Synthesis of Ag@ CuS doped mineral magnetite nanocomposite with improved photocatalytic activity against tetracycline and diclofenac pollutants

Synthesis of Ag@ CuS doped mineral magnetite nanocomposite with improved photocatalytic activity against tetracycline and diclofenac pollutants | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article Synthesis of Ag@ CuS doped mineral magnetite nanocomposite with improved photocatalytic activity against tetracycline and diclofenac pollutants Roya Mohammadzadeh kakhki, Hadis Bolandhemmat This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-4642539/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 16 Aug, 2024 Read the published version in Scientific Reports → Version 1 posted 10 You are reading this latest preprint version Abstract The contamination of water sources by pharmaceutical pollutants presents significant environmental and health hazards, making the development of effective photocatalytic materials crucial for their removal. This research focuses on the synthesis of a novel Ag@CuS-doped magnetite nanocomposite and its photocatalytic efficiency against tetracycline and diclofenac contaminants. The nanocomposite was created through a straightforward and scalable precipitation method, integrating silver nanoparticles (Ag NPs) and copper sulfide (CuS) into a magnetite framework. Various analytical techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and energy-dispersive X-ray spectroscopy (EDS), were employed to characterize the structural and morphological properties of the synthesized material. The photocatalytic activity was tested by degrading tetracycline and diclofenac under visible light. Results indicated a marked improvement in the photocatalytic performance of the Ag@CuS-doped magnetite nanocomposite compared to both pure magnetite and CuS-doped magnetite. The enhanced photocatalytic efficiency is attributed to the synergistic interaction between Ag NPs, CuS, and Fe3O4, which improves light absorption and charge separation, thereby increasing the generation of reactive oxygen species (ROS) and promoting the degradation of the pollutants. This study highlights the potential of the Ag@CuS-doped magnetite nanocomposite as an efficient and reusable photocatalyst for eliminating pharmaceutical pollutants from water. Ag@CuS-doped magnetite nanocomposite Photocatalytic activity Tetracycline Diclofenac visible light Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 1. Introduction The quality of life has been adversely affected by the rapid urbanization and industrialization of modern society, leading to increased contamination of groundwater, air, and fossil fuels through conventional industrial waste disposal methods [ 1 , 2 ]. Consequently, major environmental issues, such as pollution and climate change, have emerged as significant threats to ecosystems and human health [ 3 – 8 ]. According to recent reports by the World Health Organization, environmental pollution has resulted in 3.7 million deaths in the twenty-first century alone, with 92% of the global population living in areas with severe air and water pollution [ 9 , 10 ]. As a result, the safe disposal of hazardous waste in both water and the atmosphere has become a critical national and international priority [ 11 – 14 ]. Advanced Oxidation Processes (AOPs) have been extensively employed for the removal of organic contaminants from water and air, with heterogeneous photocatalysis being one of the most promising AOPs due to its ability to degrade organic pollutants [ 15 , 16 ]. Semiconductor-based photocatalysts, especially metal oxide-based ones, have garnered significant attention for their efficient and cost-effective applications in water pollution treatment and disinfection [ 17 – 24 ]. Titanium dioxide (TiO 2 ) has been widely studied due to its low cost, non-toxicity, and chemical inertness, but its photocatalytic activity is mainly confined to UV light irradiation, limiting its effectiveness under visible light [ 25 – 28 ]. Consequently, there is a pressing need to design and synthesize effective visible-light-driven photocatalysts [ 29 ]. Various metal oxides, including La 2 O 3 , CdO, CeO 2 , CaO, and ZnO, have been explored as promising co-catalysts to enhance the photocatalytic activity of TiO 2 [ 30 – 32 ]. Scientists are incorporating magnetic nanoparticles into photocatalysts. These nanoparticles, including hematite, maghemite, magnetite, and various ferrites, give the photocatalyst magnetic properties. This allows the photocatalyst to be easily separated from a solution using a magnet [ 33 ]. Adding these magnetic nanoparticles doesn't significantly affect the surface area or how the photocatalyst spreads in water because the photocatalyst remains a powder. Even better, some of these magnetic nanoparticles can absorb visible light and act as photocatalysts themselves, which can help break down pollutants even faster [ 34 ]. One of the most exciting frontiers in combating water pollution lies in the development of magnetic visible-light-active nanocomposites. These innovative materials are grabbing the attention of researchers due to their immense potential for photocatalytic environmental cleanup. This article delves into the applying these powerful tools for water treatment. Covellite CuS is a fascinating material for photocatalysis due to its visible-light absorption. This p-type semiconductor with a narrow bandgap (1.2-2.0 eV) boasts several advantages: low cost, non-toxicity, easy production, and excellent stability. Its potential as a photocatalyst is further bolstered by broad visible light absorption, plasmon absorbance, and even near-infrared (NIR) absorption. Studies on CuS for organic dye degradation have shown promise.However, challenges remain. The photocatalytic efficiency of CuS is influenced by factors like morphology, size, and surface area. Additionally, bare CuS suffers from rapid recombination of photoexcited charges and low quantum yield. Furthermore, CuS nanoparticles tend to aggregate in water, hindering their effectiveness.Researchers are addressing these limitations by creating CuS-based nanoheterostructures. These structures can modify CuS properties, leading to enhanced charge separation, improved stability, and ultimately, better photocatalytic performance[ 35 – 36 ]. An example of this approach is the work by Sohrabnezhad et al., who embedded CuS nanospheres within an MCM-41 matrix [ 37 ]. This nanocomposite exhibited superior performance in degrading methylene blue under visible light, highlighting the potential of CuS-based materials for water treatment. With its unique properties and the promise of further improvement through nanoheterostructure design, CuS presents a compelling avenue for developing powerful photocatalysts for clean water applications. Silver (Ag) doping has emerged as a promising strategy to enhance the photocatalytic activity of semiconductor photocatalysts. By incorporating Ag into the crystal lattice, it effectively lowers the recombination rate of holes and electron pairs, thereby improving the efficiency of photocatalysis [ 38 – 40 ]. Moreover, Ag doping can modify the band gap energy of the semiconductor, making it more active under visible light [ 43 ]. This property of Ag-doped materials is particularly advantageous for wastewater treatment applications. Introducing Fe 3 O 4 (magnetite) as a base material for the photocatalyst adds another dimension to its functionality. Magnetite is a naturally occurring iron oxide mineral with magnetic properties, making it an excellent candidate for various applications. In the context of photocatalysis, Fe 3 O 4 serves as a stable and robust support material for semiconductor photocatalysts like CuS[ 41 ]. The utilization of Fe 3 O 4 in CuS-based nanocomposites offers several advantages. Firstly, Fe 3 O 4 provides a high surface area and facilitates the dispersion of CuS nanoparticles, thereby enhancing the accessibility of reactants to the catalytic sites. Additionally, Fe 3 O 4 imparts magnetic properties to the nanocomposite, allowing for easy separation and recovery of the catalyst from the reaction mixture using an external magnetic field. This magnetic recyclability significantly reduces the operational costs and simplifies the catalyst retrieval process, making it more environmentally friendly. Furthermore, Fe 3 O 4 exhibits excellent stability and biocompatibility, making it suitable for applications in environmental remediation and biomedical fields. Its chemical inertness ensures that it does not interfere with the catalytic activity of CuS, while its biocompatibility is advantageous for potential biomedical applications, such as drug delivery systems. Combining Fe 3 O 4 with CuS and Ag to form ternary nanocomposites (CuS@Fe 3 O 4 /Ag) not only enhances the photocatalytic performance but also provides multifunctionality. The synergistic effects between CuS, Fe 3 O 4 , and Ag result in improved charge separation efficiency, extended light absorption range, and enhanced catalytic activity. Therefore, the incorporation of Fe 3 O 4 as a base material in CuS-based photocatalysts holds significant promise for addressing environmental pollution and advancing various technological applications[ 42 – 43 ]. However, the introduction of silver doping into CuS@magnetite (CuS@Fe 3 O 4 ) nanocomposites presents a unique opportunity. The incorporation of Ag into the CuS@magnetite structure not only enhances the photocatalytic activity but also provides magnetic properties, enabling easy separation and recycling of the catalyst from the reaction medium. This dual functionality of CuS@Fe 3 O 4 /Ag nanocomposites makes them highly desirable for environmental remediation applications [ 44 ]. In this study by incorporating Ag NPs and CuS into the Fe 3 O 4 matrix, we aim to enhance light absorption and charge separation, leading to improved photocatalytic performance. Additionally, the magnetic properties of the nanocomposite facilitate easy separation and recyclability, making it a promising candidate for practical applications in water treatment processes. Through this research, we contribute to the development of efficient and recyclable photocatalysts for the removal of pharmaceutical contaminants from water resources. 2.Experimental 2.1 Chemical materials and instruments Commercially available materials and reagents were obtained from Merck and Sigma Aldrich and used directly without additional purification. Characterization techniques included X-ray diffraction (XRD) using a Panalytical X'Pert Pro Holland diffractometer, Fourier transform infrared (FT-IR) spectroscopy on a Shimadzu model 8700 spectrometer, field emission scanning electron microscopy (FESEM) imaging with a Mira 3-XMU microscope, and UV-vis diffuse reflectance spectroscopy using a Photonix AR spectrometer. 2.2. Synthesis of Ag/ CuS@Fe 3 O 4 photocatalyst 3 mmol of CuCl2 was dissolved in 25 mL of deionized water. 1 gram of magnetite powder was then added to the solution and stirred for 90 minutes. In a separate beaker, 8 mmol of sodium sulfite was dissolved in 10 mL of deionized water and subsequently added to the CuCl2/magnetite mixture. The mixture was stirred for 1 hour. The resulting CuS@Fe3O4 nanoparticles were separated, washed thoroughly with deionized water, dried in an oven at 60°C for 24 hours, and finally calcined in a furnace at 550°C for 2 hours. For the preparation of the Ag/CuS@Fe3O4 photocatalyst, 1 mmol of AgNO3 was dissolved in 25 mL of deionized water. 0.3 grams of the prepared CuS@Fe3O4 nanoparticles were added to this solution and stirred for 90 minutes. Then, 3 mmol of NaOH was dissolved in 5 mL of water and added to the mixture with further stirring for 15 minutes. The Ag/CuS@Fe3O4 nanoparticles were then separated, washed thoroughly with deionized water, and dried in an oven for 24 hours. 2.3 Evaluation of Photocatalytic Activity To assess the photocatalytic performance of the synthesized nanomaterials, a degradation experiment of tetracycline (TC) under visible light illumination was conducted. First, 0.01 grams of the nanocomposite was dispersed in 40 mL of a 50 ppm TC solution. The mixture was then stirred for 15 minutes to allow for adsorption-desorption equilibrium to be reached. Following this, the solution was exposed to visible light irradiation using a 60W low consumption fluorescent lamp. At various time intervals, samples were withdrawn from the solution and centrifuged to separate the photocatalyst. The supernatant was then analyzed using a UV-Vis spectrophotometer to measure the absorbance of tetracycline. The degradation efficiency was calculated using the following formula: Degradation %=(𝐴 0 −𝐴 𝑡/ 𝐴 0 )×100 Where A 0 ​ and A t ​ are the initial absorbance and absorbance of tetracycline at time 𝑡, respectively. 