Asian Journal of Research and Reviews in Physics

5(3): 14-25, 2021; Article no.AJR2P.81418

ISSN: 2582-5992

Magnetic Characterization of Co and Zn Nano

Ferrites: Property Consideration for Oil-Spill
Clean Up
A. Musa1*, M. A. Muhammad1,2, N. M. Maharaz3 and A. S. Gidado1
1
Department of Physics, Faculty of Physical Sciences, Bayero University Kano, Nigeria.
2
Zainab Pharmacy & Gen. Ent. Ltd. No 13A Club Road Kano, Nigeria.
3
Department of Physics, Federal University Dutse, Jigawa State, Nigeria.

Authors’ contributions

This work was carried out in collaboration among all authors. All authors read and approved the final
manuscript.

Article Information
DOI: 10.9734/AJR2P/2021/v5i330164

Open Peer Review History:

This journal follows the Advanced Open Peer Review policy. Identity of the Reviewers, Editor(s) and additional Reviewers, peer
review comments, different versions of the manuscript, comments of the editors, etc are available here:
https://www.sdiarticle5.com/review-history/81418

Received 09 October 2021

Original Research Article Accepted 18 December 2021
Published 20 December 2021

ABSTRACT

Nano-magnetic particles are significantly finding applications in environmental remediation. This

work studied the magnetic properties of Co and Zn nano-ferrites, CoFe2O4 and ZnFe2O4
respectively, with considerations for the properties that are desirable for oil spill cleanup. The ferrite
nanoparticles were synthesized by the glycol-thermal method at 200 ºC for 6 hours using a stirred
pressure reactor. Single phase spinel crystal structures were obtained for both samples as
determined by an X-ray diffraction (XRD) machine. The high-resolution transmission electron
microscope and surface electron microscope images showed nano structures. The magnetic
properties and magnetic hyperfine parameters were determined using a lakeshore vibrating sample
57
magnetometer and Fe Mössbauer spectroscopy. The XRD peaks were consistent with that of a
single phase spinel structure. No impurity phase was detected. The nano-ferrites have crystallite
sizes of about 10 nm and 17 nm for CoFe2O4 and ZnFe2O4. The nano almost-spherical nature of
the samples was also confirmed from their morphology studies. The saturation magnetization of
CoFe2O4 and ZnFe2O4 were about 50 emu/g and 30 emu/g respectively. They both exhibited
superparamagnetic properties with a component of para-magnetism observed in ZnFe2O4 nano-
ferrites. CoFe2O4 nano-ferrites exhibited better desired property for oil spill cleanup. The ZnFe 2O4
nano-ferrites showed tendencies of slow response to magnetic field, however, it is more
_____________________________________________________________________________________________________

*Corresponding author: E-mail: [email protected];

 Musa et al.; AJR2P, 5(3): 14-25, 2021; Article no.AJR2P.81418

environmentally friendly. The magnetic hyperfine parameters and the isomer shift values for
CoFe2O4 and ZnFe2O4 showed strong internal magnetic fields and the obtained values are
3+
consistent with spinel structure. The oxidation state of Fe was observed to be Fe . Due to the low
coercivity and high magnetization values, these particles could be considered as potential
candidates for oil spill cleanup. These desirable magnetic properties will improve the recyclability of
the nanoparticles using low applied magnetic fields.

