Trends Sci. 2026; 23(6): 12296

Unveiling the Significant Role on Synthesis of Magnetic CuFe₂O₄ Photocatalyst for Dye Degradation

Is Fatimah^1,2,*, Lela Dwi Rahmawati^1,2, Nunung Nurlaela^1,2,

Suresh Sagadevan³, Mohd Rafie Bin Johan³ and Ruey-An Doong⁴

¹Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Islam Indonesia,

Daerah Istimewa Yogyakarta 55584, Indonesia

²Nanomaterials and Sustainable Chemistry Research Centre, Universitas Islam Indonesia,

Daerah Istimewa Yogyakarta 55584, Indonesia

³Nanotechnology & Catalysis Research Centre, University of Malaya, Kuala Lumpur 50603, Malaysia

⁴Institute of Analytical and Environmental Sciences, National Tsing Hua University, Hsinchu 300044, Taiwan

(^*Corresponding author’s e-mail: [email protected])

Received: 16 October 2025, Revised: 9 November 2025, Accepted: 16 November 2025, Published: 5 February 2026

Abstract

Metal ferrites have been known and utilized in various applications, including as photocatalyst for organic contaminated water treatment. In this work, exploration on synthesis of copper ferrite (CuFe₂O₄) by evaluating the role of synthesis method and the use of surfactant on physicochemical characteristics has been performed. Effect of hydrothermal (HT) and ultrasound-irradiation methods with and without the addition of cetyltrimethylammonium bromide (CTAB) as templating agent on physical and optical features was analysed using X-ray diffraction (XRD), scanning electron microscopy, Fourier-Transform Infra-red, particle’s size analysis, diffuse reflectance UV-Visible spectrophotometry (UV-DRS), and vibrating sample magnetometer (VSM). Photocatalytic activity of the prepared samples was examined in methyl violet photocatalytic degradation under UV and visible lights exposure. The HT treatment produced higher crystallite and particle’s size, and the increased size is correlated to decreased band gap energy of nanomaterials. In addition, the particle size which also influenced to magnetism. The band gap energy of materials are ranging at 1.71 - 2.01 eV, while magnetism ranging at 14.45 - 18.41 emu/g with the highest value gained by HT-prepared nanomaterial, while the lowest value is observed by ultrasound-irradiated method. Photocatalytic performance of the prepared materials is excellent as shown by an efficient methyl violet degradation under UV and visible light exposure. The maximum degradation of 99.9% was achieved by CuFe₂O₄ with the lowest band gap and largest crystallite size prepared under hydrothermal method without CTAB addition.

Keywords: Magnetic, Metal ferrite, Photocatalyst, Spinel ferrite

Introduction

In recent years, spinel ferrite magnetic materials have attracted the attention of researchers. Spinel ferrite magnetic materials have unique magnetic, electrical and optical properties and can be applied in various fields [1]. Spinel ferrites are materials with the general formula MFe₂O₄, where M is a divalent cation such as Zn²⁺, Ni²⁺,

Mn²⁺, or Cu²⁺. These materials have received increasing attention in recent years due to their beneficial combination of magnetic, electrical, and optical properties, suitable for a wide range of applications from data storage, biomedical and energy storage [2,3]. Spinel ferrites have shown great potential for environmental applications such as water treatment agents (heavy metal removal or catalytic destruction of organic pollutants). CuFe₂O₄ is a particle that has an inverse spinel crystal structure. CuFe₂O₄ is one of the spinel ferrites that has been utilized as catalyst and photocatalyst for various reactions. The magnetism of CuFe₂O₄ gives benefit for easy in separation and reusability [4].

