Physica B 407 (2012) 2601–2605

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Physica B
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Spin-glass-like behavior of uncompensated surface spins in NiO

nanoparticulated powder
F.H. Aragón a, P.E.N. de Souza a, J.A.H. Coaquira a,n, P. Hidalgo b, D. Gouvêa c
a
Núcleo de Fı́sica Aplicada, Institute of Physics, University of Brası́lia, Brası́lia, DF 70910-900, Brazil
b
Faculdade Gama—FGA, University of Brası́lia, Sector Central Gama, DF 72405-610, Brazil
c
Department of Metallurgical and Materials Engineering, Escola Politécnica, Universidade de Sa~ o Paulo, Sao~ Paulo, SP 05508-900, Brazil

a r t i c l e i n f o abstract

Article history: Nickel oxide nanoparticles successfully synthesized by a polymer precursor method are studied in this
Received 27 February 2012 work. The analysis of X-ray powder diffraction data provides a mean crystallite size of 227 2 nm which
Accepted 2 April 2012 is in a good agreement with the mean size estimated from transmission electron microscopy images.
Available online 7 April 2012
Whereas the magnetization (M) vs. magnetic field (H) curve obtained at 5 K is consistent with a
Keywords: ferromagnetic component which coexists with an antiferromagnetic component, the presence of two
NiO nanoparticles peaks in the zero-field-cooled trace suggests the occurrence of two blocking process. The broad
Uncompensated surface spins maximum at high temperature was associated with the thermal relaxation of uncompensated spins at
Spin-glass like the particle core and the low temperature peak was assigned to the freeze of surface spins clusters.
Static and dynamic magnetic results suggest that the correlations of surface spins clusters show a spin-
glass-like behavior below Tg ¼ 7.3 7 0.1 K with critical exponents zn ¼ 9.7 7 0.5 and b ¼ 0.7 7 0.1, which
are consistent with typical values reported for spin-glass systems.
& 2012 Elsevier B.V. All rights reserved.

1. Introduction temperature at 523 K [8]. However, nanoparticulated NiO has been

The study of small particles has become of increasing interest
due to the new properties those materials show when the crystal
size is reduced. Those new properties provide nanomaterials with a
potential for technological applications such as magneto-recording
[1] and biomedicine [2]. Nanoparticulated systems show complex
properties due to the occurrence of structural disorder, size
distribution and random orientation of the magnetization vector [3].
Those complex properties are related to the interplay between finite
size and surface effects. Meanwhile, the finite size effects are related
to the reduced number of exchange coupled spins within the
particle core, the surface effects are related to the local symmetry
breaking of the lattice which drives to fluctuations in the number of
atomic neighbors and interatomic distances.
According to the Néel model, antiferromagnetic nanoparticles
show a net moment coming from uncompensated spins of the two
sublattices whose population is enhanced by the small particle size
and morphology [4–6]. Besides, in antiferromagnetic nanoparticles
such as nickel oxide (NiO), the surface effects are enhanced due to a
much lower core moment with respect to ferromagnetic nanoparti-
cles of the same size [7]. Bulk NiO has a rhombohedral structure
(space group, R3m) with antiferromagnetic ordering and Néel
n
Corresponding author.
E-mail addresses: coaquira.ja@gmail.com, coaquira@unb.br (J.A.H. Coaquira).
reported to show a cubic crystalline structure (space group, Fm3m)
[5,9]. Reports indicate that small NiO nanoparticles show magnetic
features, such as hysteresis below a blocking temperature, irreversi-
bility between the field cooled (FC) and zero field cooled (ZFC)
magnetization curves [3,10–12], large coercivities, field shifts of the
hysteresis loop [13], superparamagnetism, and spin-glass behavior
[5,14]. All of those anomalous properties are strongly particle size
dependent.
On the other hand, interparticle interactions represent an impor-
tant effect and need to be taken into account to understand the
observed magnetic properties [5]. Furthermore, interparticle interac-
tions constitute an additional contribution to the single particle
anisotropy energy and determine the relative orientation of the
particle moments. Reports indicate the occurrence of two blocking
temperatures in NiO nanoparticles. A high blocking temperature,
which was related to the response of uncompensated moments of the
particle core, and a lower blocking temperature (below  15 K),
which was associated with the magnetic behavior of surface spins,
which randomly freeze below their blocking temperature [15]. A
comparative study of the magnetic properties of polymer dispersed
and uncoated powder of 3 nm NiO nanoparticles indicates that
the interparticle interactions lead to an increase of the effective
anisotropy energy of the core moments, shifting their blocking
temperature to higher temperatures [5].