57
Keywords: Glycol-thermal; single phase spinel; superparamagnetic; coercivity; Fe mössbauer
spectroscopy.

1. INTRODUCTION two interstitial sites known as tetrahedral A and

octahedral B ions which contains 8 tetrahedral
The emergence of nanotechnology has coordinated sites and 16 octahedral coordinated
revolutionized innovations in almost all fields of sites for divalent & trivalent metal cation
endeavors such as in agriculture, occupancy, where A and B denote divalent and
pharmaceuticals, medicals, electronics, energy, trivalent cations respectively [7-8]. For an ideal
2+
environmental management, the oil and gas normal spinel of ZnFe2O4 ferrites, Zn
industry, aerospace and automobile [1]. It is an exclusively occupies the tetrahedral A-sites while
3+
interdisciplinary technology that involves the Fe occupies the octahedral B-sites. A mixed
application of materials with a size range of cation distribution is the case for MgFe2O4. Such
about 1-100 nm, known as nanomaterials [2]. distributions of cations significantly influence the
The unique properties derived from magnetic properties of the ferrites [9].
nanomaterials found interesting applications
compared to their bulk counterpart. This is A generic example is CxD1-xFe2O4 where, 0≤x≤1.
primarily due to the nano-size effect which gives At both extreme conditions for x = 0 or x = 1,
nanomaterials a high surface to volume ratio, DFe2O4 or CFe2O4 ferrites are obtained
increased number of surface atoms and respectively. However, an intermediate case is
enhanced reactivity [3]. Magnetic, optical, and obtained for x = 0.5 as is the case for
electrical properties at the nano-scale behave C0.5D0.5Fe2O4 ferrite. Consequently, one could
very differently from the bulk samples. The vary the structural and magnetic properties of the
understanding of these properties has enabled ferrite by establishing different intermediate
the deployment of nanotechnology in the oil and cases. Also, the method of synthesis could also
gas industries in areas such as exploration, have effect on the magnetic properties of
drilling, logging, hydraulic fracturing, formation nanoparticles [10].
damage, enhanced oil recovery (EOR) and ex-
situ upgrading of oil shales/bitumen [2-5]. A more The current project synthesized single phase
recent possible application of nanomaterials for nanoparticles of CoFe2O4 and ZnFe2O4 ferrites
environmental remediation is found in the oil and using the glycol-thermal synthesis method. The
gas sector, which involves the use of amine selected elements such as Fe and Zn are
functionalized or polymer coated magnetic environmentally friendly. However, Zn has low
nanoparticles for cleaning crude oil spills [3]. anisotropy compared to Co. Therefore, Co is
Therefore, there are enormous potentials in selected because of its high anisotropy so as to
understanding the behavior of materials at nano- improve the magnetization of the sample and
scale so that the properties can be tailored help in making comparison.
towards specific application.
2. THEORETICAL BACKGRAOUND
The cubic spinel ferrites are one of such
materials that are suitable for environmental High saturation magnetization MS and low
remediation application. Ferrites belong to a
special class of ceramic oxides which generally coercivity HC are characteristic features of
has a chemical formula of AB2O4. A represents superparamagnetic materials. The magnetization
one or more of the divalent transition metals, for measures the magnetic spins response to
example zinc (Zn), iron (Fe), magnesium (Mg), magnetic field. The response is produced in a
nickel (Ni), cobalt (Co), copper (Cu), or calcium loop called the magnetic hysteresis loop. It is the
(Ca) [6], and B represents solely iron (Fe). magnetic spin response to the application and
Generally, a cubic spinel structure consists of

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 Musa et al.; AJR2P, 5(3): 14-25, 2021; Article no.AJR2P.81418

removal of magnetic field. Figs 2.4 shows a factor with a value of about 0.94 for a spherical
schematic diagram of the magnetic hysteresis shape, λ is the X-ray diffraction wavelength, W
loop responses from materials with the different is the full width at half maximum,  is the Bragg's
main classes of magnetic order in solids.
angle and hkl are the Miller indices of a selected
intensity peak [17].
The MS can be empirically calculated from the
law of approach to saturation magnetization Also, from Bragg’s law of diffraction, one could
given by [11]: establish that the lattice parameters a for a cubic
crystal structure has a relationship with hkl as;
 a b 
M ( H )  M S 1   2   H 
 H H  a h2  k 2  l 2 . (4)
(1) 2Sin 

