ISSN 1070-3632, Russian Journal of General Chemistry, 2017, Vol. 87, No. 5, pp. 899–905. © Pleiades Publishing, Ltd.

, 2017.
Original Russian Text © N.V. Chezhina, D.A. Korolev, A.V. Fedorova, N.A. Zhuk, V.A. Butin, V.P. Lutoev, B.A. Makeev, S.S. Shevchuk, A.N. Nizovtsev,
2017, published in Zhurnal Obshchei Khimii, 2017, Vol. 87, No. 5, pp. 705–711.

Structure, Magnetic, and Electrical Properties

of Bismuth Niobates Doped with d-Elements:
XVI.1 Magnetic Properties of Manganese-Containing Solid
Solutions of Bismuth Orthoniobate BiNiO4
N. V. Chezhinaa*, D. A. Koroleva, A. V. Fedorovaa, N. A. Zhukb, V. A. Butinb,
V. P. Lutoevc, B. A. Makeevc, S. S. Shevchukc, and A. N. Nizovtsevd
a
St. Petersburg State University, Universitetskaya nab. 7–9, St. Petersburg, 199034 Russia
*e-mail: n.chezhina@spbu.ru
b
Syktyvkar State University, Syktyvkar, Russia
c
Institute of Geology, Komi Scientific Center, Ural Branch, Russian Academy of Sciences, Syktyvkar, Russia
d
Institute of Biology, Komi Scientific Center, Ural Branch, Russian Academy of Sciences, Syktyvkar, Russia

Received January 26, 2017

Abstract—Magnetic susceptibility and ESR properties of manganese-containing solid solutions of bismuth

orthoniobate BiNb1–xMnxO4–δ have been studied. Mn(II), Mn(III), and Mn(IV) atoms as well as their dimers
exhibiting antiferro- and ferromagnetic types of exchange have been found in the solid solutions. Parameters of
the exchange interactions in the clusters and the distribution of monomers and dimers of manganese atoms in
the solid solutions have been calculated as functions of the paramagnetic atom fraction.
Keywords: bismuth niobate, magnetic properties, exchange interaction
DOI: 10.1134/S1070363217050012

Emerging interest to bismuth niobate is associated
with the discovery of its catalytic [2] and microwave
dielectric properties [3]. Owing to low synthesis
temperature, solid solutions of bismuth niobate are
accessible and can be used as dielectric interlayers in
monolithic condensers and in interference suppression
filters for microwave apparatus consisting of alternat-
ing thin layers of a ceramic dielectric and low-melting
electric conductors [4, 5]. To optimize dielectric
properties of bismuth orthoniobate, its composition is
modified by hetero- and isovalent substitution of
bismuth [6–13] or niobium atoms [6, 14–18]. Selection
of the composition of the ceramics is determined by
the closeness of ionic radii of atoms and by the melting
point of the substituting metal oxide. The issues of the
distribution and electronic state of substituting atoms
as well as the type of interatomic interactions between
them have not been adequately investigated so far.
1
For communication XV, see [1].
In this work, we studied the distribution and elec-
tronic state of paramagnetic manganese atoms in the
solid solutions of bismuth orthoniobate by means of
ESR and static magnetic susceptibility measurements.
The crystal structure of orthorhombic modification of
bismuth niobate (Рnna, a 0.5675, b 1.171, c 0.4980 nm)
can be regarded as a layered structure [19]. The Nb–O
octahedra connected via their side apexes form the
layers along the ac plane (Fig. 1), with niobium atoms
forming a square network. The octahedra are coupled
in such a way that their axial planes are shifted (along
the a axis) and bent with respect to each other by
certain angle. The niobium-oxygen octahedra are
distorted and exhibit three pairs of equivalent Nb–O
distances; the bond lengths vary from 1.847 to 2.159 Å.
Bismuth atoms also form layers located along the
crystallographic ac plane making up a square network
similarly to niobium atoms, but they occupy squares
not filled by niobium. Polyhedral surrounding of the
bismuth atom cannot be described in terms of regular

899
900 CHEZHINA et al.