3. Results and discussions 3.1 Characterization 3.1.1 XRD and FESEM characterization X-ray diffraction (XRD) analysis was performed to investigate the crystallographic structure of the synthesized materials, including Fe 3 O 4 (magnetite) and Ag/CuS/Fe 3 O 4 nanocomposites. The XRD patterns of Fe 3 O 4 and the doped nanocomposites revealed distinct diffraction peaks, indicating the crystalline nature of the materials. The XRD pattern of pure Fe 3 O 4 exhibited characteristic peaks at 2θ values of around 30.1°, 35.5°, 43.1°, 53.4°, 57.0°, and 62.7°, corresponding to the (220), (311), (400), (422), (511), and (440) crystal planes of cubic-phase magnetite, respectively [ 45 ]. These peaks are consistent with the standard data for magnetite (JCPDS card no. 96-900-5839), confirming the formation of pure magnetite in the synthesized sample (Figs. 1 , 2 ). In contrast, the XRD patterns of the Ag/CuS/Fe 3 O 4 nanocomposites exhibited shifts and changes in the diffraction peaks compared to pure Fe 3 O 4 . These shifts and changes suggest alterations in the crystal structure due to the doping of Ag and CuS. The appearance of additional peaks or shifts in the XRD patterns of the doped nanocomposites indicates the formation of new phases or crystal structures. The presence of peaks corresponding to Ag (JCPDS card no. 96-901-1609) and CuS (JCPDS card no. 96-153-6219) in the doped nanocomposites confirms the successful incorporation of Ag and CuS into the magnetite matrix. The shifts in diffraction peaks suggest changes in lattice parameters and crystal symmetry due to the doping. Furthermore, the broadening of peaks in the XRD patterns of the nanocomposites compared to pure Fe 3 O 4 indicates a reduction in crystallite size or the presence of smaller crystallites. This reduction in crystallite size may be attributed to the incorporation of Ag and CuS, which can affect the nucleation and growth of magnetite nanoparticles. Overall, the XRD analysis confirms the successful synthesis of pure magnetite and the doped Ag/CuS/Fe 3 O 4 nanocomposites, providing valuable insights into their crystallographic structures and phases (Figs. 1 , 2 ). The observed differences in XRD patterns between Fe 3 O 4 and Ag/CuS/Fe 3 O 4 nanocomposites can be attributed to several factors. Firstly, the doping of Ag and CuS into the Fe 3 O 4 lattice may lead to lattice distortion or strain, resulting in shifts and broadening of diffraction peaks. Additionally, the presence of Ag and CuS phases contributes to the appearance of new peaks corresponding to these materials. The presence of different phases in the nanocomposites suggests the formation of heterostructures, where Ag and CuS nanoparticles are dispersed on the surface or embedded within the Fe 3 O 4 matrix. These heterostructures could enhance the photocatalytic properties of the nanocomposites by facilitating charge separation and promoting the generation of reactive oxygen species under visible light irradiation. The shifts in diffraction peaks may also indicate changes in the crystalline structure of Fe 3 O 4 induced by doping. For example, the incorporation of Ag and CuS may lead to the formation of solid solutions or the introduction of defects in the Fe 3 O 4 lattice, affecting its crystallographic parameters. Furthermore, the presence of impurities or secondary phases in the doped nanocomposites could influence their properties. These impurities may arise from incomplete doping reactions or the presence of residual reactants. Careful analysis of the XRD patterns allows for the identification and quantification of these impurities, providing insights into the purity and composition of the synthesized materials. Overall, XRD analysis provides valuable information about the structural characteristics of Fe 3 O 4 and Ag/CuS/Fe 3 O 4 nanocomposites, shedding light on their crystallographic phases, crystallite sizes, and structural changes induced by doping. This understanding is crucial for tailoring the properties of these materials for various applications, particularly in photocatalysis and environmental remediation. Field Emission Scanning Electron Microscopy (FESEM) was employed to investigate the surface morphology and microstructure of magnetite (Fe 3 O 4 ) and Ag@CuS/Fe 3 O 4 nanocomposites(Fig. 3 ). The FESEM images of pure magnetite revealed distinct spherical particles with a relatively uniform size distribution. The surface of magnetite appeared smooth, and the particles were densely packed, indicating a well-aggregated structure. In contrast, the FESEM images of Ag@CuS/Fe 3 O 4 nanocomposites exhibited a significant change in morphology compared to pure magnetite. The presence of Ag@CuS nanoparticles on the surface of Fe 3 O 4 was evident from the images. The Ag@CuS nanoparticles appeared as small, irregularly shaped clusters dispersed uniformly on the surface of Fe 3 O 4 . This suggests successful deposition of Ag@CuS onto the magnetite surface. Furthermore, the formation of Ag@CuS nanoparticles seemed to enhance the surface roughness of the nanocomposites compared to pure magnetite. Overall, the FESEM analysis confirmed the successful synthesis of Ag@CuS/Fe 3 O 4 nanocomposites and provided valuable insights into their surface morphology, which is crucial for understanding their photocatalytic properties and applications in environmental remediation. The Energy Dispersive X-ray (EDX) analysis was conducted to determine the elemental composition of Fe 3 O 4 and Ag/CuS/Fe 3 O 4 nanocomposites(Fig. 4 ). The results are presented below: For Fe 3 O 4 :Oxygen (O): The dominant presence of oxygen is confirmed, with a weight percent (W%) of approximately 59.19%. Iron (Fe): Iron is present in the sample, constituting about 40.81% of the composition. Other Elements: No other significant elements were detected, indicating a composition primarily consisting of Fe 3 O 4 . For Ag/CuS/Fe 3 O 4 : Oxygen (O): The presence of oxygen is confirmed, although slightly lower than in pure Fe 3 O 4 , with a weight percent of approximately 64.21%. Sulfur (S): Sulfur is detected, indicating the incorporation of CuS into the nanocomposite, with a weight percent of about 1.45%. Iron (Fe): Iron is still present in the nanocomposite, although in a lower proportion compared to Fe 3 O 4 alone, constituting about 33.97% of the composition. Copper (Cu): The presence of copper suggests the incorporation of CuS into the nanocomposite, with a weight percent of approximately 0.29%. Silver (Ag): Silver is detected, indicating successful doping into the nanocomposite, with a weight percent of about 0.09%. The EDX analysis confirms the presence of oxygen, sulfur, iron, copper, and silver in the Ag/CuS/Fe 3 O 4 nanocomposite, suggesting successful doping and incorporation of these elements into the Fe 3 O 4 matrix. The slight differences in elemental composition between Fe 3 O 4 and the nanocomposite indicate changes in the chemical composition due to doping and incorporation of additional elements. 3.1.2 UV-Vis analysis The UV-Vis spectra provide valuable insights into the optical properties and bandgap energy of nanocomposites(Fig. 5 ). In the case of Fe 3 O 4 , a characteristic peak was observed at 580 nm, corresponding to its absorption of visible light. Upon the incorporation of CuS into Fe 3 O 4 to form CuS/ Fe 3 O 4 nanocomposites, a redshift in the UV-Vis spectrum was observed, with the peak shifting to 610 nm. This redshift indicates a widening of the bandgap energy and enhanced absorption of visible light. The redshift can be attributed to the presence of CuS, which has a lower bandgap energy compared to Fe 3 O 4 . The introduction of CuS nanoparticles alters the electronic structure of the nanocomposite, leading to improved light absorption and thus enhanced photocatalytic activity. Similarly, in the Ag@CuS/ Fe 3 O 4 nanocomposites, a further redshift in the UV-Vis spectrum was observed, with the peak shifting even more towards longer wavelengths. This indicates a further widening of the bandgap energy and enhanced light absorption compared to CuS/Fe 3 O 4 nanocomposites. The incorporation of silver (Ag) into the CuS/Fe 3 O 4 nanocomposites likely contributes to this redshift, as Ag nanoparticles can efficiently trap and transfer photogenerated charge carriers, leading to increased photocatalytic efficiency. Overall, the UV-Vis spectra of the nanocomposites reveal the modification of their optical properties, with the redshift indicating enhanced light absorption and improved photocatalytic activity. These results are crucial for understanding the mechanisms underlying the photocatalytic performance of the nanocomposites and for optimizing their synthesis for various environmental remediation applications. 3.1.3 FTIR analysis FTIR spectra of the Fe 3 O 4 and Ag@CuS doped magnetite is shown in Fig. 6 . The infrared (IR) spectra of Fe 3 O 4 and Ag@CuS doped magnetite (Ag/CuS@Fe 3 O 4 ) provide valuable information about their chemical composition and structural properties. In the spectral range of 400 to 1000 cm − 1 , Fe 3 O 4 exhibits multiple peaks, likely due to the presence of impurities such as SiO 2 and alumina in the mineral [ 46 – 47 ]. These peaks indicate the presence of different chemical bonds and vibrational modes associated with these impurities. In contrast, Ag/CuS doped magnetite shows fewer peaks in this range, suggesting a simpler chemical composition with fewer impurities. At 1000 cm − 1 , Ag/CuS doped magnetite displays a strong peak, indicating the presence of specific chemical bonds associated with the doping process [ 48 – 49 ]. This peak is more intense compared to Fe 3 O 4 , suggesting a higher concentration of these bonds in the doped material. In the range of 1376 to 1478 cm-1, Fe 3 O 4 exhibits a strong peak, likely related to the presence of Fe-O bonds in the magnetite structure [ 50 ]. However, in the doped material, this peak appears with lower intensity at 1427 and 1632 cm-1, indicating alterations in the bonding environment due to the doping of Ag/CuS [ 51 ]. Moreover, in Fe3O4, a broad peak is observed at 3165 cm-1, indicating the presence of O-H stretching vibrations, possibly due to surface hydroxyl groups or absorbed water molecules [ 52 ]. In contrast, the doped material shows a lower and narrower peak at 3437 cm-1, suggesting a decrease in the abundance of hydroxyl groups or water molecules on the surface [ 53 ]. Overall, these results suggest that the doping of Ag/CuS into magnetite leads to structural and chemical modifications, altering the vibrational modes and intensities observed in the IR spectra. These changes may be attributed to the incorporation of Ag/CuS nanoparticles into the magnetite structure, which influences the chemical bonding and surface properties of the material. 3.2 Evaluation of photocatalytic activity of CuS/Fe 3 O4 and Ag/CuS/Fe3O4 photocatalyst The synthesized Ag/CuS/Fe 3 O 4 nanocomposite exhibited significantly enhanced photocatalytic performance compared to pure Fe 3 O 4 and CuS/Fe 3 O 4 . The discussion focuses on the observed differences in photocatalytic activity and the factors contributing to these outcomes. In the photocatalytic degradation of tetracycline (TC), Ag/CuS/Fe 3 O 4 demonstrated remarkable efficiency, achieving complete degradation of 20 ppm TC within just 30 minutes of visible light irradiation. In contrast, pure Fe 3 O 4 exhibited a much lower degradation efficiency, with only 21% TC degradation under the same conditions. CuS/Fe 3 O 4 , while showing improved performance compared to Fe 3 O 4 , achieved a TC degradation efficiency of 27% within 30 minutes. The superior photocatalytic activity of Ag/CuS/Fe 3 O 4 can be attributed to several factors. Firstly, the incorporation of silver (Ag) and copper sulfide (CuS) onto the Fe 3 O 4 surface increases the availability of active sites for photocatalytic reactions. Ag acts as a co-catalyst, enhancing the separation of photogenerated electron-hole pairs and improving charge carrier mobility [ 54 – 55 ]. Similarly, CuS functions as a sensitizer, extending the absorption range of the photocatalyst into the visible region and enhancing light utilization efficiency [ 56 – 57 ]. Furthermore, the presence of Ag and CuS modifies the band structure of Fe 3 O 4 , leading to a reduction in the band gap energy and an increase in the absorption of visible light [ 58 – 59 ]. This modification facilitates the generation of more reactive oxygen species (ROS) and promotes the photocatalytic degradation of organic pollutants [ 60 – 61 ]. The synergistic effect between Ag, CuS, and Fe 3 O 4 is also crucial in enhancing photocatalytic performance. The combination of these materials creates a heterojunction structure, which facilitates efficient charge transfer and inhibits charge carrier recombination [ 62 – 63 ]. The unique electronic and optical properties of Ag/CuS/Fe 3 O 4 nanocomposites contribute to the improved photocatalytic activity observed in this study. 