Materials Research Bulletin 44 (2009) 1559–1564

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Materials Research Bulletin

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An investigation of structural, magnetic and dielectric properties of R2NiMnO6

(R = rare earth, Y)
R.J. Booth a, R. Fillman a, H. Whitaker b, Abanti Nag c, R.M. Tiwari c,
K.V. Ramanujachary b, J. Gopalakrishnan c, S.E. Lofland a,*
a
Department of Physics and Astronomy, Rowan University, 201 Mullica Hill Road, Glassboro, NJ 08028-1701, USA
b
Department of Chemistry and Biochemistry, Rowan University, 201 Mullica Hill Road, Glassboro, NJ 08028, USA
c
Solid State and Structural Chemistry Unit, Indian Institute of Science, Bangalore 560012, India

A R T I C L E I N F O A B S T R A C T

Article history: We have investigated the structure, magnetic and dielectric properties of the double perovskite oxides,
Received 22 January 2009 R2NiMnO6 (R = Pr, Nd, Sm, Gd, Tb, Dy, Ho and Y). We could refine powder X-ray diffraction patterns of all
Received in revised form 23 January 2009 the phases on the basis of monoclinic (P21/n) double perovskite structure where Ni and Mn atoms are
Accepted 10 February 2009
ordered at 2c and 2d sites, respectively. All the phases are ferromagnetic insulators exhibiting relatively
Available online 21 February 2009
low dielectric loss and dielectric constants in the range 15–25. The ferromagnetic ordering temperature
of the R2NiMnO6 series seems to correlate better with the radius of R3+ atoms than with the average Ni–
Keywords:
O–Mn angle (w) in the double perovskite structure. These results are consistent with all samples having
A. Oxides
Mn4+ and Ni2+ with minimal antisite disorder.
C. X-ray diffraction
D. Magnetic properties ß 2009 Elsevier Ltd. All rights reserved.
D. Dielectric properties

1. Introduction
R2NiMnO6 (R = rare earth, Y) oxides are among a special group
of double perovskite oxides [1] where a near-ideal e2g Oe0g
electronic interaction gives rise to ferromagnetic alignment of d-
electron spins, according to the classical Goodenough–Kanamori
rules [2,3]. Among these, the R = La member, La2NiMnO6, exhibit-
ing a ferromagnetic Curie temperature TC of 280 K, has received
considerable attention in recent times [4–7], not only because of
the possibility of combining multiple electronic properties
(ferromagnetism, magnetoresistance, magnetocapacitance and
semiconductivity) in this material, but also because of the
expectation that a fundamental understanding of the Ni2+–O–
Mn4+ electronic interaction would provide new guidelines for the
design of multiple property materials. The understanding has
indeed resulted in the design of a new ferromagnetic–ferroelectric
material, Bi2NiMnO6 [8] and in the prediction of a polar
ferromagnetic behavior for (La,Lu)NiMnO6 [9].
As compared to La2NiMnO6, investigations of other R2NiMnO6
oxides are relatively sparse [10–14]: while it is generally known
that the entire series of oxides are ferromagnetic with TCs smaller
than that of the R = La member, detailed structure–property
correlations especially for the interaction between R3+ and the
* Corresponding author. Tel.: +1 856 256 4382; fax: +1 856 256 4478.
E-mail address: lofland@rowan.edu (S.E. Lofland).
NiMnO6 network for this series have not been fully established.
While R = La, Nd and Y members have been shown to possess
ordered (monoclinic, P21/n) double perovskite structures [4,14,15],
the structures of other members of this series have been reported
to be orthorhombic (Pnma) [12] suggesting an incomplete ordering
of Ni and Mn atoms. An ordering of Ni and Mn atoms was assumed
(but not established) by Asai et al. [10] in their study of the
magnetic properties of this series.
In view of the foregoing, we have undertaken an investigation of
the structure and electronic properties of R2NiMnO6 series for
several R atoms. In addition to refinement of structures from
powder X-ray diffraction (XRD) data and bulk magnetization and
dielectric studies, we have also investigated the spin dynamics by
means of electron paramagnetic resonance (EPR). Our results
which are presented herein provide new insights into the role of
R3+ atoms on the magnetic properties of the series.
2. Experimental
Perovskite oxides for the composition R2NiMnO6 for R = La, Pr,
Nd, Sm, Gd, Tb, Dy, Ho and Y were prepared by reacting high purity
R2O3 (pre-dried at 900 8C), NiC2O42H2O and MnC2O42H2O in
stoichiometric proportion at the conditions given in Table 1.
Repeated grinding and heating of the samples were done to ensure
ordering of Ni/Mn atoms. The products were examined by powder
XRD. A Philips X’Pert Diffractometer (Ni filtered Cu Ka radiation)
was used to record powder XRD patterns. Lattice parameters were

0025-5408/$ – see front matter ß 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.materresbull.2009.02.003
1560 R.J. Booth et al. / Materials Research Bulletin 44 (2009) 1559–1564

Table 1
Synthesis conditions and lattice parameters of R2NiMnO6.

