Surfaces and Interfaces 38 (2023) 102862

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Surfaces and Interfaces

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Zn/Ba nanoparticles doping effect on surface interface, Morphology, and

dielectric elucidation of spinel ferrites✰
Imran Ali a, Hasan M. Khan a, h, Muhammad Naveed Akram a, Yang-Fang Chen d,
Mujahid Mustaqeem b, c, d, Tawfik A. Saleh e, *, Muhammad Ahmad f, Imran Sadiq g,
Nimra Lateef a
a
Institute of Physics, The Islamia University of Bahawalpur, Bahawalpur 63100, Pakistan
b
Department of Chemistry, National Taiwan University, No.1, Section 4, Roosevelt Road, Taipei 10617, Taiwan
c
Nano-Science and Technology Program, Academia Sinica, Taiwan International Graduate Program, Institute of Physics, Taipei 106, Taiwan
d
Department of Physics, National Taiwan University, No.1, Section 4, Roosevelt Road, Taipei 10617, Taiwan
e
Department of Chemistry, King Fahd University of Petroleum & Minerals, Dhahran 31261, Saudi Arabia
f
Department of chemistry. University of Sahiwal 57000, Pakistan
g
Centre of excellence in solid state Physics, Punjab University Lahore, Pakistan
h
Department of Physics, Bahauddin Zakariya University, Pakistan

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

Keywords: Spinel ferrites having a composition of Ca0.5Ba0.5-xZnxFe2O4, (x = 0, 0.125, 0.25, 0.350 and 0.5) was synthesized
Nanomaterials: electrical properties by sol-gel autocombustion. The acquired samples underwent a 6 h annealing process at 650 ◦ C. The FTIR and
Advanced technology XRD results verified the spinel structure. XRD data have validated the single-phase BCC structure. All samples’
Energy
average crystal diameters fall between 41.43 and 94.05 nm, and the lattice constant "a" value dropped from 8.60
Å to 8.54 Å. Other parameters such as atomic packing fraction, bulk density D-spacing, dislocation density,
number of unit cells, porosity, strain, unit cell volume, volume of particles, and X-ray density were also calcu­
lated. reveals vibrational frequencies assigned to the distinct functional groups, octahedral and tetrahedral sites.
The validation to form the spinel behavior of prepared samples is provided by FTIR bands observed in the
400–600 cm− 1 regime. The SEM was used to analyze the morphology of the produced nanocrystals. By changing
the Ba and Zn concentration, a growth in grain size was observed. Dielectric characterization has revealed a
variety of responses at different frequencies. Dielectric constant, dielectric loss, tangent loss, Q-value, electric
modulus, and A.C conductivity were explored. Small values of dielectric loss demonstrated that the reported
material can be recommended for its use in transformer cores and high-frequency devices.

1. Introduction formulas of MnZnFe2O4 and NiZnFe2O4, are two notable composites of

ferrites materials [1–6].
Iron oxides are the primary component of the ferrites, a family of To find the necessary property, both the synthesis method and
magnetic oxides. The ancient people were aware of magnetite, which compositional formulas play a critical part in the manufacturing process
has the chemical formula (Fe3O4) and is known as loadstone. It is of these alloys. The relevance of these pairings comes from the fact that
believed to be one of the earliest authentic ferrites to have magnetic these substances exhibit distinctive magnetic properties below set tem­
activity. Ferrites typically have a dark gray or black look. Commonly, perature known as Curie temperature, abbreviated CT. The importance
ferrites are represented by the formula AB2O4. In this formula A repre­ and interest in magnetic materials, such as ferrites, have grown signif­
sents several divalent ions (Co2+, Mg2+, Cu2+, Fe2+, Zn2+, and Ni2+) and icantly in the domains of science and technology. Their demand is rising
B represents trivalent metals (like Al3+, Fe3+, Cr3+, and Mn3+). Mg- steadily across a wide range of industries. Iron oxide and other metal
substituted ferrites, and Zn2+ substituted nickel ferrites, with chemical oxides are in the ferrites in the proper ratios, making them

✰
https://faculty.kfupm.edu.sa/CHEM/tawfik/research.html
* Corresponding author.
E-mail address: [email protected] (T.A. Saleh).