where a and b are constants, M S is the

3. MATERIALS AND METHODS
saturation magnetization and  hf is the high field
susceptibility. The a H term is attributed to The materials and methodology are presented
for the research work.
structural defects or nonmagnetic inclusions. The
b / H 2 term is due to uniform magneto- 3.1 Glycol-Thermal Methods
crystalline anisotropy.
The glycol-thermal method is a wet chemical
The coercivity gives a measure of the anisotropy method of synthesizing nanoparticles using a
of a magnetic material [12]. This can be stoichiometric amount of the starting chemical
estimated by: materials in their metal chlorides or nitrates
forms. These precursors are usually dissolved in
H C1  H C 2 de-ionized water. To precipitate the nitrates or
HC  , (2) the metal chloride from its solution, sodium
2 hydroxide or ammonia potassium hydroxide is
used respectively. The process is kept under
where H C1 and HC2 are the negative and continuous stirring condition while the pH value
positive coercivity respectively along the gradually increases until a desired value is
magnetic field direction [13]. Soft reached. After about 40 minutes of continuous
superparamagnetic materials are expected to stirring, the solution is washed over a thin-pore
have insignificant or almost zero coercivity filter using de-ionized water to remove the
thereby quenching the propensity for high degree chlorides or nitrates. The resulting compound is
of agglomeration of the nanoparticles and the put inside ethylene glycol and transferred to a
demand for high magnetic field. This implies that pressure reactor for certain duration. A PARR
it will be easier to recycle the magnetic 4843 stirred pressure reactor was used in the
nanoparticles after every cycle of magnetization current work. The stirring conditions in the
for reuse in the oil spoil cleaning process. reaction chamber such as temperature, speed
and pressure are recorded accordingly.
Micro-structural properties such as crystallite size
This method was used to synthesize CoFe2O4
D and lattice parameters a could significantly and ZnFe2O4nano-ferrites in this work. The
contribute to changes in structural and magnetic starting materials are FeCl3.6H2O (99%),
properties of materials [14-16]. The Scherrer’s CoCl2.6H2O (98%) and ZnCl2.6H2O (98%) as
formula; purchased from Sigma-Aldrich. The starting
materials are dissolved in about 400 ml of de-
K ionized water contained in a beaker. The beaker
D , (3)
W(hkl) Cos is placed on a magnetic stirrer at different times
for the synthesis of CoFe2O4. Similar process
was followed for the synthesis of ZnFe2O4nano-
It is often used Equation (3) to estimate D , ferrites. An initial pH value of 2.51 was recorded
where K is a constant associated with the shape and the solution was continuously stirred for

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 Musa et al.; AJR2P, 5(3): 14-25, 2021; Article no.AJR2P.81418

about 20 minutes to achieve homogeneity of the size of the nanoparticles is estimated using
mixture. Ammonium solution was carefully used Equation (3).
to raise the pH to about 9, causing a precipitation
of the metal chlorides. It was maintained under 3.2.2 High resolution transmission electron
this condition for about 30 minutes. The chloride microscopy and scanning electron
contained in the precipitate was washed off over microscopy
a glass microfibre filter in a Büchner funnel using
de-ionized water. Standard solution of silver The morphology and the physical microstructure
nitrate was used to confirm the absence of of a sample can be studied using high resolution
chlorides in the filtrate by ensuring that the transmission electron microscopy (HRTEM). It is
precipitate of silver chloride was not visible. The a technique used to study the images of a
recovered precipitate was put in about 250 ml of sample; carry out sample size investigation,
ethylene glycol and reacted using a pressure shape and crystallographic structures in the
reactor. The reaction occurred at a soak micro or nano-nanometer range. The images are
temperature of 200 ºC that was retained for 6 generated from electron beams interactions that
hours. The reactor was operated at a speed and are transmitted through the sample. The samples
pressure of about 300 rpm and 80 psi are prepared in a thin form for better results. The
respectively. Similar process of washing the objective lens magnifies and focuses the images
sample was followed after the reaction was which then appear on an imaging screen which
completed. The recovered sample was dried for has charge-couple sensor that detects. A Joel-
about 24 hours under an infra-red light to dry up JEM-2100 HRTEM was used to investigate the
any moisture, collected and stored in a vial. samples studied in this. A very little sample
quantity of about 0.0001 g was dispersed in
3.2 Sample Characterization ethanol and ultrasonically vibrated at
80Hz\40Watt for 3 minutes. A thin film of copper
3.2.1 X-ray diffraction sample holder whose diameter is about 0.0005
mm was put into prepared sample and loaded in
X-ray diffraction (XRD) is a technique used to the HRTEM equipment for measuements.
investigate the structural characteristics of
crystalline or amorphous materials. It can be Surface morphology of samples is better studied
applied to identify phases of crystalline structures using high resolution scanning electron
in a sample. It provides detailed Information microscopy (HRSEM). The machine operates
about the lattice fringes of crystalline samples with similar principle as that of the HRTEM
often known as d spacing. Microstructural except that the electron beam is focused on the
information such as crystal orientation, internal sample’s surface. The strikes of the electron
stress, crystallite size and shape can be derived beam on the surface generate signals required
from XRD data [18]. The principle of X-ray for information about the elemental composition
diffraction is such that when X-rays leave a of the sample, also referred to as energy
crystal it causes the incident beam to interfere dispersive X-ray. A Zeiss ultra plus HRSEM
with each other. However, diffraction only occurs model was used do sample surface scan in this
if Bragg's law is satisfied which is mathematically work. The sample preparation performed by
expressed as; depositing very little quantity one side of a sticky
carbon tape attached to a sample holder. The
n  2d sin  , (5) sample was coated with gold using a Polaron SC
500 sputter coater to avoid charging by the
where θ is the angle between the incident beam electron beam.
and the scattering plane, d is the interplaner
distance, λ is the wavelength of the incident 3.2.3 Magnetization measurements
beam and n is an integer,. The lattice constant a
of a cubic crystal has a relationship with the of a A LakeShore vibrating sample magnetometer
sample by the following equation; (VSM) was used to measure the magnetic
properties. The sample was measured in a
a  d h2  k 2  l 2 . (6)
magnetic field of about 14 kOe. The VSM
comprise a 735 VSM controller, a vibrating head
Therefore, substituting Bragg's law into the mounted on a cryostat, a pair of pick-up coils at
Equation (6) gives Equation (4). It is from the the faces of the poles of the electromagnet. It
XRD high intensity peak (311) that the crystallite also contains a bipolar electromagnet power

