Applied Physics A (2022) 128:1012

https://doi.org/10.1007/s00339-022-06145-0

Study of ferromagnetic and ferroelectric properties of nanocrystalline

­Bi2Mn4O10
Shereef A. Fareed1   · Makram Ibrahim1 · Ahmed E. Hannora2 · M. M. El‑Desoky3

Received: 25 August 2022 / Accepted: 12 October 2022 / Published online: 29 October 2022
© The Author(s) 2022

Abstract
Nano-crystalline bismuth manganese oxide ­Bi2Mn4O10 was prepared from ­Bi2O3 and ­MnO2 by mechanochemical technique
at different milling times followed by heat treatment at 1073 K. The crystal structural were obtained using X-ray diffraction
(XRD) and TEM. We obtained the variation of the crystallite size and micro-strain with milling time. The magnetic param-
eters include the saturation magnetization, coercivity and squareness ratio were obtained by vibrating sample magnetometer
(VSM). Each of the coercive field, Squareness ratio and saturation magnetization increased with increasing the milling time.
The electrical conduction of the prepared samples was evaluated by AC conductivity measurements at different temperature,
the dielectric parameters were plotted against temperature at different frequencies. The conduction mechanism is described
by the correlated barrier hopping model (CBH). The recoverable energy density and loss energy was obtained to calculate
the storage energy efficiency.

Keywords  Bismuth manganese oxide · Nano-structure · Mechanochemical technique · AC electrical conductivity ·

Magnetic properties

1 Introduction valuable applications [4–10]. A multiferroic material has

ferroelectricity, ferromagnetism and/or ferroelasticity or
As a part of a series of studies, we are concerned in the generally, it has two or more ferroic polarization. Bis-
current work with the ferromagnetic, ferroelectric behav- muth manganese oxides such as B ­ i2Mn4O10 crystallizes
ior and AC conductivity of a mechanical treated samples in orthorhombic structure with space group (Pbam), the
(mix of ­Bi2O3 and ­MnO2) at different milling times fol- structure has two sites octahedral and pyramidal [11–13].
lowed by heat tenement at 1073 K. In a related published The coexistence of both ferromagnetic and ferroelectric
work [1], we investigate the DC conductivity and Seebeck properties attributed to the unpaired electrons and the
coefficient of the same samples, Bismuth manganese oxide orbital ordering of Manganese cations. There are different
with the chemical formula ­Bi2Mn4O10 was described as preparation methods for bismuth manganese oxides such
a multiferroic material [2, 3]. In general, bismuth man- as sol–gel combustion and high energy ball milling. The
ganese oxides and perovskite are very promising because preparation of the constituent oxides in a ball milling tech-
they mostly owned combinational properties lead to a wide nique required high energy and high pressure [14, 15]. For
example, The perovskite formula B ­ a0.85Ca0.15Zr0.1Ti0.9O3
formed in a single crystal starting from 8 h of milling time
* Shereef A. Fareed reaching to a complete homogeneous powder after 15 h.
[email protected]
One of the important parameters is the variation of the
1
Solar and Space Research Department, National Research dielectric constant with temperature, it was obtained at dif-
Institute of Astronomy and Geophysics (NRIAG), ferent frequencies [16]. This paper is reported to study the
Helwan 11421, Cairo, Egypt effect of mechanochemical preparation technique at dif-
2
Department of Sciences and Engineering Mathematics, ferent milling times followed by heat treatment at 1073 K
Faculty of Petroleum and Mining Engineering, Suez on the structure, ferroelectric, ferromagnetic and dielectric
University, Suez 4351, Egypt
properties of nanocrystalline ­Bi2Mn4O10.
3
Department of Physics, Faculty of Science, Suez University,
Suez 43518, Egypt

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1.1 Experimental work 2 Results and discussion

