ARTICLE IN PRESS

Journal of Magnetism and Magnetic Materials 321 (2009) 12801284

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Journal of Magnetism and Magnetic Materials

journal homepage: www.elsevier.com/locate/jmmm

Superparamagnetic properties of La1xBaxCoO3 (0.0oxo0.18)

Wanju Luo , Fangwei Wang
State Key Laboratory of Magnetism, Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, P.O. Box 603, Beijing 100190, China

a r t i c l e in f o

a b s t r a c t

Article history:
Received 20 May 2008
Available online 30 November 2008

The static and dynamic magnetic properties of La1xBaxCoO3 (0oxo0.18) (LBCO) have been investigated
by the dc and ac susceptibility measurements systematically. The spin-glass-like characteristics of
magnetic behavior, which are always considered as an evidence of spin glasses for La1xSrxCoO3
(0oxo0.18) (LSCO), have been observed. However, just like that of LSCO, some magnetic behaviors,
which are different from the canonical spin-glass characteristics, for example, the difference far above
peak temperature Tp of zero-eld-cooled curve between eld-cooled magnetization (FCM) and zeroFCM (ZFCM) and the very broad peaks in the samples for x40.10, are also observed simultaneously.
Based on the comparisons with canonical spin-glass Au96Fe4 alloy and conventional superparamagnetic
(SPM) Cu97Co3 alloy, the nature of the magnetic behaviors in LBCO is ascribed to the superparamagnetic
cluster rather than spin glass. Though the magnetic properties behave as SPM, LBCO has one critical
point different from that of the conventional SPM Cu97Co3 alloy. The segregated Co nanoparticles in the
Cu97Co3 alloy are isolated by nonmagnetic background while the clusters in LBCO are embedded in an
antiferromagnetic matrix. The SPM behavior of LBCO can only exist at low temperature because the
antiferromagnetic matrix transfers to paramagnetic phase at Neel temperature TN and the SPM cluster
turns into ferromagnetic (FM) above TN.
& 2008 Elsevier B.V. All rights reserved.

Keywords:
Superparamagnetic
Spin glass
ac Susceptibility
Perovskite cobaltite

1. Introduction
The system of perovskite cobaltites oxides is very interesting
not only for the spin-state transition [13] and metalinsulator
transition [46] but also for the spin-glass-like behavior [79].
The pioneering studies on the magnetic behavior of La1xSrxCoO3
reveal that there is a transition from spin glass to cluster glass at
the magnetic percolation threshold x 0.18 [57]. For the cluster
glass region (xX0.18), the coexistence of ferromagnetic and glassy
behavior was conrmed [8]. For example, the dc magnetization of
La0.5Sr0.5CoO3 shows a Brillouin-like temperature dependence
below TC and the magnetization is time dependent at low
temperature. The samples in the range 0.0oxo0.18 were
considered as spin glasses for the cusp at the spin-glass freezing
temperature Tg in zero-eld-cooled magnetization (ZFCM) curves
and the aging behavior from long-time relaxation below Tg [57].
These magnetic behaviors could be interpreted in spin-glass
mechanism successfully but some other behaviors are far different
from the canonical spin glass such as the difference far above the
peak temperature (Tp) between eld-cooled magnetization (FCM)
and zero-FCM (ZFCM) and the very broad peaks in the samples for
x40.10. Indeed, other studies [10,11] on the spin-glass system of

 Corresponding author. Tel.:+86 1082648078.

E-mail address: wanjuluo@msn.com (W. Luo).

0304-8853/$ - see front matter & 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmmm.2008.11.045