10 μm

Fig. 2. Microscopy image of the BiNb0.94Mn0.06O4–δ sample

Fig. 1. Crystal structure of bismuth orthoniobate, BiNbO4. surface.

symmetric geometric objects; this is a figure with six
apexes, its interatomic Bi–O distances being non-
equivalent. Three pairs of various distances can be
detected, one pair of Bi–O bonds being the longest
(2.740 Å).
The BiNb1–xMnxO4–δ solid solutions with the
composition range 0.005 ≤ x ≤ 0.06 were obtained.
Scanning electron microscopy studies showed that the
solid solutions samples were porous compacts
consisting of crystalline grains (and their aggregates)
not exceeding 2.5 µm in size and close to rounded
rhombs in shape (Fig. 2). The chemical composition of
the samples corresponded to the expected formula, and
manganese atoms were incorporated in the structure of
bismuth orthoniobate (the energy dispersion X-ray
spectroscopy data).
The X-ray diffraction pattern of the solid solution
(x = 0.06) is given in Fig. 3. The unit cell parameters
of the solid solutions were close to those of bismuth
orthoniobate: a 0.5678, b 1.1719, c 0.4982 nm (x =
0.06), reflecting isomorphous substitution of Nb(V)
ions with manganese ions close in the size
{r[Nb(V)CN=6] = 0.064, r[Mn(IV)CN=6] = 0.054,
r[Mn(III)CN=6] = 0.065, r[Mn(II) CN=6] = 0.083 nm}
[20].
Using magnetic susceptibility data for the solid
solutions, we calculated paramagnetic components of
magnetic susceptibility [χpara(Mn)] and effective mag-
netic moments [μeff(Mn)] of manganese atoms at
various temperatures and concentrations of solid
solutions. The diamagnetic corrections derived from
the susceptibility of the bismuth niobate BiNbO4 matrix

2θ, deg
Fig. 3. X-ray diffraction pattern of the BiNb0.94Mn0.06O4–δ sample.

RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 87 No. 5 2017

 STRUCTURE, MAGNETIC, AND ELECTRICAL PROPERTIES… : XVI.
(a)
χpara(Mn)×106, emu/mol
Fig. 4. (a) Isotherms of paramagnetic component of magnetic susceptibility of manganese-containing solid solutions at (1) 90,
(2) 140, (3) 200, (4) 260, and (5) 320 K and (b) temperature dependences of magnetic moment of manganese atoms in
BiNb1–xMnxO4–δ at х (1) 0.005, (2) 0.02, (3) 0.06.
measured over the same temperature range were
introduced in the calculations.
In the probed temperature range, reciprocal
paramagnetic component of magnetic susceptibility of
the manganese-containing solid solutions (per a mole
of manganese atoms) as a function of temperature
followed the Curie–Weiss law. The Weiss constant
was negative, indicative of antiferromagnetic exchange
interactions. The isotherms of paramagnetic component
of manganese magnetic susceptibility [χpara(Mn)] of the
solid solutions were typical of antiferromagnets
(Fig. 4a). The increase in temperature resulted in the
increase in the effective magnetic moment of manga-
nese atoms [μeff(Mn)] (calculated by extrapolating the
paramagnetic component of magnetic susceptibility to
infinite dilution) from 5.22 (90 K) to 5.56 µB (320 K)
to approach the pure-spin value of Mn(II) (μeff =
5.92 µB, ground term 6А1g) and Mn(III) (μeff =
4.92 µB, ground term 5Eg) atoms magnetic moment.
T, K 90 140 200 260
μeff(Mn), µB 5.22 5.37 5.46 5.53
Since the precursor for the solid solutions
preparation in air was Mn2O3, the presence of Mn(II)
could be due to the disproportionation of Mn(III) into
Mn(II) and Mn(IV) (μeff 3.87 µB, 4A2g), and their
presence in the solid solutions could not be neglected.
For the orbital nondegenerate or doubly degenerate
ground states of Mn(II), Mn(III), and Mn(IV) atoms,
the effective magnetic moment is temperature-inde-
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 87 No. 5 2017
901
(b)
μeff(Mn), µB
x T, K
pendent. Hence, its increase with temperature showed
that clusters of manganese atoms with predominantly
antiferromagnetic exchange, for example Mn(II)–O–
Mn(II), Mn(III)–O–Mn(III), or Mn(IV)–O–Mn(IV),
were present even in the infinitely dilute solid
solutions. When concentration of the solid solutions
increased, the temperature dependence of the magnetic
moment was retained (Fig. 4b).
ESR spectra of the BiNb1–xMnxO4–δ solid solutions
(х = 0.005, 0.02, and 0.06) contained a broad axially
symmetric absorption band with g|| ≈ 2.8 and g┴ ≈ 2.0
(Fig. 5). A poorly resolved structure was noticed in the
“perpendicular” component, seemingly the trace of
superfine splitting of the 55Mn signal. The ESR spectra
might be attributed to paramagnetic Mn(II) and
Mn(IV) ions in the axially symmetric crystal field. The
integral intensity of the spectrum was close to the
saturation region, increasing linearly only by a factor
of 1.5 with the increase in the manganese fraction by
an order of magnitude (from 0.005 up to 0.06). That
320 evidenced the presence of paramagnetic Mn(III) atoms
predominantly, giving no ESR signal at room tem-
5.56 perature. Judging from the concentration dependence,
the relative content of paramagnetic Mn(II) and
Mn(IV) paramagnetic ions decreased by an order of
magnitude as the total fraction of the element increased
over the probed range.
To estimate the distribution of manganese atoms in
the solid solutions and describe the exchange inter-
actions in the clusters as functions of the paramagnetic
atom fraction, we carried out a theoretical calculation
of magnetic susceptibility of the solid solutions. The
902 CHEZHINA et al.
mon mon mon dim
(a) (b) aMn(II) + aMn(III) + aMn(IV) + aMn(III)–Mn(III)
dim dim
S + aMn(IV)–Mn(IV) + aMn(II)–Mn(IV) = 1. (2)

mon mon mon

x = 0.06 In Eqs. (1–2), aMn(II), aMn(III), and aMn(IV) are the
x
fractions of Mn(II), Mn(III), and Mn(IV) monomers;
dim dim dim
aMn(III)–Mn(III), aMn(IV)–Mn(IV), and aMn(II)–Mn(II) are the