https://doi.org/10.1016/j.surfin.2023.102862
Received 22 February 2023; Received in revised form 22 March 2023; Accepted 1 April 2023
Available online 7 April 2023
2468-0230/© 2023 Elsevier B.V. All rights reserved.
I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

ferromagnetic materials. For their magnetic and electric properties, shifter) that was achieved by varying concentration of Ca, Ba and Zn.
these ferrites acquire substantial electric resistance, high magneto- The objective of this work is also achieved by the altering the
crystalline anisotropy, high dielectric loss, low eddy current, high morphology of each prepared sample using different dopants in different
magnetization saturations, high values of magnetic permeability, and quantity. Optimal Q-value (14,411.01) is evidence of improved dielec­
Curie temperature CT [7–9]. Such adaptable properties of ferrites tric properties.
combine to make them crucial for numerous applications, including
magnetic recording chip, transformer core, magnetic data storage de­ 2. Experimental work
vice, and antenna rod [10,11]. These days, ferrites are synthesized in
nanocrystalline form. The nanosized ferrites can be appropriate for drug 2.1. Chemicals used to fabricate Ca0.5Ba0.5-XZnxFe2O4
delivery catalyst, magnetic sensors, hyperthermia, and among other
things because they have different and more dominant features than Barium nitrate (Ba(NO3)2, 99%), iron nitrate Fe(No3)3⋅9H2O (99%),
bulk ferrites [12–14]. These nano-sized ferrites are significant because calcium nitrate (Ca(NO3)2, 99%), Zinc nitrate (Zn(NO3)2, 99%), citric
they have various applications and multifunctional properties. Nano­ acid (C6H8O7, 99%), and ammonia nitrate (99%) were used to synthe­
particles can be used in the production and application of ferrites in the size Ca0.5Ba0.5-XZnxFe2O4 (x = 0, 0.125, 0.25, 0.350 and 0.5) (x = 0,
field of developing technologies. Nano-size ferrites are manufactured 0.125, 0.250, 0.350 and 0.50) via auto combustion sol-gel method. All
with particular attention paid to their electrical, structural, optical, these chemicals were acquired from Sigma-Aldrich and were utilized as
dielectric, and magnetic properties, among other qualities. Because of received.
this, a considerate approach to choosing and synthesizing relevant
components is the key to obtaining the acceptable standard with the 2.2. Experimental details
desired qualities. The ability to adjust the particle size or crystallite and
location of dopants makes the auto combustion sol-gel approach the Barium nitrate Ba(No3)2, iron nitrate Fe2(No3)3⋅9H2O, calcium ni­
optimum method for creating nano-size ferrites [15]. trate Ca(No3)2, and zinc nitrate Zn(No3)2, were employed to accomplish
The fourth type of ferrite is the spinel ferrites which exhibit the the necessity of barium (Ba), calcium (Ca), iron (Fe) and zinc (Zn). The
general formula MFe2O4 where M is showing the divalent metal ions for quantity of all the chemicals is listed in Table 1. Five beakers containing
examples Ni, Zn, Cd, Cu, Mn, and Fe. There are two interstitial sites in the stoichiometrically correct quantity of citric acid were filled with de-
the crystal spinel ferrite structure which are fabricated of tetrahedral (A ionized water after correctly mixed with the acid in the proper propor­
– site) as well as octahedral (B-site). The spinel ferrites have no specific tion. All beakers are set on the hot plate at 30 ◦ C for continuous stirring
direction of magnetization because the crystal spinel ferrite structure is until the citric acid has cooled. The aforementioned ingredients were
cubic due to this cause the spinel ferrites are magnetically soft and, in then added to the citric acid solution at room temperature to produce
this way, it is easier to alter the orientation of magnetic moments upon five stock solutions and five of the zinc-based calcium-barium
the implementation of the external magnetic field. The formed materials substituted spinel ferrites. To prepare the intended series of the Zn-based
are normal spinel ferrites if divalent metal cations that are (M) engage Ca-Ba substituted spinel ferrites, the nitrate solutions in the stoichio­
the A- site trivalent iron cations Fe3+ occupies the B-site. The crystal metric ratios were mixed at room temperature with the C6H8O7 solution
structure is called inverse spinel if all A- sites reside in Fe3+ metallic in a molar ratio of 1.3. The stock solutions were placed on the hot plate
cations and the B-sites with both M and Fe3+ metal cations. The orien­ and heated for 5 to 6 h at 70 ◦ C while stirring. Citric acid’s electro­
tations of magnetic moments of metallic cations like a Fe3+. This mag­ negative ion interacts with nitrates’ (salts’) electropositive cations
netic moment shows parallel to one another in A-site but antiparallel in during the vaporization of water molecules to change the solution into
the B-sites. The number of A-sites is twice that of B-sites due to the di­ precipitate. Few ammonia drops were added for maintaining the pH
rection of these moments. In this way, we can say that the whole level of the solutions. Once a loose gel had formed, and the temperature
structure of spinel ferrites is like ferrimagnetic material. was maintained at 80 ◦ C, and the stirring was turned off. When the
The advancement of magnetic Nano sized spinel ferrites has attracted temperature reached 100 ◦ C, the gel exploded. The gel was ultimately
the intentness of researchers and engineers toward industry due to their ground into a fine powder after being entirely burned into ashes at a
fascinating and significant applications. The spinel ferrites have a temperature of 110 ◦ C. All ground samples were put into ceramic cru­
different area of field such as drug delivery agents, biomedicine, elec­ cibles and were annealed for 6 h at 650 ◦ C. In the end, different char­
tromagnets, switching devices, photo catalysts, paramagnetic, micro­ acteristics techniques like, Tensor 27 Bruker was used for FTIR analysis
wave devices, cancer treatment, power transformer, loading coils, water in 400–4000 cm− 1 range, X-ray diffractometer (XRD) examination of the
purification, radar and communication systems, magnetic storage de­ Ca0.5Ba0.5-xZnxFe2O4, (x = 0, 0.1250, 0.25, 0.35 and 0.5) nano ferrites
vices, etc. Since the spinel ferrites exhibit distinguished properties such was done by Brucker D8 diffractometer from 20 -70 at the rate 2◦ per
○ ○