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 Musa et al.; AJR2P, 5(3): 14-25, 2021; Article no.AJR2P.81418

supply, a Gaussmeter for magnetic field based on the structural studies, morphological
measurements, a temperature controller, a chiller and magnetization measurement.
and a data card for data collection.
The VSM operates on the Faraday’s law of 4.1 X-ray Diffraction
magnetic induction which is due to the induced
voltage that is generated from the pair of pick-up The X-ray powder diffraction patterns for
coils. The voltage is proportional to the CoFe2O4 and ZnFe2O4nano-ferrites are shown in
magnetization of the sample. According to Figs. 2 and 3 respectively. The XRD instrument
Faraday's law; used in the current work was equipped with a
diffracted beam monochromator in the receiving
d optics equipped with a Cobalt anode at
  E, (7) wavelengths λ1=1.7892 Å, and λ2=1.7931 Å. The
dt calculated average wavelength λ was 1.7903 Å.
The data were collected in a 2θ-range of 10° to
d 80° at an angular resolution of 0.02°. The results
show that nano-ferrites samples are pure phases
where dt is the rate of change of magnetic flux
without impurities. All the peaks are well indexed
and E is the induced voltage. This principle helps
with reference to the spinel structure (Joint
to measure the magnetic moment by using the
Committee on Powder Diffraction Standards
AC signal produced from the vibrating
(JCPDS No. 022-1086) associated with the
magnetized sample. The degree of the
space group Fd3m [19]. The prominent 311 peak
magnetization of the sample bears a direct
associated with spinel structure can be clearly
relationship with the amplitude of the induced
seen. The broadness of the peaks, especially for
signal.
the CoFe2O4 nano-ferrites is indicative of the
57 nano-particle nature of the sample. Therefore,
3.2.4 Fe Mössbauer setup and measure-
the expectation is that the crystallite size of the
ments
CoFe2O4 nano-ferrites should be smaller
Fig. 1 shows a typical block diagram of a 57Fe compared to that of ZnFe2O4 nano-ferrites.
Mössbauer spectroscopy deployed for the
current work. It shows a Mössbauer drive unit The crystal structure analysis were performed
(MDU), a CANBERRA amplifier, a pre-amplifier, using the 311 peak to determine parameters
a power supply, a detector and a multichannel such as the crystallite size D and the lattice
analyzer (MCS). The device contains a 25 parameters a. The D and a were calculated using
57
mCi Co source that is sealed in a Rh matrix and equations 3 and 4 respectively, and the obtained
attached to the transducer. The calibration was values are presented in Table 3. As expected
done at room temperature using an alpha-iron from the broadness of ZnFe2O4nano-ferrites XRD
foil. A thin sample of about 0.2 g was sufficient peaks, the crystallite size of the ZnFe2O4nano-
for the measurement. The γ ray of energy particles is bigger by about 8 nm compared to
intensity of 14.4 keV from the source interacts CoFe2O4nano-ferrites. This might not be
with the nucleus of the sample and the unconnected to the ionic radii of Co and Zn,
transmitted rays through the sample are detected which are 125 pm and 137 pm respectively [20].
by the detector. The signals are therefore This implies that Zn with larger ionic radius could
amplified at high voltage (HV) and transmitted lead to expansion of the unit cell of
through a single channel analyser (SCA). They ZnFe2O4nano-ferrites. The values of the lattice
are further processed for data capture using a parameters, a, are consistent with reported
multi-channel analyzer (MCA). The data are values for ferrite spinel structure. No significant
interpreted on the computer screen as increase was, however, observed for a in both
Mössbauer spectra. The collection of samples.
the data is carried out for a minimum of
about 15 minutes. However, analytical 4.2 Morphological Studies
Mössbauer recoil software is used for the data
analysis. The shape of the nano-particles and their surface
were examined using high resolution
4. RESULTS AND DISCUSSION transmission electron microscopy and high
resolution scanning electron microscopy
This section provides details on results and (HRTEM and HRSEM) respectively. The
analysis of the magnetic nano ferrites material morphologies of the samples are shown in Figs.

