Materials Science for Energy Technologies 2 (2019) 455–462

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Materials Science for Energy Technologies

CHINESE ROOTS
GLOBAL IMPACT
journal homepage: www.keaipublishing.com/en/journals/materials-science-for-energy-technologies

Variation in structural and mechanical properties of Cd-doped Co-Zn

ferrites
Akshay B. Kulkarni a, Shridhar N. Mathad b
a
Department of Physics, Jain College of Engineering, Belagavi 590014, India
b
K.L.E. Institute of Technology, Hubballi 580030, India

a r t i c l e i n f o a b s t r a c t

Article history: Synthesis of cadmium doped cobalt zinc ferrite (Co0.5Zn0.5Cd1.5xFe2
xO4) series with x = 0.0, 0.1, 0.2, 0.3,
Received 2 February 2019 0.4, 0.5 by solid state method and analysis of structural properties using XRD, FTIR, and SEM character-
Revised 19 March 2019 ization. To understand the decomposition behavior of the precursors of samples TG/DTA analysis was car-
Accepted 20 March 2019
ried out. TG/DTA/DSC shows that reaction is endothermic in nature and the reaction completion
Available online 29 March 2019
temperature at around 730 °C. The XRD characterization of the samples affirms the cubic spinel structure.
Grains in the samples are having nature of octahedron, tetrahedron and granular depicted by SEM
Keywords:
images. The FTIR spectra of synthesized ferrites evidenced two strong absorption bands (m1 and m2) in
Co-Zn ferrite
TG/DTA/DSC
the range of 400–600 cm
1 belonging to tetrahedral (A) and octahedral (B) interstitial sites. In XRD anal-
FTIR ysis, the shrinkage of unit cell is observed at higher doping concentration. The peak (3 1 1) shown the
XRD maximum intensity for x = 0.0, whereas peak (3 1 0) shown maximum intensity for x = 0.5. Williamson
SEM Hall (WH) plot and size-strain plot (SSP) results show the variation in the grain size with change in dop-
ing concentration. The doping of cadmium plays an important role in crystal growth as observed in SEM
images. In FTIR analysis, peaks shift towards lower wave number with raise in doping concentration.
Ó 2019 The Authors. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-
nd/4.0/).

1. Introduction isolation and purification of genomic (DNA) and the separation of

polymerase chain reaction (PCR) ready DNA [5] and especially in
Ferrites are beneficial dielectric materials having low conduc- hyperthermia treatment [6].
tivity and have across-the-board applications in the field of micro- Cobalt zinc ferrite (Co0.5Zn0.5Fe2O4) magnetic nano-particles
wave devices [1]. Nano crystalline ferrites are technologically were used for further contrast enhancement in magnetic resonance
important materials owing to their unparalleled electric, dielectric, imaging (MRI) [7]. Zinc doped cobalt ferrites are subjected to alter-
magnetic and optical properties. Which make them suitable for nating magnetic field it demonstrates low energy loss [8]. Co-Zn
tons of technological applications like microwave devices, trans- ferrites in the bulk crystalline form prepared by usual ceramic
formers, electric generators, storage instrumentations, etc [2]. technique [9], chromium substituted nano particles of cobalt zinc
Use as photo-catalysts for the waste water treatment is a hot topic ferrites by co-precipitation method [10,11]. Structural and dielec-
for the environmental researcher [3]. CoFe2O4 has substantially tric studies of nickel doped cobalt zinc ferrites [12] and structural
been invoking on account of its large magnetic multi-axial aniso- studies of cadmium doped Co-Zn ferrites are widely reported [13].
tropy, moderate saturation magnetization, very high Curie temper- Mn doped Co-Zn ferrites (Co0.6Zn0.4MnxFe2
xO4) were successfully
ature (Tc) and remarkable chemical stability [4]. The nano cobalt synthesized by the sol–gel auto-combustion method and its elec-
ferrites particles are worthy contenders in the medical field like trical, magnetic properties and photo catalytic degradation activi-
ties reported [14,15].
However, the addition of cadmium transition metal effects on
Peer review under responsibility of KeAi Communications Co., Ltd. structural properties Co0.5Zn0.5Cd1.5xFe2
xO4 (x = 0.0, 0.1, 0.2, 0.3,
0.4, 0.5) have never been reported to our best knowledge. In this
manuscript we established the properties of Co0.5Zn0.5Cd1.5xFe2
xO4
synthesized by solid state method. The structural properties of fer-
Production and hosting by Elsevier rites have been explored by XRD, SEM and FTIR studies. The lattice