Source-materials from bismuth and manganese oxides 2.1 Structure

­(Bi2O3/MnO2) with high purity 99% were prepared using
the mechanochemical process, the oxides were mixed by Figure  1(a) shows the XRD patterns of mechanically
a ball milling machine for different milling times followed treated samples, it’s clear that the broadening increased
by heat treatment at 1073 K. The structure was investi- with increasing the milling time reaching to an amorphous
gated at different milling times (1, 5, 10, 30 and 50 h) state. The effect of heat treatment on the mechanically
using X-ray diffraction and High resolution magnified prepared samples at 1037 K and different times is shown
images of the transmission electron microscope using in Fig. 1b. According to The ICCD card “01-074-1096”,
the “SIEMENS D5000” X-ray diffractometer with tar- bismuth manganese oxide phase with chemical formu-
get CuKα radiation and the “JEOL 2100 HRT” HRTEM las ­Bi2Mn4O10 was formed after 5 h of milling time fol-
respectively. A portion of each sample was pressed using lowed by heat treatment at 1073 K. The phase ­Bi2Mn4O10
a uniaxial hydraulic press to form pellets with 10  mm formed in orthorhombic crystal structure and space group
diameter under applying pressure of five tons. The mag- Pbam. The samples at 30 and 50 h showed a small amount
netic parameters were obtained using the vibrating sample of tetragonal ­Mn3O4 phase with space group I41/amd, the
magnetometer (VSM) at room temperature using the “Lake orthorhombic phase B ­ i2Mn4O10 decreased after 10 h of mill-
shore 7410” VSM. ing time and it decomposes to α-Bi2O3 and α-Mn2O3. The
A computerized LCR meter bridge up to 1 MHz was ICCD card 03-065-2776 represents a few amount of M ­ n 3O 4
connected with electrical-controlled furnace to measure with tetragonal structure and space group 141/amd while the
the temperature-dependent AC electrical parameters. Saw- card 01-081-0563 represents the spectrum of bismuth oxide
yer–Tower circuit was used to obtain the electrical hystere- ­Bi12.8O12 with tetragonal system and space group 141/amd.
sis loop of one of the prepared samples to assure the value Figure 2 shows different formation percentages of the
of the ferroelectric/paraelectric transition temperature as phases ­Bi2Mn4O 10, ­Mn3O4 and ­Bi12.8O19.2 at each mill-
obtained from dielectric measurements. ing time. 88% of the phase B ­ i2Mn4O10 is formed with the

Fig. 1  XRD patterns of a mechanical treatment of the mixed oxides ­Bi2O3/MnO2 without heat treatment, b samples after heat treatment at
1037 K

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stoichiometry of some manganites on the magnetic and

electric properties is reported in many studies [1].
The full-width at half maximum (β) is obtained from the
highest peaks to calculate the crystallite size (L) of each
sample using Hall–Williamson as given in Eq. (1) [19]:
k𝜆
𝛽 cos 𝜃 = (1)
L
where λ is the wavelength, k is the Scherrer constant (shape
factor) and (θ) is the Bragg angle, β represent the full width
at half maximum of the highest peak which obtained using
“Origin” software. As shown in Fig. 3, the micro-strains
was estimated from the Hall-Williamson relation, it is var-
ied from 0.078 to 0.210 (%). The micro-strain generated in
the samples is related to their reaction during mechanical
treatment, this enhanced the destabilization of the crystal
Fig. 2  Percentages of the formed phases with milling time
structure.
Figure 4 shows The TEM images of the prepared samples
(heated at 1073 K) at different milling time of 5, 10 and 50 h,
the graphs show the multigrain structure at 50 nm magni-
fication scale clarifying the d-spacing, it was 2.7 Å for the
sample milled at 5 h, 2.4 Å for the sample milled at 10 h and
2.9 Å for the sample milled at 50 h. this agreed well with the
corresponding d values from XRD spectrum data. Figure 5
shows their diffraction patterns, spots and concentric cir-
cles confirmed the poly crystalline structure of the prepared
samples. The main phase planes are labeled at the sample
of 5 h of milling time.
As appeared from the TEM graphs, the sample (a) owned
the lower polycrystallinity compared with the samples
milled at 10 and 50 h. From XRD, the obtained average
crystallite size for the samples (a), (b) and (c) are 58, 108
and 101 nm respectively.
Fig. 3  Variation of crystallite size and micro-strain of heat-treated
samples against milling time in hours 2.2 Magnetic properties

