J Supercond Nov Magn (2017) 30:2135–2141
DOI 10.1007/s10948-017-4003-y
ORIGINAL PAPER
Structural, Mössbauer Effect, Magnetic, and Thermal
Properties of Gadolinium Erbium Iron Garnet
System Gd3−x Erx Fe5O12
Qassem I. Mohaidat1 · Mahdi Lataifeh1 · Sami H. Mahmood2 ·
Ibrahim Bsoul3 · Mufeed Awawdeh1
Received: 2 November 2016 / Accepted: 1 February 2017 / Published online: 23 February 2017
© Springer Science+Business Media New York 2017
Abstract In this article, Gd3−x Erx Fe5 O12 powders with
x = 0.0, 0.5, 1.0, 1.5, 2.0, 2.5, and 3.0 were prepared by
solid-state reaction method. The properties of the prepared
samples were examined by X-ray diffraction, Mössbauer
spectroscopy, vibrating sample magnetometry, and differen-
tial scanning calorimetry. The XRD patterns of the powders
show a single-phase structure and were found to agree with
the standard pattern of rare earth iron garnet. Room temper-
ature Mössbauer spectra of the powders indicate that iron is
present in three magnetic sites corresponding to two octahe-
dral sites and one tetrahedral site. The saturation magnetiza-
tion increased with increasing erbium substitution, and the
Curie temperature decreased slightly.
 Qassem I. Mohaidat
q.muhaidat@yu.edu.jo
Mahdi Lataifeh
mahdi.q@yu.edu.jo
Sami H. Mahmood
s.mahmood@ju.edu.jo
Ibrahim Bsoul
ibrahimbsoul@yahoo.com
Mufeed Awawdeh
amufeed@yu.edu.jo
1 Physics Department, Yarmouk University, Irbid 21163, Jordan
2 Physics Department, The University of Jordan, Amman
11942, Jordan
3 Physics Department, Al al-Bayt University, Mafraq
13040, Jordan
Keywords Mössbauer spectroscopy · Magnetic
properties · X-ray diffraction · Differential scanning
calorimetry
1 Introduction
The interest in rare earth iron garnets (R3 Fe5 O12 ) still
attracts many researchers due to their numerous technolog-
ical applications and scientific importance. The discovery
of yttrium iron garnet (YIG) in 1956 had paved the way
for the evolution of advanced technologies in the fields of
microwave devices and magnetic bubble domain type digital
memories [1, 2]. Also, the garnet end members have impor-
tant applications in the laser industry [3]. The microscopic
and macroscopic properties of rare earth ion substitutions
(R = Gd3+ − Yb3+ ) for Y3+ ions in the YIG lattice have
received considerable interest, leading to the understand-
ing of the magnetic structure and underlying magnetic
interactions in garnets [1, 4–8].
The crystal structure of rare earth iron garnets is des-
cribed by the body-centered cubic unit cell with space group
Ia3d (230), containing eight formula units (160 ions). The
cations in the chemical formula R3 Fe5 O12 are distributed
among three different sublattices as 3R3+ -dodecahedral {c}
sites (24 ions/unit cell), 2Fe3+ -octahedral {a} sites (16
ions/unit cell), and 3Fe3+ -tetrahedral {d} sites (24 ions/unit
cell) [1].
The rare earth iron garnets (RIGs) exhibit ferrimagnetic
ordering at room temperature. This property is related to
the distribution of the magnetic ions over the three different
crystallographic sublattices mentioned above. The strongest
a-d superexchange interaction constrains the magnetiza-
tions of the iron sublattices to be coupled antiparallel, with
2136
net magnetization of (Md − Ma ). Since the magnetizations
of the iron sublattices are independent of the rare earth ion
at the c-site, the Curie temperature is nearly the same for all
RIGs, being (550 ± 10 K) [1, 4, 5].
The superexchange interactions between the rare earth
ions in the c sublattice, and the iron ions in the a and d sub-
lattices, are an order of magnitude smaller than the a–d one
and lead to antiparallel coupling of the magnetization of the
{c} sublattice (Mc ) with the resultant (Md − Ma ) [1, 9, 10].
The bulk garnet magnetization as a function of temperature
can be written as
M(T ) = {Md (T ) − Ma (T )} − Mc (T ) (1)
This magnetization may vanish at the compensation tem-
perature Tcomp that is because the rare earth sublattice
and the iron sublattices randomize at different temperature
dependencies. For Ho0.01 Gd0.99 Fe5 O12 , Tcomp was found to
be 280 K [9].
In the system to be studied, Gd3−x Erx Fe5 O12 , the
gadolinium ion is an S-state ion with J = 7/2, so the
effect of the crystalline electric field is negligible when we
compare it with the effect of the exchange field [9]. In
Gd3+ -rich samples, the system became more isotropic, and