R2NiMnO6 Preparation conditionsa Lattice parametersb

La2NiMnO6 1000 8C/24 h, 1150 8C/24 h, 1150 8C/48 h a = 5.5099(7) Å, b = 5.4562(6) Å, c = 7.7703(1) Å, b = 89.82(1)8, V = 233.60(5) Å3

Pr2NiMnO6 1000 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.4453(8) Å, b = 5.4701(7) Å, c = 7.6966(1) Å, b = 90.030(3)8, V = 229.257(7) Å3

Nd2NiMnO6 1000 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.4145(9) Å, b = 5.4842(1) Å, c = 7.6742(1) Å, b = 90.011(2)8, V = 227.883(9) Å3

Sm2NiMnO6 1000 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.3524(9) Å, b = 5.5119(1) Å, c = 7.6103(1) Å, b = 90.034(3)8, V = 224.522(1) Å3

Gd2NiMnO6 1000 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.2955(1) Å, b = 5.5418(1) Å, c = 7.5630(1) Å, b = 90.126(1)8, V = 221.953(1) Å3

Tb2NiMnO6 1150 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.2740(9) Å, b = 5.5417(9) Å, c = 7.5302(1) Å, b = 89.814(1)8, V = 220.090(9) Å3

Dy2NiMnO6 1000 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.2477(1) Å, b = 5.5462(1) Å, c = 7.5059(1) Å, b = 90.232(1)8, V = 218.460(1) Å3

Ho2NiMnO6 810 8C/24 h, 1000 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.2277(1) Å, b = 5.5470(1) Å, c = 7.4895(1) Å, b = 89.726(1)8, V = 217.185(1) Å3

Y2NiMnO6 810 8C/24 h, 1000 8C/24 h, 1200 8C/24 h, 1300 8C/24 h, 1300 8C/24 h a = 5.2285(1) Å, b = 5.5518(1) Å, c = 7.4872(2) Å, b = 89.744(1)8, V = 217.337(1) Å3
a
All the oxides were prepared by reacting high purity R2O3 (pre-dried at 900 8C), NiC2O42H2O and MnC2O42H2O in stoichiometric proportion at the conditions given.
b
Monoclinic P21/n.

obtained by least squares refinement of powder XRD data by
means of the program PROSZKI [16], and XRD patterns were
simulated by the program POWDERCELL [17]. For structure
refinement, XRD data were collected in the 2u range 5–1008 with
a step size of 0.028 and a residence time of 9 s. Rietveld refinement
of powder XRD data was carried out with the program GSAS [18].
The patterns were refined for the lattice parameters, scale factor,
background (shifted Chebyshev background function), pseudo-
Voigt profile function (U, V, W and X), atomic coordinates, and
isothermal temperature factors (Uiso).
The magnetization M was measured on a Physical Properties
Measurement System (Quantum Design) at magnetic fields H up to
50 kOe and temperatures ranging from 5 to 350 K. Dielectric
constant (e) and loss (tan d) were measured at room temperature
with a coaxial resonator [19] for frequencies between 1 and 5 GHz.
EPR data were recorded at temperatures ranging from 100 to 570 K
at 9.2 GHz with a Varian E-9 spectrometer.
3. Results and discussion
3.1. Structure

Powder XRD patterns of all the R2NiMnO6 oxides synthesized

could be indexed on monoclinic (P21/n) cells similar to those of
La2NiMnO6 [4] and Y2NiMnO6 [15] (Table 1). We could refine
powder XRD data of all the oxides on the basis of P21/n model of the
double perovskite structure–refinement with typical perovskite
orthorhombic Pnma structure led to unsatisfactory results.
Representative refinement profiles and structural parameters
derived from the refinement are given in Fig. 1 and Tables 2 and
3, while Table 4 lists the relevant structural parameters derived
from the refinement. Although the refinement of the XRD data is
insensitive to Ni/Mn disorder, the Mn–O and Ni–O bond lengths
and bond valence sums (BVS) obtained (Table 4) for the ordered
structure are in agreement with the values expected [4,8] for
MnIV–O and NiII–O bonds. Moreover, the ferromagnetism of the
oxides (discussed later) with near ideal ordered moments (5mB)
provides additional support for a near complete ordering of Ni/Mn
in all the R2NiMnO6 oxides.
While we see that the hMn–Oi and hNi–Oi bond lengths remain
nearly the same in all the R2NiMnO6, there is a distinct decrease of
the hNi–O–Mni bond angle (w) with the decrease of R-ion radius
that is characteristic of RMO3 perovskite oxides in general [20] as
well R2NiMnO6 oxides [10].