https://doi.org/10.1016/j.mset.2019.03.003
2589-2991/Ó 2019 The Authors. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
456 A.B. Kulkarni, S.N. Mathad / Materials Science for Energy Technologies 2 (2019) 455–462

parameters, crystallite size, hopping lengths, strain, dislocation

density, and mechanical properties of ferrites reported.

2. Experimental

All of the starting materials CoCl26H2O, ZnCl2, FeCl36H2O, and

CdCl2H2O were of analytical grade (molychem) used for the
synthesis of ferrites series samples by standard solid state reaction
method (shown in Fig. 1). The chemicals are taken in stoichiomet-
ric proportion and the mixture of chemicals is finely powdered and
thoroughly mixed in agate mortar, few drop of distilled water is
used as media for better uniformity. The mixture is heated in a
muffle furnace (meta lab scientific industries, mumbai) at 800 °C
for 4 h. The chemical reaction is given below.

CoCl2  6H2 O þ ZnCl2 þ FeCl3  6H2 O þ CdCl2  H2 O Fig. 2. TG/DTA/DSC graph of Co0.5Zn0.5Cd1.5xFe2
xO4 with x = 0.2.

! Co0:5 Zn0:5 Cdx Fe2
x O4 þ nH2 O " þnCl2 " ð1Þ

Structural characterization of the ferrite powders are carried

out. The TG/DTA/DSC curves of the sample have been obtained
on Perkin Elmer, Diamond TG/DTA and Mettler Toledo DSC 822e.
The X-ray diffraction patterns of the samples have been obtained
on Bruker AXS D8 Advance Diffractometer (XRD) with Cu-Ka radi-
ation, wavelength, k = 1.5406 Å. The FTIR of the samples have been
obtained on Thermo Nicolet, Avatar 370. And the SEM images of
the samples have been obtained on JEOL Model JSM
6390LV.

3. Results and discussion

3.1. TG/DTA/DSC

The chemicals are taken in stoichiometric proportion, TG-DTA

analysis of mixture of the chemicals is carried out from room
temperature to 800 °C, so as to understand the decomposition Fig. 3. XRD comparative intensity plot for cadmium doped Co-Zn ferrites.
behavior of the precursors. The TG/DTA/DSC of sample
Co0.5Zn0.5Cd1.5xFe2-xO4 for x = 0.2 is shown in Fig. 2, confirms the
formation of final product at 730 °C. The graphs indicate that the 3.1.1. XRD
formation process is endothermic in nature and the active region The structure of sample is analyzed using the XRD analysis. The
of formation ferrite is from 426 °C (699 K) to 715 °C (988 K). XRD image of cadmium doped Co-Zn ferrites series is presented in

CoCl2.6H2O

FeCl3.6H2O

ZnCl2 The samples are

charcteried by
Heang the FTIR, XRD and
CdCl2.H2O
mixture at SEM
800 °C for 4
Grinding the hours
mixture
thouroughly
in agate
Mixing all mortar, ll
chlorides in uniformity is
stoichiometric achieved
proporon

Fig. 1. Schematic diagram of synthesis of ferrite samples by solid state reaction method.
 A.B. Kulkarni, S.N. Mathad / Materials Science for Energy Technologies 2 (2019) 455–462 457

Table 1
XRD peak intensities for Co0.5Zn0.5Cd1.5xFe2
xO4 series with x = 0.0, 0.1, 0.2, 0.3, 0.4, 0.5 and calculated lattice parameter values.