3.2.1 Effect of Catalyst Dose The effect of catalyst dose on the photocatalytic degradation of tetracycline (TC) was investigated by varying the amount of Ag/CuS/Fe 3 O 4 nanocomposite from 0.002 g to 0.02 g while keeping the TC concentration constant at 20 ppm. The results revealed a clear correlation between the catalyst dose and the photocatalytic efficiency. At the lowest catalyst dose of 0.002 g, approximately 60% of TC was degraded after 30 minutes of visible light irradiation [ 64 ]. Increasing the catalyst dose to 0.005 g resulted in a slight improvement in the degradation efficiency, with around 60–70% degradation observed [ 65 ]. Further increasing the catalyst dose to 0.007 g significantly enhanced the photocatalytic activity, achieving approximately 84% degradation of TC within the same time frame [ 66 ]. Interestingly, a dose of 0.02 g of Ag/CuS/Fe 3 O 4 nanocomposite led to the highest photocatalytic efficiency, with approximately 90% degradation of TC achieved in just 30 minutes [ 67 ]. This indicates that the photocatalytic performance is highly dependent on the amount of catalyst present in the reaction system.The observed trend suggests that an optimal catalyst dose is crucial for achieving maximum photocatalytic activity. At lower doses, insufficient active sites may limit the degradation rate, resulting in lower efficiency. On the other hand, excessively high doses may lead to aggregation of catalyst particles, reducing the available surface area for photocatalytic reactions.The enhanced photocatalytic activity at higher catalyst doses can be attributed to the increased number of active sites available for TC adsorption and photocatalytic reactions. Moreover, higher catalyst doses may also promote more efficient light absorption and utilization, leading to improved charge carrier generation and separation(Fig. 7 ). These findings emphasize the importance of optimizing the catalyst dose to maximize photocatalytic performance and underscore the potential of Ag/CuS/Fe 3 O 4 nanocomposites for environmental remediation applications. 3.2.2 Effect of Tetracycline Concentration The effect of tetracycline (TC) concentration on the photodegradation efficiency using Ag/CuS/Fe 3 O 4 nanocomposites was investigated. The concentration of TC varied from 25 ppm to 100 ppm(Fig. 8 ). At lower concentrations (25 ppm, 30 ppm, and 40 ppm), the photodegradation efficiency exhibited an increasing trend. Specifically, at 25 ppm, 30 ppm, and 40 ppm, the degradation efficiencies were 94%, 96%, and 97%, respectively. This suggests that lower concentrations of TC lead to more efficient photodegradation, possibly due to better accessibility of the photocatalytic sites on the nanocomposites. However, as the TC concentration increased to 50 ppm, 60 ppm, 80 ppm, and 100 ppm, the photodegradation efficiency relatively decreased. At 50 ppm, 60 ppm, 80 ppm, and 100 ppm, the degradation efficiencies were 97%, 98%, 81%, and 78%, respectively. This decrease in efficiency with higher TC concentrations could be attributed to factors such as increased competition for active sites on the nanocomposites, saturation of the photocatalytic surface, and reduced light penetration due to higher turbidity caused by increased TC concentration. Overall, the photodegradation efficiency of TC using Ag/CuS/Fe 3 O 4 nanocomposites is influenced by the initial concentration of TC, with lower concentrations demonstrating higher efficiencies, while higher concentrations exhibit a diminishing trend in efficiency. 3.2.3 Effect of pH solution The effect of pH on the photocatalytic activity of Ag/CuS/Fe 3 O 4 nanocomposites was systematically investigated to understand its impact on the degradation of tetracycline (Fig. 9 ). The results revealed a significant dependence of photocatalytic performance on pH levels. At pH 2, the photoactivity was observed to be relatively low, achieving only about 20% degradation of tetracycline. This decrease in activity at acidic pH can be attributed to several factors, including reduced adsorption of tetracycline molecules and hindered generation of reactive oxygen species (ROS) due to the protonation of surface hydroxyl groups. However, as the pH increased to 4, 6, 7, 11, and 12, a substantial enhancement in photocatalytic activity was observed. In these alkaline conditions, the photoactivity exceeded 90%, indicating a remarkable improvement in tetracycline degradation efficiency. The higher activity at alkaline pH can be attributed to the increased adsorption of tetracycline molecules and facilitated generation of ROS, both of which are crucial for the photocatalytic degradation process. The isoelectric pH of the photocatalyst was found to be 8.7, further confirming the pH-dependent behavior observed in the photocatalytic activity. Overall, the results emphasize the importance of pH in controlling the photocatalytic performance of Ag/CuS/Fe 3 O 4 nanocomposites, with alkaline conditions being particularly favorable for efficient tetracycline degradation. 3.4 Isoelectric pH Determination The isoelectric point (pH iep ) of the photocatalyst was determined using a sodium chloride (NaCl) solution with varying pH values. The pH iep is a crucial parameter that indicates the pH at which the surface charge of the photocatalyst is neutral[ 70 – 71 ]. In this experiment, NaCl solutions with pH values ranging from acidic to alkaline were prepared and used to suspend the photocatalyst. The suspensions were then stirred for 24h to ensure equilibrium. Subsequently, the pH of the photocatalyst particles was measured. The results revealed that the pH iep of the photocatalyst was determined to be 8.7 (Fig. 10 ). This indicates that at a pH of 8.7, the surface charge of the photocatalyst becomes neutral, and the material exhibits minimum electrostatic repulsion between particles. The isoelectric pH is an essential parameter as it affects the surface chemistry and colloidal stability of the photocatalyst. Understanding the pH iep allows for the optimization of photocatalytic processes, as it influences the adsorption of reactants and intermediates onto the photocatalyst surface. By knowing the pH iep , appropriate pH conditions can be chosen to enhance the photocatalytic activity and stability of the material. Additionally, the pH iep value provides valuable insights into the surface properties of the photocatalyst, which are crucial for various applications, including pollutant degradation and water treatment. The determination of the isoelectric pH of the photocatalyst provides fundamental information that can be utilized to optimize its performance and enhance its effectiveness in environmental remediation processes. 3.5 Kinetic Study The photocatalytic degradation of tetracycline (TC) using Ag/CuS/Fe3O4 nanocomposites was investigated to understand the reaction kinetics. The study involved varying the dosage of the catalyst from 0.002 g to 0.02 g and analyzing the degradation kinetics. The degradation rate of TC was calculated using the following equation: ln (𝐶 0/ 𝐶 𝑡 )=𝑘𝑡 Where: C₀ is the initial concentration of TC (ppm) Cₜ is the concentration of TC at time t (ppm) k is the rate constant (L/min or cm³/min) t is the reaction time (min) By measuring the TC concentration at different time intervals throughout the experiment, the rate constant (k) can be determined using this equation. The rate constant reflects the efficiency of the photocatalyst in degrading TC. From the kinetic analysis, it was observed that increasing the dosage of the catalyst led to higher degradation rates of TC. The rate constant 𝑘 ranged from 0.026 min −1 to 0.2 min −1 for catalyst dosages ranging from 0.002 g to 0.02 g (Fig. 11 ). Specifically, at a catalyst dosage of 0.002 g, the rate constant was 0.026 min −1 , whereas at a dosage of 0.02 g, the rate constant increased to 0.2 min −1 . This result indicates that higher catalyst dosages promote faster degradation kinetics due to increased active sites available for the adsorption of TC molecules and subsequent generation of reactive species. The first-order kinetic behavior suggests that the degradation rate is directly proportional to the concentration of TC remaining in the solution. Furthermore, the observed first-order kinetics imply that the photocatalytic degradation of TC by Ag/CuS/Fe 3 O 4 nanocomposites is primarily controlled by the availability of active sites on the catalyst surface. As the dosage of the catalyst increases, the number of active sites also increases, leading to enhanced degradation rates. Overall, the kinetic study demonstrates that the Ag/CuS/Fe 3 O 4 nanocomposites exhibit efficient photocatalytic degradation of TC, and the process follows a first-order kinetic model across different catalyst dosages [ 72 ]. 3.6 Mechanism of Photodegradation The photocatalytic degradation of tetracycline (TC) using Ag/CuS/Fe3O4 nanocomposites involves a complex series of reactions driven by the generation of reactive oxygen species (ROS) upon exposure to visible light [ 73 ]. The mechanism can be described as follows: 1. Adsorption: Initially, tetracycline molecules adsorb onto the surface of the Ag/CuS/Fe3O4 nanocomposites due to electrostatic interactions and hydrogen bonding between the TC molecules and the catalyst surface. 2. Generation of Reactive Species: Under visible light irradiation, the Ag/CuS/Fe 3 O 4 nanocomposites absorb photons, leading to the excitation of electrons from the valence band to the conduction band. This excitation creates electron-hole pairs (𝑒− -h+). 3. ROS Generation: The photogenerated electrons (𝑒 − ) react with molecular oxygen (𝑂 2 ) adsorbed on the catalyst surface, leading to the formation of superoxide radicals (O 2 • − ). Similarly, the photogenerated holes (h + ) react with water molecules (𝐻 2 𝑂) to form hydroxyl radicals (OH•). These ROS are highly reactive and play a crucial role in the degradation of TC. 4. TC Degradation: The ROS, including superoxide radicals and hydroxyl radicals, attack the adsorbed TC molecules, leading to the degradation of TC into smaller, less complex organic molecules, and eventually into harmless byproducts such as carbon dioxide and water. 5. Effect of Scavengers: The presence of scavengers such as hydrogen peroxide (H2O2), ethylenediaminetetraacetic acid (EDTA), ethanol (EtOH), and potassium chloride (KCl) significantly affects the photocatalytic degradation process(Fig. 12 ). In the initial stages of photodegradation, scavengers compete with tetracycline (TC) molecules for the reactive oxygen species (ROS). Hydrogen peroxide (H2O2), as a strong oxidizing agent, readily scavenges ROS, leading to a decrease in their concentration. EDTA, a strong chelating agent, also competes with TC for ROS, effectively reducing their availability for TC degradation. Ethanol (EtOH) acts as a sacrificial agent by absorbing photons and generating hydroxyl radicals (••OH), thus scavenging ROS. Potassium chloride (KCl) likely acts as an electron scavenger, intercepting electrons and reducing the formation of ROS. During the early stages of the reaction, the scavengers' competition with TC for ROS leads to a decrease in photodegradation efficiency compared to the control (without scavenger). This decrease is most pronounced for H2O2 and EDTA due to their strong scavenging abilities. However, as the reaction progresses, the scavengers begin to saturate, and their scavenging capacities diminish. At this point, the differences in photodegradation efficiency between the scavenger-containing samples and the control diminish. Eventually, in the later stages of photodegradation, all scavengers and the control without scavenger exhibit similar high photodegradation efficiencies, typically around 90%. This behavior suggests that while scavengers initially hinder the degradation process by competing with TC for ROS, their effect diminishes over time, allowing the photocatalyst to efficiently degrade TC regardless of the scavenger present. 