La1xSrxCoO3 (0.0oxo0.18) (LSCO) revealed that there is no true

spin glass in the samples for x40.08, although glassy dynamics
is observed.
It is well known that the magnetic characteristics, such as
susceptibility maximum, irreversibility between FC and ZFC
magnetization, and time-dependent magnetization, exist in both
spin glass and superparamagnetic (SPM) materials [1215].
Previous works [16,17] on the comparison between the canonical
spin-glass Au96Fe4 and the conventional superparamagnetic
Cu97Co3 revealed the differences of magnetic behaviors between
the two systems in detail. The difference between FCM and ZFCM
of Cu97Co3 exists far above Tp, while that of Au96Fe4 exists only
below Tg. The FCM of Cu97Co3 increases monotonically with
decreasing temperature, but FCM below Tg in Au96Fe4 is nearly
temperature independent. With increasing the magnetic eld,
ZFCM/H and FCM/H of Cu97Co3 decrease and Tp shifts to lower
temperature considerably. On the other hand, ZFCM/H of Au96Fe4
slightly decreases only near Tg. For the temperature dependence of
linear and nonlinear susceptibilities, the positive peak of the
linear part and the negative peak of the nonlinear part for Cu97Co3
are very broad, while they are very sharp in the case of Au96Fe4.
Comparing the reported magnetic behaviors of previous
studies [7,911] on LSCO in the spin-glass region with those of
Cu97Co3 and Au96Fe4 [1619], it is found that the magnetic
features in the system of LSCO are very similar to that of Cu97Co3
rather than those of Au96Fe4. Therefore, it is reasonable to believe

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that the light-doped perovskite cobaltites should be superparamagnetic cluster rather than spin glass. For this reason, the
nature of the magnetic properties in the system of divalent ionsdoped perovskite cobaltite is denitely worthwhile to be claried.
Ba2+ has larger ionic radius [20] and it can introduce holes into
CoO bonds as Sr2+ or Ca2+ does. Unfortunately, however, there are
only a few studies [2124] about La1xBaxCoO3 and most of them
are focused on the transport properties. In the present work, the
magnetic properties of La1xBaxCoO3 (0.0oxo0.18) are investigated in detail. The static and dynamic properties have been
discussed based on the dc magnetization and ac susceptibility
measurements.

2. Experiments
Polycrystalline samples of La1xBaxCoO3 (LBCO) in the range
of 0.0oxo0.18 were fabricated from La2O3, BaCO3 and Co3O4
starting materials by the standard solid-state reaction method
and X-ray powder diffraction conrmed that the samples were in
high purity [25]. dc Magnetization as a function of temperature
and external magnetic eld was derived using a SQUID magnetometer (Quantum Design MPMS-7). These temperature-dependent data were taken on heating under an external eld of 100 Oe
after cooling in the zero-magnetic eld or in a eld of 100 Oe. ac
Susceptibilities at different frequencies in the range from 33 to
9999 Hz were taken in a commercial device physical properties
measurement system (PPMS).

3. Experimental results and discussion

3.1. dc Magnetization
Figs. 1 and 2 show the temperature dependence of FCM/H (M/H
in a eld-cooled process) and ZFCM/H (M/H in a zero-eld-cooled
process) measured at H 100 Oe for x 0.03 and 0.12, respectively. Obviously, the ZFC curve in Fig. 1 shows a sharp peak at
about 10 K while the FC magnetization increases with decreasing
temperature in the whole measured temperature range. These
characteristic features had also been observed in La0.95Sr0.05CoO3
and had been ascribed to the spin glass [9]. The canonical spin
glass [13,15] exhibits a cusp in ZFC magnetization curve near
freezing temperature (Tf) indeed. However, the FC curve of
canonical spin glass is temperature independent below Tf, which
is contrary to that of the perovskite cobaltites. In addition, the
bifurcation between ZFC and FC curves is just below Tf in

Fig. 1. Temperature dependence of the FC and the ZFC susceptibility (M/H) for
x 0.03 measured at H 100 Oe. ZFC data are shown as open symbols, whereas
FC data are shown as solid symbols. Inset shows the inverse of ZFC susceptibility,
and the solid line represents a t to the CurieWeiss law.

Fig. 2. Temperature dependence of FC and ZFC susceptibility (M/H) for x 0.12

measured at H 100 Oe. Inset shows the inverse of ZFC susceptibility, and the
solid line represents a t to the CurieWeiss law above TC.