Table 2
Atomic positions, occupancy and isotropic temperature factors for Sm2NiMnO6
(P21/n)a.

Atom Site x y z Uiso (Å2) Occupancy

Sm 4e 0.0128(4) 0.0542(1) 0.2483(1) 0.0258(3) 1

Ni 2c 0.5 0.0 0.5 0.0265(1) 1
Mn 2d 0.5 0.0 0.0 0.0245(1) 1
O1 4e 0.0925(1) 0.4732(1) 0.2724(2) 0.0440(4) 1
O2 4e 0.7180(4) 0.2740(4) 0.0323(2) 0.0261(4) 1
Fig. 1. Rietveld refinement of the structure of (a) Sm2NiMnO6 and (b) Tb2NiMnO6 O3 4e 0.7066(3) 0.2986(2) 0.4408(1) 0.0260(5) 1
from powder XRD data. Observed (*), calculated (–) and difference profiles
a
(bottom) are shown. The vertical bars indicate positions of the Bragg reflections. Reliability factors (%): Rp = 1.94, Rwp = 3.08, R2F ¼ 7:02; x2 = 4.201.
 R.J. Booth et al. / Materials Research Bulletin 44 (2009) 1559–1564 1561

Table 3 and Mn ions per unit cell, the valence states are either Mn3+ (3d4
Atomic positions, occupancy and isotropic temperature factors for Tb2NiMnO6 (P21/
S = 2) and Ni3+ (3d7 S = 3/2) or Mn4+ (3d3 S = 3/2) and Ni2+ (3d8
n)a.
S = 1). Assuming g = 2 for Mn and 2.2 for Ni, the former yields an
Atom Site x y z Uiso (Å2) Occupancy
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
P 2 ffi
effective moment for the Mn–Ni network meff ¼ gi Si ðSi þ 1Þ of
Tb 4e 0.0151(3) 0.0658(1) 0.2526(7) 0.0252(3) 1
6.50 and the latter 4.97. The fit to the susceptibility yields
Ni 2c 0.5 0.0 0.5 0.01591(1) 1
Mn 2d 0.5 0.0 0.0 0.0252(1) 1 5.18  0.08, which is consistent with the Mn4+/Ni2+ scenario. This is
O1 4e 0.0917(1) 0.4680(1) 0.2577(2) 0.0251(2) 1 in contrast to the claim by Bull and McMillan [12] that the oxidation
O2 4e 0.6935(2) 0.2779(2) 0.0454(1) 0.0140(4) 1 states of the transition metal are not integral.
O3 4e 0.7012(2) 0.3066(2) 0.4468(1) 0.0102(4) 1
Fig. 2 also shows the temperature-dependent magnetization of
a
Reliability factors (%): Rp = 1.47, Rwp = 2.20, R2F ¼ 6:74; x2 = 2.694. Y2NiMnO6. The low-field magnetization (not shown) yields
TC  79 K. The moment is 4.5mB/unit cell at 50 kOe (inset), close
3.2. Magnetic properties to the expected value of 5.2mB/unit cell for ferromagnetic
alignment of spin only values for Mn4+ and Ni2+ to be compared
Fig. 2 shows the molar paramagnetic susceptibility x of with the >7mB/unit cell expected for Mn3+ and Ni3+. Note the small
Y2NiMnO6. The dotted line in the insets represents a fit to a hysteresis in contrast to the metamagnetic behavior observed by
Curie–Weiss law: Troyanchuk et al. [11]. By extrapolating M vs. 1/H to 1/H = 0, one
finds the saturation magnetization to be 4.6mB/unit cell; this slight
P reduction could be due to a finite antisite disorder [10].
NA gi2 m2B Si ðSi þ 1Þ
x¼ (1) The other compounds in this series, which contain rare earths
3kB ðT  uÞ
with nonzero moment, also show ferromagnetic behavior, as
where gi is the Lande spectroscopic splitting factor and Si the spin reported earlier [10,12,13]. While the high-temperature values of
of the ith ion, respectively, NA Avogadro’s number, mB the Bohr x (Fig. 2) for these compounds can be fit to Eq. (1), the effective
magneton, u the Weiss temperature, and kB Boltzmann’s constant. moment values are unreasonable. Since, except at the lowest
Since the compounds in this system are insulators (i.e. no temperatures, the magnetization of the other compounds is 5mB/
indication of mixed valence) and there is only one pair of Ni unit cell in the ferromagnetic state, we propose that the rare earth

Table 4
Structural parameters of R2NiMnO6.