as larger chemical stability, large surface to volume ratio, larger prin­ minute, JEOL JSM-5910 SEM was used to study the morphology of the
ciples of saturation magnetization, dc resistivity with minute value of prepared samples. Grain size was measured and analyzed using image J
dielectric loss, retentivity. Few of them some other types of magnetic software. Dielectric analysis was utilized to examine the impact of
Nano particles like gold Nano-sized particles are the same as to Nano bairam calcium and zinc on the characteristics of prepared samples. LCR
sized spinel ferrites and also exhibit large surface-to-volume ratios [16] meter was used for dielectric analysis in the range 0–3 GHz [18], Fig. S1.
In the modernistic age, MNPs (magnetic Nano particles) have a great Each prepared sample was named as follows:
amount of consideration due to their extraordinary SPM (super Para
magnetic) characteristics and high adsorption capacities. The founda­ N1=Ca0.5Ba0Zn0.5Fe2◦ 4
tion on their magnetic and crystal structure ferrites are categorized as N2=Ca0.5Ba0.125Zn0.35Fe2◦ 4
spinel ferrite, garnet ferrite, ortho ferrite, hexagonal ferrite. From all of
them, great consideration has been given to the (SFNPs) spinel ferrite N3=Ca0.5Ba0.25Zn0.25Fe2◦ 4
Nano particles. The reason behind this is that spinel ferrites exhibit
N4=Ca0.5Ba0.35Zn0.125Fe2◦ 4
quality magnetic characteristics and simple chemical composition and
extensive applications in numerous areas which are biomedical, water N5=Ca0.5Ba0.5Zn0Fe2◦ 4
treatment, and electronic devices. [17]
The present work is to enhance the dielectric properties of
Ca0.5Ba0.5-xZnxFe2O4, (x = 0, 0.125, 0.25, 0.350 and 0.5) for high
frequency devices (microwave absorber, recording media and phase

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I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

Table 1
Mass of salts for the Synthesis of Ca0.5Ba0.5-xZnxFe2O4.
Formulation Named Ca(NO3)2 (0.1 Ba(NO3)2 Zn(NO3)2 (0.1 Fe(NO3)3⋅9H2O (0.2 Citric acid (0.2 Ratio as per the ICP-OES analysis
as M/mL) (0.1 M/ M/mL) M/mL) M/mL) (Ca:Ba:Zn:Fe)
mL)

Ca0.5Ba0Zn0.5Fe2O4 N1 50 0.0 50 100 100 1:0:1:4

Ca0.5Ba0.125Zn0.35Fe2O4 N2 50 15 35 100 100 4:1:3:16
Ca0.5Ba0.25Zn0.25Fe2O4 N3 50 25 25 100 100 2:1:1:8
Ca0.5Ba0.35Zn0.125Fe2O4 N4 50 35 15 100 100 4:3:1:16
Ca0.5Ba0.5Zn0Fe2O4 N5 50 50 0.0 100 100 1:1:0:4

3. Results and discussion parameters. In Ca0.5Ba0.5-xZnxFe2O4 sample quantity of highest ionic

radius element Ba2+= 1.38 starts decreasing from maximum value at the
3.1. XRD analysis same time second subtituient Zn2+=0.74 Å is in very small quantity
directaly affect the lattice parameter “a”. The variation in the lattice
XRD patterns of Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, and parameter and unit cell volume is similar for N3 and N4. Many structural
0.5) are shown in Fig. 1. Peaks related to cubic structure were obtained parameters are the same or have comparatively closed values for N3 and
at different 2θ values 30.04 (220), 32.89 (311), 35.50 (222), 40.34 N4, and this is due to the reason that these compositions have maximum
○ ○ ○ ○

