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A R T I C LE I N FO A B S T R A C T
Keywords: Polycrystalline ZneZr substituted barium hexaferrite (BaFe12-xZnx/2Zrx/2O19 where x = 0.3, 0.5, 0.7 and 1.0)
Barium hexaferrite specimen have been synthesized by two different methods, namely conventional and microwave sintering. The
Microwave sintering latter has resulted in magnetoplumbite phase in 5 min at a lower temperature (1000 °C). The values of magnetic
Cation substitution parameters of different samples are extracted from the corresponding M − H loops using law of approach to
Raman spectroscopy
saturation magnetization. A high value of saturation magnetization (Ms = 76 emu/g) is obtained for a con-
Saturation magnetization
Coercivity
ventionally sintered sample. Still higher value of saturation magnetization (Ms = 104 emu/g) has been obtained
for the microwave sintered cation substituted sample. The increase in the magnetization has been attributed to
the magnetic reordering of iron cations in the non-magnetic Zn2+-Zr4+ substituted samples. The coercivity of
the microwave processed substituted samples has been drastically reduced to 163 Oe (from 2961 Oe for con-
ventionally sintered pristine sample). The observed decrement can be ascribed to the increase in particle size and
reduction in magnetocrystalline anisotropy (2.58 × 106 erg/cc). Raman spectra of the substituted samples have
shown a shift in the vibrational frequencies (characteristic of magnetoplumbite phase) with cation substitution.
This suggests that the non-magnetic ZneZr cations replace Fe3+ from certain interstitial sites (4f1, 4f2, 2b and
12k).
1. Introduction and iron ions occupy the interstitial sites. The interstitial sites are oc-
tahedral (2a, 12k, 4f2), tetrahedral 4f1, and trigonal bipyramidal (2b).
Hexaferrites are known to be very promising candidates for their The M-hexaferrites substituted in Fe-positions with Al or In are pro-
technical use in magnetic recording, permanent magnets, microwave mising for practical uses [5–8].
devices, etc. [1,2]. The importance of these materials lies in their The properties of pristine and cation substituted BHF samples can be
striking properties like high saturation magnetization, high coercivity, modified by the method of preparation and processing conditions [9]. A
high anisotropy field, high resistivity, chemical inertness, etc. The number of preparation techniques, including crystallization of glass
properties in turn depend on their preparation method, particle size, ceramic [10], low temperature cofiring of ceramics [11], salt melt
sintering technique, and most importantly on their composition/struc- technique [12], hydrothermal synthesis [13], ammonium nitrate melt
ture. The structure of barium hexaferrite is same as that of magneto- method [14], water-in-oil micro-emulsion procedure [15], chemical co-
plumbite, and hence it is known as M-Barium hexaferrite (M-BHF or precipitation [16], one step solvent free gel synthesis technique [17],
simply BaM). The crystal structure of diamagnetically doped barium and citrate precursor method [18] have been employed to prepare
hexaferrites may be described by two space groups. One of them is pristine and substituted BaM samples. New techniques such as micro-
classical P63/mmc (No.194). Second of them is P63/mc (No.186) space wave sintering, thin film formation, ion irradiation etc. are being ap-
group. Second space group has been used for describing the crystal plied to modify the structure and hence magnetic properties of hex-
structure to explain the existence of non-zero spontaneous polarization. aferrites [19–21]. Microwave sintering is a new, rapid, green, economic
This is a polar non-centrosymmetric space group [3,4]. A unit cell of technique of heating/modifying the materials including nonmetals and
BaM consists of two formula units of BaFe12O19, i.e. a total of 64 ions. alloys [22].
Oxygen ions form the closed packed arrangement (as in hcp and fcc) The large spontaneous polarization and multiferroic properties at
∗
Corresponding author.
E-mail address: phz118138@physics.iitd.ac.in (M. Sharma).
1
Present Address: Department of Physics, Government College for Women Jind, Jind-126102, India.
2
Former Professor, Department of Physics, Indian Institute of Technology Delhi.
https://doi.org/10.1016/j.ceramint.2019.02.136
Received 25 June 2018; Received in revised form 19 February 2019; Accepted 19 February 2019
Available online 20 February 2019
0272-8842/ © 2019 Published by Elsevier Ltd.
