanoparticles at 10 K is 48 emu/g, which is about
14% lower than that of bulk NiFe2O4. In order to
investigating the physical principle of the decrease of
Fig. 4 a Hysteresis loops of the NiFe2O4 nanoparticles
measured at 10 K and 300 K. Inset shows the 10 K and 300 K
hysteresis loops at low magnetic field range. b The ZFC and FC
curves of the NiFe2O4 nanoparticles measured at temperature
ranging from 10 K to 300 K and with an applied magnetic field
of 100 Oe from SQUID measurements
J Nanopart Res (2012) 14:751
Ms value, we take a simple treatment that there is a
uniform thickness of magnetic dead layer (t) on the
surface of individual NiFe2O4 nanoparticles. Using
the geometry of the measured NiFe2O4 nanoparticles,
the dead layer thickness (t) is calculated by the
following formula (Tahar et al. 2007):
 
6t
MS ¼ MS ð1Þ 1  ð1Þ
D
where D is the nanoparticle diameter measured by
TEM, Ms and Ms(?) correspond to the saturation
magnetization of nanoparticles and bulk at room
temperature respectively. The calculated thickness of
dead layer (t) is 0.45 nm. This shows that the magnetic
dead layer of 9.5 nm NiFe2O4 nanoparticles is very
thin. The volume ratio of the magnetically disordered
phase to the total phase can be then calculated to be
approximately 13.5%.
Figure 4b shows zero-field-cooled (ZFC) and field-
cooled (FC) curves of the NiFe2O4 nanoparticles
measured at temperature ranging from 10 K to 300 K
and with an applied magnetic field of 100 Oe from
SQUID measurements. The curves reveal a 80 K
blocking temperature (TB) where ZFC and FC curves
start to nearly overlap with each other, indicating the
9.5 nm NiFe2O4 nanoparticles become superparamag-
netic when the temperature is equal or higher than 80 K
(Beji et al. 2006). When the temperature is lower than
TB, the FC curve is almost flat, which is probably due to
the spin-glass effect (Bitoh et al. 1995). The distinction
between the FC and ZFC curve below TB is governed by
the energy barriers associated with magnetic anisotropy
of nanoparticles (Li et al. 2010b). Using the measured
TB value, the effective magnetic anisotropy constant Keff
of the 9.5 nm NiFe2O4 nanoparticles is calculated to be
6.2 9 105 erg/cm3 according to the formula Keff V ¼
25kB TB ; where kB is the Boltzmann constant and V is
the average volume of one particle determined from a
HRTEM image of the same NiFe2O4 nanoparticles.
This value is much larger than the bulk magnetocrys-
talline anisotropy (-7 9 104 erg/cm3). The enhance-
ment of Keff is believed to be mainly due to the surface
anisotropy as the particle size is reduced (Pérez et al.
2008; Thakur et al. 2008).
This hexane-dispersed NiFe2O4 solution can be
used as magnetic fluid. As an example, Figure S-2
(Supporting information) shows a typical solution of
9.5 nm NiFe2O4 nanoparticles dispersed in hexane
Page 7 of 9
contained in a centrifuge tube in. It can be seen that
this black solution is homogeneous and is stabilized
for more than half a year before aggregation. After a
permanent magnet was placed alongside, the 9.5 nm
NiFe2O4 hexane solution clearly climbed along the
wall of centrifuge tube.
Conclusion
In conclusion, we have demonstrated that virtually
monodispersed 9.5 nm NiFe2O4 nanoparticles can be
prepared by a modified LSS-assisted hydrothermal
route. A single NiFe2O4 nanoparticle has been inves-
tigated by a CBED technique for the first time, clearly
showing a single crystal with spinel structure. It is
shown that the chemical composition is consistent
with the expected NiFe2O4 formula. The surface of
each NiFe2O4 nanoparticle is successfully capped with
a surfactant of oleic acid, which causes individual
NiFe2O4 nanoparticles to be well dispersed in non-
polar solvent without a agglomerating. The investiga-
tion of magnetic properties reveals that NiFe2O4
nanoparticles behave superparamagnetic when the
temperature is equal or higher than 80 K. When the
temperature is greater than 80 K, the nanoparticles
become ferromagnetic. Its effective magnetic anisot-
ropy constant Keff is calculated to be 6.2 9 105 erg/
cm3. NiFe2O4 nanoparticles are expected to have
potential application in biomedicine and magnetic
fluid.
Acknowledgments This study was supported by the National
Basic Research Program of China (973 program) (Grant No.:
2012CB933104), the Natural Science Foundation of Gansu
Province of China (Grant No.: 1107RJZA221), the Fundamental
Research Funds for Central Universities from the Ministry of
Education of the People’s Republic of China (Grant No:
860521), and the National Natural Science Foundation of China
(Grant No: 11034004). We would like to thank Prof. Roger R
Ford, School of Computing, Science & Engineering, the
University of Salford, UK, for the correction of English.
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