(400), 50.19 (311), 53.62 (422), 56.28 (333), 63.61 (440). These ions of both substituents (Ba2+= 1.38 Å and Zn2+=0.74 Å) are getting
○ ○ ○ ○

peaks are coordinated with the ICDD# (01–082–1049) [19,20]. All the the position at the interstitial site of Ca2+= 1.12 Å and Fe2+= 0.78 Å.
peaks show cubic spinel ferrite characteristics [21,22]. No extra peak The Effect of Ba and Zn variation on x-ray density (ρx), bulk density (ρb)
related to the second phase was observed in the XRD spectrum due to the and% porosity (P) is illustrated in Fig. 4. The x-ray density (ρx) has an
successful substitution of Ba and Zn. Particle size (D), D-spacing (d), inverse relation with lattice constant, so it decreases with the upsurge in
Lattice parameter (a), Unit cell volume (V), Atomic Packing fraction Zn and decreases in Ba. Bulk density (ρb) and% porosity (P) are altering
(APF), Dislocation density (δ), No. of the unit cells (n), Strain (ε), Par­ inversely. It can also be noticed that dislocation density (δ), Strain (ε),
ticles Volume (υ), X-ray density (ρx), Bulk density (ρb) and Porosity (P) and x-ray density (ρx) show a decreasing trend for all Ca0.5Ba0.5-
were computed, Table 2, using various formulas; xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, and 0.5), Table 1.
Particle size, with the number of unit cells, and the particles volume
are directly affected by barium and zinc alteration, Table 1. These pa­ 3.2. Spectral analysis (FTIR)
rameters are linearly increasing with an increase in Zn with a decrease in
Ba. This Effect is elaborated in Fig. 2. The particle size increased from The FTIR results of Ca0.5Ba0.5-xZnxFe2O4 were recorded in the wave
41.94 to 94.05 nm, owing to differences in the ionic radius of the Ba2+= number range of 400 cm− 1 to 4000 cm− 1. The absorption bands
1.38 Å, Ca2+= 1.12 Å, Fe2+= 0.78 Å and Zn2+=0.74 Å. generated by the inter-atomic vibrations inside the materials were
It can be determined that the volume and size of the particle, and the examined using FTIR, Fig, S2. The differences in the structure and
number of units are governed by the larger ionic radius (Ba2+= 1.38 Å). chemistry of the synthesized spinel ferrites caused by various parame­
As the quantity of Barium ions decreases, these parameters increase ters including combustion reaction, degree of doping concentration,
linearly. The unit cell volume and lattice parameter exhibited a sinu­ annealing process or heat treatment, are also shown by FTIR analysis
soidal trend for different Barium and Zinc values, Fig. 3. First, both fall [14,23]. The force constant which may exist between the tetrahedral
from the highest values, increase to a sustained position, and then again and octahedral sites in the material’s unit cells are calculated using FTIR
fall to the lowest value. Different ionic radii and varying quantities of analysis. [24]. High-frequency absorption peaks are seen at 3730 to
Barium and Zinc play a vital role in fluctuation of all the structural 3987 cm− 1 for all prepared samples, due to the H–O-H and O–H
stretching vibration due to the moistures [25]. The peaks around 2071
cm− 1 for all synthesized samples indicate C–H bonds stretching vibra­
tion due to the residual citric acid [26]. The peak near 874 cm− 1 can be
observed for all N1–N5 due to the bonding of Fe3O4 particles with sur­
face O.H. groups [27]. The range 400–600 cm− 1 is related to metal oxide
(M-O) stretching vibrations. In the regime 458–479 cm− 1 and 525–544
cm− 1 two absorption bands υ1 and υ2 are detected in all compositions
that are associated with M-O bond. Absorption bands υ1 and υ2 arising
from intrinsic vibrations of M-O bonds justified the creation of Fe+2 and
O+2 ions at tetrahedral and octahedral sites. Due to the different ionic
radius of Ba+2 and Zn+2 ions the position of υ1 and υ2 transfer from low
to high wavenumber due to the altering the Ba and Zn concentrations.
The transfer of υ1 and υ2 from low to high wavenumber due to the
different concentrations of Ba and Zn is displayed in Fig. 5 and Table 3.

3.3. Morphological studies (SEM)

The morphology of synthesized spinel ferrites has been examined

through JEOL JSM-5910 scanning electron microscope. The prepared
samples’ surface morphology, grain size distribution, energy dispersive
spectroscopy (EDS) and elemental mapping images and the atomic ratio
of the synthesized samples is presented in Fig. S3. The ICP-OES analysis
was conducted for the prepared materials and the ratio of the elemental
Fig. 1. XRD patterns of Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, analysis is recorded in Table 1. ICP-OES results of atomic ratio of metal
and 0.5). species indicated the successful preparation of the samples. The amount

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I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

Table 2
The structural values of Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35 and 0.50).
Parameters Equations N1 N2 N3 N4 N5