M. Sharma and S.C. Kashyap Ceramics International 45 (2019) 11226–11232
Fig. 1. X-ray diffractograms of (a) Conventionally Sintered (CS) and (b) microwave sintered (MS) polycrystalline BaFe(12-x)Znx/2Zrx/2O19 samples.
room temperature have been recently discovered in diamagnetic ca- CSBHFZZ07, CSBHFZZ10, and MSBHFZZ03, MSBHFZZ05 and
tions substituted barium hexaferrites. Herewith the magnetoelectric MSBHFZZ07, where ZZ represent zinc and zirconium, and the numbers
characteristics of M-type hexaferrites fabricated by a modified ceramic following the alphabets are 10x values (represented in 2 digits) in
technique are more advanced than those for the well-known room BaFe12-xZnx/2Zrx/2O19.
temperature BiFeO3 orthoferrite multiferroics [23–26]. The magnetic The structural characterization of the prepared samples was carried
properties of BaM can also be altered simply by the spin imbalance out using x-ray diffraction (X-Pert PRO Philips) technique in θ–2θ
induced either by cation substitution or by cation rearrangement in the geometry using Cu Kα radiation (λ = 1.54060 Å) with a step size Δ (2θ)
unit cell. It may be noted that the double cation pairs like ZneZr, of 0.05°. The morphology and particle size were investigated by em-
ZneSn, MgeTi, CoeTi, LaePr, NieZr substitute iron cations in BHF ploying a scanning electron microscope (Zeiss EVO 50). The magnetic
from spin up/down sites and hence modify the magnetic properties parameters like magnetization (M) and coercivity (Hc) of the samples
[27–32]. It is reported that by varying the concentration of ZneSn, were estimated from the room temperature hysteresis measurements
optimal magnetic properties are achieved for high density magnetic (M − H curves) which were carried out by using VSM option of 14-T
recording applications [28]. The high value of Hc in NieZr substituted PPMS (Quantum Design) at a maximum field of 50 kOe. Raman spectra
BHF is attributed to the single domain particles. Further reduction in of the samples were recorded using Renishaw Invia Raman microscope
coercivity has been reported in NieZr substituted BHF with increase in equipped with a 10 mW HeeNe laser of wavelength 632.8 nm and a
the concentration of substituents because of decrease in magnetocrys- Leica microscope.
talline anisotropy [33]. It is found that the crystallinity of triple cation
substituted BHF decreases with increase in substituent concentration.
The perfect hexagonal particles with improved magnetic parameters 3. Results and discussion
were formed at lower temperature and even at lower concentration of
triple ions e.g CoeZneSn which can make it suitable for different uses 3.1. Structural characterization
[34].
In our laboratory the Fe3+ cations are successfully substituted in Oxygen excess or deficit in a sample can increase and decrease the
bulk barium hexaferrite specimen by either one cation (Zn), two cation oxidation degree of 3d-metals. The changing of charge state of 3d-
pair (MgeZr) or three cations (MgeZneZr) in either conventionally metals as a consequence of changing of oxygen content changes the
sintered (CS) and/or microwave sintered samples [22]. In this paper, a magnetic parameters such as the Curie temperature and magnetic mo-
brief account of modification of magnetic properties of M-BHF realized ment and electrical parameters such as the resistivity and value of band
by both, substitution of ZneZr ions for iron ions and by microwave gap which either increase or decrease [35]. The oxidation degree of 3d
sintering (MS), is presented. metals may change the unit cell parameters also [36]. The cation or-
dering is reported to enhance the Curie temperature (Tc) by two times
the Tc of cation disordered compounds [37]. The magnetic parameters
2. Experimental are assumed to be unchanged because of the oxygen deficiency because
of sintering in oxygen atmosphere.