canonical spin glass while it is far above Tf in perovskite cobaltites

as shown in the gure. Moreover, for canonical spin glasses, the
paramagnetic Curie temperature yp, extrapolated from susceptibility data taken well above Tf, is close to zero [13]. On the
contrary, the paramagnetic Curie temperature yp is far below zero
for La0.97Ba0.03CoO3 and La0.88Ba0.12CoO3 as indicated in the insets
of Fig. 1 and Fig. 2.
Based on the above characteristics analysis it is obviously
inaccurate to ascribe the nature of magnetic behavior in
perovskite cobaltites to spin glasses. On the other hand, these
magnetic behaviors in La0.97Ba0.03CoO3 are analogical to the
typical characteristics in the conventional SPM material Cu97Co3
[14,16,17]. Therefore, we speculate that the divalent ions-doped
perovskite cobaltites LBCO belong to SPM cluster rather than the
spin glass.
Several previous works [47] suggest that the system of
La1xSrxCoO3 separates into hole-rich ferromagnetic clusters
and hole-poor nonmagnetic matrix. The clusters are dominated
by the ferromagnetic double exchange interaction between Co3+
and Co4+, while the nonmagnetic matrix is dominated by the
Co3+Co3+ interaction, which is known to be antiferromagnetic
superexchange. This point of view is supported by recent cold
inelastic neutron scattering studies, and it is conformed that the
clusters increase in size and number with increasing concentration of x [26]. Ba2+ doping has a similar effect of introducing holes
into CoO bonds as Sr2+ doping, except that Ba2+ ion has larger
ionic radius than Sr2+ ion [2024]. Therefore, it is reasonable to
believe that the phase-separated picture of La1xSrxCoO3 described above is also true for the system of LBCO. If the clusters are
single-domain clusters without interaction between them, then
the magnetic system of LBCO is very similar to that of the SPM
Cu97Co3 alloy, in which the segregated Co nanoparticles are
isolated by nonmagnetic background. In the frame of SPM, these
phenomena of LBCO as described in the above section, which
could not be well-explained in spin glass, could be interpreted
consistently by the SPM blocking model [14,16]. In SPM blocking
model, the dc ZFC and FC magnetizations are given by the
Langevin function, which is determined by the cluster volume and
the saturation magnetization [16,19,27]. And the ZFCM and FCM
are different from each other below blocking temperature TB.
Please see Refs. [14,16] for the detailed description of this SMP
blocking model. The blocking model reproduces the following
characteristic features for the system of SPM particles being
embedded in nonmagnetic background [16,17]. The ZFC shows a
round peak at Tp. The FCM increases with the decreasing
temperature until all clusters are blocked, and it becomes larger
than ZFCM far above Tp. Such features reect the distribution of
the blocking temperature, i.e., the distribution of the particles

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W. Luo, F. Wang / Journal of Magnetism and Magnetic Materials 321 (2009) 12801284

volume [16]. These features coincide with experimental results

of LBCO very well, which suggested that the hypothesis of LBCO
belonging to SPM clusters is reasonable.
SPM materials and spin glasses share some common features
such as a cusp in ZFCM curve and long-time relaxation
magnetization while they are different from each other in other
aspects of dc and ac magnetic behaviors [1419], which will be
further illustrated below.
The magnetic eld dependence of ZFCM/H and FCM/H for
La0.95Ba0.05CoO3 is shown in Fig. 3. With increasing magnetic eld,
ZFCM/H and FCM/H signicantly decrease and the bifurcation
temperature shifts to lower temperature from 205 K under 100 Oe
to 185 K under 300 Oe. This magnetic feature is also similar to that
of Cu97Co3, while it is inconsistent with that of the canonical spinglass Au96Fe4 [16].
The sharp peak in ZFCM curve, which is an evidence of
ascribing the light-doped samples to spin glasses, becomes
broader and broader with increasing concentration x and displays
a plateau in the range 0.10oxo0.18, for example, of La0.88Ba0.12
CoO3, as shown in Fig. 2. This broad peak cannot be interpreted in
spin glass while it is a natural result of large volume SPM clusters.
In the SPM system, it is believed that the cluster size has a
distribution and the large volume clusters form different shapes.
These factors result in a distribution of the blocking temperature,
so the peak broadens.
Hysteresis loops at 5 K up to 100 kOe after zero-eld cooling
are shown in Fig. 4 for LBCO (0.0oxo0.18). Obviously, the
magnetizations for all samples are not saturated even up
to 100 kOe. Lack of saturation in high elds is a characteristic feature of spin glasses [6]. On the other hand, the magnetization too will not saturate at a moderate eld in the system
of the SPM clusters embedded in the hole-poor region nonmagnetic matrix, which is dominated by the antiferromagnetic
interaction between Co3+ and Co3+. Surprisingly, the slope of
the magnetization curve at high eld (H410 kOe) increases
with increasing concentration of x though the magnetization
does not saturate.