Particle size ‘D’ (nm) Kλ 41.43 57.99 71.64 71.96 94.05

D =
βcosθ
d-spacing ‘d’ (Å) nλ 0.229 0.228 0.228 0.228 0.228
d =
2sinθ( )
Lattice parameter ‘a’ (Å) 1 4 h2 + hk + k2 l2 8.60 8.55 8.59 8.59 8.54
= + 2
d2hkl 3 a2 c
Unit cell volume ‘V’ (Å) V = a3 636.960 625.860 635.340 635.340 622.970
4
Dislocation density ‘δ × 10− 1 5.82 2.97 1.95 1.93 1.13
δ = 2
D √̅̅̅
Atomic Packing fraction% 2π 3a3 67.935 67.941 67.870 67.870 68.016
APF = × 100
V
No. of the unit cells (n) D3 67.466 188.293 349.714 354.421 806.978
n = 0.6043 × 3
a
Volume of particles ‘υ’ (nm)3
( )
4 D 3 37,214.851 102,054.183 192,414.685 195,004.640 435,359.356
υ = π
3 2
Strain ‘ε’ β 0.052 0.041 0.033 0.032 0.031
ε = hkl
4tanθ
3
X-ray density ‘ρx’ (g/cm ) Z×M 5.514 5.421 5.152 5.002 4.871
ρx =
N × a3
Bulk density ‘ρb’ (g/cm )3 m 3.106 2.410 2.667 2.438 2.492
ρb = 2
πr h )
Porosity ‘P’ (%) ( ρ 43.666 55.544 48.226 51.259 48.832
P = 1 − b × 100
ρx

Fig. 2. Alteration in the volume of particles (ν), number of the unit cells (n), and particle size (D).

of Ba and Zn impacts the crystallinity and agglomeration. SEM images 3.4. Dielectric studies
have revealed nonuniform distribution but clearly defined boundaries in
low Zn samples. It can also be observed from SEM micrographs and The electrical characteristics of ferrites make them significant in
histograms for the low Zn samples, in which the small grains are in the various fields, particularly in high-frequency applications like inte­
large amount. The number of small grains is decreasing by increasing Zn grated chip and microwave absorption properties. The method of
content. The interconnectivity of the structure also increases by dielectric characteristics of the ferrite materials is based on the prepa­
increasing Zn content. From the higher resolution of SEM images, it can ration technique, material’s composition and structure, method of
be observed that the grain boundaries are not well defined. A highly fabrication, and cation distribution. The dielectric features also relied on
connected net-like structure can be observed in N4 and N5. Grains with a the practical field, crystallite size, heat treatment or annealing process,
large structure are also increased. It can be seen that the number of large and time [28]. Behavior data of electric polarization effect and localized
microns is increasing. From all histograms, the data revealed that the charge carriers in ferrites were provided by the measurement of
grains in the range 0.1–0.3 μm are maximum. The changing concen­ dielectric parameters. Large values of dielectric materials are used for
tration of Ba and Zn affects the grain size and the number of microns in high-frequency uses, specifically in integrated chip components and
different regimes. The number of 0.1–0.4 μm grains are maximum in N1 microwave absorption features. Based on polarization, the dielectric
that decreases exponentially by increasing the concentration of Zn. dispersion in ferrites was studied by the Maxwell-Wagner theory. The
Similarly, the quantity of 0.4–0.7 μm is maximum in N5, which de­ dielectric properties of synthesized ferrite materials having composition
creases from N5 to N1 exponentially, Fig. 6. Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, and 0.5) spinel ferrites

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I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

Dielectric loss can be observed at 0.89 GHz, shown by N1.

3.4.2. Dielectric constant

The dielectric constant can be considered as electrostatic energy
stored per unit gradient; per unit volume, which is denoted by ε′ [31].
The dielectric constant is calculated as Eq. (2)
Cd
(2)
′
ε =
Aε o

where ‘A’ is the cross-sectional area, ‘C’ is the capacitance, ‘d’ is the
thickness of the pellet, ‘εo’ permittivity of free space [32]. Dielectric
properties of Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, 0.5) spinel
ferrites were explored in a frequency from 1 to 3 GHz. By increasing the
frequency, the dielectric constant ε′ declines. This indicates a dispersive
performance at high frequency because of space-charge polarization
[33], Fig. 8, Tables 6 and 7. By increasing the frequency, the dielectric
constant ε′ declines for all ferrites due to hooping phenomenon between
Fe+2 and Fe+3 and Maxell-Wagner model and interfacial polarization
Fig. 3. Alteration in lattice constant (a) and volume of the unit cell (V). based on Koop’s theory [34,35]. Thus, changing the concentrations of
Zn and Ba alters the value of the dielectric constant. A minimal dielectric
were measured. constant can be observed at 1.8 GHz frequency that N4 presented. The
optimal value of the dielectric constant was displayed by N1 at 0.031
3.4.1. Dielectric loss factor GHz.
The dielectric loss factor is the measure of energy loss in a material
having the symbol ε′′ , which is the dielectric loss factor. Dielectric loss 3.4.3. Tangent loss
factor is computed by using Eq. (1). It is the dissipation factor and the fraction of the dielectric loss factor
into the dielectric gain factor. The formula to calculate the tangent loss is
(1)
′
ε′′ = ε tanδ given by [36].
In this Eq. 1 ε′′ represents dielectric loss, tanδ is the tangent loss while ε′′
ε′ represents dielectric constant [29,30]. The alteration in dielectric loss tanδ = (3)
ε′
of composition Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, and 0.5)
is shown in Fig. 7, Tables 4 and 5. The reasons which provoke the rate of tanδ =
σac
(4)
dielectric loss in ferrites are defects in dipoles and electron hopping. 2πf ε′
When the value frequency is small, then dipole interactions are clear, Eq. (3) represents the charging current by ε′ and loss current by ε’’
and by increasing the frequency range, dipole interactions decrease the [37]. The essential part of the core loss in a material is calculated
dielectric loss [28]. It can be seen that N1 and N2 showed rapidly through the value of tangent loss in ferrite materials. For Ca0.5B­
varying dielectric loss in high frequency while other prepared samples a0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, and 0.50) spinel ferrites. When
show almost uniform behavior. All samples showed a very low dielectric frequency increases, then tangent loss declines, and this trend is also the
loss, which is confined in the range of -2 to 2.5. Thus, various concen­ same as for ε’ and ε’’ . Fig. 9 displays that tangent loss declines by the
trations of Ba and Zn change the dielectric loss value at different fre­ increase in frequency. According to Koop’s phenomenological
quencies. N4 shows minimal dielectric loss at 2.01 GHz. Maximum