In this work we present a study on NiO nanoparticles carried
out by DC magnetization and AC susceptibility measurements.

0921-4526/$ - see front matter & 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.physb.2012.04.003
2602 F.H. Aragón et al. / Physica B 407 (2012) 2601–2605
The aim of this work is to characterize the static and dynamic
properties of the surface spins in the region of low temperatures
and determine spin-glass-like features of the NiO nanoparticu-
lated system.
2. Experimental details
NiO nanoparticles have been synthesized by a polymeric
precursor method. Ni(NO3)2  6H2O has been used as a cationic
precursor. Further preparation details are reported elsewhere
[16]. The crystal quality and average crystallite size were deter-
mined by X-ray powder diffraction (XRD) in a commercial
diffractometer (Bruker, D8 advanced) with the Cu Ka radiation
and using the Bragg–Brentano geometry. The mean particle size
and size distribution were determined by transmission electron
microscopy (TEM) (JEOL 1011 microscope with 100 keV electron
beam). The AC and DC magnetic measurements were performed
in a physical properties measurement system (PPMS) (quantum
design). Those measurements were carried out in a broad range of
temperatures (5–340 K) and magnetic fields up to 790 kOe. The
AC excitation field frequencies were in the range from 33 Hz to
9000 Hz.
3. Results and discussion
3.1. Structural characterization
The XRD pattern of the nickel oxide sample is shown in Fig. 1.
All Bragg reflections are consistent with the rhombohedral struc-
ture of NiO compound, which exclude the occurrence of extra
crystalline or amorphous phases in the sample. In order to obtain
further information such as crystallite size and residual strain, the
whole set of Bragg reflections were refined using the Rietveld
method. The peak shape was modeled using the Thompson–Cox–
Hastings pseudo-Voigt function (TCH-pV) given by [17]
TCH-pV ¼ ZLþ ð1ZÞG ð1Þ
where L and G are the Lorentzian and Gaussian peak function
respectively, and Z is the mixing parameter. The line broadening
related to the instrumental contribution was corrected by adequately
subtracting the linewidth (full width at half maximum) of a standard
sample (Si single crystal) from the linewidth of the sample. The
experimental linewidth represented by Eq. (1) is decomposed into
the Gaussian and Lorentzian peak contributions according to the
Fig. 1. Room temperature XDR patterns of the NiO nanoparticles, the size and
strain was obtaining by Rietveld refinement (Rexp and RWP are parameters which
represent the refinement quality). The observed and calculated data are repre-
sented by the points and solid line, respectively. The solid line at the bottom
represents the difference between the observed and calculated data.
relations: HG ¼ ðU tan2 y þ V tan y þ W þZ=cos2 yÞ1=2 and HL ¼ X tan y
þ Y=cos y, respectively [18].
Assuming that the final linewidth (H) is related to the crystal-
lite size and residual strain, the following relation can be used to
evaluate both parameters:
H cos y ¼ K l=/DS þ4e sin y ð2Þ
where /DS is the mean crystallite size, e is the residual strain and
K is a dimensionless factor that depends on the particle shape
(K 0.9 for spherical shape). Those parameters can be estimated
from the plot of H cos y as a function of sin y (Williamson–Hall
plot). The results obtained from the Rietveld refinement is
showed in Table 1. A value of /DS¼(2272) nm and e ¼0.07%
were obtained. The latter indicates that the residual strain is
small, but not negligible and must have originated at the interface
between the particle core and the surface layer where the
symmetry breaks and the broken chemical bonds modify the
local environment.
In order to corroborate the XRD results, TEM images were
carried out. Fig. 2 shows one of the TEM images obtained for the
NiO nanoparticles. The particle sizes of the TEM images were
counted using the ImageJ software. Several images were used to
obtain a total of N ¼483 particle sizes. Subsequently, a particle
size histogram was mounted using the Sturges method [19]. The
bin-width (W) is obtained from the relation: W¼(Dmax  Dmin)/k,
where k¼1 þ3.322 log(N).