because the gadolinium moment follows the applied mag-
netic field, it is easy to rotate other anisotropic ions such
as erbium toward the hard direction of magnetization when
we look at single crystals. On the other hand, the erbium
(Er3+ ) ion being a non-S-state ion, the crystalline electric
field (CEF) causes quenching of the orbital angular momen-
tum L. The exchange field plus the CEF causes the Er3+
moments to have double conical arrangement (umbrella
structure) relative to the easy direction of magnetization
[1, 9, 11].
In the present work, we report the results of the struc-
tural, magnetic, and hyperfine studies on Gd3−x Erx Fe5 O12
(x = 0.0, 0.5, 1.0, 1.5, 2.0, 2.5, and 3.0), synthesized by
ball milling and appropriate heat treatment. X-ray diffrac-
tion (XRD) measurements were used to examine the phase
purity and structural characteristics of the prepared gar-
nets. Mössbauer spectroscopy (MS) measurements at room
temperature (RT) were made on the above samples to inves-
tigate the effect of Er substitution on the hyperfine field,
the isomer shift, and other MS parameters. Further, RT
magnetic measurements on the garnets were carried out to
investigate the effect of such substitution on the magnetic
properties of these compounds. Furthermore, thermal mea-
surements using differential scanning calorimetry (DSC)
were made in order to examine the magnetic phase tran-
sitions and determine the Curie temperature for all the
samples under investigation [12]. This work is a result of
the continuation of our previous research program concern-
ing garnets and involving NMR studies of holmium ions in
J Supercond Nov Magn (2017) 30:2135–2141
single crystals of rare earth iron garnet [13], as well as MS
and magnetization measurements [9, 10, 14, 15].
2 Experimental Procedures
Gd3−x Erx Fe5 O12 powders with x = 0.0, 0.5, 1.0, 1.5, 2.0,
2.5, and 3.0 were prepared by solid-state reaction method.
Metallic oxides Gd2 O3 , Er2 O3 , and Fe2 O3 were used to
fabricate Gd3−x Erx Fe5 O12 powder samples. Stoichiometric
ratios of the metallic oxides were loaded into a hardened
stainless steel cup with a ball to powder ratio of 8:1. The
milling process was carried out at 250 rpm for 16 h. The
resulting precursor was annealed at 1300 ◦ C for 2 h. X-ray
diffraction (XRD) patterns were collected using a Philips
X’pert PRO X-ray diffractometer (PW3040/60) operating
at (45 kV, 40 mA),with Cu-Kα radiation (λ = 1.5405 Å).
The samples were scanned over angular range 15◦ < 2θ <
75◦ with a 0.02◦ scanning step and a speed of 1◦ /min. XRD
patterns were analyzed using X’pert HighScore software to
identify the phases present in each sample. Rietveld refine-
ment of the XRD patterns for all fabricated samples was
carried out using FullProf suite 2000 software to obtain the
values of refined structural parameters.
Samples for Mössbauer spectroscopy studies were pre-
pared by gently pressing a thin layer of the powdered
sample between two circular Teflon disks with diameter 2
cm, which is small compared with the distance between
the γ -ray source and the sample, in order to avoid angu-
lar broadening of the spectrum. Room temperature (RT)
Mössbauer spectra were collected using a standard constant
acceleration Mössbauer spectrometer over 1024 channels.
The γ -ray source was a 50-mCi 57 Co in rhodium matrix.
The spectra were then analyzed using fitting routines based
on least-squares analysis.
The magnetic measurements were carried out using a
vibrating sample magnetometer (VSM MicroMag 3900,
Princeton Measurements Cooperation), providing a maxi-
mum applied magnetic field of 10 kOe.
The differential scanning calorimetry (DSC) model
(NETZSCH-Gerätebau GmbH 204 F1 Phoenix) was used
to measure the thermal properties of the Gd3−x Erx Fe5 O12
powder samples. The DSC analysis depends on the mea-
surement of the difference in heat fluxes, recorded for the
sample analyzed and a reference sample. DSC is a thermal
analysis technique which measures heat flow related to tran-
sitions in materials as a function of time and temperature;
this can provide quantitative and qualitative information
about physical and chemical changes that involve endother-
mic or exothermic processes, or changes in the heat capacity
of the sample under investigation. Measurements were made
at a heating rate of 5 degrees per minute in the temperature
range 30 to 350 ◦ C.
J Supercond Nov Magn (2017) 30:2135–2141 2137

