CHAPTER-4

RESULTS AND DISCUSSIONS

The objective of this study was the synthesis and characterization of Cu doped SnFe 2O4 to
investigate their structural and morphological properties. Ferrite-based nanomaterials like
SnFe2O4 are promising due to their excellent magnetic, electrical, and photocatalytic
performance, which can often be improved through metal ion doping. Incorporating copper ions
is specifically expected to enhance the material's crystallinity, surface morphology, and electronic
behavior, thereby boosting its overall functional properties. To confirm the successful synthesis
and phase purity, the resulting nanomaterials were analyzed using X-ray Diffraction (XRD) for
crystalline structure, Scanning Electron Microscopy (SEM) for surface morphology, and Energy-
Dispersive X-ray Spectroscopy (EDS) for elemental composition. The combined data provides
essential insights into how doping influences the characteristics of SnFe 2O4
4.1 XRD Analysis:
Pure and Cu-doped SnFe₂O₄ nanomaterials X-ray diffraction (XRD) pattern are shown in the
Figure 4.1.

Figure 4.1: XRD images of (a) SnFe2O4 (b, c, d) Cu/SnFe2O4

The X-ray diffraction (XRD) pattern of Cu-doped SnFe₂O₄ nanomaterials confirms the
formation of a single-phase cubic spinel structure without any secondary or impurity phases,

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indicating successful incorporation of Cu²⁺ ions into the SnFe₂O₄ lattice. The diffraction peaks
observed at 2θ values around 29.8°, 35.2°, 42.7°, 53.1°, 56.5°, and 62.2° correspond to the (220),
(311), (400), (422), (511), and (440) planes, respectively, matching well with the standard JCPDS
card No. 01-071-0695 for spinel ferrite structures. A slight shift in peak positions with Cu doping
suggests minor lattice distortion due to the difference in ionic radii between Cu²⁺ and Sn⁴⁺ ions.
The average crystallite size estimated using the Debye–Scherrer equation, lies in the range of 22–
38 nm, confirming the nanocrystalline nature of the synthesized samples. The overall structural
analysis reveals that Cu doping does not alter the spinel phase but induces slight modifications in
peak intensity and width, which can be attributed to changes in crystal strain and particle size.
4.2 SEM and EDS Analysis:
The surface morphology and elemental composition of the synthesized Cu-doped SnFe₂O₄
nanomaterials were thoroughly examined using Scanning Electron Microscopy (SEM) and Energy
Dispersive X-ray Spectroscopy (EDS). The SEM micrographs clearly reveal that the Cu-doped
SnFe₂O₄ nanoparticles possess a predominantly spherical morphology with a uniform and
homogeneous distribution across the surface. The particles appear well-defined and finely
dispersed, exhibiting minimal agglomeration, which indicates that the incorporation of copper ions
contributes to enhanced surface stability and uniform growth during the synthesis process.

Figure 4.2: SEM images of (a) SnFe2O4 (b, c, d) Cu/SnFe2O4

The average particle size of the Cu-doped SnFe₂O₄ nanoparticles was estimated to be
approximately 28 nm, confirming the formation of nanocrystalline particles. The relatively small
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and consistent particle size suggests that Cu doping effectively influences the nucleation and grain
growth mechanisms, leading to a reduction in particle aggregation and an improvement in surface
smoothness. Such morphological refinement can be attributed to the substitution of Cu²⁺ ions into
the ferrite lattice, which modifies the crystallization kinetics and enhances structural compactness.
Furthermore, the presence of well-defined and uniformly distributed grains confirms the successful
synthesis of Cu-doped SnFe₂O₄ nanoparticles with controlled morphology and high structural
integrity. These characteristics are particularly advantageous for catalytic and optical applications,
as the nanoscale dimensions and smooth surface texture provide a larger active surface area and
improved interaction with reactive species.

Figure 4.3: EDX spectrs of Cu/ SnFe2O4

The Energy Dispersive X-ray Spectroscopy (EDS) analysis was carried out to verify the
elemental composition and purity of the synthesized Cu-doped SnFe₂O₄ nanomaterials. The EDS
spectrum shown in Figure 4.3 confirms the presence of tin (Sn), iron (Fe), oxygen (O), and copper
(Cu) as the major constituent elements, validating the successful incorporation of Cu ions into the
SnFe₂O₄ lattice. The absence of any extraneous peaks or impurity-related signals in the spectrum
indicates the high purity of the synthesized sample and confirms that the hydrothermal synthesis
route effectively prevented contamination during material formation. The elemental mapping
further reveals a uniform spatial distribution of Sn, Fe, O, and Cu throughout the sample surface,
demonstrating homogeneous doping and consistent compositional uniformity. The presence of Cu
at low intensity levels corresponds to its controlled doping concentration, ensuring that it
substitutes partially for Fe sites within the ferrite framework without altering the overall
stoichiometric balance. This uniform incorporation of Cu ions is likely to influence the electronic
structure and surface activity, enhancing charge transfer efficiency during photocatalytic
processes. Weight percentage of elements in both the nanomaterial are given in Table 4.1