Fig. 4. Alteration in X-ray density (ρx), bulk density (ρb) and% porosity (P).

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I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

maximum value of the tangent loss is 0.476, which N2 displayed at 2.27

GHz.

3.4.4. Quality factor

The reciprocal of tangent loss is called the dielectric material’s
quality factor or Q value. The dissipation factor of the dielectric mate­
rials. Mathematically, it can be written as;

Fig. 5. Movement of υ1 and υ2 due to the different concentrations of Ba and Zn.

Table 3
Position of υ1 and υ2 .
Formulation Named as υ1 υ2
Ca0.5Ba0Zn0.5Fe2O4 N1 458 525
Ca0.5Ba0.125Zn0.35Fe2O4 N2 464 531
Ca0.5Ba0.25Zn0.25Fe2O4 N3 469 535
Ca0.5Ba0.35Zn0.125Fe2O4 N4 473 543
Ca0.5Ba0.5Zn0Fe2O4 N5 479 546
Fig. 7. Dielectric loss against frequency graph of Ca0.5Ba0.5-xZnxFe2O4 (x = 0,
0.125, 0.25, 0.35, and 0.5) spinel ferrites.

hypothesis, the largest loss appears at small frequencies because the

electron at the octahedral site jumps between Fe3+ and Fe2+ ions more Table 4
Dielectric loss at 1, 1.5, and 2.5 GHz.
frequently in relation to the applied electric field [38]. According to the
Debye relaxation, resonance peaks were detected near 2.5 GHz. [39]. Formulation Named as Dielectric loss
The dielectric constant is vital in a capacitor because to the minimal 1 GHz 1.5 GHz 2.5 GHz

tangent loss factor’s intensification. This suggests that these ferrites have Ca0.5Ba0.5Zn0Fe2O4 N1 2.18154 -0.21925 -0.96284
amazing uses in magnetic recording heads due to their extremely low Ca0.5Ba0.35Zn0.125Fe2O4 N2 0.33906 0.5036 − 0.4845
Ca0.5Ba0.25Zn0.25Fe2O4 N3 0.47184 0.10666 0.52628
dielectric losses, Tables 8 and 9. Thus, varying quantity of Ba and Zn
Ca0.5Ba0.125Zn0.35Fe2O4 N4 0.12821 − 0.06006 − 0.01179
affects the value of the tangent loss at different frequencies. Minimum Ca0.5Ba0Zn0.5Fe2O4 N5 0.5688 0.36022 0.22243
tangent loss can be observed at 2.63 GHz, exhibited by N1. The

Fig. 6. Changes in grain size distribution and quantity of microns.

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I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

Table 5
Minimal and optimal dielectric loss along with frequency.
Formulation Named as Minimum Maximum
Frequency (GHz) Dielectric Frequency (Hz) Dielectric
loss loss

Ca0.5Ba0.5Zn0Fe2O4 N1 2.63 -1.51549 8.86 × 108 2.54725

Ca0.5Ba0.35Zn0.125Fe2O4 N2 2.52 -0.48527 2.24 × 109 1.5867
Ca0.5Ba0.25Zn0.25Fe2O4 N3 1.70 -0.16346 3.10 × 107 1.32035
Ca0.5Ba0.125Zn0.35Fe2O4 N4 2.01 -0.06006 3.10 × 107 0.28442
Ca0.5Ba0Zn0.5Fe2O4 N5 2.63 0.0987 3.10 × 107 0.86648

ferrites have a significant value of the quality factor. By owing these

characteristics, these ferrites have various applications in large fre­
quency resonant circuits, choke, inductors, multi-layer chips, satellite
communication, microwave devices, magnetic storage devices, nano­
electronic devices, sensors, power transformers, etc. [41,42], Tables S1
and S2. Thus, it can be observed that Q-value is affected by Ba and Zn as
it showed a varying response at different frequencies. The nominal
Q-value is − 3625.92, which N4 presents at 1.68 GHz. Similarly, the
optimal Quality factor is at 1.81 GHz, which N3 displays.