3 Results and Discussion

Gd3Fe5O12 IExp
Figure 1 shows the XRD patterns for all samples examined ICalc

Intensity (arb. units)

in this work. The XRD pattern for the sample with x = 0 IExp- ICalc
was identified by a single ICDD file (00-048-0077) which Bragg Position
belongs to cubic gadolinium iron oxide ferrite (Gd3 Fe5 O12 ).
The XRD pattern for the sample with x = 3, however,
was identified with a single cubic erbium iron oxide fer-
rite (Er3 Fe5 O12 ) consistent with the standard pattern ICDD
file (00-023-0240). As one might observe from Fig. 1, all
samples revealed the presence of a single garnet phase, indi-
cating the suitability of the present synthesis route for the
preparation of a highly pure garnet phase, where the Er3+ 20 30 40 50 60 70
ions diffused completely into the lattice of Gd3 Fe5 O12 .
Rietveld refinements for all fabricated samples are shown Er3Fe5O12 IExp
in Fig. 1. Also, an enlarged view of the samples with x = ICalc
0 and x = 3 are presented in Fig. 2. The theoretical pat-

Intensity (arb. units)

IExp- ICalc
tern (black continuous line) is in good agreement with the
Bragg Position
experimental data (red dots), where the residual difference
curve (in blue) is a straight horizontal line with small rip-
ples at the peak positions. The Bragg factor (RB ) and the
goodness-of-fit quality (χ 2 ) are shown in Table 1. The
value of χ 2 for all fitted samples is less than 0.4, which
indicates an excellent fit. The structural parameters, as well

x = 3.0 20 30 40 50 60 70
o
2 θ (deg.)
Fig. 2 Refined XRD patterns for Gd3−x Erx Fe5 O12 samples with x =
x = 2.5 0 and x = 3. The residual difference between the experimental and
calculated data is given in the lower part of the plots (blue line)

x = 2.0
as the x-ray density (ρx ) for all samples, are also tabulated in
Intensity (arb. units)

Table 1. The refined lattice constant a for the two end com-
pounds (x = 0 and x = 3) are in excellent agreement with
x = 1.5
reported values [1]. Also, the analysis revealed that the lat-
tice constant and cell volume decreased monotonically with
x = 1.0 the increase of the substitution level of Er. This decrease
can be associated with the difference in ionic radii, since the

x = 0.5 Table 1 Bragg factor, χ 2 , lattice constant a, unit cell volume, and
density for all fabricated samples

Composition (x) χ2 RB a (Å) V (Å3 ) ρ x (g/cm3 )

x = 0.0
(± 0.01)

Gd3 Fe5 O12 0.151 2.15 12.469(9) 1939.0 6.46

00-048-0077
Gd2.5 Er0.5 Fe5 O12 0.149 2.89 12.450(3) 1929.9 6.52
Gd2.0 Er1.0 Fe5 O12 0.148 1.97 12.426(4) 1918.8 6.59
20 30 40 50 60 70 Gd1.5 Er1.5 Fe5 O12 0.176 1.68 12.410(1) 1911.3 6.65
o
2θ Gd1.0 Er2.0 Fe5 O12 0.216 1.88 12.386(8) 1900.6 6.73
Gd0.5 Er2.5 Fe5 O12 0.278 1.72 12.365(4) 1890.7 6.80
Fig. 1 Refined XRD patterns for Gd3−x Erx Fe5 O12 samples along Er3 Fe5 O12 0.315 1.59 12.346(1) 1881.9 6.86
with the standard ICDD pattern for Gd3 Fe5 O12
2138 J Supercond Nov Magn (2017) 30:2135–2141