Several methods are used for the synthesis of copper ferrite, and these play an important factor to create physicochemical characters for furthermore determine the chemical activity of the material. The methods consist of the sol-gel, mechanochemical method, coprecipitation, microemulsion, hydrothermal method (HT), ultrasound-irradiation (US) and mechanochemical methods. The coprecipitation method is one of the most used methods for synthesis due to its simple and easiness. Additionally, the combination with HT, US or microwave irradiation were applied to intensity the crystallization and particles growth [5]. Similar to some other nanoparticles synthesis, synthesis routes control the physicochemical features of material, including optical properties [6]. In addition, surfactants influence the growth of nanoparticles.

The physicochemical features are theoretically affecting the chemical activity, including optical properties and photocatalytic activity. Considering the magnetic photocatalyst is a required form in dye degradation by photocatalysis mechanisms recently, evaluation on the photocatalytic activity of CuFe₂O₄ is interesting to be explored. Previous works investigated the effect of HT-method and US-method on the morphology, magnetism, optical, crystallite size and infra-red radiance performance [7-9] and study of the effect of cationic surfactant on physicochemical feature of CuFe₂O₄ has been performed [10]. An intensive wavelength and energy supported by US accelerate coprecipitate to the fast nucleation environmentally friendly, safe and inexpensive [11,12]. Particularly, US irradiation leads to faster and more efficient material production, so it is expected to be easily controlled and produce materials that have a specific diameter with a faster rate in the deposition process [2]. However, comparative study on both HT and US methods along with effect of surfactant to the physicochemical character of CuFe₂O₄ nanoparticles for advance applicability as photocatalyst is not reported yet. Within this scheme, cetyltrimethylammonium bromide (CTAB) is considered as an effective templating agent by the succeed for some nanoparticles synthesis with small concentration required to control nanoparticles growth [13,14]. From these backgrounds, this study is expected to unveil the role of the use of HT method and US irradiation along with the effect of the addition of CTAB in synthesizing CuFe₂O₄. The comparison of HT and US method and study on the effect surfactant addition to the physicochemical and photocatalytic activity is the novelty of this work which never explored before. The physicochemical characterization was observed is using X-ray diffraction (XRD), Fourier-Transform Infra-Red (FTIR), particle size distribution (PSD), diffuse reflectance UV-Vis Spectrophotometer (UV-DRS), and VSM instruments, while got photocatalytic activity examination, methyl violet was chosen as model of dye molecule. The phenomenon on intensification during nanoparticles formation and was aimed to be studied to get an effective synthesis of CuFe₂O₄.

Materials and methods

Preparation of CuFe₂O₄

About 4 g of FeCl₃.6H₂O, 2.72 g of Cu(II) acetate, 2.05 g of sodium acetate and 0.007 g of sodium citrate were mixed with 200 mL of demineralized water. Into the solution, 50 mL of 0.2% of CTAB was added followed by seting up the solution to get pH 10 with the addition of NaOH solution. After furthermore followed by stirring for 1 h, the solution was transferred into a Teflon-lined autoclave, heated at 180 °C overnight. The obtained slurry from these steps was calcined at 500 °C for 2 h, and the sample was encoded as CFO-HTC.

Similar procedure was performed without the addition of CTAB but in HT treatment, and the sample was encoded as CFO-HT. From US treatment, the HT traetment after coprecipitation was replaced by US irradiation to the precipitate for 1 h using commercial ultrasound chamber, and other steps are in same condition. The samples obtained from the synthesis by using CTAB and without CTAB were designated as CFO-S and CFO-SC. Figure 1 depicts the scheme of synthesis, and the summary of synthesis conditions is provided in Table 1.

Figure 1 Scheme of synthesis.

Table 1 Resume of samples synthesis condition.