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2 and 3.respectively The nano-ferrites sample of sizes of the ZnFe2O4nano-ferrites are bigger than
CoFe2O4 shows a better crystalline structure with that of CoFe2O4nano-ferrites. This supports the
particles of almost spherical shape compared to crystallite size estimation from the XRD data.
ZnFe2O4nano-ferrites. The HRSEM images of The surface images also show the fairly spherical
both nano-ferrites measured at the same nature of the nano-particles.
magnification of 100 nm reveal that the particle

Fig. 1. Mössbauer spectroscopy block diagram

(a) ZnFe2O4 Ferrites (b) CoFe2O4 Ferrites

Fig. 2. X-ray diffraction patterns for (a) ZnFe2O4 ferrites and (b) CoFe2O4 ferrites

Fig. 3. HRTEM image of nano-ferrites synthesized by glycol-thermal method

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4.3 Magnetization Measurements superparamagnetic behavior associated with

smaller particle. The nano-ferrite had coercivity
Magnetization measurements at room HC of about 0.03 kOe and saturation
temperature were performed on the nano-ferrites magnetization MS of about 50 emu/g. These
samples, using LakeShore model 735 VSM features are desirous for practical application of
equipment. The magnetic properties such as nano-particles for oil spill cleanup. The
coercivity HC and saturation magnetizat sizes as implication is that a small magnet will be
already shown in the VSM results. Similar sufficient to magnetize and demagnetize the
magnetization results for CoFe2O4 have been sample without significant remnant or residual
reported by Xing-Hua et. al. [12] MS were magnetization in the sample. It also implies that
estimated from magnetic hysteresis loops. The during the recycling process of the nano-
HC and MS were estimated based on Equations 2 particles, magnet with little magnetic field
and Equation 1 respectively. The magnetic strength can help perform the cycle of
hysteresis loop for CoFe2O4 nano-ferrites is magnetization with swift response to the
presented in Fig. 4 (a). The fit is shown in Fig. magnetic field.
4(b). The hysteresis loop show evidence of

Table 1. Crystal structure parameters, size (D), LATTICE PARAMETER (a) for CoFe 2O4 and
ZnFe2O4 nano-ferrites
2
Sample D (nm)±0.24 a (Å)±0.005 R
CoFe2O4 10.04 8.384 0.9869
ZnFe2O4 17.82 8.386 0.9871

(a) HRSEM image of CoFe2O4 Nano-Ferrites (b) HRSEM image of ZnFe2O4 Nano-Ferrites

Fig. 4. HRSEM image of nano-ferrites synthesized by glycol-thermal method

(a) (b)