hkl x = 0.0 x = 0.1 x = 0.2 x = 0.3 x = 0.4 x = 0.5

Observed Intensity % Observed Intensity % Observed Intensity % Observed Intensity % Observed Intensity % Observed Intensity %
210 20.2 16.9 9.9 9.1 26.1 30.8
220 27.9 27.5 25.6 23.7 5.5 14.7
310 71.5 57.2 38.5 38.8 100 100
311 100 100 100 100 77.4 83.9
321 19.1 15.4 12.2 13.1 24.6 29.3
400 20.3 20.9 24.1 21.3 4.9 11.3
421 27.7 25.6 26.9 24.6 46.3 50
422 35.6 32.8 20.9 29.1 51.9 61.7
511 26.5 34.5 31.8 36.8 13.1 10.9
440 58.8 65.3 55.2 61.4 35.7 42.4
441 24.8 23.9 14.8 17.4 31.1 43
620 5.7 7 6.1 5.1 13 17.4
533 8.2 14.3 10.3 11.6 7.7 14.4
444 5.2 5.4 3.4 4.3
Lattice Parameter 8.4044 8.3925 8.4268 8.4227 8.3822 8.3801

Fig. 3. The diffraction pattern peaks are matched with ferrite sam- cell parameters can be described by using 2nd order polynomial
ple JCPDS card #00–22-1086, the matching of (2 2 0), (3 1 1), (2 2 2), fits to the data,
(4 0 0), (4 2 2), (5 1 1), and (4 4 0) reflection planes confirms cubic
spinel structure. The lattice parameter of series is calculated using a ¼
0:111x2 þ 0:089x þ 8:397 ð3Þ
Eq. (2) and tabulated in Table 1.
The lattice parameter show an initial increase with doping till
a x = 0.2, then the unit cell show a significant shrinkage. The varia-
d¼ ð2Þ
2 2 2 1=2 tion of lattice parameter is shown if Fig. 6. This is due to occupation
ðh þ k þ l Þ
of cadmium ion at octahedral and tetrahedral sites [16].
where d - interplanar spacing, a - lattice parameter and (h k l) - The X-ray density, hopping length for A and B sites of anions,
Miller indices bond length and ionic radii, stacking fault coefficients and micro-
The cell parameters slightly change with increase in cadmium strain are calculated using Eq.5 to Eq. (13) and tabulated in Table 2.
concentration. This may be due to the smaller ionic radii of Fe+2 The volume of unit cell shown an expansion till doping concen-
(0.67 Å), Zn (0.82 Å) and Co (0.79 Å) as compared to Cd+2(1.03 Å). tration of x = 0.2 and then shown a continuous shrinkage till
It may be due partial replacement of Cd+2 with Fe+2 causing the x = 0.5. The hopping length, bond length and ionic radii follow
shrinkage of dimension of the unit cell resulting in lattice parame- the same pattern. The stacking fault coefficient show very low val-
ter change. For the composition dependent comparison, the unit ues, indicating that the peaks not much variation compared to

Table 2
Calculated values of volume of unit cell, hopping length, bond length, ionic radii, X-ray density, and stacking fault coefficient.

Concentration (x) 0 0.1 0.2 0.3 0.4 0.5

Volume of unit cell V (e-30) 593.64 591.12 598.4 597.52 588.94 588.5
Hopping length LA (Å) 3.6392 3.6341 3.6489 3.6471 3.6296 3.6287
Hopping length LB (Å) 2.9714 2.9672 2.9793 2.9779 2.9636 2.9628
Bond Length A-O (Å) 1.9215 1.9188 1.927 1.926 1.916 1.9159
Bond length A-B (Å) 2.0423 2.0394 2.048 2.047 2.037 2.0364
Ionic Radii rA (Å) 0.5715 0.5688 0.577 0.576 0.566 0.5659
Ionic Radii rB (Å) 0.6923 0.6894 0.698 0.697 0.687 0.6864
x-ray density Dx (g/cm3) 5.3226 5.5995 5.7826 6.0337 6.3857 6.6459
Stacking fault coefficient a 0.00323 0.00324 0.00309 0.00306 0.00443 0.00577

Table 3
Calculated values of crystallite size, micro strain and dislocation density using W-H plots, SSP and standard formula (Eq. (4)).