Material’s characterization

The crystallinity and phase of the prepared samples were analysed by using X-ray diffractometer (XRD) spectroscopy on Phenom X’. Ni-filtered Cu Kα irradiation (λ = 1.54) was utilized as photon source, and the measurement was recorded from 10° - 70° of diffraction angles (2θ), step size of 0.1°/step. The morphology of the prepared samples was examined by using field emission scanning electron microscope (FE-SEM). Fourier-transform Infrared Spectroscopy (FT-IR) analysis (Perkin Elmer Spectrum One, USA) was used to investigate the functional groups in the samples recorded at the 4,000 to 500 cm⁻¹ wavelength range. Vibrating magnetometer 7400 Series VSM System (Lake Shore, Ohio) was employed for magnetism analysis, and the hysteresis measurements were performed at 300 K with magnetic field up to 0.9 T to obtain the demagnetisation corrections. Zetta-sizer Nanoseries instrument (Malvern, United Kingdom was utilized to measure the surface potential of the samples. UV-DRS of JASCO V760 was used for the band gap energy determination.

Photocatalytic activity examination

The capability of prepared CuFe₂O₄ as photocatalyst was evaluated by batch photocatalytic degradation experiments. Close batch experiments of photocatalytic degradation of methyl violet (MV) were conducted using a reactor equipped with UV lamp (Philips, 20 Watt) with the light intensity of 34.9 W/cm² and xenon lamp (Philips, = 500 nm, 30 watt) with the light intensity of 32.0 W/cm²  as visible light source. In each experiment, about 0.1 g of the CuFe₂O₄ sample was dispersed into 100 mL of 20 mg/L of MV solution. Stirring for 15 min in a dark condition was performed prior UV light exposure. An aliquot of 5 mL was taken out from that solution after every 15 min, filtered by using syringe filters and then the MV concentration was determined by UV-Visible spectrophotometer (HITACHI U-2080, Japan). Degradation efficiency (DE) was calculated based on the percentage of reduced concentration measured by colorimetric analysis.

Results and discussion

Physicochemical characterization

The XRD diffraction patterns of the prepared sample is presented in Figure 2. From the figure, it is seen that all sample show the characteristic peaks of CuFe₂O₄ at 2 of 16.2°, 33.2°, 35.6°, 38.7°, 49.5°, 54.1° and 62.5° that are in good agreement with the (111), (220, (311), (222), (400), (422), (511) and (440) planes, respectively referred to the Joint Committee on Powder Diffraction (JCPDS) No. 35-0425. In addition, the HT-prepared samples; CFO-HT and CFO-HTC express additional peak at 2 = 24.22° which potentially demonstrated the presence of Fe₂O₃. The formation of Fe₂O₃occurred due to the excess Fe ions in the precursor which accelerate to be hydrated under HT pressure and temperature. Similar phenomenon was obtained in the synthesis of CuFe₂O₄ reported in previous works [15].

Further calculations on crystallite size based on some peaks were performed by following equation Eq. (1), and the results are provided in Table 2.

With K is k is a constant related to the crystalline shape, λ is wavelength, β is full width and half maximum (FWHM), and θ is reflection angle.

Figure 2 XRD patterns of prepared CuFe₂O₄

Table 2 Calculation of crystallite size based on XRD measurement.

Based on the results obtained in Table 2, it is seen that CFO-HT, CFO-HTC, CFO-S and CFO-SC have crystal sizes of 34.72, 33.20, 18.40 and 23.51 nm, respectively. The addition of CTAB into a-HT-synthesized material reduces the crystal size, meanwhile the effect is on opposite way for US-irradiation method. The reduced crystallite size by the presence of the surfactant in the crystal gowth is similar to was reported in the synthesis of CuO nanoparticles. The decomposed gel formation of CuO was obtained with the addition of CTAB surfactant and it confirmed the presence of compressive strain in the crystal lattice [16]. Similarly, the addition of Triton-X gave the smaller crystallite size of SnO₂ [17]. The addition of surfactant acted as templating agent to fix the better crystallinity of the particles. As also confirmed by the FWHM data and available peaks of CuFe₂O₄, the HT-synthesized materials have better crystallinity rather than US-irradiated materials [18]. However, as the energy sufficiently provide faster aggregation of the particles, the surfactant promotes particle’s growth for greater size as reported in the use of polyethylene glycol (PEG) in the synthesis of ZnO [19]. Surfactant could increase monodispersion of each reactant to enhance stability of the growth particles. The surfactant concentration modulates the size of nanoparticles due to the hindrance of surfactants and interparticle interaction. Referred to the investigation on effect of surfactants for NiFe₂O₄ and gold nanoparticles syntheses [20,21], mechanism on hindered aggregation is represented in Figure 3.