Fig. 5. (a) Room temperature hysteresis loops of CoFe2O4nano-ferrites, (b) A fit approach to
saturation magnetization of the high field initial magnetization of CoFe2O4 (Equation 1)

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Similar analysis was performed on the ZnFe2O4 fitting of the magnetic components using the
nano-ferrites particles. The hysteresis loop is Lorentzian site analysis.
presented in Fig. 5(a). The magnetic loop
appears to show mixed magnetic phases of Two sextets’ δ1 and δ2, were best suited to model
super-paramagnetism and paramagnetism. The the CoFe2O4 nano-ferrites as shown in Fig. 6.
paramagnetic component can be observed from The spectra shows a well ordered magnetic
the steep shape of the hysteresis loop. phase where sextets’ δ1 and δ2 are associated
3+
Coercivity, HC, of about 0.20 kOe and saturation with Fe ions at tetrahedral A-sites and
magnetization MS of about 30 emu/g were octahedral B-sites of the spinel crystal structure
obtained. The low magnetization value when [23]. Table 2 gives the values of the magnetic
compare to that obtained for CoFe2O4 nano- hyperfine field, HBf, isomer shift, IS, quadrupole
ferrites could be attributed to unpaired electrons splitting, ΔEQ, and the fraction population, f, of
3+
in the valence shell of Zn atoms, thereby causing Fe ions. The higher field of about 482 kOe is
a poor magnetic response of the ZnFe2O4 nano- attributed to the B-sites and the lower field of
ferrites. Thus could also explain why there is a about 445 kOe associated with the A-sites. The
slight increase in the coercivity because, non- isomer shift values are in the appropriate range
3+
magnetic atoms within a cluster of magnetic for Fe [24] and the hyperfine magnetic field are
spins could increase coercivity [22]. Although, close to reported values [25]. Therefore, no
2+
CoFe2O4 nano-ferrites showed the most desirous evidence of Fe is observed.
properties for application, ZnFe2O4 nano-ferrites
is less toxic. Therefore, its response to the However, the ZnFe2O4 nano-ferrite was not a
application and removal of magnetic field could well ordered sextet compared to CoFe2O4 nano-
be slow, it will be environmentally friendly. ferrite, and it was best fitted with two sextets and
two doublets as shown in Fig. 7. The results are
The obtained parameters from the fit to the law of shown in Table 3. The effect of the paramagnetic
approach to saturation magnetization of Equation component can be seen to have a dropping
1 are presented in Fig. 5(b). The significant effect and broadness of the spectra. The two
change in the parameter for ZnFe2O4nano- sextets are associated with the coordination of
ferrites is indicative of a nonmagnetic inclusions 3+
Fe ions at tetrahedral A and octahedral B sites
arising from Zn atoms. of the spinel crystal structure [26,27]. The
57 doublets account for the paramagnetic
4.4 Fe Mössbauer Spectroscopy
component as was observed in the magnetic
Measurements hysteresis loops. Again, the isomer shift values
3+
The
57
Fe Mössbauer spectroscopy are in the appropriate range for Fe . Higher
measurements for the CoFe2O4 and ZnFe2O4 values of quadrupole splitting indicate that the
nano-ferrites were performed at room ions are imbedded in non-cubic surroundings,
temperature. α-Fe foil was used for the while the relatively small values of the
calibration at a constant acceleration. The Recoil quadrupole splitting indicate that A and B sites
Mössbauer analysis software was used for the have nearly cubic symmetry.

(a) (b)

Fig. 6. (a) Room temperature hysteresis loops of ZnFe2O4nano-ferrites, (b) A fit approach to
saturation magnetization of the high field initial magnetization of ZnFe 2O4 (Equation 1)

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Table 2. Mössbauer parameters of CoFe2O4nano-ferrites samples obtained from fit, where δ

isomer shifts, (IS) Hbf is the hyperfine magnetic field, quadrupole splitting (ΔEQ), fraction
2 2
populations (f ) and reduced chi (R ) of Fe ions
2
Sample Sites HBf(kOe) δ (mm/s) ΔEQ (mm/s) f (%) R
±1.3 ±0.02 ±0.00 ±2 1.3110
CoFe2O4 δ1 (A-site) 445.3 0.31 0.01 30
δ2 (B-site) 482.3 0.31 0.01 70

