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Unusual metallic behavior in nanostructured cobalt ferrite at
superparamagnetic regime
R. Kannan, S. Rajagopan, A. Arunkumar, D. Vanidha, and R. Murugaraj
Citation: J. Appl. Phys. 112, 063926 (2012); doi: 10.1063/1.4754855

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JOURNAL OF APPLIED PHYSICS 112, 063926 (2012)
Unusual metallic behavior in nanostructured cobalt ferrite

at superparamagnetic regime
R. Kannan,1,a) S. Rajagopan,2 A. Arunkumar,1 D. Vanidha,1 and R. Murugaraj3
1
Department of Physics, Pondicherry Engineering College, Puducherry 605 014, India
2
Department of Chemistry, Pondicherry Engineering College, Puducherry 605 014, India
3
Department of Physics, MIT Campus, Anna University, Chennai 600 044, India
(Received 12 January 2012; accepted 29 August 2012; published online 28 September 2012)
Cobalt ferrite nanoparticles have been synthesized by coprecipitation method by varying the
precipitation temperatures. The samples have been characterized by x-ray diffraction, impedance
analysis, ac conductivity, dielectric, and vibrating sample magnetometer. When the average
crystallite size is in the range of 2–16 nm, these compounds behave as metallic, and upon thermal
activation, they become semiconducting, indicating anomalous conducting behavior. Impedance
analysis reveals a metallic to semiconducting phase transition, accompanied by grain boundary
effect, gradually replaced by grain contribution. Ac conductivity measurements and dielectric
analysis also confirmed the transformation, when the slope changed from positive to negative as a
function of temperature. Particle size independent magnetic behavior was observed in finite size limit
C 2012 American
due to site exchange of cations between tetrahedral (A) and octahedral (B) sites. V
Institute of Physics. [http://dx.doi.org/10.1063/1.4754855]
INTRODUCTION Variations in the synthesis technique with varying pH

content have been studied by various authors.3,8,9 In this
Nanosized cobalt ferrite is highly preferred in bio-
report, stoichiometrically controlled pH was used for prepara-
medical applications due to thermal stability and high satura-
tion of optimized and reproducible cobalt ferrite. When the
tion magnetization. The most common problem found in
particle size reached the lower size limit of 2 nm, grain bound-
nanoferrite is agglomeration leading to the formation of
ary conduction has been found to change to grain conduction
grains and grain boundaries. The presence of excess alkaline
with increase of temperature. Simultaneously, a metallic to
base, unreacted metal chlorides, if any and adsorbed water
semiconducting transition took place at around 453 K and
content complicates the nucleation and growth process.1
403 K for samples sintered at 350 C and 600 C, respectively.
Several outcomes on the correlation behavior between parti-
cle size and conductivity, through grain and grain boundaries EXPERIMENTAL
of nanoparticles of different ferrites, are available.2–5 The
physio-chemical properties of ferrite in nanosize are CoFe2O4 ferrite was prepared by conventional co-
expected to be strongly dependent on synthesis condition precipitation technique using AR grade of anhydrous FeCl3
and subsequently on the particle size. (Qualigens), CoCl2 (Merck), and NaOH (Rankem) of high pu-
Few reports are available on the effect of precipitation rity in stoichiometric proportion. Metal chlorides were dis-
temperature on the formation of cobalt ferrite. However, par- solved separately in double distilled water and added to the
ticle behavior at finite size has not yet been studied in detail. NaOH solution at room temperature (RT) dropwise, following
Cation-cation (c-c) and cation-anion-cation (c-a-c) interac- the sequence of FeCl3 and CoCl2 under constant stirring until
tions at B-site are responsible for electrical and magnetic a brown precipitate was obtained. It was filtered and washed
properties of ferrite. Further magnetic exchange interactions with distilled water followed by acetone and dried in air. The
are controlled by the distance between the A and B cations. dried sample was ground, pelletized, and sintered at two dif-
When the separation between the nanoparticles goes below a ferent temperatures namely 350 C and 600 C. The experi-
certain limit, quantum mechanical interactions dominate ment was repeated for 60 C and 90 C of NaOH solution.
over long range interaction giving rise to anomaly at finite All the prepared samples were characterized by PXRD
size.6 Normally, nanocobalt ferrite exhibit semiconducting using XPERT-PRO x-ray diffractometer. AC conductivity
behavior in the temperatures up to 650 K.7 Atta ur Rahman and dielectric measurements were carried out using HP
et al.3 observed a semiconducting to metallic transition for a 4284A LCR meter (USA Make) in the frequency range
particle size of 10 nm. Grain and grain boundary contributed 20 Hz to 1 MHz. Room temperature magnetization was
conductivity changes to grain conduction around 340 K. measured using vibrating sample magnetometer (VSM).
Hence it is clear that the particle size and as a consequence
the volume ratio of grain boundary to grain decide, the na- RESULTS AND DISCUSSION
ture of conductivity in nanoferrite. X-ray diffraction
a)
Author to whom correspondence should be addressed. Electronic mail: The powder x-ray diffraction (XRD) patterns of copreci-
[email protected]. Tel.: þ 91 9442787484. Fax: þ91 413 2655101. pitated CoFe2O4 sintered at 350 C and 600 C shown in
0021-8979/2012/112(6)/063926/8/$30.00 112, 063926-1 C 2012 American Institute of Physics