Powders of BaFe12-xZnx/2Zrx/2O19 (where x = 0.3, 0.5, 0.7 and 1.0) Fig. 1(a) and (b) illustrate the x-ray diffractograms of all the con-
were prepared by solid state reaction technique. A mixture of stoi- ventionally- and microwave-sintered samples of BaFe12-xZnx/2Zrx/2O19.
chiometric amounts of BaCO3, Fe2O3, ZnO and ZrO2 powders was ball Single magnetoplumbite phase (JCPDS#39–1433) formation is con-
milled for 24 h. The mixed powder was dried and subjected to calci- firmed in all the conventionally sintered samples. However in case of
nation at 1000 °C for 10 h. Thereafter 2 wt % binder (Polyvinyl alcohol) MSBHFZZ05 sample, an impurity peak is observed near 33° in the dif-
was added to the calcined powder. The pellets of this powder were fractogram. A shift of all the peaks in the diffractograms to lower angle
sintered separately in a conventional furnace at 1200 °C for 5 h and in a side indicates an increase in the lattice parameters. The lattice para-
single mode (H-field) microwave cavity at 1000 °C for 5 min. The meters are calculated using the following relation:
emissivity of pyrometer was set at 0.64. The samples of different
composition synthesized either by conventional sintering (CS) or mi- 1 4(h2 + hk + k 2 ) l2
2
= 2
+ 2
crowave sintering (MS) have been named as CSBHFZZ03, CSBHFZZ05, d 3a c
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M. Sharma and S.C. Kashyap Ceramics International 45 (2019) 11226–11232
Table 1 ratio of c/a, in CS as well as MS samples, is lower than 3.98 (Table 1),
Lattice parameters (a and c), c/a ratio, unit cell volume, average crystallite size, and hence supports the formation of the M-type hexagonal structure
and average particle size of conventionally sintered (CS) and microwave sin- [38]. It may be noted from the Table that the lattice parameter a in-
tered (MS) pristine and cation substituted BHF specimen. creases marginally (up to a maximum of 0.34%) whereas c shows a
Sample a (Å) c (Å) c/a Unit cell Average Average higher increment (up to a maximum of 0.75%) with an increase in the
volume Crystallite Particle concentration of substituents (ZneZr cations) upto 8.33% of iron ca-
(Å3) Size (D) (nm) Size (nm) tions in CS samples. The lattice parameters may change with oxygen
a
CSBHF00 5.888 23.210 3.942 696.83 52 598
stoichiometery [36], however, the variation in the same has been stu-
CSBHFZZ03 5.897 23.279 3.947 701.04 24 412 died with concentration of the substituted ions and plotted with non-
CSBHFZZ05 5.901 23.315 3.951 703.08 27 474 linear interpolation in Fig. 2. In MS samples, the value of a increases
CSBHFZZ07 5.907 23.362 3.955 705.93 24 579 from 5.885 to 5.919 (0.58%) and c increases from 23.261 to 23.429 Å
CSBHFZZ10 5.908 23.384 3.960 706.83 23 627
b (0.72%) as concentration of ZneZr cations is increased up to 6.19% of
MSBHF00 5.885 23.261 3.953 697.65 46 650
MSBHFZZ03 5.905 23.314 3.948 704.00 46 880 Fe cations. This is because of larger ionic radii of the zinc and zirconium
MSBHFZZ05 5.913 23.392 3.956 708.27 51 – cations as compared to that of iron cations. The ionic radii of iron
MSBHFZZ07 5.919 23.429 3.958 710.83 37 2000 (Fe3+), zinc (Zn2+) and zirconium (Zr4+) cations in tetrahedral co-
a
ordination are 0.49 Å, 0.60 Å, and 0.59 Å; whereas in octahedral co-
Reference [15]. ordination the corresponding values are 0.55 Å, 0.74 Å and 0.72 Å re-
b
Reference [16].
spectively [39].
The crystallite size (Dhkl) is calculated using Scherrer equation:
0.89λ
Dhkl =
β cos θ hkl
Fig. 3. Scanning electron micrographs of BaFe(12-x)Znx/2Zrx/2O19 samples: (a),(b),(c), and (d) correspond to CS samples; (e) and (f) correspond to microwave sintered
at 1000 °C for 5 min. In addition to size distribution, average particle size is also depicted in the histograms.