The magnetic behavior of the prepared samples was inves-

smallest percentages of the other oxides (5% of ­Bi12.8O19.2 tigated by vibrating sample magnetometer. The obtained
and 7% of ­Mn3O4) at the milling time 5 h. Such a method magnetic ordering is generated from the unpaired electrons
in Fig. 2 has appeared in many published studies [17, 18]. of manganese cations [20]. As illustrated in Fig. 6 the mag-
The crystallite size varied from 47.6 to 110 nm, the vari- netic hysteresis loop of the samples milled at 5, 10 and 50 h
ation of micro-strain and crystallite size against milling showed soft magnetic behavior at room temperature, the cor-
time is illustrated in Fig. 3. The orthorhombic structure responding values of saturation magnetization (­ Ms), retentiv-
of ­Bi2Mn4O10 has (001) preferred orientation after 1 and ity ­(Mr), Coercivity (­ Hc) and squareness ratio are listed in
5 h of heat treatment. The octahedral-coordinated M ­ n4+ (Table 1). The sample at 5 h of milling time owned the mini-
3+
cations and M­ n cations are located in square pyramids. mum value of the coercive field (­ Hc) which is the required
The cation distribution and oxygen stoichiometry are con- field to minimize the magnetization to its minimum value.
sidered as the origin of the relatively phase difference at The obtained values of squareness ratio confirmed the soft
each milling time as well as the changes in the unit cell magnetic behavior of the three samples at room tempera-
volume and concentration of manganese cations “N”, so ture, it’s obvious that the softness decreased by increasing
the exchange interaction and the resultant magnetic and the milling time while each of the saturation magnetization
electric properties will be influenced. The effect of oxygen ­(Ms), retentivity (­ Mr) and Coercivity (­ Hc) was increased

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Page 4 of 11 S. A. Fareed et al.

Fig. 4  TEM of the heat-treated samples (1073 K) milled at different milling time a 5 h, b 10 h and c 50 h

with increasing the milling time. According to the obtained and 66 K for bismuth manganite [20, 22] which means
data in (Table 1), the samples can be used in high frequency that the ferromagnetic behavior take a place in lower tem-
applications or high energy conversion transducers [21]. perature. As clearly obtained, the increasing in magnetic
However, according to the above results it’s recom- parameters with increasing the milling time is backed to
mended to obtain the magnetic behavior at low tempera- structural distortion or different dopant ionic radii which
ture, this is agreed with previous research work stated reflect different percentages of the formed phases [23,
that, the Curie temperature lie approximately between 40 24].

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Fig. 5  TEM diffraction patterns of the heat-treated samples (1073 K)

milled at different milling time a 5 h, b 10 h and c 50 h

2.3 Dielectric properties
Fig. 6  VSM at room temperature for the heat-treated samples
(1073 K) milled at differentmilling time a 5 h, b 10 h and c 50 h
It is known that, the electrical energy storage in dielectric
materials is represented by the dielectric constant (ɛ‵) while
the dissipated energy is denoted by ɛ‶, the variation of ɛ‵, the dipoles polarization lag behind the applied electric field,
ɛ‶ and tan δ with temperature at different frequencies is ­ c is really matched with ferro-
to assure that the values of T
obtained in Figs. 7, 8 and 9 for the heat-treated samples electricity, we plot the electric hysteresis loop (Fig. 10) of
milled at 5, 10 and 50 h. The highest appeared peaks are the sample milled at 50 h, we noted that the loop is nearly
due to the ferroelectric transition temperature (­ Tc) where disappeared at 453  K which is approximately the same

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Page 6 of 11 S. A. Fareed et al.