R2NiMnO6 Bond angles (8) Ni–O1–Mn, Ni–O2–Mn, Average bond Average bond Bond valence sums
Ni–O3–Mn, hNi–O–Mni length (Å) hNi–Oi length (Å) hMn–Oi (BVS) Ni, Mn, R

La2NiMnO6 160.3 2.020 1.917 2.232

162.2 3.852
158.7 2.772
160.4

Pr2NiMnO6 158.1 2.029 1.928 2.178

161.4 3.738
156.5 3.049
158.6

Nd2NiMnO6 160.1 2.039 1.915 2.118

157.9 3.871
155.9 2.848
157.9

Sm2NiMnO6 149.4 2.046 1.902 2.112

160.6 4.08
146.8 3.178
152.3

Gd2NiMnO6 149.4 2.070 1.895 1.954

152.4 4.094
146.8 3.315
149.5

Tb2NiMnO6 146.7 2.033 1.907 2.136

153.2 3.968
145.5 2.945
148.5

Dy2NiMnO6 144.9 2.034 1.924 2.144

148.7 3.782
147.2 2.895
146.9

Ho2NiMnO6 146.5 2.031 1.924 2.172

146.6 3.778
146.4 3.137
146.5

Y2NiMnO6 145.2 2.018 1.938 2.282

146.6 3.676
146.1 3.053
145.9
1562 R.J. Booth et al. / Materials Research Bulletin 44 (2009) 1559–1564

Fig. 2. Temperature dependence of the inverse susceptibility and magnetization at 10 kOe. The modified Curie–Weiss fit (dotted line) describes the susceptibility data rather
well. The inset shows the field dependence of the magnetization at 5 K.

moments are effectively non-interacting and that x can be written as
C MnNi C RE
x¼ þ (2)
T u T
where CRE and CMnNi are the Curie constants of the rare earths and
Mn–Ni networks, respectively. From Van Vleck’s values for the Curie
constants for the trivalent rare earths [21], the resulting fits yield
values (Table 5) for the effective moment of the Mn–Ni network that
are consistent with ferromagnetic alignment of Mn4+ and Ni2+. The
downturn in the magnetization at lowest temperatures seen in some
samples (Sm and Nd) is presumably related to large magnetocrystal-
line anisotropy due to spin–orbit coupling of the Mn–Ni network to
the rare earth (see below). The effect is not seen for rare earths with
large moments (Tb, Gd, Ho, Dy) probably because the paramagnetic
susceptibility of the rare earth is so large that it gives rise to the
upturn in magnetization at low temperatures.
At 5 K, the high-field magnetization was used calculate the
corresponding extrapolated moment values (inset, Fig. 2). Those
values, as well as the expected total moment, with the theoretical
rare earth moments [22], are also listed in Table 5 along with the TC
values determined by low-field magnetization studies. The present
TC values are generally higher than those reported by Troyanchuk

Table 5
Magnetic properties of R2NiMnO6.

Compound ua (K) Effective rare Effective Ni–Mn TCd (K) Rare earth Theoretical saturation Measured moment Extrapolated
earth momentb (mB) momentc (mB) momente (mB) momentf (mB) at 50 kOe (mB) Momentg (mB)

Pr2NiMnO6 226  3 3.6 5.50  0.08 212 3.2 11.6 5.0 5.7
Nd2NiMnO6 213  2 3.6 5.37  0.08 194 3.27 11.8 5.6 7.1
Sm2NiMnO6 176  1 0.84 5.50  0.06 157 0.71 6.6 4.9 5.1
Gd2NiMnO6 149  2 7.9 5.22  0.08 128 7 19.2 15.6 21.7
Tb2MnNiO6 132  2 9.7 5.17  0.06 111 9 23.2 13.5 15.4
Dy2NiMnO6 107  2 10.6 4.94  0.07 93 10 25.2 13.6 16.9
Ho2NiMnO6 99  1 10.6 4.90  0.05 82 10 25.2 14.1 21.7
Y2NiMnO6 101  1 0 5.18  0.05 79 0 5.2 4.5 4.6
a
Results from modified Curie–Weiss plot (Fig. 2).
b
Theoretical rare earth moment mcalc = g[J(J + 1)]1/2 (Ref. [21]).
c
Results from modified Curie–Weiss plot (Fig. 2) including theoretical rare earth moment.
d
Determined from low-field measurements.
e
Rare earth moment calculated from gJ (Ref. [22]).
f
Total theoretical saturation moment [2gJ + 5.2] where theoretical Ni–Mn moment = 5.2.
g
Experimental data from M vs. 1/H extrapolated to 1/H = 0.
 R.J. Booth et al. / Materials Research Bulletin 44 (2009) 1559–1564 1563