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M. Sharma and S.C. Kashyap Ceramics International 45 (2019) 11226–11232
There are 64 atoms in a unit cell of barium hexaferrite which give The magnetic moment of pure BHF is only because of magnetic
rise to 189 modes of vibration. Forty two of these modes are Raman cations i.e. Fe3+. At absolute zero, the spin direction of magnetic ca-
active (11A1g+ 14E1g + 17E2g); 30 are IR active (13A2u +17E1u) and tions at 2a, 2b and 12k (a total of 16) is in one direction (upward di-
the remaining modes i.e. 3A1u + 4A2g+ 13B1g + 4B1u + 3B2g + 12B2u rection) whereas spin of cations at 4f1 and 4f2 (a total of 8) is in another
+ 15E2u are silent. Out of the 42 Raman active modes, 32 frequencies (downward) direction [46]. Thus net magnetization per formula unit of
(A1g, E1g, and E2g) were observed at room temperature in the range of BaFe12O19 is given by M = M2a (↑) + M2b (↑) + 6M12k (↑) – 2M4f1 (↓) –
173–713 cm−1 and assigned to various polyhedra in the unit cell 2M4f2 (↓) which is equal to 20 μB.
The M − H loops of ZneZr substituted BHF samples, sintered
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M. Sharma and S.C. Kashyap Ceramics International 45 (2019) 11226–11232
Table 2
Raman frequencies and area under the peaks (shown inside the bracket) in the spectra of conventionally sintered pristine and substituted BHF specimen.
Mode (1) A1g, E2g (2) A1g, E2g (3) A1g (4) E1g (5) A1g (6) A1g (7) A1g
CSBHF 338 (5.1) 412 (7.0) 469 (3.0) 526 (6.93) 615 (10.3) 685 (28.3) 721 (6.3)
CSBHFZZ03 337 (5.0) 412 (4.1) 466 (3.0) 523 (5.45) 614 (9.2) 684 (33.5) 718 (4.2)
CSBHFZZ05 337 (6.1) 412 (3.6) 466 (2.2) 522 (4.74) 615 (8.0) 685 (32.6) 718 (3.8)
CSBHFZZ07 335 (7.6) 410 (4.2) 463 (2.9) 519 (6.38) 613 (8.1) 683 (34.7) 717 (3.2)
CSBHFZZ10 336 (8.3) 409 (4.9) 463 (2.5) 518 (6.17) 614 (8.8) 683 (32.5) 717 (2.9)
Fig. 5. The M − H loops of polycrystalline BaFe(12-x)Znx/2Zrx/2O19 samples: (a) Conventionally sintered (CS) at 1200 °C for 5 h and (b) its expanded M − H loops (c)
microwave sintered (MS) at 1000 °C for 5 min (d) its expanded M − H loops. Figures (b) and (d) clearly depict the changes in magnetic parameters with composition
and processing techniques.
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M. Sharma and S.C. Kashyap Ceramics International 45 (2019) 11226–11232
are 1653 Oe and 1000 Oe. The observed high value of coercivity of
pristine samples is expected to result from the strong uniaxial aniso-
tropy along c-axis. The non magnetic cation substitution disrupts the
uniaxial anisotropy, as evidenced by the decrease in anisotropy field
(Table 3), and results in drastic decrease in coercivity (by nearly 92% in
CS samples and by 83% in MS samples). In addition the variation in
particle size also contributes to the change in Hc.
The variation in estimated anisotropy field (Ha) and effective ani-
sotropy constant (K1) due to addition of substituents is shown in Fig. 6.
It can be clearly seen from the figure that the effective anisotropy
constant decreases rapidly with increase in the concentration of sub-
stituents. It is reported that the maximum contribution to the aniso-
tropy comes from 2b site (1.40 cm−1/ion) and minimum contribution
from 4f1 site (0.18 cm−1/ion) whereas contribution from 12k site is
negative (−0.18 cm−1/ion). The contributions from the other sites 2a
and 4f2 are reported to be 0.23 and 0.51 respectively [52]. The aniso-
Fig. 6. Variation of first anisotropy constant (K1) and anisotropy field (Ha) with tropy constant (K1) is expected to decrease when Zn2+ ions substitute
concentration (x) of ZneZr cations in polycrystalline BaFe(12-x)Znx/2Zrx/2O19
Fe3+ ions at 4f1/4f2 sites and Zr4+ ions occupy the bipyramid (2b) or
samples.
octahedral sites in BHF samples.
2 3 4. Conclusions
C=− Ha
105
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M. Sharma and S.C. Kashyap Ceramics International 45 (2019) 11226–11232
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