Figure 3 Mechanism of nanoparticles growth by the addition of surfactant.

These data imply that that the addition of surfactants consisting of heads (hydrophilic) and tails (hydrophobic) can improve the properties of the synthesized particles. With the presence of surfactants, the surface tension of the solution is reduced so that it can form nucleation and the formation of new phases. However, in the US- irradiation method, the crystal size does not decrease because the reaction takes place quickly, so that the surfactant does not affect the nucleation process or it influenced to force faster aggregation.

Figure 4 FTIR spectra of materials.

FTIR spectra of the samples (Figure 4) show the absorption peaks at around 3,420 - 3,034 cm⁻¹ associated to the peaks at around 1,622 cm⁻¹ refer to water absorption and surface O-H groups in the spectrum of the oxides. In HT-method synthesized samples (CFO-HT and CFO-HTC), some peaks at around 900 - 800 cm⁻¹ are reflected which are assigned to the the binding of OH with Fe and Cu [22]. In addition, there are some peaks observed at around 560 cm⁻¹ corresponded to the vibrations of the Fe-O bonding and the peaks at around 460 - 475 cm⁻¹ revealing the O-Cu binding. The bands are assigned to the Fe-O tetrahedral group which related to Cu-O demonstrating bond formation between iron and oxygen and cupper and oxygen, respectively [23].

Figure 5 SEM images of prepared materials.

Surface morphology of the prepared samples is expressed irregular forms of the particles, and it is a distinctive surface image presented in Figure 5. The hypothesized aggregation is confirmed by the bigger particle’s size in CFO-SC compared to other samples. In addition, both CFO-HT and CFO-HTC display the rod-like forms that are presumable for Fe₂O₃ as also presented from XRD analysis results [24]. Dynamic light scattering (DLS) was used to evaluate the particle’s size distribution (PSD) of the prepared materials, and the results are presented in Figure 6.

Figure 6 Particle’s size distribution of (a) CFO-S, (b) CFO-SC, (c) CFO-HT, and (d) CFO-HTC.

The particle’s size of HT-prepared materials demonstrated the larger particle’s size compared to coprecipitation method. The faster crystal growth could be provided temperature and pressure in HT condition. In more detail, the addition of CTE reduces the particle’s size suggesting the capping agent effect of secondary metabolite of the extract referred to the colloidal stability of crystal growth in the system. Effect of extract concentration influences the colloidal system and sintering to form the particles. This phenomenon was expressed in the formation of SnO₂ and GdPO₄·nH₂O nanoparticles [25,26].

Magnetic properties

The magnetic properties of the samples were studied using VSM at room temperature, and the hysteresis curves are depicted in Figure 7. It can be observed that in general, all samples exhibit ferromagnetic behaviour with magnetism (Ms) and finite coercivity (Hc). The highest magnetism is expressed by CFP-HT with the magnetism of 18.41 emu/g and the less magnetism is observed from CFO-S with 14.45 emu/g. By plotting the relationship between crystallite size and magnetism, it could be concluded that the magnetism is associated with the larger crystallite size as similar to was reported by the synthesized CuFe₂O₄ using honey mediated sol-gel combustion method [27]. Meanwhile the coercivity is related to the phase anisotropy of tetragonal and hexagonal in spinel ferrite structure. The magnetism values from these are also comparable to was reported as with similar range of crystallite size, the magnetisms area at around 11 - 19 emu/g. Similar range is also considered by the prepared CuFe₂O₄ with crystallite size of 15 nm expressing the magnetism of 11 emu/g [28]. The smaller crystallites generally lead to increase surface effects and disordered layers meanwhile larger crystallites can alter the transition from single domain to multi-domain states, but some other factors such as the morphology of nanoparticles and the presence of other minerals or organic component could influence reduce the magnetism. Thus, the smaller crystallite size influences the magnetic properties for weaker magnetization and higher coercivity [29]. Table 3 summarizes the crystallite size and magnetism of similar works.