Conc. Crystallite size (in Å) Micro strain Dislocation density

X (q)
From W-H From From formula Micro strain Micro strain e = 2*sqrt From formula q = 1/D2 q = 15e/
graph SSP sD ¼ b Kk
:cosh
e = slope/4 (slope) e = bcosh/4 aD
D
(WH) (SSP)
0.0 235 241 240 0.000047 0.003883 0.001453 1.77E 3.53E
+ 15 + 13
0.1 223 228 251 0.000423 0.006556 0.001392 1.63E 3.38E
+ 15 + 14
0.2 263 278 268 0.000018 0.004954 0.001302 1.42E 1.23E
+ 15 + 13
0.3 312 173 216 0.000690 0.011224 0.001636 2.27E 3.93E
+ 15 + 14
0.4 171 181 237 0.001345 0.011799 0.001483 1.86E 1.41E
+ 15 + 15
0.5 214 222 237 0.000393 0.005829 0.001464 1.79E 3.28E
+ 15 + 14
458 A.B. Kulkarni, S.N. Mathad / Materials Science for Energy Technologies 2 (2019) 455–462

pffiffiffi
standard values. Average crystallite size is calculated by Debye- a 3
Scherrer’s formula [17].
LA ¼ ð6Þ
4
pffiffiffi
K k a 2
D¼ ð4Þ LB ¼ ð7Þ
bD :cosh 4
where, D- crystallite size, k- wavelength of X-ray used (1.5406 Å), where, LA-The distance between magnetic ions (hopping length) in
K- crystallite shape factor which is taken as 0.9 in this case consid- A site (tetrahedral) and LB- The distance between magnetic ions B
ering the particles to be spherical in general. bD- pure diffraction site (octahedral).
broadening. pffiffiffi
A
O ¼ ðu
1=4Þa 3 ð8Þ
8M
ðDxFerrite Þ ¼ ð5Þ B
O ¼ ð5=8
uÞa ð9Þ
Na3
where, Dxferrite-X-ray density, M- molecular weight of sample, where, A–O – bond length between A ion and Oxygen, B–O – bond
N- Avogadro’s number length between A ion and oxygen, u-oxygen ion parameter is taken
as 0.382 [18] for Zn-Cd-ferrite.

Fig. 4. Williamson-Hall plot for cadmium doped Co-Zn ferrites.

 A.B. Kulkarni, S.N. Mathad / Materials Science for Energy Technologies 2 (2019) 455–462 459

pffiffiffi
r A ¼ ðu
1=4Þa 3
rðO2
Þ ð10Þ 1
Dislocation DensityðqD Þ ¼ ð14Þ
D2
r B ¼ ð5=8
uÞa
rðO2
Þ ð11Þ
15e
where, rA– ionic radius for A site, rB– ionic radius for B site, r(O 2

)- qD ¼ ð15Þ
aD
ionic radius of oxygen ion (1.35 Å).
  The crystallite size, micro-strain and dislocation density are
2p2 ½D2h tabulated in Table 3
a¼ pffiffiffi ð12Þ
45 3 tanhhkl
3.1.2. Williamson hall plot and size-strain plot method
a- stacking fault coefficient, D2h- difference in standard and
The size-strain broadening are additive components of the total
observe 2h values.
breadth of a bragg peak [19]. The distinct h dependencies laid the
bcosh basis for the separation of size and strain broadening in the analy-
micro
strainðeÞ ¼ ð13Þ
4 sis of Williamson and Hall. The W-H plots are plotted using Eq. (16)
are plotted in Fig. 4a–f.

Fig. 5. Size strain plot for cadmium doped Co-Zn ferrites.