V
063926-2 Kannan et al. J. Appl. Phys. 112, 063926 (2012)
FIG. 1. XRD pattern of cobalt ferrite for the

samples RT, 60 C, and 90 C (a) sintered at
350 C and (b) sintered at 600 C.
Figs. 1(a) and 1(b) confirm the nanocrystalline nature and tivity comes from grain boundaries because the grain bound-
single-phase formation. The intensity of XRD peaks has been ary volume is very large due to smaller particle size.2 Higher
found to increase as the sintering temperature increased, indi- resistance (Rgb ¼ grain boundary resistance) values obtained
cating the crystallinity has significantly improved with higher from the diameter of the semicircle also indicate that the con-
sintering temperature. Peak broadening of (311) was used to ductivity is due to grain boundaries instead of grains.15–17
estimate the average size of the crystallite using Scherrer’s Semicircle behavior as a function of temperature with differ-
formula.10 The particle size and lattice parameters of CoFe2O4 ent shapes is attributed to structural inhomogeneities origi-
are shown in Table I. From the calculated value, it was found nating from grain and grain boundaries present in the
that the particle size has been found to increase upon increas- samples.3,5 It has been found that the semicircle plots show a
ing the sintering temperature,11 and the lattice parameter of gradual change into an arc-like behavior indicating crossover
spinel cubic was found to be “a” ¼ 7.63 Å instead of the from grain boundary to grain conduction and subsequently
reported value (“a” ¼ 8.34 Å). Ayyub et al.12–14 elaborately straight line nature is observed which is indicative of elec-
discussed the size effect on various structural and thermody- trode effect.
namic parameters like lattice parameter, unit cell volume Rgb is found to increase with increase in temperature as
(UCV), and temperature. The anisotropic variation of lattice shown in Figs. 3(a) and 3(b), reaching a maximum and then
constant with particle size is attributed to the different long decreases indicating that the system has undergone metallic
range and short range molecular forces to realize phases with to semiconducting transition accompanied by the transforma-
physical properties (e.g., lattice parameter) that are in tune tion from grain boundary conduction to grain conduction.
with the size effect. This transition occurs at 403 K, 403 K, and 453 K for 350 C
sintered samples and at 353 K, 403 K, and 353 K for 600 C
sintered samples, respectively for RT, 60 C and 90 C. The
Impedance analysis
variation in phase transition temperature for different sam-
Impedance measurements have been carried out for all ples is attributed to size effect.12
the samples at selected temperatures in the frequency range The activation energy (Ea) is obtained, by fitting the dc
20 Hz to 1 MHz and the Nyquist plots corresponding to the conductivity data of the Rgb values, using Arrhenius relation
sample RT of 350 C and 600 C sintered are shown in Figs. r ¼ r0 exp(Ea/kBT), where r0 is pre-exponential factor
2(a) and 2(b). In the present study, only one semi-circle was with dimension of (Xcm)1 and kB is the Boltzmann con-
obtained, suggesting that the main contribution for conduc- stant.18 It is found that the slope changes from a positive to
TABLE I. Particle size, lattice parameter (a), saturation magnetization (Ms), and coercivity (Hc) of cobalt ferrite.
Sample Sintering temperature ( C) Particle size D (nm) Lattice parameter (a) Å Saturation magnetization Ms (emu/g) Coercivity Hc (G)
RT 350 2.0 7.66 12.71 382.7