6. Later Stage Degradation: However, as the reaction progresses, the concentration of ROS decreases, and the availability of active sites on the catalyst surface becomes limiting. At this point, the presence of scavengers has a minimal effect on the degradation efficiency. Therefore, in the later stages of photodegradation, the photodegradation efficiency of the scavenger-containing solutions approaches that of the control (without scavenger). 7. Overall Efficiency: Despite the presence of scavengers, the overall photodegradation efficiency remains high (around 90%), indicating the robustness of the Ag/CuS/Fe 3 O 4 nanocomposites in degrading TC under visible light irradiation. This mechanism highlights the importance of ROS generation and scavenger effects in the photocatalytic degradation of tetracycline using Ag/CuS/Fe 3 O 4 nanocomposites. 3.7 Application of Ag/CuS/Fe 3 O 4 nanocomposites in photodegradation of diclofenac The photocatalyst demonstrated high efficiency in the degradation of diclofenac (Dic) when tested alone, achieving an impressive degradation rate of 84% (Fig. 13 .A). This indicates the excellent photocatalytic activity of the material in degrading this particular pharmaceutical compound under visible light illumination. Furthermore, in a simultaneous photodegradation experiment involving both diclofenac (Dic) and tetracycline (TC), the photocatalyst exhibited remarkable performance. The degradation of tetracycline (TC) reached an impressive efficiency of 95%, indicating the photocatalyst's strong capability to degrade this antibiotic compound. Moreover, despite the simultaneous degradation of both diclofenac (Dic) and tetracycline (TC), the photocatalyst also demonstrated substantial efficacy in degrading diclofenac (Dic), achieving a degradation efficiency of 50%. This highlights the versatility of the photocatalyst in simultaneously degrading multiple organic pollutants, even when present in complex mixtures (Fig. 13 .B). Overall, the results underscore the potential of the photocatalyst for efficient photodegradation of pharmaceutical compounds, both individually and in complex mixtures, contributing to the mitigation of organic pollutant contamination in water bodies. The efficiency of the photocatalyst for the photodegradation of diclofenac alone was found to be 84%. Diclofenac, a commonly used nonsteroidal anti-inflammatory drug, is known for its persistence in the environment and potential ecological risks. However, when the photocatalyst was used for the simultaneous photodegradation of both diclofenac and tetracycline (TC), the results showed remarkable performance. The degradation efficiency for tetracycline was as high as 95%, indicating the excellent ability of the photocatalyst to break down this antibiotic compound efficiently. Interestingly, despite the simultaneous degradation of both diclofenac and tetracycline, the efficiency for diclofenac was slightly lower, achieving a degradation rate of 50%. This suggests that while the photocatalyst is effective in degrading diclofenac, the presence of tetracycline may have a slight inhibitory effect on its degradation efficiency for diclofenac. Overall, the simultaneous photodegradation of diclofenac and tetracycline demonstrates the potential of the photocatalyst for the efficient removal of these emerging contaminants from water sources. Further optimization of the photocatalytic process may enhance the degradation efficiency for diclofenac and other pharmaceutical compounds, contributing to the development of advanced water treatment technologies. 4. Conclusion This study demonstrates the effective utilization of Ag/CuS/Fe 3 O 4 nanocomposites as photocatalysts for the degradation of organic pollutants, particularly tetracycline (TC) and diclofenac. The synthesized nanocomposites exhibited superior photocatalytic activity, outperforming pristine Fe 3 O 4 and CuS/Fe 3 O 4 counterparts. The enhanced performance of Ag/CuS/Fe 3 O 4 nanocomposites can be attributed to the synergistic effects of Ag and CuS, which improve the charge carrier separation and extend the light absorption range, leading to increased photocatalytic efficiency. The presence of Ag also contributes to lowering the bandgap energy, making the nanocomposites more active under visible light. EDX analysis confirmed the successful doping of Ag and CuS into the Fe 3 O 4 lattice, which was further supported by XRD analysis showing distinct diffraction peaks corresponding to the different phases. FESEM images revealed the morphological characteristics of the nanocomposites, indicating the formation of well-defined structures with enhanced surface areas. UV-Vis and FTIR spectroscopy provided insights into the optical and chemical properties of the nanocomposites, highlighting the shifts in absorption peaks and the presence of functional groups associated with photocatalytic activity. The photocatalytic activity of Ag/CuS/Fe 3 O 4 nanocomposites was evaluated through the degradation of tetracycline under visible light irradiation. The nanocomposites exhibited excellent performance, achieving a degradation efficiency of 100% within 30 minutes, compared to lower efficiencies observed for Fe 3 O 4 and CuS/Fe 3 O 4 . Furthermore, the effect of catalyst dosage, pH, and scavengers on the photocatalytic activity was investigated. The results showed that higher catalyst dosages and alkaline pH conditions significantly enhanced the degradation efficiency, while scavengers initially reduced the efficiency but had minimal impact in the later stages of the reaction. Additionally, the simultaneous photodegradation of diclofenac and tetracycline revealed the versatility of Ag/CuS/Fe 3 O 4 nanocomposites in treating multiple pollutants, with promising degradation efficiencies observed for both compounds. In conclusion, Ag/CuS/Fe 3 O 4 nanocomposites show great potential for environmental remediation applications, particularly in the treatment of wastewater contaminated with organic pollutants. Further studies could focus on optimizing the synthesis parameters and exploring the recyclability and long-term stability of the nanocomposites for practical applications. 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Cite Share Download PDF Status: Published Journal Publication published 16 Aug, 2024 Read the published version in Scientific Reports → Version 1 posted Editorial decision: Revision requested 10 Jul, 2024 Reviews received at journal 09 Jul, 2024 Reviews received at journal 04 Jul, 2024 Reviewers agreed at journal 28 Jun, 2024 Reviewers agreed at journal 27 Jun, 2024 Reviewers invited by journal 27 Jun, 2024 Editor assigned by journal 27 Jun, 2024 Editor invited by journal 27 Jun, 2024 Submission checks completed at journal 27 Jun, 2024 First submitted to journal 26 Jun, 2024 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-4642539","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":325029998,"identity":"7ccc2a98-9e46-47cc-b5f2-56b8b9dbb155","order_by":0,"name":"Roya Mohammadzadeh 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20:33:44","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":1282147,"visible":true,"origin":"","legend":"\u003cp\u003eComparison of XRD patterns of magnetite and Ag/CuS/magnetite (CuFeAg) nanoparticles with reference standards\u003c/p\u003e","description":"","filename":"floatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/ee5a49ac90270896aa3950b7.png"},{"id":60713475,"identity":"0ff595e4-d4c6-4d26-a0e9-855b5a96dfdf","added_by":"auto","created_at":"2024-07-19 20:33:44","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":195464,"visible":true,"origin":"","legend":"\u003cp\u003eFESEM images of (A) CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and (B) Ag@CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites\u003c/p\u003e","description":"","filename":"floatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/99ca754d37724351d2b82fa6.png"},{"id":60713737,"identity":"94afb92d-910a-4719-88fc-03501975c69c","added_by":"auto","created_at":"2024-07-19 20:41:44","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":26542,"visible":true,"origin":"","legend":"\u003cp\u003eEDX analysis of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposite\u003c/p\u003e","description":"","filename":"floatimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/64bfbba7e3714ca7aa2216c3.png"},{"id":60713473,"identity":"688af47f-ebde-42cd-a477-4ce7cfa83840","added_by":"auto","created_at":"2024-07-19 20:33:44","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":17846,"visible":true,"origin":"","legend":"\u003cp\u003eUV-Vis spectra of the synthesized nanocomposites\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/b18e6506495b0e47f3e0250c.png"},{"id":60713477,"identity":"a7444c24-bbbc-44f1-aefc-fb8535200d2f","added_by":"auto","created_at":"2024-07-19 20:33:44","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":84408,"visible":true,"origin":"","legend":"\u003cp\u003eFTIR spectra of (A)Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and (B)Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposite\u003c/p\u003e","description":"","filename":"floatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/ab8ee79f3431a01c74404f43.png"},{"id":60713476,"identity":"952707ab-6a97-4e57-beec-4609a7110133","added_by":"auto","created_at":"2024-07-19 20:33:44","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":43144,"visible":true,"origin":"","legend":"\u003cp\u003eEffect of dose of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposite on TC photodegradation\u003c/p\u003e","description":"","filename":"floatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/6ca0c6978feb0354a0b78c16.png"},{"id":60713469,"identity":"b348e1b1-5c78-43d5-866b-c34f01c31848","added_by":"auto","created_at":"2024-07-19 20:33:43","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":41881,"visible":true,"origin":"","legend":"\u003cp\u003eEffect of TC concentration on photodegradation efficincy\u003c/p\u003e","description":"","filename":"floatimage8.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/64bdfd6d52423367c9f5f2e1.png"},{"id":60713472,"identity":"f49f6c7e-8146-49ed-86e7-fc21e1027395","added_by":"auto","created_at":"2024-07-19 20:33:44","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":38400,"visible":true,"origin":"","legend":"\u003cp\u003eEffect of pH solution on the photodegradation efficiency of TC\u003c/p\u003e","description":"","filename":"floatimage9.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/ed43c44ed34c1805acca9866.png"},{"id":60713480,"identity":"3bccd2f2-6490-4ab2-beb6-e246fb1dc874","added_by":"auto","created_at":"2024-07-19 20:33:45","extension":"png","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":10177,"visible":true,"origin":"","legend":"\u003cp\u003eIsoelectric pH determination\u003c/p\u003e","description":"","filename":"floatimage10.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/f3e866b619af69c5ac1840fd.png"},{"id":60713470,"identity":"957163ec-8af1-4fb2-b669-0c6f2bf3b7f5","added_by":"auto","created_at":"2024-07-19 20:33:44","extension":"png","order_by":11,"title":"Figure 11","display":"","copyAsset":false,"role":"figure","size":46706,"visible":true,"origin":"","legend":"\u003cp\u003eKinetic study of TC photodegradation with various doses of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites\u003c/p\u003e","description":"","filename":"floatimage11.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/dfcbf14538686756e0f1e101.png"},{"id":60713479,"identity":"3e25bef9-0ed8-4cd7-b8c1-7f3e9043fd26","added_by":"auto","created_at":"2024-07-19 20:33:45","extension":"png","order_by":12,"title":"Figure 12","display":"","copyAsset":false,"role":"figure","size":9451,"visible":true,"origin":"","legend":"\u003cp\u003eEffect of scavengers on the photocatalytic efficiency\u003c/p\u003e","description":"","filename":"floatimage12.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/0851a7d202338710bbbd7232.png"},{"id":60713478,"identity":"9d322c7c-5b9b-4615-927b-0c684b3e9535","added_by":"auto","created_at":"2024-07-19 20:33:45","extension":"png","order_by":13,"title":"Figure 13","display":"","copyAsset":false,"role":"figure","size":50417,"visible":true,"origin":"","legend":"\u003cp\u003ePhotodegradation of (A) Diclofenac and(B) binary mixture solution of Diclofenac-Tetracycline\u003c/p\u003e","description":"","filename":"floatimage13.png","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/5ccdc3c4181b86bb76f60360.png"},{"id":63070771,"identity":"dbc38b29-2067-4e92-a4f6-0453c5c1e420","added_by":"auto","created_at":"2024-08-22 19:53:58","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2700289,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-4642539/v1/5717bfb5-2978-4c3f-a652-2864dbf8d36e.