radius of the Gd3+ ion (0.97 Å) is appreciably larger than Table 2 The hyperfine parameters and the percentage relative inten-
that of the Er3+ ion (0.89 Å). This property of lanthanide sities (I ) obtained at room temperature for the Gd3−x Erx Fe5 O12
samples
contraction is observed on rare earth elements as one goes
from left to right in the periodic table. Hence, the crystal Site Bhf (kOe) CS (mm/s) Width (mm/s) I (%)
structure becomes more compact and the unit cell volume (± 0.5) (± 0.002) (± 0.02) (± 1)
decreases as a result of Er3+ substitution.
Room temperature (RT) Mössbauer spectra (MS) of the x=0
system Gd3−x Erx Fe5 O12 with x = 0.0, 0.5, 1.0, 1.5, 2.0, Octahedral(s) 499 0.39 0.30 27
2.5, and 3.0 are shown in Fig. 3. The spectra shown are 489 0.40 0.30 10
similar to those reported by others for rare earth iron gar- Tetrahedral 406 0.16 0.40 63
nets (RIG). MS were fitted with three magnetic sextets [16]
x = 0.5
corresponding to iron ions (Fe3+ ) in three different envi-
Octahedral(s) 499 0.38 0.30 27
ronments, two octahedral sites and one tetrahedral site, and
489 0.39 0.30 10
the fitting parameters are listed in Table 2. Previous stud-
Tetrahedral 406 0.16 0.45 63
ies showed that MS can be fitted by either two or three
magnetic sextets [14–18]. The assumption made for the two-
x = 1.0
component model is that one sextet corresponds to Fe3+
Octahedral(s) 498 0.38 0.29 27
ions in the octahedral (16a) site, while the other sextet
486 0.39 0.30 10
Tetrahedral 404 0.16 0.47 63

x = 3.0 x = 1.5
Octahedral(s) 497 0.38 0.30 27
485 0.39 0.31 10
Tetrahedral 403 0.16 0.50 63
x = 2.5
x = 2.0
Octahedral(s) 496 0.38 0.30 27
484 0.39 0.31 10
x = 2.0
Tetrahedral 401 0.16 0.51 63
Intensity (a.u)

x = 2.5
Octahedral(s) 495 0.37 0.31 27
x = 1.5 484 0.39 0.31 10
Tetrahedral 399 0.16 0.54 63

x = 3.0
x=1
Octahedral(s) 494 0.37 0.31 27
482 0.39 0.32 10
Tetrahedral 398 0.15 0.52 63

x = 0.5
corresponds to iron ions in the tetrahedral site (24d). The two
sextets are characterized by negligible quadrupole splitting
x=0 and relative intensities of about 40:60 [14–16]. According
to other investigators [17, 19, 20], the different orientations
of the main axis of the electric field gradient and the mag-
-12 -9 -6 -3 0 3 6 9 12 netic hyperfine field Bhf on the octahedral sites result in
Velocity (mm/sec) two magnetic sextets having the same center shift (CS) and
quadrupole splitting, with a relative intensity ratio of 3:1.
Fig. 3 Mössbauer spectra for the Gd3−x Erx Fe5 O12 samples (filled It is clear that the CS for each site does not change
circles) together with the theoretical spectrum obtained from the fitting
software (continuous red line). The component corresponding to octa-
with the substitution of Er3+ . This confirms the fact that
hedral sites is represented by the blue sextet, while that corresponding Er3+ replaces Gd3+ in the dodecahedral site of the {c}
to tetrahedral sites is represented by the green sextet sublattice, and neither of the iron sublattices is influenced
J Supercond Nov Magn (2017) 30:2135–2141
by the substitution. Moreover, the relative intensities of the
components corresponding to the {a} and {d} iron sublat-
tices are in good agreement with the theoretical prediction
and with the results of previous studies [14, 15].
The experimental data in Table 2 show that the values
of the hyperfine magnetic field Bhf at the iron nucleus in
the octahedral and tetrahedral sites decreased slightly as
the concentration of the erbium ions increased. The small
reduction in the values of Bhf could be due to small varia-
tions of the a − c and d − c interactions as a result of Er3+
substitution at the {c} sites. The hyperfine magnetic field
Bhf at the iron nucleus originates mainly from the net spin
density through the Fermi contact potential. The net spin
density is affected by the interaction of the electronic wave
functions of the Mössbauer ion Fe3+ with the surrounding
ions. The prevailing a − c and d − c magnetic interactions
are of two types: the magnetic dipole-dipole (direct) interac-
tion between the R3+ ions and the Fe3+ ions, and the super
transferred hyperfine interaction between these ions via the
intervening oxygen [21, 22].
Magnetization measurements on polycrystalline samples
of Gd3−x Erx Fe5 O12 have been made at room temperature.
These measurements include hysteresis loops and initial
magnetization curves (Figs. 4 and 5). It is clear from the
hysteresis loops that all samples are nearly magnetically
saturated at relatively low applied magnetic fields, and
the saturation magnetization Ms was therefore estimated
directly from the curves, without the need for applying the
law of approach to saturation. From Fig. 4, one can see that
Ms (measured in emu/g) increased systematically by nearly
an order of magnitude with the increase of x from 0 to 3.
Fig. 4 Magnetization hysteresis
loops for Gd3−x Erx Fe5 O12 16
samples
12
4
M (emu/g)
0
-4
-8
-12
-16
-10000
2139
The results are consistent with the data provided by [1] for
the end compounds. From the initial magnetization curves
(Fig. 5), it is also clear that the initial magnetic susceptibility
χin increased with increasing Er substitution.
For RIGs, the net magnetic moment per formula unit at 0
K could be given by
μnet = 3μ(R3+ )dod − 3μ(Fe3+ )tet + 2μ(Fe3+ )oct
= 3μ(R3+ )dod − μ(Fe3+ )tet
At this temperature, the saturation magnetization of
GdIG is greater than that of ErIG. This can be attributed to
the fact that Gd3+ has a larger magnetic moment (μGd =
7 μB ) than Er3+ (μEr = 5 μB ). As a result, ErIG has
a lower compensation temperature (Tcomp ≈ 80 K) than
GdIG (Tccomp ≈ 290 K) [7]. In this work, the magnetization
measurements were performed at room temperature. Due
to the strong temperature dependence of the magnetic Gd
sub-lattice {c}, the Gd sub-lattice dominates the magnetic
behavior for T < Tcomp , while for T > Tcomp , the magnetic
behavior is mainly caused by the antiferromagnetically cou-
pled Fe sub-lattices ({d} and {a} sites) which explains the
fact that ErIG possesses a higher saturation magnetization
than GdIG at room temperature [23, 24].
Differential scanning calorimetry (DSC) measurements
were performed on all samples (Fig. 6). The Curie temper-
ature Tc was determined from the dip in each thermal scan
as indicated by the insets in Fig. 6. The Curie temperature
of the different Gd3−x Erx Fe5 O12 samples was found to be
286.9, 284.6, 282, 279.5, 275.9, 274.8, and 271.9 ◦ C, for
x = 0, 0.5, 1.0, 1.5, 2.0, 2.5, and 3.0, respectively. In all
x = 0.0
x = 0.5
x = 1.0
x = 1.5
x = 2.0
x = 2.5
x = 3.0
-5000 0 5000 10000
H (Oe)
2140 J Supercond Nov Magn (2017) 30:2135–2141