Fig. 8. Dielectric constant against frequency graph of Ca0.5Ba0.5-xZnxFe2O4 (x

= 0, 0.125, 0.25, 0.35, and 0.5) spinel ferrites.

Table 6
Dielectric constant at 1, 1.5, and 2.5 GHz.
Formulation Named as Dielectric constant
1 GHz 1.5 GHz 2.5 GHz

Ca0.5Ba0.5Zn0Fe2O4 N1 5.90819 6.37885 7.02336

Ca0.5Ba0.35Zn0.125Fe2O4 N2 3.82789 4.35221 3.73447
Ca0.5Ba0.25Zn0.25Fe2O4 N3 3.93265 4.34102 4.33976 Fig. 9. Tangent loss against frequency graph of Ca0.5Ba0.5-xZnxFe2O4 (x = 0,
Ca0.5Ba0.125Zn0.35Fe2O4 N4 2.20139 2.11959 2.24856 0.125, 0.25, 0.35, and 0.5) spinel ferrites.
Ca0.5Ba0Zn0.5Fe2O4 N5 4.53055 3.90873 4.2396

Table 8
1
Q value = (5) Tangent loss at 1, 1.5, and 2.5 GHz.
tanδ
Formulation Named as Tangent loss (GHz)
The quality factor or Q-value of dielectric material varies inversely 1 1.5 2.5
with the dielectric tangent loss. The graphical representation of the
Ca0.5Ba0.5Zn0Fe2O4 N1 0.36924 -0.03437 -0.13709
Quality factor versus applied frequency is shown in Fig. S4. The Q-value Ca0.5Ba0.35Zn0.125Fe2O4 N2 0.08858 0.11571 -0.12974
or quality factor is considered a very significant characteristic of ferrites Ca0.5Ba0.25Zn0.25Fe2O4 N3 0.11998 0.02457 0.12127
material [40]. Ca0.5Ba0.125Zn0.35Fe2O4 N4 0.05824 -0.02834 -0.00525
Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, and 0.50) spinel Ca0.5Ba0Zn0.5Fe2O4 N5 0.12555 0.09216 0.05247

Table 7
Minimal and optimal dielectric constant along with frequency.
Formulation Named as Minimum Maximum
Frequency (GHz) Dielectric constant Frequency (Hz) Dielectric constant

Ca0.5Ba0.5Zn0Fe2O4 N1 1.26 5.21045 3.10 × 107 11.75294

Ca0.5Ba0.35Zn0.125Fe2O4 N2 2.31 2.34749 3.10 × 107 5.75157
Ca0.5Ba0.25Zn0.25Fe2O4 N3 1.34 3.8048 3.10 × 107 6.45371
Ca0.5Ba0.125Zn0.35Fe2O4 N4 1.8 2.0425 3.10 × 107 2.63238
Ca0.5Ba0Zn0.5Fe2O4 N5 1.89 3.79137 3.10 × 107 5.99348

7
I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

Table 9
Minimal and optimal tangent loss along with frequency.
Formulation Named as Minimum Maximum
Frequency (GHz) Tangent loss Frequency (Hz) Tangent loss

Ca0.5Ba0.5Zn0Fe2O4 N1 2.63 -0.19194 9.46 × 108 0.38058

Ca0.5Ba0.35Zn0.125Fe2O4 N2 2.5 -0.12974 2.27 × 109 0.47658
Ca0.5Ba0.25Zn0.25Fe2O4 N3 1.70 -0.03912 3.10 × 107 0.20459
Ca0.5Ba0.125Zn0.35Fe2O4 N4 2.01 -0.02834 3.10 × 107 0.10805
Ca0.5Ba0Zn0.5Fe2O4 N5 2.63 0.02214 1.50 × 109 0.18891