Table 3 Crystallite size and magnetism of prepared CuFe₂O₄ with present work.

Figure 7 (a) Magnetism of samples and (b) Correlation of crystallite size and magnetism.

Optical properties

The optical property of the prepared materials was evaluated by UV-DRS spectroscopy to determine the band gap energy (Eg). Based on the spectra, Eg was calculated using the Tauc’s method referred to equation:

With is absorption co-efficient, ħ isPlankʼs constant, and is the frequency of a photon, with n = 2. The Eg values are based on the intrapolation of the graphs between (ahv)² versus hv as depicted in Figure 8. The calculation gives the Eg values of 2.00, 2.01, 1.71 and 1.81 eV for CFO-S, CFO-SC, CFO-HT and CFO-HTC, respectively. By The smaller crystallite size and higher bandgap energy for NZMF are correlated by the quantum confinement effect. Based on previous research, the crystallite size and particle’s size determine the band gap energy as the higher size contributes to reducing the band gap energy. Investigations into CdTe, ZnS, CdSe, ZnSe, and ZnTe nanoparticles revealed that increased particle size the band gap energy of semiconductor nanomaterials reduces as their particle size increases [34,35].

Investigation resumed the altering optoelectronic properties of InX semiconductor nanoparticles with X = As, Sb, and P significantly dependent on the size and nanoparticles. The blue shifts of optical absorption spectra related to an improved exciton confinement and stronger quantum size effects by smaller nanoparticles. Additionally, morphology and shape of the nanoparticles affect to the density and electronic band structures to change the dynamics and recombination of charge carriers [36]. The correlation between particle’s size and band gap energy of prepared samples is plotted in Figure 8(e). The plot tends a non-linear correlation which is similar to was reported from InX nanoparticles and Nano-TiO₂ [37,38].

Figure 8 (a) - (d) UV-DRS spectra of prepared materials, (e) Effect of particle’s size on E_g.

Photocatalytic activity

The photocatalytic behaviour of the prepared materials was examined on MV degradation on a batch reaction system under UV and visible light exposure. The kinetics evaluation based on concentration change of MV at interval time. The spectral changes of treated MV under UV and visible light are presented in Figures 7(a) - 7(b). Based on the spectral changes, the kinetics plots and the resumed DE are provided in Figures 7(c) - 7(e). There is significant reduced absorbance of the solution by the photocatalytic treatments either by UV or visible light, implying the degradation mechanism of towards MV. The identified degradation is confirmed by the significant difference among the spectral changes and the plots obtained from the photocatalytic treatments respect to the adsorption treatment. Based on the kinetics data, the provided optical properties of all prepared samples are sufficiently supporting the formation of oxidant to degrade MV compound by their interactions with light sources. Based on RE values, it is considered that the activity of the samples is with following order: CFO-HT>CFO-HTC>CFO-S>CFO-SC. The highest photocatalytic activity achieved by CFO-HT was 99.9%, and it seems that it is in opposite directions with the increased band gap energy. In addition, for all sample, the DE values gained under visible light exposure are higher than that of UV-light exposed treatment.

In this case, the lower band gap energy allows to the faster electron excitation to create radicals for faster oxidation mechanism. Similar phenomenon was observed in the Cu/ZnO composite which the enhanced activity is related to the lowering band gap energy [39]. Similarly, the reduction of band gap of NiSnO₃ and ZnS/TiO₂ causes enhanced optical absorption to facilitate photocatalytic degradation [40,41]. The data suggest that the capability of the samples to absorb photon is suitable with the range of the band gap energy. The higher photoactivity of HT samples could be related to the presence of Fe₂O₃. As byproduct or impurity of the synthesis, the combination of small amount Fe₂O₃ with CuFe₂O₄ could support the photocatalytic mechanism via Z-scheme as also reported by previous works [42,43]. The proposed scheme is presented in Figure 9.