600 16.2 7.57 74.36 1617.7
60 350 3.5 7.46 14.61 662.9
600 8.4 7.60 55.05 1232.8
90 350 2.0 7.39 21.09 466.9
600 7.9 7.60 59.00 1303.6
FIG. 2. Nyquist plots of cobalt ferrite of RT sample (a) sintered at 350 C and (b) sintered at 600 C.
negative value with increase in temperature [Figs. 4(a) and (Fe-Fe) interaction dominates, the conduction become metal-
4(b)], indicating metallic to semiconducting transition. lic and when c-a-c(Fe-o-Fe/Co-o-Co) is dominant, it become
It is known that conduction in ferrite takes place by tem- semiconducting.19 In the superparamagnetic regime, some of
perature dependent hopping mechanism. In an inverse spinel, the Co atoms from B-site occupy A-site equally replacing Fe
all cobalt atoms occupy B-site and Fe is equally shared atoms from A-site to B thus making cation-cation (c-c) inter-
between tetrahedral (A) and the octahedral (B) sites, i.e., actions more predominant leading to metallic behavior with
(Fe)[FeCo]O4 under normal conditions. The interaction positive slope at low temperature.20 When temperature
between the cations (c-c), and the cations and anion (c-a-c) increases, the slope becomes negative indicating cation-
at B-site decides the nature of conductivity. When c-c anion-cation (c-a-c) interaction is dominant over c-c
FIG. 3. Variation of Rgb with temperature

for the samples RT, 60 C, and 90 C (a)
sintered at 350 C and (b) sintered at
600 C.
AC conductivity analysis
The variations of ac conductivity as a function of fre-
quency is measured for all the samples at different tempera-
tures, out of which RT of 350 C and 600 C sintered sample
is shown in Figs. 5(a) and 5(b). The conductivity almost
remains the same at low frequency and increases strongly at
high frequency exhibiting dispersion. The straight-line por-
tion of dc conductivity tends to be short in metallic regime
and increases in the semiconducting state with increase of
temperature. The dc to ac changeover takes place in the fre-
quency range of 105 Hz to 106 Hz and for certain tempera-
tures greater than 453 K, which shows near constant loss
(NCL) behavior.3,5,22
The ac conductivity of the system can be explained on
the basis of the expression21
rac ¼ r1 ðTÞ þ r2 ðx; TÞ;
where r1(T) is due to band conduction and is related to dc

conductivity which is temperature dependent. r2(x, T) is
due to hopping conduction which occurs among the octahe-
dral B-sites and it is both temperature and frequency depend-
ent.21 Temperature dependent hopping is represented by the
Arrhenius equation r1(T) ¼ r0 exp (Ea/kBT), where Ea is
the activation energy and r0 is pre-exponential factor. Acti-
vation energy was calculated from ln r1 T versus 1000/T
plot, where the slope changes from positive to negative as
shown in Figs. 6(a) and 6(b).
FIG. 4. Calculation of activation energy from ln r(Scm1) vs 1000/T for the
samples RT, 60 C, and 90 C (a) sintered at 350 C and (b) sintered at The occupation index of A and B-sites strongly depends
600 C. on the synthesis conditions, like particle size, temperature
and pressure. The transition between Fe2þ $ Fe3þ or Co2þ
$ Co3þ ions might be responsible for conduction in ferrite
interactions leading to semiconducting behavior. A similar due to hopping of charge carriers between adjacent octahe-
transition is reported by Ata-Allah et al. in copper doped dral sites (B).17,21 Non-equilibrium site occupancy is one of
nickel ferrite.21 This finding is commensurate with the fact the common characteristics of nanostructured materials.23
that unambiguous metallicity is always accompanied by c–c Atta ur Rahman et al.3 have reported semiconducting behav-
interactions which are enabled by migration of atoms ior for cobalt ferrite and Younas et al.18 have reiterated the
between A and B sites. same for nickel ferrite. Upon thermal activation, the system
FIG. 5. Variation of ac conductivity with fre-

quency for the sample RT (a) sintered at 350 C
and (b) sintered at 600 C.
FIG. 6. Calculation of activation energy from ac conductivity (ln r1T