x = 0.02
fractions of dimers with antiferromagnetic exchange;
dim
aMn(II)–Mn(IV) is the fraction of dimers with ferro-
magnetic exchange.
x = 0.005 Formula (1) implicitly included the parameters of
antiferromagnetic exchange between manganese atoms
JMn(III)–Mn(III) and JMn(IV)–Mn(IV), and that of ferromagnetic
exchange JMn(II)–Mn(IV).
B, mТ According to the Heisenberg–Dirac–van Vleck
Fig. 5. (a) ESR spectra of the BiNb1–xMnxO4–δ solid solu- model [21], magnetic susceptibility of dimers con-
tions at х = 0.005, 0.02, and 0.06 and (b) dependences of sisting of paramagnetic atoms could be calculated
integral intensity of the spectral band g|| ~2.8 and g┴ ~2.0 on using Eq. (3).
manganese fraction x in BiNb1–xMnxO4–δ.
Σ g2(S')S'(S' + 1)(2S' + 1)e−E(J,S')/kT
experimental dependences of χpara(Mn) on concentra- S1−S2 1 S'
, (3)
χdim =
tion of the solid solutions were processed within the 2 8TΣ (2S' + 1)e−E(J,S')/kT
framework of the diluted solid solution model, which S'
implied that the susceptibility an additive sum of
contributions of single paramagnetic atoms with E(J, S') = –J[S'(S' + 1) – Sa(Sa + 1) – Sb(Sb + 1)],
(monomers) and their M–O–M aggregates (dimers). S' = Sa + Sb, Sa + Sb – 1,…, |Sa – Sb|, Sа, Sb being spins
We considered the presence of the following species in of the atoms in a dimer [Sа = Sb = 2 for the Mn(III)–O–
the BiNb1–xMnxO4–δ solid solutions: monomers [Mn(II) Mn(III) dimer, Sа = Sb = 3/2 for the Mn(IV)–O–
and Mn(IV) atoms] exhibiting signals in the ESR Mn(IV) dimer, and Sа = 5/2, Sb = 3/2 for the Mn(II)–O–
spectra along with the Mn(III) monomers and dimers Mn(IV)] dimer, g being the g-factor for Mn(III) and
with antiferromagnetic [Mn(III)–O–Mn(III), Mn(IV)– Mn(IV) atoms, J being the exchange parameter, and T
O–Mn(IV)] and ferromagnetic [Mn(II)–O–Mn(IV)] being absolute temperature.
types of exchange. We neglected the presence of the
The amount of experimental data on magnetic
Mn(II)–O–Mn(II) dimers due to low probability of
susceptibility as function of temperature and solid
their formation. The final formula for calculating the
solution concentration, was sufficient for estimating
paramagnetic component of manganese atoms as the
the exchange parameters and the fraction of clusters of
sum of contributions of monomers and dimers was as
paramagnetic atoms (cf. [22–24]).
shown in Eq. (1) under the condition Eq. (2).
para mon mon mon mon mon
χcalc(Mn) = aMn(II)χMn(II) + aMn(III)χMn(III) + aMn(IV)χMn(IV)
mon
Paramagnetic components of magnetic suscepti-
dim dim dim dim bility of Mn(II)–O–Mn(IV), Mn(III)–O–Mn(III), and
+ aMn(III)–Mn(III)χMn(III)–Mn(III) + aMn(IV)–Mn(IV)χMn(IV)–Mn(IV)
Mn(IV)–O–Mn(IV) dimers were calculated using
dim dim
+ aMn(II)–Mn(IV)χMn(II)–Mn(IV), (1) Eqs. (4)–(6), respectively.
5/2–3/2
1 180exp(7.5x) + 84exp(–0.5x) + 30exp(–6.5x) + 6exp(–10.5x)
χdim = —– ——–—————————————————————— , (4)
4T 9exp(7.5x) + 7exp(–0.5x) + 5exp(–6.5x) + 3exp(–10.5x)
2–2
1 180exp(8x) + 84 + 30exp(–6x) + 6exp(–10x)
χdim = —– —————————————————————— , (5)
4T 9exp(8x) + 7 + 5exp(–6x) + 3exp(–10x) + exp(–12x)
3/2–3/2
1 84exp(4.5x) + 30exp(–1.5x) + 6exp(–5.5x)
χdim = —– —————————————————————— , (6)
4T 7exp(4.5x) + 5exp(–1.5x) + 3exp(–5.5x) + exp(–7.5x)