460 A.B. Kulkarni, S.N. Mathad / Materials Science for Energy Technologies 2 (2019) 455–462

K k
bhkl cosh ¼ þ 4esinh ð16Þ
D

The evaluation of the SSP parameters are obtained by consider-

ing peaks in intermediate range. This gives less weight to data from
high angle reflections where the precision is usually less. The SSP
plots are shown in Fig. 5a–f which are plotted using Eq. (17). In this
approximation, SSP plots assume that the ‘‘strain profile” by a
gaussian function and the ‘‘crystallite size” profile is lorentzian
[20,21].
Accordingly, we have:

K:k 2  e 2
2
ðdh k l bh k l coshÞ ¼ ðd b coshÞ þ ð17Þ
D hkl hkl 2
The correlation between W-H plot and SSP has been reported in
Table 3.
Fig. 6. Lattice parameter and crystallite size variation for cadmium doped Co-Zn
ferrites.

Fig. 7. SEM images of cadmium doped Co-Zn ferrites.

 A.B. Kulkarni, S.N. Mathad / Materials Science for Energy Technologies 2 (2019) 455–462 461

be due to the shorter bond length of the tetrahedral site than that
of the octahedral site.
This confirms that the presence of cadmium ion change the
internal structure at micro level. The absorption bands m1 and m2
are found in the expected range and the difference in band position
is due to the difference in the Fe3+ - O2
for the octahedral and
tetrahedral complexes. The positions of absorption bands are com-
position dependent whose dependence could be attributed to the
variation in cation – oxygen bond distances.

4. Conclusions

The Co0.5Zn0.5Cd1.5xFe2
xO4 series with x = 0.0, 0.1, 0.2, 0.3, 0.4,

0.5 are successfully synthesized by solid state reaction method.
The TG-DTA curves show that the ferrite synthesis reaction com-
pletes at 730 °C. The reaction is endothermic in nature. The FTIR
curves show shift of absorption bands towards lower wave number
region with increase in cadmium doping concentration. The two
absorption bands at 560 cm
1 and 400 cm
1 confirm the presence
Fig. 8. FTIR curves for cadmium doped Co-Zn ferrites.
tetrahedral and octahedral positions inside lattice structure. The
shift towards lower wave number region is due to shrinkage of unit
cell. The X-ray diffraction results for the samples confirms the for-
Table 4
mation of single phase cubic spinel structure with lattice parame-
FTIR peaks for Co0.5Zn0.5Cd1.5xFe2
xO4 series with x = 0.0, 0.1, 0.2, 0.3, 0.4, 0.5.
ter showing initial increase till x = 0.2 and then showing a
Concentration m2 (cm
1) v1 (cm
1) continuous shrinkage unit cell till x = 1.0. We have also discussed
0.0 418 570 dislocation density (qD); mechanical properties (strain), hopping
0.1 416 569 length {tetrahedral site (LA) and octahedral site (LB)}, bond length
0.2 416 571
(A–O and B–O), ionic radii (rA and rB) and stacking fault probability
0.3 408 568
0.4 — 568 (a) of cadmium doped cobalt zinc ferrite also reported. The SEM
0.5 — 566 images show that the structures are octahedron, tetrahedron and
granular in nature. The size of particles varies in terms of few
micrometers as expected in case of solid state reaction method.
3.2. SEM The SEM shows that the cadmium doping plays an important role
in grain growth.
The microstructure of ferrite samples were shown in Fig. 7a, b.
SEM images show regular tetrahedron, octahedron and bead like
Conflict of interest
structured grains with grain size more than 2 lm. With increase
in cadmium doping, the grain size of the ferrites goes on increasing
The authors have declared no conflict of interest.
systematically. The high magnification image clearly shows that
the tetrahedral and octahedral grains are perfect with sharp
boundaries and pointed angles getting sharper on cadmium addi- Appendix A. Supplementary data
tion. The results indicate that the presence of cadmium play an
important role in the formation of grain growth. Supplementary data to this article can be found online at
https://doi.org/10.1016/j.mset.2019.03.003.
3.3. FTIR
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