In the inset of Fig. 2 is shown the obtained histogram. As
observed, this histogrampffiffiffiffiffiffi
is well modeled by a log-normal
2
distribution: f ðDÞ ¼ ð1=sD 2pÞexp½ln ðD=D0 Þ=2s2 . Here, D0 is
the median value and s is the size distribution dispersion. From
the fit a D0 ¼20.1 nm and s ¼0.36 are obtained from the fit. Those
values provide a mean particle size /DS ¼21.472.0 nm. Con-
sidering the uncertainties, the mean value determined from TEM
data is in good agreement with the mean crystallite size deter-
mined from the analysis of XRD data.
The polydispersion as well as the size are important factors
and determine the magnetic properties of the system, since the
surface to volume ratio increases as the nanoparticle size
decreases (surface/volume E4pr2/(4pr3) ¼1/r). As reported in
Table 1
Parameters obtained from the Rietveld refinement of the X-ray diffractogram of
NiO nanoparticles.
Mean size (nm) Strain (%) a¼ b¼ c (Å) Density (g/cm3) RExp =Rwp RBragg (%)
22 72 0.069 4.179 6.796 0.650 6.99
Fig. 2. TEM image of the NiO nanoparticles. In the inset is shown the histogram
mounted as described in the text and modeled by the log-normal function.
 F.H. Aragón et al. / Physica B 407 (2012) 2601–2605
the literature, the magnetization saturation in nanosized systems
is proportional to that ratio [20]. It is worth mentioning that the
1/r dependence was predicted for spherical particles, whereas real
particles have irregular shape which implies to have a relatively
different dependence in a real system.
3.2. DC magnetic properties
Fig. 3 shows the magnetization (M) of NiO nanoparticles as a
function of the magnetic field (H) obtained at T ¼5 K and 300 K.
The low temperature M vs. H curve shows a hysteretic behavior
with a coercive field HC ¼200 Oe, which seems to be consistent
with a ferromagnetic response. A non-zero coercive field is also
observed at 300 K, as inferred from the figure (see the bottom
inset in Fig. 3), and a much smaller magnetization signal. Similar
results were reported by Kodama et al. [21] for 32-nm size NiO
nanoparticles, although with larger coercive field (HC 410 kOe)
and opened loop up to 70 kOe. In the region of high magnetic
fields, the magnetization shows a linear behavior with a tendency
to saturation. A linear data fit to the relation M¼ wH in the
magnetic field range from 750 to 790 kOe provides an average
magnetic susceptibility w ¼ (1171)  10  6 emu/g Oe, which is
very near to the value 8.8  10  6 emu/g Oe reported for the
antiferromagnetic bulk system [22]. At T¼5 K, the magnetization
seems to be composed by a saturating contribution and a
contribution linearly dependent on the applied field in agreement
with the reports [5]. This data has been analyzed by using the
modified saturation magnetization law given by [23]
M ¼ M S ð1a=Hb=H2 Þ þ w1 H ð3Þ
where a is a parameter usually related to structural defects or
nonmagnetic inclusions, b is related to the magnetocrystalline aniso-
tropy and w1 represents the linear contribution. In sufficiently high
magnetic fields, the term related to a is negligible [24]. Using Eq. (3)
to fit the experimental data in the high field region provides an
MS ¼(0.4370.1) emu/g, b¼(3.370.3)  107 Oe2 and w1 ¼(1.007
0.01)  10-5 emu/g Oe. The saturation magnetization is assigned to
the ferromagnetic response of uncompensated spins and corresponds
to a fraction of 0.3% of the whole population of spins in a particle.
Assuming that the NiO nanoparticles have a cubic symmetry, the b
parameter is given by b ¼ 8K 2eff =105M 2s [23]. Using the latter relation,
an estimative of the effective anisotropy constant provides a
Keff ¼ (0.670.1)  105 erg/cm3. This Keff value is relatively smaller
than those reported values for NiO nanoparticles, although smaller
values are expected when the particle size is increased [7]. The w1
value representing the linear contribution is near to the value
obtained from the M vs. H curve at room temperature. This
contribution could represent the magnetic response of bigger NiO
nanoparticles which behave essentially as bulk antiferromagnets due
Fig. 3. Hysteresis loops obtained at 5 K and 300 K. The inset at the upper part
shows the M vs H at 300 K. The inset at the lower part shows the magnification of
the central of the M vs. H field at both temperatures.
2603
Fig. 4. Zero-field-cooled (ZFC) and field-cooled (FC) curves in the region of
temperatures below 25 K, where the ZFC curve shows a cusp at T  7 K. The inset
shows the ZFC and FC curves in the whole temperature range in which the
experiments were carried out. A broad maximum was determined for the ZFC
curve at T  160 K.
to their small surface to volume ratio, although no evidences of a
bimodal size distribution (just one peak is determined from the
histogram) has been determined from TEM images.