Fig. 4. M versus H of LBCO at 5 K after zero-eld cooling.

3.2. ac Susceptibility
Previous theoretical and experimental works [1219,2831] on
the spin glasses and SPM clusters conrmed that detailed study
of the ac susceptibility corresponding to eld and frequency
Fig. 5. The temperature dependence of the in-phase ac susceptibility for the
compounds of (a) x 0.03, (b) x 0.05 and (c) x 0.08, at different frequencies in
the range 339999 Hz.

dependence could provide a missing link between spin glasses

and SPM. For a canonical spin glass, the peak in the in-phase
component of ac susceptibility is frequency dependent and
it shifts towards higher temperatures with higher frequencies.
The magnitude of the peak below freezing temperature (Tf) is
frequency dependent. This is indeed the case for LSCO [5,9] and
LBCO with xo0.10, as shown in Fig. 5. However, these features are
never present in the samples with x40.10. As shown in Fig. 6, the
peaks become so broad that it is even impossible to determine the
exact freezing temperature Tf.
In the spin-glass studies of the cobaltites samples LSCO [5,9], it
is proposed that the characteristic relaxation time t0 could be
derived as follows:
Fig. 3. Magnetic eld dependence of FCM/H (solid symbols) and ZFCM/H (open
symbols) for x 0.05. The data measured at 100 Oe are shown as squares, whereas
the data measured at 300 Oe are shown as circles.

Tf  Tg
t
/
Tg
t0

zn

(1)

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W. Luo, F. Wang / Journal of Magnetism and Magnetic Materials 321 (2009) 12801284

Fig. 6. The temperature dependence of the in-phase ac susceptibility for (a)

x 0.10, (b) x 0.12 and (c) x 0.15, at different frequencies in the range
339999 Hz.

where t ( f1) is the relaxation time, Tf is the peak temperature

of ac susceptibility with frequency of f, and Tg is the critical
temperature for the spin glass. Here, the value of Tg is chosen by
minimizing the least-square deviation from a straight-line t. The
values of t0 and zn are extracted from the intercept and slope,
respectively. The best ts of LBCO are shown in Fig. 7 for x 0.03,
0.05, and 0.08. These obtained magnitudes of t0 (6.0  109,
6.1 1011, and 3.0  1011 s, respectively) are larger than those of
canonical spin glasses (t0E1013 s) [14], which indicates that the
microscopic spin magnetic entities in the samples of LBCO are not
single atomic spins, but nano-sized clusters of ferromagnetically
coupled spins [9]. In the system of spin glass, zn is a constant
exponent, which should not be changed with x. In the present
paper for LBCO, however, it varies from 6.85, 6.11, to 4.93 for
x 0.03, 0.05, and 0.08, respectively. This exponent of zn is also
changed from 10.30 to 9.33 for La0.95Sr0.05CoO3 and La0.91Sr0.09CoO3 [4,9]. The changing zn reects that the critical exponent of
the correlation length n or the dynamic exponent z is varying with
x, or both [15], which could be considered as the SPM cluster size
and collective magnetic moment varies with x.
For the samples with x40.10, as shown in Fig. 6, the peaks
become so broad that it is impossible to determine the freezing
temperature Tf and nothing could be done about the t of
characteristic relaxation time t0. For the sample of La0.90Ba0.10
CoO3, it seems to show the frequency-dependent feature at rst
glance, but a meaningful characteristic relaxation time t0 cannot
be derived from formula (1) any more. This phenomenon further
conrms that it is inadequate to ascribe the nature of the
magnetic behavior in LBCO to spin glasses. On the other hand, it
is a natural result of SPM cluster growth and of different shapes
of clusters.
In the frame of SPM blocking model, the temperature
dependence of the SPM linear susceptibility corresponding to

1283

Fig. 7. The best t of Tf(o) data extracted from the ac susceptibility measurements
to Eq. (1) for (a) x 0.03, (b) x 0.05 and (c) x 0.08.