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 STRUCTURE, MAGNETIC, AND ELECTRICAL PROPERTIES… : XVI. 903

Calculated distribution of manganese atoms in BiNb1-xMnxO4–δ solid solutionsa

mon min mon dim dim dim χexp(calc)×103, emu/mol

x aMn(II) aMn(III) aMn(IV) aMn(III)–Mn(III) aMn(IV)–Mn(IV) aMn(II)–Mn(IV)
140 K 200 K 260 K 320 K
0.000 0.080 0.198 0.070 0.255 0.0345 0.3625 25.5 18.5 14.6 12.0
(24.5) (17.4) (13.4) (10.8)
0.005 0.050 0.245 0.055 0.350 0.030 0.270 22.8 17.0 13.7 11.4
(22.4) (16.1) (12.5) (10.1)
0.001 0.040 0.275 0.050 0.395 0.026 0.214 21.4 15.9 12.8 10.7
(21.3) (15.4) (12.0) (9.8)
0.015 0.030 0.300 0.044 0.423 0.023 0.180 20.5 15.3 12.3 10.2
(20.6) (15.0) (11.7) (9.6)
0.020 0.018 0.325 0.037 0.457 0.020 0.143 19.9 14.9 12.0 10.0
(19.8) (14.5) (11.3) (9.3)
0.030 0.010 0.350 0.029 0.500 0.010 0.101 19.0 14.3 11.5 9.6
(19.0) (14.0) (11.0) (9.1)
0.040 0.000 0.370 0.020 0.530 0.000 0.080 18.5 13.8 11.1 9.3
(18.6) (13.7) (10.8) (8.9)
0.060 0.000 0.390 0.005 0.560 0.000 0.045 17.7 13.3 10.7 8.9
(18.0) (13.4) (10.6) (8.8)
a mon mon mon dim dim
aMn(II), aMn(III), aMn(IV) are fractions of monomers of Mn(II), Mn(III) and Mn(IV) atoms; aMn(III)–Mn(III), aMn(IV)–Mn(IV) are fractions of dimers
dim
with antiferromagnetic exchange; aMn(II)–Mn(IV) is fraction of dimers with ferromagnetic exchange type.

The agreement between the calculated and
experimental values was achieved by minimizing the
Σ Σ (χijcalc – χijexp)2 function, with Σ denoting summation
i j
j
over the concentrations, and Σj reflecting summation
over the temperatures; χijcalc and χijexp were experimental
and calculated paramagnetic components of magnetic
susceptibility of the solid solutions, respectively.
The best agreement between experimental and
calculated data for the solid solutions was obtained
with the following parameters: JMn(III)–Mn(III) = –9 cm–1
and JMn(IV)–Mn(IV) = –6 cm–1 for antiferromagnetic
exchange and JMn(II)–Mn(IV) = 50 cm–1 for ferromagnetic
exchange; the correlation between experimental and
theoretical magnetic susceptibilities of manganese
atoms in the BiNb1–xMnxO4–δ solid solutions is given in
the Table. The difference between experimental and
calculated molar magnetic susceptibility of manganese
atoms in the solid solutions did not exceed 5%.
The performed calculations revealed the presence
of Mn(II), Mn(III), and Mn(IV) atoms and their dimers
with antiferromagnetic and ferromagnetic exchange
types in the infinitely diluted solid solution (Fig. 6).
The simultaneous presence of Mn(II) and Mn(IV)
atoms was seemingly due to the disproportionation of
Mn(III) in dilute solid solutions, as evidenced by their
almost equal fractions in the solid solutions and by the
presence of Mn(II) atoms predominantly as ferro-
magnetically bound Mn(II)–O–Mn(IV) dimers.
Since the unit cell parameter was marginally changed
at low concentration of paramagnetic atoms, we
suggested that a fraction of isolated Mn(II) atoms with
larger ionic radius than that of niobium {r[Nb(V)CN=6]
0.064 and r[Mn(II)CN=6] 0.083 nm} was located in the
cation sites of Bi(III). Such a possibility of Mn(II)
atoms distribution has been earlier revealed for com-
plex bismuth niobates with the pyrochlore structure
[25]. The appearance of Mn(IV) atoms at low con-
centrations of the solid solutions partially compensates
for the charge misbalance resulting from the hetero-
valent substitution of niobium atoms [26, 27].
The increase in the concentration of the solid
solutions resulted in the decrease in the fractions of
Mn(II) and Mn(IV) atoms along with the increase in
the total fraction of Mn(III) atoms (in the forms of
monomer and exchange-bound dimers). The ESR data
showed that the integral intensity of the absorption
band of Mn(II) and Mn(IV) atoms in the solid solution
with x = 0.06 was only 1.5 times higher than that in the

RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 87 No. 5 2017

904
а paramagnetic atoms seems to be associated with the
Fig. 6. Fraction of dimers (1) Mn(III)–O–Mn(III),
(2) Mn(II)–O–Mn(IV) and monomers (3) Mn(III), (4) Mn(IV)
as functions of manganese ions in BiNb1-–xMnxO4–δ.
solution with x = 0.005, reflecting the increase in the
fraction of Mn(III) atoms that gave no ESR signal
down to very low temperatures. Hence, the stabiliza-
tion of the solid solution structure at high con-
centrations was due to the aggregation of paramagnetic
Mn(III) atoms.
The Mn(III) atoms were present in the solid
solutions as monomers and antiferromagnetically
bound dimers, their fraction increasing with the
growing solid solution concentration. The simulta-
neous increase in the magnetic moment with tem-
perature at various concentrations of manganese atoms
in the solid solutions showed that the exchange
parameter was independent of the total fractions of
paramagnetic clusters, coinciding with the calculation
results (Fig. 4b).
The parameters of antiferro- and ferromagnetic
exchange [JMn(III)–Mn(III) –9 cm–1 and JMn(II)–Mn(IV) 50 cm–1]
were substantially different, due to deviation of the
bond angle between exchange-bound manganese
atoms in the niobium sites (120°) from 180°. Accord-
ing to the theory of magnetic exchange [28], the
deviation of the exchange angle from 180° activates
the ferromagnetic-type channels dxy||py┴pz||dxz,
dx2–y2||px ┴pz||dxz and hampers the antiferromagnetic-
type channels dx2–y2||px||dx2–y2, and dx2–y2||py||dx2–y2,
dxy|py|dxy, and dxz|pz|dxz. Moreover, geometric distor-
tions of coordination polyhedrons and anion vacancies
also favor the ferromagnetic exchange. The mentioned
factors resulted in low value of the antiferromagnetic
exchange parameter. The formation of dimers rather
than the more complex aggregates or chains of
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 87 No. 5 2017
CHEZHINA et al.
low concentration of paramagnetic atoms in the solid
solutions.
EXPERIMENTAL
The solid solution samples were obtained via the
standard ceramic procedure from “special pure” grade
Bi(III), Nb(V), and Mn(III) oxides at 650 and 950°C.
Phase composition of the samples were monitored by
means of scanning electron microscopy (a Link energy
dispersion spectrometer) and X-ray phase analysis (a
х
DRON-4-13, CuKα emission). The unit cell parameters
of the solid solutions were calculated using the CSD
program package [29].
We determined manganese contents in the BiNb1–x·
MnxO4–δ solid solutions by means of atom emission
spectrometry (a SPECTRO CIROS spectrometer with
inductively bound plasma), the accuracy being ±5% of
x in the solid solution formula. We measured magnetic
susceptibility of the solid solutions by Faraday method
at 16 temperatures over the 77–400 K range. The
accuracy of the relative measurements was of ±1%.
The ESR spectra of polycrystalline samples of the
solid solutions were recorded using a RadioPAN SE/X
2547 radiospectrometer of X-diapason (Center for
Collective Usage “Geonauka,” Komi Scientific Center,
Ural Branch, Russian Academy of Sciences). The
spectra were recorded using a rectangular resonator
(RX102, TE 102 mode) at room temperature as the
first derivative at the HF modulation frequency of 100
MHz with the amplitude of 0.25 mT and the SHF field
power of 35 mW. A batch of a sample (≈100 mg) was
put into a quartz tube (external diameter 4 mm). We
used the ESR signal of miniature reference sample
(anthracite, singlet line g0 2.0032, ∆Bpp 0.5 mT) to
calibrate the amplification of the apparatus. The quartz
ampoule with the reference sample was rigidly fixed in
the resonator coaxially to the test tube with the
measured sample. For each sample, the spectrum in the
magnetic field range 0–700 mT and the lines of the
reference were separately recorded with the scan step
of 5 mT. Then the total spectra were normalized to the
reference line intensity and then to 100 mg of the
sample.
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