Fig. 4 shows the field-cooled (FC) and zero-field-cooled (ZFC)
magnetization curves as a functions of the temperature obtained
with a field of H¼100 Oe for the NiO nanoparticles. The ZFC curve
shows two maxima at high temperatures (see inset), a weak and
broad maximum centered at Tp  160 K and at low temperatures,
a cusp centered at T1 ¼7 K are determined. The FC curve shows an
irreversible behavior with respect to the ZFC below T1. Curiously,
the FC curve crosses the ZFC curve in the region of high
temperatures as can be inferred from the inset. The presence of
two maxima is in agreement with the works reported in the
literature for uncoated and polymer dispersed NiO nanoparticles
[5,7,25]. The high temperature maximum (Tp) has been com-
monly associated with the progressive blocking of uncompen-
sated magnetic moments of the particle core (whose population
depends on the particle size). Although there are reports suggest-
ing that the uncompensated core moments show a spin-glass
behavior [14], it is more generally accepted that the magnetiza-
tion response is satisfactorily explained by the superparamag-
netic behavior of the interacting particles [5,7].
However, as the temperature is decreased below the high-
temperature maximum, the uncompensated surface spins start to
correlate and those correlations become stronger enough to form
spin clusters. Those spin clusters induce strong interparticle
interactions due to the direct contact between the particles and
lead to a frustrated magnetic states as the temperature is
decreased [26]. Therefore, as reported in the literature [27], the
low temperature peak (T1) marks the transition to correlated
states of the surface spins clusters, which are randomly coupled
and a spin-glass behavior seems to be established.
3.3. Static magnetic properties
In order to understand the thermal dependence of the surface
spins clusters and determine the nature of the spin-glass behavior,
ZFC curves are obtained under several DC magnetic fields which are
shown in Fig. 5. As observed, the peak shows a shift towards lower
temperatures as the magnetic field is increased. The maximum
showed by the susceptibility could represent the blocking tempera-
ture of the collection of surface spins clusters. If the progressive
blocking of those entities were ruled by the superparamagnetic
phenomenon, the field dependence of the blocking temperature
(peak position) would be given by T 1 pVðHK HÞ2 , where V is the
volume of the spin cluster, HK is the anisotropic field and H is the
2604 F.H. Aragón et al. / Physica B 407 (2012) 2601–2605
Fig. 5. DC susceptibility vs. temperature curves obtained under several applied
field. The inset shows the peak temperature (T1) as a function of H2/3. The solid line
represents the linear fit.
Fig. 6. Plot of the in-phase component of the AC susceptibility as a function of the
temperature and at different field frequencies. The inset shows the log–log plot of
the critical slowing down law (Eq. (5)) and the line is the fit.
applied field [14,28]. It was experimentally determined that the
peak temperature shows a linear decrease with H2/3 as shown in the
inset of Fig. 5. This field dependence corresponds to the so-called de
Almeida–Thouless line (AT line) given by [29]
Hpð1T 1 =T g Þ3=2
This is a strong evidence which suggests that the thermal
freezing of the surface spins clusters is better described by a spin-
glass-like behavior rather than the superparamagnetism of inter-
acting particles and the transition temperature to the spin-glass
state (Tg) can be estimated by extrapolating the AT line to H¼0.
Several spin glasses [30] and low dimensional systems, such as
g-Fe2O3 nanoparticles [31] show that field dependence and it is
considered as a strong evidence for the existence of a spin-
glass phase.
3.4. Dynamic susceptibility measurements
Fig. 6 shows the real part (w0 ) of the AC susceptibility as a
function of the temperature obtained by applying an alternating
field at different frequencies (o). As can be observed each w0 vs. T
curve shows a cusp whose position shifts towards higher tem-
peratures as the field frequency increases. This indicates the
existence of thermal relaxations whose nature needs to be
determined. The dynamics of low-dimensional non-interacting
magnetic entities are usually described by the Arrhenius law:
t ¼ t0 exp ðEa =kB TÞ
where t ¼1/o is the relaxation time and t0 is a characteristic time
with usual values in the range 10  9 10  13 s, Ea is the energy
barrier which separates two low energy states. Considering the
susceptibility peak as the representative freezing temperature,
Tf(o), when tobs E1/o, and using Eq. (5) one can estimate the
values of Ea and t0 values. The plot of ln(o) vs. 1/Tf(o) shows
a linear tendency of experimental data and the fit provides an
Ea/kB ¼406 K and t0 ¼ 10  23 s. The latter value is physically
unacceptable and usually seen in spin-glass systems [19] and it
suggests that the low temperature peak of the susceptibility and
its frequency dependence could provide evidences for a spin-glass
behavior of surface spin clusters in NiO nanoparticles.