(Scm1 K) vs 1000/T) for the samples RT, 60 C, and 90 C (a) sintered at
underwent metallic phase transition indicating domination of FIG. 7. Variation of “n” with temperature for the samples RT, 60 C, and
90 C (a) sintered at 350 C and (b) sintered at 600 C.
c-c interactions.
We found that cobalt ferrite in the superparamagnetic
regime underwent a transition from metallic to semiconduct- 353 K, 403 K, and 353 K for 600 C sintered samples, respec-
ing state with increase in temperature. Unusual behavior of tively for RT, 60 C, and 90 C indicating similar transition
metallicity in low temperature is due to strong (c-c) and temperature dependence as reported earlier.
weak (c-a-c) interaction at B-site,19 which is attributed to
reverse cation migration due to size effect. Hence, experi- Dielectric studies
mentally observed positive slope is attributed to metallicity
and negative slope to semiconducting state. The phase transi- The effect of frequency on the dielectric constant (e0 ) of
tion due to thermally activated process was found to be in the sample 60 C of CoFe2O4 sintered at 350 C and 600 C is
agreement with impedance analysis. illustrated in Figs. 8(a) and 8(b). The dispersion of dielectric
Frequency dependent ac conductivity is given by constant is found to decrease at lower frequencies and remains
Jonscher’s universal conduction mechanism24 constant at higher frequencies. It is due to the fact that beyond
a certain frequency of ac electric field, the electron exchange
r2 ðx; TÞ ¼ BðTÞxn ðTÞ cannot follow the alternating field giving rise to relaxation
mechanism.25–29 The variation of dielectric constant e0 with
where “n” is the dimensionless parameter obtained from the temperature, for a selected frequency value (102, 103, 104,
slope of log (rac) versus log (x) graph. The frequency de- 105 Hz), is depicted in Figs. 9(a) and 9(b) for the sample of
pendent hopping conduction is further divided and analyzed 60 C sintered at 350 C and 600 C. The increase of e0 with
based on the variation of “n” as a function of temperature. temperature shows normal behavior of semiconducting fer-
Four different models9 were proposed namely, (i) quantum rites.30 However, in our system, the dielectric constant has
mechanical tunneling if “n” is independent of temperature, been found to decrease anomalously and then showed an
(ii) small polaron hopping (SPH) conduction when “n” increase with increase in temperature. The changeover was
increases with temperature, (iii) correlated barrier hopping observed at the same temperature and the anomalous change
(CBH)18 occurs with a decrease in “n” for increase in tem- in the dielectric constant can be explained by the similar
perature and (iv) overlapping large polaron tunneling mechanism of migration of Fe ions from A-site to B20 as that
(OLPT)3,9,18 takes place, if the “n” value decreases and then in the case of impedance and ac conductivity analysis.
increases for increasing temperature. Dielectric constant (e0 vs Temperature), impedance anal-
With increase in temperature, the value of “n” increases ysis (Rgb vs Temperature) and AC conductivity (“n” vs Tem-
and then decreases, thereby indicating SPH followed by perature) studies confirm that the phase transition can be
CBH as shown in Figs. 7(a) and 7(b). In support of our argu- attributed to the (c-c) interactions enabled by cation migra-
ment, a similar trend was reported by Farea et al.17,18 The tion between A and B sites due to size effect.
transition from SPH to CBH occurs at temperatures of The activation energy of dielectric relaxation process
403 K, 403 K, and 453 K for 350 C sintered samples and at was calculated from electrical modulus (M00 versus log (f))30
FIG. 8. Variation of dielectric constant (e0 ) with