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 Table 4.1: Wt% of individual element in SnFe2O4 and Cu/ SnFe2O4

Element (Wt%) SnFe2O4 Cu/ SnFe2O4

Sn 24.84 24.18
Fe 47.09 47.13
O 28.07 26.76
Cu - 1.93

4.3 Photocatalytic activity:

The study examines the photocatalytic performance of SnFe₂O₄ and Cu-doped SnFe₂O₄
nanocomposites in the degradation of Rhodamine B (RHB) dye under light irradiation. Figure 4.4
presents the variation in RHB dye concentration during the photocatalytic process. The SnFe₂O₄
and Cu/SnFe₂O₄ samples exhibit strong degradation efficiency, which varies with different Cu
doping concentrations. The undoped SnFe₂O₄ sample shows a baseline degradation efficiency of
78.5%, reflecting its inherent photocatalytic capability. Upon doping with 1% Cu, the efficiency
improves to 89.6%, indicating enhanced electron–hole separation and surface reactivity.
Efficiencies further increase significantly to 97.4% at 3% Cu doping, demonstrating optimal
photocatalytic performance at this concentration. However, a slight decline in degradation
efficiency to 92.4% is observed at 5% Cu doping, likely due to excess dopant acting as
recombination centers that hinder photocatalytic activity. Overall, the results confirm that Cu
incorporation enhances the photocatalytic efficiency of SnFe₂O₄, with the 3% Cu/SnFe₂O₄
composition exhibiting the highest degradation performance, making it the most effective catalyst
for RHB dye degradation under visible light irradiation.

Figure 4.4: Photocatalytic activity of SnFe2O4 and Cu/ SnFe2O4 nano composites

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 The photodegradation behavior of RHB dye was analyzed using a pseudo-first-order
kinetic model, expressed by the equation ln(C₀/C) = k t, where C₀ and C represent the initial and
instantaneous dye concentrations, respectively, t is the irradiation time, and k is the rate constant.
Figure 4.5 presents the linear fitting plots of ln(C₀/C) versus time (t) for the degradation of RHB
dye using SnFe₂O₄ and Cu/SnFe₂O₄ nanocomposites. The linearity of these plots confirms that the
degradation process follows pseudo-first-order kinetics. The relatively lower correlation observed
for pure SnFe₂O₄ indicates limited photocatalytic activity, as evidenced by its smaller k value.
Upon Cu doping, the value of k increases significantly, reflecting an improvement in the rate of
photocatalytic degradation. The kinetic rate constant (k) represents the reaction speed and serves
as an essential parameter for evaluating catalytic efficiency under specific conditions. From the
kinetic rate constant data, it is evident that the 3% Cu-doped SnFe₂O₄ nanocomposite exhibits the
highest k value, indicating the fastest degradation rate of RHB dye. This result confirms that 3%
Cu doping provides the most effective enhancement of photocatalytic activity, leading to superior
degradation efficiency compared to both undoped and higher dopant concentrations.

Figure 4.5: Kinetic rate constants of SnFe2O4, Cu/SnFe2O4 nano composites

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 Conclusions
The SnFe₂O₄ and Cu-doped SnFe₂O₄ nanocomposites were successfully synthesized using the
hydrothermal method. The prepared nanocomposites were characterized using Scanning Electron
Microscopy (SEM) coupled with Energy-Dispersive X-ray Spectroscopy (EDS) to analyze their
morphology and elemental composition. Based on the experimental findings, the following
conclusions can be drawn:
 The average crystallite size of both pure SnFe₂O₄ and Cu-doped SnFe₂O₄ nanocomposites
was measured to be approximately 28 nm.
 SEM analysis revealed that the SnFe₂O₄ and Cu/SnFe₂O₄ nanocomposites possess a
spherical morphology with a uniform and homogeneous distribution of particles, indicating
a well-defined nanostructure.
 EDS spectra confirmed the presence of Sn, Fe, O, and Cu elements, verifying the successful
incorporation of copper into the SnFe₂O₄ lattice and confirming the purity of the
synthesized nanocomposites with no detectable impurities.
 The Cu/SnFe₂O₄ nanocomposites exhibited enhanced photocatalytic activity compared to
pure SnFe₂O₄ for the degradation of Rhodamine B (RHB) dye under visible light
irradiation.
 The photocatalytic degradation efficiency of the Cu/SnFe₂O₄ nanocomposites reached
97.4% after 80 minutes of light exposure, which is significantly higher than the degradation
efficiency of the pure SnFe₂O₄ nanocomposites.

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