3.4.5. Electric modulus the conductivity’s value throughout a wider frequency range. Ac con­
This property is the fundamental parameter to understanding the ductivity rises as zinc increases before decreasing noticeably more as
factors provoking the process of electrical change. The components dopant absorption expands. Thus, varying quantity of Ba and Zn affects
include charge carriers, relaxation time, and hopping rate between the value of A.C conductivity at different frequencies. Minimum A.C
conductions. The material’s impedance analysis aids in identifying its conductivity can be observed at 2.63 GHz, exhibited by N1. The
electric features, such as grain boundaries and the role that grains play maximum value of A.C conductivity is 0.19079, which N2 displayed at
in the conductivity of the substance. 2.25 GHz.
Mathematically,
′ 4. Conclusion
ε
(6)
′
M = ′
ε 2 + ε′′ 2 Spinel ferrites having a composition of Ca0.5Ba0.5-xZnxFe2O4, (x = 0,
ε′′ 0.125, 0.25, 0.35, 0.5) were synthesized. The acquired samples under­
M ′′ = ′ (7) went a 6 h annealing process at 650 ◦ C. To explore structural, spectral,
ε 2 + ε′′ 2
morphological, and dielectric features, XRD, FTIR, SEM, and dielectric
Eqs. (6) and (7) represent the real and imaginary parts of electric analysis were used. FTIR and XRD results verified these ferrites’ spinel
modulus, which gives the total electric modulus of ferrites material. The structure. XRD data have validated the single-phase BCC structure.
sum of the real and imaginary parts of the electric modulus results in the Nanoparticle ferrites’ octahedral and tetrahedral sites and specific
entire electric modulus of fabricated ferrites [43]. The plot of Mʹ vs. functional groups are revealed by FTIR to have vibrational frequencies.
frequency of Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, 0.35, and 0.5) Using the SEM technique, the morphology of the synthesized nano­
spinel ferrites is presented in Fig. S5. The graph reveals that at low crystals was investigated. The size of the grains increased when the Ba
frequency the values of Mʹ is small that increase with frequency [44]. and Zn concentrations changed. Different responses at various fre­
The graph of Mʹʹ vs. frequency for Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, quencies have been identified via dielectric characterization. The
0.25, 0.35, and 0.5) spinel ferrites are represented in Fig. S6. The plot of frequency-dependent parameters such as A.C conductivity, Q-value,
Mʹʹ displays the energy dissipation in dielectric material ferrites [45]. electric modulus, tangent loss, dielectric constant, and dielectric loss
With the addition of Zn content, the peaks are slightly shifting toward a were investigated. Small values of dielectric loss demonstrated that the
wider frequency range. The underlying cause of the entire pattern re­ materials are suitable to be used in transformer cores and high-
veals that charge transport, like electrical transport and conduction frequency devices.
relaxation transfer, is responsible [41], Tables S3–S6. Thus, it can be
observed that M’ and M” is affected by varying the concentration of Ba CRediT authorship contribution statement
and Zn as it exhibited varying response at different frequencies. Minimal
values of M’ and M” are 0.07562 and − 0.03417 which presented by N1 Imran Ali: Investigation, Data curation, Formal analysis, Writing –
and N2 at 1.60 × 107Hz and 2.51 GHz, respectively. In the same way, the original draft. Hasan M. Khan: Investigation, Data curation, Formal
maximum M’ and M” can be observed at 0.39967 GHz and 0.13819 GHz, analysis, Writing – original draft. Muhammad Naveed Akram: Inves­
which are displayed by N2, respectively. tigation, Data curation, Formal analysis, Writing – original draft. Yang-
Fang Chen: Investigation, Data curation, Formal analysis, Writing –
3.4.6. A.C conductivity original draft. Mujahid Mustaqeem: Investigation, Data curation,
This property known as σac is given by the following relation; Formal analysis, Writing – original draft. Tawfik A. Saleh: Writing –
′
σ ac = ωεo ε tanδ = 2π f εo ε′′ (8) review & editing. Muhammad Ahmad: Investigation, Methodology,
Visualization. Imran Sadiq: Investigation, Methodology, Visualization.
where ω= angular frequency, tanδ= tangent loss, εo= permittivity of Nimra Lateef: Investigation, Methodology, Visualization.
free space, ε′ = dielectric constant, and ε′′ =dielectric loss [46]. The
change in AC conductivity of Ca0.5Ba0.5-xZnxFe2O4 (x = 0, 0.125, 0.25, Declaration of Competing Interest
0.35, and 0.5) with frequency and Ba, Zn concentration is shown in
Fig. S6 and S7. From the graph, it can be seen that A.C. conductivity The authors declare that they have no known competing financial
rises with frequency, which is typical behavior of ferrites. The conduc­ interests or personal relationships that could have appeared to influence
tivity of A.C. is seen to change rapidly in the high-frequency region the work reported in this paper.
while nearly remaining constants in low-frequency zone. Because of this,
the mechanism of the dielectric polarization is similar to the electrical Data availability
conduction process. From Koop’s model as well as Maxwell-Wagner’s
theory, ferrite’s grains are kept apart by the grain boundary of the thin No data was used for the research described in the article.
layer [46–51].
A grain boundary affects the conductivity of the grain at a higher
frequency and the conductivity of the A.C. at a lower frequency. While
Acknowledgements
boundaries and grains are randomly positioned at low frequencies, they
become more systematically structured as frequency increases, boosting
The author T.A Saleh thanks KFUPM, Saudi Arabia, for the support

8
I. Ali et al. Surfaces and Interfaces 38 (2023) 102862

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