Table 1  Magnetic parameters of the sample milled for 50 h at room

temperature
`Milling Squareness ratio Mr (emu/g) Ms (emu/g) Hc (G)
time (h)

5 0.014 0.00117 0.0842 41.157

10 0.021 0.00184 0.0864 55.277
50 0.194 0.35990 1.8552 119.67

temperature (456 K) at the highest peak. The other small

peak is related to structural changes as reported previously
[25]. It’s obvious that the ferroelectricity transition tem-
perature is decreasing with increasing the milling time. We
evaluate the energy storage properties of the samples, Eqs. 2,
3 and 4 show how we can obtain the recoverable energy den-
sity (Wr), total energy density (Wt) and the energy storage
efficiency (η) respectively. At room temperature (303 K), the
value of Wr was 0.0496 mj/cm3 with energy loss W(loss) of
3.8895 mj/cm3 while at 453 K, Wr increased to 68.789 mj/
cm3 and the energy loss decreased to be 0.99 mj/cm3.
P max

∫Pr
Wr = EdP (2)

P max

∫0
Wt = EdP (3)

Wr
𝜂= × 100 (4)
Wr + W(loss)

where Pmax, E, Pr, and W(loss) are maximum polarization,

applied electric field, remnant polarization, and energy loss
density. The Wt, Wr and W(loss) are calculated by measur-
ing the internal and external areas of the polarization versus
electric field (P–E) curves. The energy storage efficiency (η)
increased from 1.26% at 303 K to be 98% at 453 K.
The dielectric constant varied with milling time due to
the different percentage of the formed phases which illus-
trated in Fig. 2, it's obvious that the sample after 5 h of mill-
ing time owned the maximum value of dielectric constant
(approximately 20,000 at 100 Hz). The dissipation factor or
loss tangent tanδ is given from the ratio in Eq. 5.

𝜀� (𝜔)
Tan𝛿 = (5)
𝜀�� (𝜔)
Fig. 7  Variation of ɛ/ with temperature at different frequencies for the
where ω = 2πf. [21, 22]s heat-treated samples (1073 K) milled at different milling time a 5 h, b
10 h and c 50 h
The temperature-dependence of loss tangent is shown
in Fig.  9 its clear that tan δ increases with increasing

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Fig. 8  Variation of ɛ// with temperature at different frequencies for the

heat-treated amples (1073 K) milled at different milling time a 5 h, b
10 h and c 50 h Fig. 9  Variation of tan δ with temperature at different frequencies for
the heat-treated samples (1073  K) milled at different milling time a
5 h, b 10 h and c 50 h

temperature, this is due to the thermal activation of elec-

trons, the observed peaks at low temperature is attrib- the relaxation is belong to the oxygen vacancies [24].
uted to the electrons hopping frequency matching with Figure 11 represents the frequency dependent electrical
frequency of applied electric field. At high temperature modulus where the semi-circular arcs of the real modulus

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Page 8 of 11 S. A. Fareed et al.

Fig. 10  ferroelectric hysteresis loops of the prepared sample (milled

at 50 h) at different temperature a at 303 K, b at 353 K and c at 453 K

Fig. 11  Variation of M" versus M‵for the heat-treated samples

(M‵) versus the imaginary (M‶) is plotted for the samples (1073 K) milled at different milling time a 5 h, b 10 h and c 50 h
milled at 5, 10 and 50 h, the modulus M‵ and M‶ are given
by the following equations [26]: 𝜀�
M� = (6)
𝜀�2 + 𝜀��2

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Study of ferromagnetic and ferroelectric properties of nanocrystalline ­Bi2Mn4O10 Page 9 of 11  1012

𝜀��
M �� = (7)
𝜀�2 + 𝜀��2

The peaks are attributed to the short and long range hop-
ping of charge carrier from an ionic state to neighboring
ionic one.
As appeared from the Relaxation processes, At high
frequency, the large semi-circular arcs represent the bulk
or grain response while at low frequencies, the weak grain
boundaries effect took a place [27]
Figure 12 shows the variation of logarithmic AC con-
ductivity with 1000/T at different frequencies for the heat-
treated samples (at 1073 K) milled at different time 5, 10
and 50 h.
The logarithmic a.c. conductivity increased with increas-
ing temperature for all samples except the sample at 5 h of
milling time where at low temperature it increased with
temperature and then decreased gradually to its minimum
value and redirected again to increased with the higher tem-
perature degrees, at the first vertex point, the hopping of
charge carrier is influenced by the applied frequency more
than the thermal energy and inversely, at the second vertex,
the thermal energy overcame the frequency effect.
The a.c. conductivity is related to the DC by Jonscher
relation:

𝜎ac = 𝜎dc + A𝜔S (8)

where ω is the angular frequency. A 𝜔S represents the pure

AC conductivity. A is constant, A = πN2e2/6KBT(2α) N is the
number of sites per unit volume among which hopping takes
place. S is the frequency exponent, 0 ≤ s ≤ 1.
The conductivity mechanism could be explained by the
temperature-dependent behavior of (s), Several models were
proposed in previous work [28–32], the exponent s can be
calculated from the slope of ln σ versus ln ω at different
temperature as shown in Fig. 13, the temperature depend-
ency of s values are obtained in Fig. 14. It’s obvious that the
exponent s decreased with increasing temperature, in this
range the conduction mechanism can be described by the
correlated barrier hopping (CBH).

3 Conclusion

The mechanochemical milling time is not linear param-

eter for preparing the phase ­Bi2Mn4O10. According to the Fig. 12  Variation of logarithm A.C. conductivity with 1000/T at dif-
squareness ratio which is ranged from 0.014 to 0.194, all ferent frequencies for the heat-treated samples (1073 K) milled at dif-
the prepared samples behave a soft magnetic ordering ferent milling time a 5 h, b 10 h and c 50 h
at room temperature. The sample milled at 5 h which is

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Page 10 of 11 S. A. Fareed et al.

is the same temperature of the transition peak of the tem-

perature-dependent dielectric constant. The energy storage
efficiency (η) of the sample milled at 50 h increased from
1.26% at 303 K to 98% at 453 K, accordingly, the prepared
samples can be applied as energy transducer (due to their
ferroelectricity) at the temperature range (450–600 K).
The conduction mechanism can be described by the cor-
related barrier hopping (CBH). The above results leading
us to try more different milling times to shift up the ferro-
electric transition temperature to get an energy transducer
works at high temperature.

Author contributions  Study conception—SAF, MI, AEH, MMEl-D.

Data collection—SAF. Analysis and interpretation of results—SAF,
AEH, MMEl-D. Draft manuscript preparation—SAF, MIb, AEH,
MMEl-D. All authors reviewed the results and approved the final ver-
sion of the manuscript. The author confirms sole responsibility for
Fig. 13  Variation of Ln σ with Ln ω at different temperature for the “study conception”, “data collection”, “analysis and interpretation of
samples milled at 5 h results”, and “manuscript preparation”.

Funding  Open access funding provided by The Science, Technology

& Innovation Funding Authority (STDF) in cooperation with The
Egyptian Knowledge Bank (EKB). We declare that, no funding was
received for this work.

Declarations 
Conflict of interest  The authors declare that they have no known com-
peting financial interests or personal relationships that could have ap-
peared to influence the work reported in this paper.

Ethical approval  We confirm that we took in consideration all the ethi-

cal rules in the this research work.

Open Access  This article is licensed under a Creative Commons Attri-

bution 4.0 International License, which permits use, sharing, adapta-
tion, distribution and reproduction in any medium or format, as long
as you give appropriate credit to the original author(s) and the source,
provide a link to the Creative Commons licence, and indicate if changes
were made. The images or other third party material in this article are
included in the article's Creative Commons licence, unless indicated
otherwise in a credit line to the material. If material is not included in
Fig. 14  Variation of exponent S with temperature for the samples the article's Creative Commons licence and your intended use is not
milled at 5 h permitted by statutory regulation or exceeds the permitted use, you will
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formed by 88% of ­Bi2Mn4O10 with only 5% of B ­ i12.8O19.2

and 7% of ­Mn3O4 is magnetically the softer one relatively
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