Fig. 3. TC and u as a function of the ionic radius of the rare earth. The dependence is Fig. 4. Representative EPR data of Sm2MnNiO6 taken at 243 K. The line represents a
quite linear. The inset shows the dependence of TC and u on hcos2 fi. fit with Lorentzian lineshapes.

Fig. 5. Temperature dependence of the EPR linewidth.

1564 R.J. Booth et al. / Materials Research Bulletin 44 (2009) 1559–1564

Table 6 have measured the dielectric constant and tan d values of

EPR parameters for R2NiMnO6 oxides.
R2NiMnO6 and the values are listed in Table 7. The low dielectric
Compound g constants (e = 15–25) with no dispersion suggest that there is
perhaps no microwave magnetocapacitance effect in these
Pr2NiMnO6 2.10
Nd2NiMnO6 2.06 materials. Small dielectric constants with low loss together with
Sm2NiMnO6 2.09 high resistivity (107 V-cm at 300 K) of R2NiMnO6 oxides are
Gd2NiMnO6 2.03 consistent with the ordered double perovskite structure [24].
Tb2MnNiO6 2.25
Dy2NiMnO6 2.07
Ho2NiMnO6 2.20
4. Conclusions
Y2NiMnO6 2.07
In summary, we have investigated R2NiMnO6 (R = Pr, Nd, Sm,
Gd, Tb, Dy, Ho and Y) perovskite oxides. All phases could be refined
et al. [11] and lower than those of Bull and McMillan [12] although to monoclinic double perovskite structure, and our studies
the latter measurements were done at relatively large field (1 kOe) suggest that the transition metal ions were Mn4+ and Ni2+ as
which may have skewed the values. Note, as expected, the TC values determined by refinement of the X-ray powder diffraction and
are consistently slightly less than the corresponding u values. subsequent bond valence analysis as well as the studies of the
R2NiMnO6 oxides show the characteristic ferromagnetic TC and ferromagnetic moment and paramagnetic susceptibility. All the
positive u values that vary systematically with the radius of the R3+ phases were insulators exhibiting relatively low dielectric loss
atom (Fig. 3). The variation of TC in this series of oxides has been and dielectric constants in the range 15–25, another indication of
correlated with cos2 w where w is hNi–O–Mni bond angle [10]. integral valency. The Curie temperature of the R2NiMnO6 series is
While the TC in general decreases with w which in turn depends on a linear function of the radius of R3+. Electron paramagnetic
the radius of the R3+ atom, we find a better correlation between TC resonance measurements indicate that the Mn–Ni network
and R3+ radius (VIII coordination) [23] (Fig. 3) than with w alone. interacts only weakly with the rare earth ions, as one might have
From 55Mn NMR experiments, Asai et al. [13] have shown that for expected from the dependence of Curie temperature on ionic
the R2NiMnO6 oxides, NMR hyperfine magnetic fields suggest a radius.
decrease of covalency of Ni–O and Mn–O bonds in these oxides as R
goes from La to Lu. TC is controlled not only by the angle w but also Acknowledgements
by the variation of covalency/ionicity of the Ni–O and Mn–O bonds.
R3+ radius seems to reflect both these effects and hence provides a We thank Mamata Tripathy for her help with the synthesis of
better correlation for the TC. R2NiMnO6 oxides. JG thanks the Department of Science and
Technology, Government of India, for the award of a Ramana
3.3. EPR studies Fellowship. KVR appreciates the support of DST, Government of
India, for the award of a CP-STIO fellowship. SEL acknowledges
The spin dynamics were studied by EPR. EPR lineshapes (cf. support by the University of Maryland NSF MRSEC DMR 0520471.
Fig. 4) were fit to a pair of Lorentzian curves centered at
H ¼ v h=g mB , where  h is Planck’s constant, and v the angular References
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