frequency for the sample 60 C (a) sintered at
by linearizing the equation, xp ¼ x0 exp(EP/kBT) as shown 2 nm to 4 nm, Ms increases from 12.7 emu/g to 14.6 emu/g.
in the Figs. 10(a) and 10(b). The similarity in the change of However for the particles (2.09 nm) synthesized at 90 C,
slope in the activation energy graph for electrical conduction Ms again increases to 21.1 emu/g instead of decreasing,
(ac and dc) and dielectric polarization further ascertained the indicating non-equilibrium site occupancy.23,35 The abnor-
phase transition which occurs at the same temperature. mality is explained by the same mechanism of migration of
Co ions from B-site to A as discussed earlier. We observed
similar trend for 600 C sintered samples. Improved crys-
Magnetization studies
tallinity and increase in the volume fraction are responsible
Figs. 11(a) and 11(b) show the M-H curve for the nano- for high saturation magnetization of 74.4 emu/g
cobalt ferrite samples and the magnetic behavior of ferrite is for16.21 nm. Ms has been found to decrease to 55.1 emu/g
explained based on the particle size and coercivity.31–34 As when the particle size is decreased to half the size. Even a
discussed earlier in the cobalt inverse spinel, magnetization minor decrease in particle size (8.46 nm to 7.97 nm) gives
contribution arises from cobalt ion only, which occupies the rise to anomalous increase in Ms 59.0 emu/g as tabulated in
B-site, whereas magnetic moments of the Fe ions occupying Table I. This inconsistency is explained based on the same
A and B-site will cancel each other as their spins point in op- concept of non-equilibrium site occupancy commonly
posite directions. found in nanostructured materials. Thus, magnetization
Saturation magnetization (Ms) is found to be a func- studies independently confirm the migration of cations
tion of particle size in the superparamagnetic limit for between A and B-sites due to size effect apart from electri-
350 C sintered samples. When the particle size lies within cal studies.
FIG. 9. Temperature dependence of e0 at vari-

ous frequencies for the sample 60 C (a) sin-
tered at 350 C and (b) sintered at 600 C.
indicative that the particles are in the superparamagnetic re-

gime with single domain nature, since particle size and coer-
civity increase with temperature.
CONCLUSIONS
Co-precipitated cobalt ferrite at the lower boundary limit
(2–16 nm) is found to undergo anomalous metallic to semi-
conducting transition accompanied by grain boundary to grain
conduction. Our argument is supported by dc and ac conduc-
tivity and dielectric analysis in which variations in Rgb, “n”,
and e0 as a function of temperature ascertain the phase transi-
tion. Similar transition is also verified from the activation
energy graph where the slope changes from positive to nega-
tive for all the electrical characterization. Moreover, the
change in slope confirms metallic nature which arises due to
c-c interactions and to enable c-c interaction, migration of Co
ions from B-site to A is an essential condition. Independently
magnetization studies reveal non-equilibrium site occupancy
due to finite size effect. As a function of particle size, it could
be possible to switch between the conductivities for applica-
tions in the medical field of hyperthermia.
FIG. 10. Calculation of activation from ln xp(radian) vs 1/T for the samples
RT, 60 C, and 90 C (a) sintered at 350 C and (b) sintered at 600 C.
ACKNOWLEDGMENTS
Magnetic coercivity (Hc) was found to be a function of
This work has been supported by the grant in aid of
particle size (RT, 60 C, 90 C) and sintering temperature as
AICTE-RPS project of R. Kannan, of Department of
shown in Table I. Coercivity increases with sintering temper-
Physics, Pondicherry Engineering College, Pondicherry,
ature indicating that the particles are below the critical size
India. We thank Alagappa University, Karaikudi for provid-
having single-domain.31–34 Normally, enhancement of coer-
ing PXRD data and SAIF, IIT Madras for VSM data.
civity is associated with increase in the crystallite size within
the single-domain range as a function of temperature. Further 1
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Unusual metallic behavior in nanostructured cobalt ferrite at

Citation: J. Appl. Phys. 112, 063926 (2012); doi: 10.1063/1.4754855

Additional information on J. Appl. Phys.

Unusual metallic behavior in nanostructured cobalt ferrite

INTRODUCTION Variations in the synthesis technique with varying pH

0021-8979/2012/112(6)/063926/8/$30.00 112, 063926-1 C 2012 American Institute of Physics

FIG. 1. XRD pattern of cobalt ferrite for the

RT 350 2.0 7.66 12.71 382.7

FIG. 3. Variation of Rgb with temperature

rac ¼ r1 ðTÞ þ r2 ðx; TÞ;

where r1(T) is due to band conduction and is related to dc

FIG. 5. Variation of ac conductivity with fre-

FIG. 6. Calculation of activation energy from ac conductivity (ln r1T

FIG. 8. Variation of dielectric constant (e0 ) with

FIG. 9. Temperature dependence of e0 at vari-

indicative that the particles are in the superparamagnetic re-

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