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Synthesis of Ag@ CuS doped mineral magnetite nanocomposite with improved photocatalytic activity against tetracycline and diclofenac pollutants","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eThe quality of life has been adversely affected by the rapid urbanization and industrialization of modern society, leading to increased contamination of groundwater, air, and fossil fuels through conventional industrial waste disposal methods [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. Consequently, major environmental issues, such as pollution and climate change, have emerged as significant threats to ecosystems and human health [\u003cspan additionalcitationids=\"CR4 CR5 CR6 CR7\" citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. According to recent reports by the World Health Organization, environmental pollution has resulted in 3.7\u0026nbsp;million deaths in the twenty-first century alone, with 92% of the global population living in areas with severe air and water pollution [\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e, \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. As a result, the safe disposal of hazardous waste in both water and the atmosphere has become a critical national and international priority [\u003cspan additionalcitationids=\"CR12 CR13\" citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e]. Advanced Oxidation Processes (AOPs) have been extensively employed for the removal of organic contaminants from water and air, with heterogeneous photocatalysis being one of the most promising AOPs due to its ability to degrade organic pollutants [\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eSemiconductor-based photocatalysts, especially metal oxide-based ones, have garnered significant attention for their efficient and cost-effective applications in water pollution treatment and disinfection [\u003cspan additionalcitationids=\"CR18 CR19 CR20 CR21 CR22 CR23\" citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]. Titanium dioxide (TiO\u003csub\u003e2\u003c/sub\u003e) has been widely studied due to its low cost, non-toxicity, and chemical inertness, but its photocatalytic activity is mainly confined to UV light irradiation, limiting its effectiveness under visible light [\u003cspan additionalcitationids=\"CR26 CR27\" citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. Consequently, there is a pressing need to design and synthesize effective visible-light-driven photocatalysts [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. Various metal oxides, including La\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, CdO, CeO\u003csub\u003e2\u003c/sub\u003e, CaO, and ZnO, have been explored as promising co-catalysts to enhance the photocatalytic activity of TiO\u003csub\u003e2\u003c/sub\u003e [\u003cspan additionalcitationids=\"CR31\" citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eScientists are incorporating magnetic nanoparticles into photocatalysts. These nanoparticles, including hematite, maghemite, magnetite, and various ferrites, give the photocatalyst magnetic properties. This allows the photocatalyst to be easily separated from a solution using a magnet [\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e]. Adding these magnetic nanoparticles doesn't significantly affect the surface area or how the photocatalyst spreads in water because the photocatalyst remains a powder. Even better, some of these magnetic nanoparticles can absorb visible light and act as photocatalysts themselves, which can help break down pollutants even faster [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eOne of the most exciting frontiers in combating water pollution lies in the development of magnetic visible-light-active nanocomposites. These innovative materials are grabbing the attention of researchers due to their immense potential for photocatalytic environmental cleanup. This article delves into the applying these powerful tools for water treatment.\u003c/p\u003e \u003cp\u003eCovellite CuS is a fascinating material for photocatalysis due to its visible-light absorption. This p-type semiconductor with a narrow bandgap (1.2-2.0 eV) boasts several advantages: low cost, non-toxicity, easy production, and excellent stability. Its potential as a photocatalyst is further bolstered by broad visible light absorption, plasmon absorbance, and even near-infrared (NIR) absorption. Studies on CuS for organic dye degradation have shown promise.However, challenges remain. The photocatalytic efficiency of CuS is influenced by factors like morphology, size, and surface area. Additionally, bare CuS suffers from rapid recombination of photoexcited charges and low quantum yield. Furthermore, CuS nanoparticles tend to aggregate in water, hindering their effectiveness.Researchers are addressing these limitations by creating CuS-based nanoheterostructures. These structures can modify CuS properties, leading to enhanced charge separation, improved stability, and ultimately, better photocatalytic performance[\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. An example of this approach is the work by Sohrabnezhad et al., who embedded CuS nanospheres within an MCM-41 matrix [\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e]. This nanocomposite exhibited superior performance in degrading methylene blue under visible light, highlighting the potential of CuS-based materials for water treatment.\u003c/p\u003e \u003cp\u003eWith its unique properties and the promise of further improvement through nanoheterostructure design, CuS presents a compelling avenue for developing powerful photocatalysts for clean water applications.\u003c/p\u003e \u003cp\u003eSilver (Ag) doping has emerged as a promising strategy to enhance the photocatalytic activity of semiconductor photocatalysts. By incorporating Ag into the crystal lattice, it effectively lowers the recombination rate of holes and electron pairs, thereby improving the efficiency of photocatalysis [\u003cspan additionalcitationids=\"CR39\" citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e]. Moreover, Ag doping can modify the band gap energy of the semiconductor, making it more active under visible light [\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. This property of Ag-doped materials is particularly advantageous for wastewater treatment applications.\u003c/p\u003e \u003cp\u003eIntroducing Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e (magnetite) as a base material for the photocatalyst adds another dimension to its functionality. Magnetite is a naturally occurring iron oxide mineral with magnetic properties, making it an excellent candidate for various applications. In the context of photocatalysis, Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e serves as a stable and robust support material for semiconductor photocatalysts like CuS[\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe utilization of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e in CuS-based nanocomposites offers several advantages. Firstly, Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e provides a high surface area and facilitates the dispersion of CuS nanoparticles, thereby enhancing the accessibility of reactants to the catalytic sites. Additionally, Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e imparts magnetic properties to the nanocomposite, allowing for easy separation and recovery of the catalyst from the reaction mixture using an external magnetic field. This magnetic recyclability significantly reduces the operational costs and simplifies the catalyst retrieval process, making it more environmentally friendly.\u003c/p\u003e \u003cp\u003eFurthermore, Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e exhibits excellent stability and biocompatibility, making it suitable for applications in environmental remediation and biomedical fields. Its chemical inertness ensures that it does not interfere with the catalytic activity of CuS, while its biocompatibility is advantageous for potential biomedical applications, such as drug delivery systems.\u003c/p\u003e \u003cp\u003eCombining Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e with CuS and Ag to form ternary nanocomposites (CuS@Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e/Ag) not only enhances the photocatalytic performance but also provides multifunctionality. The synergistic effects between CuS, Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e, and Ag result in improved charge separation efficiency, extended light absorption range, and enhanced catalytic activity.\u003c/p\u003e \u003cp\u003eTherefore, the incorporation of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e as a base material in CuS-based photocatalysts holds significant promise for addressing environmental pollution and advancing various technological applications[\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. However, the introduction of silver doping into CuS@magnetite (CuS@Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e) nanocomposites presents a unique opportunity. The incorporation of Ag into the CuS@magnetite structure not only enhances the photocatalytic activity but also provides magnetic properties, enabling easy separation and recycling of the catalyst from the reaction medium. This dual functionality of CuS@Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e/Ag nanocomposites makes them highly desirable for environmental remediation applications [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eIn this study by incorporating Ag NPs and CuS into the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e matrix, we aim to enhance light absorption and charge separation, leading to improved photocatalytic performance. Additionally, the magnetic properties of the nanocomposite facilitate easy separation and recyclability, making it a promising candidate for practical applications in water treatment processes. Through this research, we contribute to the development of efficient and recyclable photocatalysts for the removal of pharmaceutical contaminants from water resources.\u003c/p\u003e"},{"header":"2.Experimental","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Chemical materials and instruments\u003c/h2\u003e \u003cp\u003eCommercially available materials and reagents were obtained from Merck and Sigma Aldrich and used directly without additional purification. Characterization techniques included X-ray diffraction (XRD) using a Panalytical X'Pert Pro Holland diffractometer, Fourier transform infrared (FT-IR) spectroscopy on a Shimadzu model 8700 spectrometer, field emission scanning electron microscopy (FESEM) imaging with a Mira 3-XMU microscope, and UV-vis diffuse reflectance spectroscopy using a Photonix AR spectrometer.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2. Synthesis of Ag/ CuS@Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e photocatalyst\u003c/h2\u003e \u003cp\u003e3 mmol of CuCl2 was dissolved in 25 mL of deionized water. 1 gram of magnetite powder was then added to the solution and stirred for 90 minutes. In a separate beaker, 8 mmol of sodium sulfite was dissolved in 10 mL of deionized water and subsequently added to the CuCl2/magnetite mixture. The mixture was stirred for 1 hour. The resulting CuS@Fe3O4 nanoparticles were separated, washed thoroughly with deionized water, dried in an oven at 60\u0026deg;C for 24 hours, and finally calcined in a furnace at 550\u0026deg;C for 2 hours.\u003c/p\u003e \u003cp\u003eFor the preparation of the Ag/CuS@Fe3O4 photocatalyst, 1 mmol of AgNO3 was dissolved in 25 mL of deionized water. 0.3 grams of the prepared CuS@Fe3O4 nanoparticles were added to this solution and stirred for 90 minutes. Then, 3 mmol of NaOH was dissolved in 5 mL of water and added to the mixture with further stirring for 15 minutes. The Ag/CuS@Fe3O4 nanoparticles were then separated, washed thoroughly with deionized water, and dried in an oven for 24 hours.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Evaluation of Photocatalytic Activity\u003c/h2\u003e \u003cp\u003eTo assess the photocatalytic performance of the synthesized nanomaterials, a degradation experiment of tetracycline (TC) under visible light illumination was conducted. First, 0.01 grams of the nanocomposite was dispersed in 40 mL of a 50 ppm TC solution. The mixture was then stirred for 15 minutes to allow for adsorption-desorption equilibrium to be reached. Following this, the solution was exposed to visible light irradiation using a 60W low consumption fluorescent lamp.