Figure 9 (a) and (b) Spectral changes of treated MV using CFO-HT under UV and visible light, respectively, (c) and (d) Kinetics plots of MV degradation using prepared samples under UV and visible light, e. Resumed DE gained by treatment on the prepared samples.

Based on kinetics data, the photocatalytic degradation of MV obeys first-order kinetic model theory expressed by equation:

where k represents reaction rate constant (min⁻¹), C₀ and C_t are the concentrations of MV at initial and at reaction time of t. The plots and calculated k values referred to the equation are presented in Figure 10. Resumed DE and k values for each process using prepared materials are presented in Table 4.

Table 4 Recapitulated DE and k values of the treatments using prepared materials.

The values evidence and in accordance with the performance of materials. In general, all DE data represents a comparable activity to similar materials were reported by previous works as listed in Table 5. In addition, the fitness of MV degradation reaction to the pseudo-first order kinetics is summarized from all listed works.

Figure 10 Pseudo-first order plots of MV degradation using prepared samples using (a) UV light and (b) visible light.

Table 5 Comparison on photocatalytic activity of CuFe₂O₄ and related materials for MV degradation.

Mechanism of photocatalysis

It has been discussed elsewhere that the photocatalyst play role to create the radicals as the surface absorb energy from light. The sufficient energy from photon leads to electron excitation and the formation of hole (h⁺). The interaction among h⁺ and ^OH creates radicals which furthermore, by interactions with O₂ could form superoxide radicals OOH. From the excited electron, the interaction of surface with O₂ could produce can produce superoxide radicals (O₂^). The oxidation potential of these species is the main reactant for dye degradation. To investigate the contributing species in the dye degradation mechanism, kinetics evaluation of the reaction by the addition of scavengers was performed. Isopropanol (IPR), EDTA and BQ were employed as OH, h+ and OOH scavengers, respectively. The chart provided in Figure 11 suggests that the addition of IPR is the most influential scavenger to inhibit the reaction, followed by BQ and EDTA. This implies that the excitation of electron plays the most important role for creating oxidant. Furthermore, the created radicals propagate the formation of other oxidant species, referred to following mechanism:

Figure 11 Effect of scavengers on DE and kinetics constant.

Conclusions

This study provides a detailed analysis on effect of hydrothermal and ultrasound-irradiation procedures in the synthesis of CuFe₂O₄. The results indicate that the synthesis route affected the crystallite size, magnetism, and band gap energy of the nanoparticles. The presence of CTAB surfactant and templating agent governs the crystallite growth, which also depends on the temperature and pressure of the crystallization. This impact to different effect on crystallization under ultrasound-irradiation and hydrothermal condition. The increased crystallite size led to the enhanced magnetism and higher band gap energy. Moreover, the lower band gap energy determines as an important factor to increase photocatalytic activity. An excellent photocatalytic activity was expressed by the high efficiency towards methyl violet degradation. Maximum degradation efficiency of 99.9% was achieved on 120 min photocatalytic treatment under visible light on CuFe₂O₄ prepared under hydrothermal synthesis without CTAB addition.

Declaration of Generative AI in Scientific Writing

There is no AI tools used for research and manuscript preparation.

CRediT Author Statement

Is Fatimah: Conceptualization; Methodology; Software. Lela Dwi Rahmawati: Data curation; Writing - Original draft preparation. Nunung Nurlaela: Data curation; Writing - Original draft preparation. Suresh Sagadevan: Visualization; Investigation. Mohd Rafie bin Johan: Supervision- Reviewing and Editing. Ruey-an Doong: Methodology- Data Curation-Reviewing and Editing.

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