Fig. 5 Initial magnetization 16

curves for Gd3−x Erx Fe5 O12 x=3
samples
x = 2.5
12
x=0
x=2 x = 0.5
x=1

M (emu/g)
x = 1.5 x = 1.5
x=2
8 x = 2.5
x=3
x=1

4 x = 0.5

x=0

0
0 2000 4000 6000 8000 10000
H (Oe)

samples, Tc represents the magnetic transition from ferro-
magnetic to paramagnetic behavior since all samples were
composed of the RIG single phase. Moreover, Tc did not
change appreciably with Er3+ substitution, indicating that
the magnetic ordering of the rare earth iron garnet system is
mainly determined by the strong superexchange interaction
between the two iron a and d sublattices and within each
individual iron sublattice. The slight decrease in Tc with Er
substitution indicates that the effect of the rare earth sub-
lattice on the strength of the superexchange interaction is
nearly negligible.

O
4 Conclusions
Tc=271.9 C
x=3 XRD measurements indicated that all the samples under in-
O
vestigation were composed of a single RIG phase.
Tc=274.8 C Mössbauer spectra at RT show that the Er3+ ion substitutes
x = 2.5 Gd3+ in the dodecahedral csite, introducing no structural
or chemical environmental effects. The spectra were fitted
Tc=275.9 C
O
with three magnetic sextets corresponding to Fe3+ ions in
x=2
three different environments, two octahedral and one tetra-
DSC(mW/mg)

hedral site, respectively. The saturation magnetization Ms

for the samples exhibited a systematic increase with Er3+
O
Tc=279.5 C
x = 1.5 substitution, due to the strong temperature dependence of
O
the magnetic Gd sub-lattice {c}. Second-order phase tran-
Tc=282 C sitions were observed in DSC thermal measurements for
all compositions, from which the ordering (Curie) tempera-
x=1
O
tures were deduced. It is clear that the strong superexchange
Tc=284.6 C
interaction between the two iron (a–d) sublattices is highly
responsible for magnetic ordering.
x = 0.5
O
Tc=286.9 C
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