\u003c/p\u003e \u003cp\u003eAt various time intervals, samples were withdrawn from the solution and centrifuged to separate the photocatalyst. The supernatant was then analyzed using a UV-Vis spectrophotometer to measure the absorbance of tetracycline. The degradation efficiency was calculated using the following formula:\u003c/p\u003e \u003cp\u003eDegradation %=(\u0026#119860;\u003csub\u003e0\u003c/sub\u003e\u0026minus;\u0026#119860;\u003csub\u003e\u0026#119905;/\u003c/sub\u003e\u0026#119860;\u003csub\u003e0\u003c/sub\u003e)\u0026times;100\u003c/p\u003e \u003cp\u003eWhere \u003cem\u003eA\u003c/em\u003e\u003csub\u003e0\u003c/sub\u003e​ and \u003cem\u003eA\u003c/em\u003e\u003csub\u003e\u003cem\u003et\u003c/em\u003e​\u003c/sub\u003e are the initial absorbance and absorbance of tetracycline at time \u0026#119905;, respectively.\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results and discussions","content":"\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e3.1 Characterization\u003c/h2\u003e \u003cdiv id=\"Sec8\" class=\"Section3\"\u003e \u003ch2\u003e3.1.1 XRD and FESEM characterization\u003c/h2\u003e \u003cp\u003eX-ray diffraction (XRD) analysis was performed to investigate the crystallographic structure of the synthesized materials, including Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e (magnetite) and Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites. The XRD patterns of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and the doped nanocomposites revealed distinct diffraction peaks, indicating the crystalline nature of the materials.\u003c/p\u003e \u003cp\u003eThe XRD pattern of pure Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e exhibited characteristic peaks at 2θ values of around 30.1\u0026deg;, 35.5\u0026deg;, 43.1\u0026deg;, 53.4\u0026deg;, 57.0\u0026deg;, and 62.7\u0026deg;, corresponding to the (220), (311), (400), (422), (511), and (440) crystal planes of cubic-phase magnetite, respectively [\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e]. These peaks are consistent with the standard data for magnetite (JCPDS card no. 96-900-5839), confirming the formation of pure magnetite in the synthesized sample (Figs.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e,\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eIn contrast, the XRD patterns of the Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites exhibited shifts and changes in the diffraction peaks compared to pure Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e. These shifts and changes suggest alterations in the crystal structure due to the doping of Ag and CuS. The appearance of additional peaks or shifts in the XRD patterns of the doped nanocomposites indicates the formation of new phases or crystal structures. The presence of peaks corresponding to Ag (JCPDS card no. 96-901-1609) and CuS (JCPDS card no. 96-153-6219) in the doped nanocomposites confirms the successful incorporation of Ag and CuS into the magnetite matrix. The shifts in diffraction peaks suggest changes in lattice parameters and crystal symmetry due to the doping. Furthermore, the broadening of peaks in the XRD patterns of the nanocomposites compared to pure Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e indicates a reduction in crystallite size or the presence of smaller crystallites. This reduction in crystallite size may be attributed to the incorporation of Ag and CuS, which can affect the nucleation and growth of magnetite nanoparticles. Overall, the XRD analysis confirms the successful synthesis of pure magnetite and the doped Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites, providing valuable insights into their crystallographic structures and phases (Figs.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e,\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThe observed differences in XRD patterns between Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites can be attributed to several factors. Firstly, the doping of Ag and CuS into the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e lattice may lead to lattice distortion or strain, resulting in shifts and broadening of diffraction peaks. Additionally, the presence of Ag and CuS phases contributes to the appearance of new peaks corresponding to these materials. The presence of different phases in the nanocomposites suggests the formation of heterostructures, where Ag and CuS nanoparticles are dispersed on the surface or embedded within the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e matrix. These heterostructures could enhance the photocatalytic properties of the nanocomposites by facilitating charge separation and promoting the generation of reactive oxygen species under visible light irradiation. The shifts in diffraction peaks may also indicate changes in the crystalline structure of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e induced by doping. For example, the incorporation of Ag and CuS may lead to the formation of solid solutions or the introduction of defects in the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e lattice, affecting its crystallographic parameters. Furthermore, the presence of impurities or secondary phases in the doped nanocomposites could influence their properties. These impurities may arise from incomplete doping reactions or the presence of residual reactants. Careful analysis of the XRD patterns allows for the identification and quantification of these impurities, providing insights into the purity and composition of the synthesized materials. Overall, XRD analysis provides valuable information about the structural characteristics of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites, shedding light on their crystallographic phases, crystallite sizes, and structural changes induced by doping. This understanding is crucial for tailoring the properties of these materials for various applications, particularly in photocatalysis and environmental remediation.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eField Emission Scanning Electron Microscopy (FESEM) was employed to investigate the surface morphology and microstructure of magnetite (Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e) and Ag@CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites(Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThe FESEM images of pure magnetite revealed distinct spherical particles with a relatively uniform size distribution. The surface of magnetite appeared smooth, and the particles were densely packed, indicating a well-aggregated structure.\u003c/p\u003e \u003cp\u003eIn contrast, the FESEM images of Ag@CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites exhibited a significant change in morphology compared to pure magnetite. The presence of Ag@CuS nanoparticles on the surface of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e was evident from the images. The Ag@CuS nanoparticles appeared as small, irregularly shaped clusters dispersed uniformly on the surface of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e. This suggests successful deposition of Ag@CuS onto the magnetite surface. Furthermore, the formation of Ag@CuS nanoparticles seemed to enhance the surface roughness of the nanocomposites compared to pure magnetite.\u003c/p\u003e \u003cp\u003eOverall, the FESEM analysis confirmed the successful synthesis of Ag@CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites and provided valuable insights into their surface morphology, which is crucial for understanding their photocatalytic properties and applications in environmental remediation.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe Energy Dispersive X-ray (EDX) analysis was conducted to determine the elemental composition of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites(Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e). The results are presented below:\u003c/p\u003e \u003cp\u003eFor Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e:Oxygen (O): The dominant presence of oxygen is confirmed, with a weight percent (W%) of approximately 59.19%. Iron (Fe): Iron is present in the sample, constituting about 40.81% of the composition. Other Elements: No other significant elements were detected, indicating a composition primarily consisting of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e. For Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e: Oxygen (O): The presence of oxygen is confirmed, although slightly lower than in pure Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e, with a weight percent of approximately 64.21%. Sulfur (S): Sulfur is detected, indicating the incorporation of CuS into the nanocomposite, with a weight percent of about 1.45%. Iron (Fe): Iron is still present in the nanocomposite, although in a lower proportion compared to Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e alone, constituting about 33.97% of the composition. Copper (Cu): The presence of copper suggests the incorporation of CuS into the nanocomposite, with a weight percent of approximately 0.29%. Silver (Ag): Silver is detected, indicating successful doping into the nanocomposite, with a weight percent of about 0.09%. The EDX analysis confirms the presence of oxygen, sulfur, iron, copper, and silver in the Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposite, suggesting successful doping and incorporation of these elements into the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e matrix. The slight differences in elemental composition between Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and the nanocomposite indicate changes in the chemical composition due to doping and incorporation of additional elements.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec9\" class=\"Section3\"\u003e \u003ch2\u003e3.1.2 UV-Vis analysis\u003c/h2\u003e \u003cp\u003eThe UV-Vis spectra provide valuable insights into the optical properties and bandgap energy of nanocomposites(Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e). In the case of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e, a characteristic peak was observed at 580 nm, corresponding to its absorption of visible light.\u003c/p\u003e \u003cp\u003eUpon the incorporation of CuS into Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e to form CuS/ Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites, a redshift in the UV-Vis spectrum was observed, with the peak shifting to 610 nm. This redshift indicates a widening of the bandgap energy and enhanced absorption of visible light. The redshift can be attributed to the presence of CuS, which has a lower bandgap energy compared to Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e. The introduction of CuS nanoparticles alters the electronic structure of the nanocomposite, leading to improved light absorption and thus enhanced photocatalytic activity.\u003c/p\u003e \u003cp\u003eSimilarly, in the Ag@CuS/ Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites, a further redshift in the UV-Vis spectrum was observed, with the peak shifting even more towards longer wavelengths. This indicates a further widening of the bandgap energy and enhanced light absorption compared to CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites. The incorporation of silver (Ag) into the CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites likely contributes to this redshift, as Ag nanoparticles can efficiently trap and transfer photogenerated charge carriers, leading to increased photocatalytic efficiency.\u003c/p\u003e \u003cp\u003eOverall, the UV-Vis spectra of the nanocomposites reveal the modification of their optical properties, with the redshift indicating enhanced light absorption and improved photocatalytic activity. These results are crucial for understanding the mechanisms underlying the photocatalytic performance of the nanocomposites and for optimizing their synthesis for various environmental remediation applications.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec10\" class=\"Section3\"\u003e \u003ch2\u003e3.1.3 FTIR analysis\u003c/h2\u003e \u003cp\u003eFTIR spectra of the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and Ag@CuS doped magnetite is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e. The infrared (IR) spectra of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and Ag@CuS doped magnetite (Ag/CuS@Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e) provide valuable information about their chemical composition and structural properties.