Table 3. Mössbauer parameters obtained from fit, where Hbf is the hyperfine magnetic field, δ
2 2
isomer shifts (IS), quadrupole splitting (ΔEQ), fraction populations (f ) and reduced chi (R ) of
Fe ions of ZnFe2O4nano-ferrites samples
2
Sample Sites HBf(kOe) δ (mm/s) ΔEQ (mm/s) f (%) R
±1.2 ±0.02 ±0.00 ±1
ZnFe2O4 δ1 (A-site) 408 0.32 0.00 24 1.1102
δ2 (B-site) 470 0.31 -0.00 15
D1 0.37 7.22 30
D2 0.35 1.03 32

57
Fig. 7. Fit to Fe mössbauer Spectra for CoFe2O4 nano-ferrites

57
Fig. 8. Fit to Fe Mössbauer spectra for ZnFe2O4nano-ferrites

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 Musa et al.; AJR2P, 5(3): 14-25, 2021; Article no.AJR2P.81418

5. CONCLUSIONS oxidation state of Fe was seen. The hyperfine

fields based on the Lorentzian site analysis for
Magnetic nano-particles possess the potential to ZnFe2O4 nano-ferrites were lower compared to
be used for environmental remediation. Certain CoFe2O4 nano-ferrites. The glycol-thermal
magnetic properties are expected for such synthesis method is a viable method to produce
application. This work studied the structural and nano-ferrites with single phase.
magnetic properties of CoFe2O4 and
ZnFe2O4nano-ferrites synthesized by glycol- From the single phase of CoFe2O4 nano-ferrites
thermal technique. The properties that support and ZnFe2O4 nano-ferrites which ware
their application for oil spill cleanup are synthesized by glycol-thermal method at 200 ºC
57
considered. Structural properties were we are able to show from Fe Mössbauer
investigated by X-ray diffraction technique from spectroscopy measurement that the oxidation
3+
which information such as crystallite size and state of Fe was stable at Fe such stability in the
lattice parameters were determined. The oxidation state of Fe helps in reusability of the
CoFe2O4 and ZnFe2O4nano-ferrites samples nanoparticles after every cycle of clean up. This
were single phase cubic spinel structure without is important because the magnetic properties of
any impurity phase. Larger crystallite size of the nanoparticles can be fairly predicted not
about 17 nm was obtained for ZnFe2O4nano- change significantly to affect its application
ferrites compared to about 10 nm obtained for around room temperature. We are also able to
CoFe2O4nano-ferrites. Such large size was find that CoFe2O4has a low desirable coercivity
attributed to lager atomic radii of Zn atoms. No property making it a better candidate for possible
significant changes occurred in the lattice oil spill cleanup compared to the ZnFe2O4studied
parameters. The high resolution transmission in the current work.
electron microscopy and surface microscopy
showed that nano structure and the almost- DISCLAIMER
spherical shape of the nanoparticles.
The products used for this research are
Room temperature magnetization results of the commonly and predominantly use products in our
two samples show evidence of area of research and country. There is absolutely
superparamagnetic behavior for CoFe2O4nano- no conflict of interest between the authors and
ferrites. However, a mixed magnetic phase of producers of the products because we do not
superparamagnetism and paramagnetism intend to use these products as an avenue for
appear to be the case for ZnFe2O4 nano-ferrites. any litigation but for the advancement of
CoFe2O4 has a low coercivity and high knowledge. Also, the research was not funded by
magnetization compared to ZnFe2O4 nano- the producing company rather it was funded by
ferrites. This suggests that the nanoparticles will personal efforts of the authors.
respond to small magnetic field when such
particles are used for environmental remediation COMPETING INTERESTS
such as oil spill cleanup. However, it has a
disadvantage of toxicity at high concentration Authors have declared that no competing
dosage compared to ZnFe2O4 nano-ferrites that interests exist.
is environmentally friendly. Hence, ZnFe2O4
nano-ferrites might have a slow response to REFERENCES
magnetic field, it possess higher potential for
environmental sustainable when considering the 1. Kirubakaran S, Thiruvenkatam V. Diverse
two samples studied in this work. The room applications of nanotechnology in
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