The existence of a true spin-glass phase transition implies that
the relaxation times of magnetic entities show a critical behavior
by approaching the transition temperature from above. The
description of this critical phenomenon is usually ruled by the
critical slowing down law given by [19]
t ¼ tn ½T f ðoÞ=T g 1zn ð6Þ
where z is the dynamic critical exponent, n is the critical exponent
describing the divergence of the correlation length (x), tn is a
microscopic relaxation time and Tg is the transition temperature.
The existence of a true phase transition can be tested using the
cusp position in the in-phase component of the AC susceptibility
data. A good linearity is obtained in the log–log plot as shown in
the inset of Fig. 6 and the linear fit provides a Tg ¼ 7.270.1 K and
zn ¼ 9.570.2. The latter value is consistent with those values
reported for canonical three-dimensional Ising and Heisenberg
spin glasses, for which zn ¼8  10 [32–35], strongly interacting g-
Fe2O3 nanoparticles [31], and NiO nanoparticles with a mean size
of 3 nm [5]. That spin-glass like transition is additionally corro-
borated by the criterion of the relative variation of Tf per
frequency decade, which provides a (DTf/Tf)/D log(o)  8  10  2.
This value is near to the one reported for (Eu,Sr)S spin-glass
insulator (  6  10  2) and larger than the values reported for
canonical spin glasses (  5  10  3) [36,37].
On the other hand, using linear response theory and the spin
auto-correlation function [38] it is possible to derive the full
dynamic scaling relation for the out-of-phase component of the
AC susceptibility given by [39]
w00 ðo,TÞ ¼ eb Gðoezn Þ ð7Þ
where b is the critical exponent defining how the order parameter
ð4Þ approaches zero (within the mean field theory, b ¼1) and (e ¼
T/Tg  1), is the reduced temperature. The asymptotic behavior of
G(x) for large values of x is given by GðxÞpxb=zn .
Using the out-of-phase susceptibility data shown in Fig. 7a, the
dynamic scaling analysis according to Eq. (7) results in a best data
collapse for zv ¼9.770.5, Tg ¼ 7.370.1 K and b ¼0.7 70.1
(Fig. 7b). The zn value is in agreement with that obtained in the
previous analysis. The value of b is in good agreement with
typical values of b ¼0.5–0.8 reported for three-dimensional Ising
and Heisenberg spin glasses [34,38,40–42], but slightly smaller
than those found for dipolar spin glasses [39]. Moreover, the value
of b/zn E0.07, extracted from the asymptotic behavior of the
scaling function G(x) for large x is consistent with the derived
values of b and zn. Although additional studies are needed, all of
the evidences of a spin-glass-like behavior determined in this
work must be related to the thermal freezing of surface spin
clusters which shows critical character near to the spin-glass like
phase transition. Although those evidences indicate a spin-glass-
like behavior, measurements using other techniques are needed
to confirm the relation between the spin-glass behavior and the
dynamics of the uncompensated surface spins in this nanoparti-
culated system.
ð5Þ
4. Conclusions
NiO nanoparticles synthesized by a polymer precursor method
show a rhombohedral structure and particle size of  22 nm. The
 F.H. Aragón et al. / Physica B 407 (2012) 2601–2605
Fig. 7. (a) Plot of the out-of-phase component of the AC susceptibility as a
function of the temperature at different field frequencies. (b) The scaling data plot
according to Eq. (6).
magnetic features of the NiO nanoparticles are compatible with
the presence of an antiferromagnetically ordered particle core and
disordered spins clusters at the particle surface. DC and AC
magnetic susceptibility data analysis support the critical slowing
down phenomenon and the glassy nature of the surface spin
correlations. The dynamic critical exponent (zn ¼9.5), the relative
variation of the transition temperature per frequency decade
(  8  10  2), the observation of the AT line, as well as the
dynamic scaling of the out-of-phase component of the AC sus-
ceptibility indicate a true transition to a spin-glass state at
Tg  7 K.
Acknowledgments
This work was financially supported by the Brazilian agencies
CNPq, CAPES and FAP/DF.
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