\u003c/p\u003e \u003cp\u003eIn the spectral range of 400 to 1000 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e exhibits multiple peaks, likely due to the presence of impurities such as SiO\u003csub\u003e2\u003c/sub\u003e and alumina in the mineral [\u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e]. These peaks indicate the presence of different chemical bonds and vibrational modes associated with these impurities. In contrast, Ag/CuS doped magnetite shows fewer peaks in this range, suggesting a simpler chemical composition with fewer impurities.\u003c/p\u003e \u003cp\u003eAt 1000 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, Ag/CuS doped magnetite displays a strong peak, indicating the presence of specific chemical bonds associated with the doping process [\u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e]. This peak is more intense compared to Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e, suggesting a higher concentration of these bonds in the doped material.\u003c/p\u003e \u003cp\u003eIn the range of 1376 to 1478 cm-1, Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e exhibits a strong peak, likely related to the presence of Fe-O bonds in the magnetite structure [\u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e50\u003c/span\u003e]. However, in the doped material, this peak appears with lower intensity at 1427 and 1632 cm-1, indicating alterations in the bonding environment due to the doping of Ag/CuS [\u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e51\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eMoreover, in Fe3O4, a broad peak is observed at 3165 cm-1, indicating the presence of O-H stretching vibrations, possibly due to surface hydroxyl groups or absorbed water molecules [\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e52\u003c/span\u003e]. In contrast, the doped material shows a lower and narrower peak at 3437 cm-1, suggesting a decrease in the abundance of hydroxyl groups or water molecules on the surface [\u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e53\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eOverall, these results suggest that the doping of Ag/CuS into magnetite leads to structural and chemical modifications, altering the vibrational modes and intensities observed in the IR spectra. These changes may be attributed to the incorporation of Ag/CuS nanoparticles into the magnetite structure, which influences the chemical bonding and surface properties of the material.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003e\u003cb\u003e3.2 Evaluation of photocatalytic activity of CuS/Fe\u003c/b\u003e\u003csub\u003e\u003cb\u003e3\u003c/b\u003e\u003c/sub\u003e\u003cb\u003eO4 and Ag/CuS/Fe3O4 photocatalyst\u003c/b\u003e\u003c/h2\u003e \u003cp\u003eThe synthesized Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposite exhibited significantly enhanced photocatalytic performance compared to pure Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e. The discussion focuses on the observed differences in photocatalytic activity and the factors contributing to these outcomes.\u003c/p\u003e \u003cp\u003eIn the photocatalytic degradation of tetracycline (TC), Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e demonstrated remarkable efficiency, achieving complete degradation of 20 ppm TC within just 30 minutes of visible light irradiation. In contrast, pure Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e exhibited a much lower degradation efficiency, with only 21% TC degradation under the same conditions. CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e, while showing improved performance compared to Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e, achieved a TC degradation efficiency of 27% within 30 minutes.\u003c/p\u003e \u003cp\u003eThe superior photocatalytic activity of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e can be attributed to several factors. Firstly, the incorporation of silver (Ag) and copper sulfide (CuS) onto the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e surface increases the availability of active sites for photocatalytic reactions. Ag acts as a co-catalyst, enhancing the separation of photogenerated electron-hole pairs and improving charge carrier mobility [\u003cspan citationid=\"CR54\" class=\"CitationRef\"\u003e54\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR55\" class=\"CitationRef\"\u003e55\u003c/span\u003e]. Similarly, CuS functions as a sensitizer, extending the absorption range of the photocatalyst into the visible region and enhancing light utilization efficiency [\u003cspan citationid=\"CR56\" class=\"CitationRef\"\u003e56\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR57\" class=\"CitationRef\"\u003e57\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eFurthermore, the presence of Ag and CuS modifies the band structure of Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e, leading to a reduction in the band gap energy and an increase in the absorption of visible light [\u003cspan citationid=\"CR58\" class=\"CitationRef\"\u003e58\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR59\" class=\"CitationRef\"\u003e59\u003c/span\u003e]. This modification facilitates the generation of more reactive oxygen species (ROS) and promotes the photocatalytic degradation of organic pollutants [\u003cspan citationid=\"CR60\" class=\"CitationRef\"\u003e60\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR61\" class=\"CitationRef\"\u003e61\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe synergistic effect between Ag, CuS, and Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e is also crucial in enhancing photocatalytic performance. The combination of these materials creates a heterojunction structure, which facilitates efficient charge transfer and inhibits charge carrier recombination [\u003cspan citationid=\"CR62\" class=\"CitationRef\"\u003e62\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR63\" class=\"CitationRef\"\u003e63\u003c/span\u003e]. The unique electronic and optical properties of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites contribute to the improved photocatalytic activity observed in this study.\u003c/p\u003e \u003cdiv id=\"Sec12\" class=\"Section3\"\u003e \u003ch2\u003e3.2.1 Effect of Catalyst Dose\u003c/h2\u003e \u003cp\u003eThe effect of catalyst dose on the photocatalytic degradation of tetracycline (TC) was investigated by varying the amount of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposite from 0.002 g to 0.02 g while keeping the TC concentration constant at 20 ppm. The results revealed a clear correlation between the catalyst dose and the photocatalytic efficiency.\u003c/p\u003e \u003cp\u003eAt the lowest catalyst dose of 0.002 g, approximately 60% of TC was degraded after 30 minutes of visible light irradiation [\u003cspan citationid=\"CR64\" class=\"CitationRef\"\u003e64\u003c/span\u003e]. Increasing the catalyst dose to 0.005 g resulted in a slight improvement in the degradation efficiency, with around 60\u0026ndash;70% degradation observed [\u003cspan citationid=\"CR65\" class=\"CitationRef\"\u003e65\u003c/span\u003e]. Further increasing the catalyst dose to 0.007 g significantly enhanced the photocatalytic activity, achieving approximately 84% degradation of TC within the same time frame [\u003cspan citationid=\"CR66\" class=\"CitationRef\"\u003e66\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eInterestingly, a dose of 0.02 g of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposite led to the highest photocatalytic efficiency, with approximately 90% degradation of TC achieved in just 30 minutes [\u003cspan citationid=\"CR67\" class=\"CitationRef\"\u003e67\u003c/span\u003e]. This indicates that the photocatalytic performance is highly dependent on the amount of catalyst present in the reaction system.The observed trend suggests that an optimal catalyst dose is crucial for achieving maximum photocatalytic activity. At lower doses, insufficient active sites may limit the degradation rate, resulting in lower efficiency. On the other hand, excessively high doses may lead to aggregation of catalyst particles, reducing the available surface area for photocatalytic reactions.The enhanced photocatalytic activity at higher catalyst doses can be attributed to the increased number of active sites available for TC adsorption and photocatalytic reactions. Moreover, higher catalyst doses may also promote more efficient light absorption and utilization, leading to improved charge carrier generation and separation(Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThese findings emphasize the importance of optimizing the catalyst dose to maximize photocatalytic performance and underscore the potential of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites for environmental remediation applications.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec13\" class=\"Section3\"\u003e \u003ch2\u003e3.2.2 Effect of Tetracycline Concentration\u003c/h2\u003e \u003cp\u003eThe effect of tetracycline (TC) concentration on the photodegradation efficiency using Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites was investigated. The concentration of TC varied from 25 ppm to 100 ppm(Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eAt lower concentrations (25 ppm, 30 ppm, and 40 ppm), the photodegradation efficiency exhibited an increasing trend. Specifically, at 25 ppm, 30 ppm, and 40 ppm, the degradation efficiencies were 94%, 96%, and 97%, respectively. This suggests that lower concentrations of TC lead to more efficient photodegradation, possibly due to better accessibility of the photocatalytic sites on the nanocomposites.\u003c/p\u003e \u003cp\u003eHowever, as the TC concentration increased to 50 ppm, 60 ppm, 80 ppm, and 100 ppm, the photodegradation efficiency relatively decreased. At 50 ppm, 60 ppm, 80 ppm, and 100 ppm, the degradation efficiencies were 97%, 98%, 81%, and 78%, respectively. This decrease in efficiency with higher TC concentrations could be attributed to factors such as increased competition for active sites on the nanocomposites, saturation of the photocatalytic surface, and reduced light penetration due to higher turbidity caused by increased TC concentration.\u003c/p\u003e \u003cp\u003eOverall, the photodegradation efficiency of TC using Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites is influenced by the initial concentration of TC, with lower concentrations demonstrating higher efficiencies, while higher concentrations exhibit a diminishing trend in efficiency.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec14\" class=\"Section3\"\u003e \u003ch2\u003e3.2.3 Effect of pH solution\u003c/h2\u003e \u003cp\u003eThe effect of pH on the photocatalytic activity of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites was systematically investigated to understand its impact on the degradation of tetracycline (Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e). The results revealed a significant dependence of photocatalytic performance on pH levels. At pH 2, the photoactivity was observed to be relatively low, achieving only about 20% degradation of tetracycline. This decrease in activity at acidic pH can be attributed to several factors, including reduced adsorption of tetracycline molecules and hindered generation of reactive oxygen species (ROS) due to the protonation of surface hydroxyl groups. However, as the pH increased to 4, 6, 7, 11, and 12, a substantial enhancement in photocatalytic activity was observed. In these alkaline conditions, the photoactivity exceeded 90%, indicating a remarkable improvement in tetracycline degradation efficiency. The higher activity at alkaline pH can be attributed to the increased adsorption of tetracycline molecules and facilitated generation of ROS, both of which are crucial for the photocatalytic degradation process. The isoelectric pH of the photocatalyst was found to be 8.7, further confirming the pH-dependent behavior observed in the photocatalytic activity. Overall, the results emphasize the importance of pH in controlling the photocatalytic performance of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites, with alkaline conditions being particularly favorable for efficient tetracycline degradation.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec15\" class=\"Section2\"\u003e \u003ch2\u003e3.4 Isoelectric pH Determination\u003c/h2\u003e \u003cp\u003eThe isoelectric point (pH\u003csub\u003eiep\u003c/sub\u003e) of the photocatalyst was determined using a sodium chloride (NaCl) solution with varying pH values. The pH\u003csub\u003eiep\u003c/sub\u003e is a crucial parameter that indicates the pH at which the surface charge of the photocatalyst is neutral[\u003cspan citationid=\"CR70\" class=\"CitationRef\"\u003e70\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR71\" class=\"CitationRef\"\u003e71\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eIn this experiment, NaCl solutions with pH values ranging from acidic to alkaline were prepared and used to suspend the photocatalyst. The suspensions were then stirred for 24h to ensure equilibrium. Subsequently, the pH of the photocatalyst particles was measured.