thermal equilibrium for clusters having a volume V is given

by[14]:

wsp

m2s V
3kB T

(2)

and the linear susceptibility in the blocked state when the

particles are unable to reach equilibrium within the measuring
time is calculated by

wbl

m2s
,
3K u

(3)

where ms is the saturation magnetization, kB is the Boltzmann

constant, and Ku is the anisotropy constant.
The blocking temperature TB is given by setting relaxation time
t equals to the measurement time as
TB

KuV
,
kB ln1=ot0 

(4)

where the characteristic relaxation time t0 has been estimated to

be in the range 1091013 s [32,33]. This formula indicates that
the blocking temperature TB increases with increasing frequency,
the anisotropy constant and the size of superparamagnetic cluster.
About the frequency dependence, this is indeed the case for
x 0.03, 0.05, and 0.08, as shown in Fig. 5. For the high-doped
samples such as x 0.12 and 0.15, it is believed that the cluster
volume is so large that it could form far different shapes, so the
anisotropy constant Ku varies. For example, a cluster constructed
by sixteen units could be in the shapes of 1  2  8, 1  4  4, and
2  2  4, and so on. This characteristic makes the peak very broad
as shown in Fig. 6.
Fig. 8 displays the temperature dependence of ac susceptibility
measured at an ac eld of 10 Oe, 33 Hz for the samples LBCO.
Obviously, the cusp peak temperature Tp in ac susceptibility

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W. Luo, F. Wang / Journal of Magnetism and Magnetic Materials 321 (2009) 12801284

Co4+, and the clusters embedded in a hole-poor nonmagnetic

matrix. This matrix is dominated by the Co3+Co3+ interaction,
which known to be antiferromagnetic superexchange. It is
proved that the SPM clusters increase in size with increasing
concentration x by the analysis of SPM blocking model. In
addition, the clusters have a volume distribution for a certain
sample. Due to the antiferromagnetic background matrix transfers
to paramagnetic phase, the SPM behavior of LBCO can only exist at
low temperature and the SPM cluster turns into ferromagnetic
phase above TN.

Acknowledgement
This work was supported by the Natural Science Foundation of
China (Contract no. 10375088).
References
Fig. 8. The temperature dependence of ac susceptibility measured at an ac eld of
10 Oe, 33 Hz for the samples of LBCO.

curves increases and the magnitude of the peaks decreases with

the increasing concentration x, especially, the peak becomes
broader and broader and the magnitude of the peak suddenly
increases to a very large value at the magnetic percolation
threshold x 0.18 as shown in the inset of Fig. 8. This feature of
increasing Tp reects that the cluster increases with increasing
concentration x [26]. In addition, the magnitude of the peaks
decreases with the increasing concentration x. This behavior could
be interpreted by the two formulas (2) and (3). The anisotropy
constant increases and the saturation magnetization decreases as
indicated by the slopes in Fig. 4 with increasing concentration of x,
which make the peak decreasing with increasing concentration x.
When x reaches 0.18, the compound will become cluster glass
[47] and the SPM blocking model will not take effect any more.
The static and dynamic magnetic properties of LBCO exhibit
the SPM behavior as described above. However, there is one
critical point different from that of the conventional SPM Cu97Co3.
The segregated Co nanoparticles in the Cu97Co3 alloy are isolated
by nonmagnetic background, while the clusters in LBCO are
embedded in an antiferromagnetic matrix. This antiferromagnetic
matrix will transfer to paramagnetic phase above Neel temperature TN. (Due to the FM cluster disturbance, it is impossible to
derive the exact Neel temperature TN from the CurieWeiss law.)
That means the SPM cluster will be turned into FM above TN for
LBCO and the SPM behavior can only exist at low temperature.

4. Conclusion
The static and dynamic magnetic properties of La1xBaxCoO3
(0.0oxo0.18) have been investigated. Based on the comparisons
with the canonical spin-glass Au96Fe4 and the conventional SPM
Cu97Co3, the nature of magnetic behaviors in LBCO is ascribed to
the SPM clusters rather than spin glasses. This result indirectly
supports that the system of low-doped LBCO separates into
hole-rich ferromagnetic clusters, which is dominated by the
ferromagnetic double exchange interaction between Co3+ and

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