\u003c/p\u003e \u003cp\u003eThe results revealed that the pH\u003csub\u003eiep\u003c/sub\u003e of the photocatalyst was determined to be 8.7 (Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e10\u003c/span\u003e). This indicates that at a pH of 8.7, the surface charge of the photocatalyst becomes neutral, and the material exhibits minimum electrostatic repulsion between particles.\u003c/p\u003e \u003cp\u003eThe isoelectric pH is an essential parameter as it affects the surface chemistry and colloidal stability of the photocatalyst. Understanding the pH\u003csub\u003eiep\u003c/sub\u003e allows for the optimization of photocatalytic processes, as it influences the adsorption of reactants and intermediates onto the photocatalyst surface. By knowing the pH\u003csub\u003eiep\u003c/sub\u003e, appropriate pH conditions can be chosen to enhance the photocatalytic activity and stability of the material. Additionally, the pH\u003csub\u003eiep\u003c/sub\u003e value provides valuable insights into the surface properties of the photocatalyst, which are crucial for various applications, including pollutant degradation and water treatment.\u003c/p\u003e \u003cp\u003eThe determination of the isoelectric pH of the photocatalyst provides fundamental information that can be utilized to optimize its performance and enhance its effectiveness in environmental remediation processes.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec16\" class=\"Section2\"\u003e \u003ch2\u003e3.5 Kinetic Study\u003c/h2\u003e \u003cp\u003eThe photocatalytic degradation of tetracycline (TC) using Ag/CuS/Fe3O4 nanocomposites was investigated to understand the reaction kinetics. The study involved varying the dosage of the catalyst from 0.002 g to 0.02 g and analyzing the degradation kinetics.\u003c/p\u003e \u003cp\u003eThe degradation rate of TC was calculated using the following equation:\u003c/p\u003e \u003cp\u003eln (\u0026#119862;\u003csub\u003e0/\u003c/sub\u003e\u0026#119862;\u003csub\u003e\u0026#119905;\u003c/sub\u003e)=\u0026#119896;\u0026#119905;\u003c/p\u003e \u003cp\u003eWhere:\u003c/p\u003e \u003cp\u003e \u003cul\u003e \u003cli\u003e \u003cp\u003e \u003cb\u003eC₀\u003c/b\u003e is the initial concentration of TC (ppm)\u003c/p\u003e \u003c/li\u003e \u003cli\u003e \u003cp\u003e \u003cb\u003eCₜ\u003c/b\u003e is the concentration of TC at time t (ppm)\u003c/p\u003e \u003c/li\u003e \u003cli\u003e \u003cp\u003e \u003cb\u003ek\u003c/b\u003e is the rate constant (L/min or cm\u0026sup3;/min)\u003c/p\u003e \u003c/li\u003e \u003cli\u003e \u003cp\u003e \u003cb\u003et\u003c/b\u003e is the reaction time (min)\u003c/p\u003e \u003c/li\u003e \u003c/ul\u003e \u003c/p\u003e \u003cp\u003eBy measuring the TC concentration at different time intervals throughout the experiment, the rate constant (k) can be determined using this equation. The rate constant reflects the efficiency of the photocatalyst in degrading TC.\u003c/p\u003e \u003cp\u003eFrom the kinetic analysis, it was observed that increasing the dosage of the catalyst led to higher degradation rates of TC. The rate constant \u0026#119896; ranged from 0.026 min\u003csup\u003e\u0026minus;1\u003c/sup\u003e to 0.2 min\u003csup\u003e\u0026minus;1\u003c/sup\u003e for catalyst dosages ranging from 0.002 g to 0.02 g (Fig.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e). Specifically, at a catalyst dosage of 0.002 g, the rate constant was 0.026 min\u003csup\u003e\u0026minus;1\u003c/sup\u003e, whereas at a dosage of 0.02 g, the rate constant increased to 0.2 min\u003csup\u003e\u0026minus;1\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003eThis result indicates that higher catalyst dosages promote faster degradation kinetics due to increased active sites available for the adsorption of TC molecules and subsequent generation of reactive species. The first-order kinetic behavior suggests that the degradation rate is directly proportional to the concentration of TC remaining in the solution.\u003c/p\u003e \u003cp\u003eFurthermore, the observed first-order kinetics imply that the photocatalytic degradation of TC by Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites is primarily controlled by the availability of active sites on the catalyst surface. As the dosage of the catalyst increases, the number of active sites also increases, leading to enhanced degradation rates.\u003c/p\u003e \u003cp\u003eOverall, the kinetic study demonstrates that the Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites exhibit efficient photocatalytic degradation of TC, and the process follows a first-order kinetic model across different catalyst dosages [\u003cspan citationid=\"CR72\" class=\"CitationRef\"\u003e72\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e\u003c/p\u003e\n\u003ch2\u003e3.6 Mechanism of Photodegradation\u003c/h2\u003e\n\u003cp\u003eThe photocatalytic degradation of tetracycline (TC) using Ag/CuS/Fe3O4 nanocomposites involves a complex series of reactions driven by the generation of reactive oxygen species (ROS) upon exposure to visible light [\u003cspan class=\"CitationRef\"\u003e73\u003c/span\u003e]. The mechanism can be described as follows:\u003c/p\u003e\n\u003cp\u003e\u003cspan\u003e1. Adsorption: Initially, tetracycline molecules adsorb onto the surface of the Ag/CuS/Fe3O4 nanocomposites due to electrostatic interactions and hydrogen bonding between the TC molecules and the catalyst surface.\u003cbr\u003e\u003c/span\u003e \u003cspan\u003e2. Generation of Reactive Species: Under visible light irradiation, the Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites absorb photons, leading to the excitation of electrons from the valence band to the conduction band. This excitation creates electron-hole pairs (𝑒\u0026minus; -h+).\u003cbr\u003e\u003c/span\u003e \u003cspan\u003e3. ROS Generation: The photogenerated electrons (𝑒\u003csup\u003e\u0026minus;\u003c/sup\u003e) react with molecular oxygen (𝑂\u003csub\u003e2\u003c/sub\u003e) adsorbed on the catalyst surface, leading to the formation of superoxide radicals (O\u003csub\u003e2\u003c/sub\u003e\u0026bull;\u003csup\u003e\u0026minus;\u003c/sup\u003e). Similarly, the photogenerated holes (h\u003csup\u003e+\u003c/sup\u003e) react with water molecules (𝐻\u003csub\u003e2\u003c/sub\u003e𝑂) to form hydroxyl radicals (OH\u0026bull;). These ROS are highly reactive and play a crucial role in the degradation of TC.\u003cbr\u003e\u003c/span\u003e \u003cspan\u003e4. TC Degradation: The ROS, including superoxide radicals and hydroxyl radicals, attack the adsorbed TC molecules, leading to the degradation of TC into smaller, less complex organic molecules, and eventually into harmless byproducts such as carbon dioxide and water.\u003cbr\u003e\u003c/span\u003e \u003cspan\u003e5. Effect of Scavengers: The presence of scavengers such as hydrogen peroxide (H2O2), ethylenediaminetetraacetic acid (EDTA), ethanol (EtOH), and potassium chloride (KCl) significantly affects the photocatalytic degradation process(Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e12\u003c/span\u003e).\u003cbr\u003e\u003c/span\u003e\u003c/p\u003e\n\u003cp\u003eIn the initial stages of photodegradation, scavengers compete with tetracycline (TC) molecules for the reactive oxygen species (ROS). Hydrogen peroxide (H2O2), as a strong oxidizing agent, readily scavenges ROS, leading to a decrease in their concentration. EDTA, a strong chelating agent, also competes with TC for ROS, effectively reducing their availability for TC degradation. Ethanol (EtOH) acts as a sacrificial agent by absorbing photons and generating hydroxyl radicals (\u0026bull;\u0026bull;OH), thus scavenging ROS. Potassium chloride (KCl) likely acts as an electron scavenger, intercepting electrons and reducing the formation of ROS.\u003c/p\u003e\n\u003cp\u003eDuring the early stages of the reaction, the scavengers\u0026apos; competition with TC for ROS leads to a decrease in photodegradation efficiency compared to the control (without scavenger). This decrease is most pronounced for H2O2 and EDTA due to their strong scavenging abilities. However, as the reaction progresses, the scavengers begin to saturate, and their scavenging capacities diminish. At this point, the differences in photodegradation efficiency between the scavenger-containing samples and the control diminish. Eventually, in the later stages of photodegradation, all scavengers and the control without scavenger exhibit similar high photodegradation efficiencies, typically around 90%. This behavior suggests that while scavengers initially hinder the degradation process by competing with TC for ROS, their effect diminishes over time, allowing the photocatalyst to efficiently degrade TC regardless of the scavenger present.\u003c/p\u003e\n\u003cp\u003e\u003cspan\u003e6. Later Stage Degradation: However, as the reaction progresses, the concentration of ROS decreases, and the availability of active sites on the catalyst surface becomes limiting. At this point, the presence of scavengers has a minimal effect on the degradation efficiency. Therefore, in the later stages of photodegradation, the photodegradation efficiency of the scavenger-containing solutions approaches that of the control (without scavenger).\u003cbr\u003e\u003c/span\u003e \u003cspan\u003e7. Overall Efficiency: Despite the presence of scavengers, the overall photodegradation efficiency remains high (around 90%), indicating the robustness of the Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites in degrading TC under visible light irradiation.\u003cbr\u003e\u003c/span\u003e\u003c/p\u003e\n\u003cp\u003eThis mechanism highlights the importance of ROS generation and scavenger effects in the photocatalytic degradation of tetracycline using Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites.\u003c/p\u003e\n\u003cp\u003e\u003c/p\u003e\n\u003cdiv id=\"Sec18\" class=\"Section2\"\u003e\n \u003ch2\u003e3.7 Application of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites in photodegradation of diclofenac\u003c/h2\u003e\n \u003cp\u003eThe photocatalyst demonstrated high efficiency in the degradation of diclofenac (Dic) when tested alone, achieving an impressive degradation rate of 84% (Fig. \u003cspan class=\"InternalRef\"\u003e13\u003c/span\u003e.A). This indicates the excellent photocatalytic activity of the material in degrading this particular pharmaceutical compound under visible light illumination.\u003c/p\u003e\n \u003cp\u003eFurthermore, in a simultaneous photodegradation experiment involving both diclofenac (Dic) and tetracycline (TC), the photocatalyst exhibited remarkable performance. The degradation of tetracycline (TC) reached an impressive efficiency of 95%, indicating the photocatalyst\u0026apos;s strong capability to degrade this antibiotic compound. Moreover, despite the simultaneous degradation of both diclofenac (Dic) and tetracycline (TC), the photocatalyst also demonstrated substantial efficacy in degrading diclofenac (Dic), achieving a degradation efficiency of 50%. This highlights the versatility of the photocatalyst in simultaneously degrading multiple organic pollutants, even when present in complex mixtures (Fig. \u003cspan class=\"InternalRef\"\u003e13\u003c/span\u003e.B).\u003c/p\u003e\n \u003cp\u003eOverall, the results underscore the potential of the photocatalyst for efficient photodegradation of pharmaceutical compounds, both individually and in complex mixtures, contributing to the mitigation of organic pollutant contamination in water bodies.\u003c/p\u003e\n \u003cp\u003eThe efficiency of the photocatalyst for the photodegradation of diclofenac alone was found to be 84%. Diclofenac, a commonly used nonsteroidal anti-inflammatory drug, is known for its persistence in the environment and potential ecological risks.\u003c/p\u003e\n \u003cp\u003eHowever, when the photocatalyst was used for the simultaneous photodegradation of both diclofenac and tetracycline (TC), the results showed remarkable performance. The degradation efficiency for tetracycline was as high as 95%, indicating the excellent ability of the photocatalyst to break down this antibiotic compound efficiently.\u003c/p\u003e\n \u003cp\u003eInterestingly, despite the simultaneous degradation of both diclofenac and tetracycline, the efficiency for diclofenac was slightly lower, achieving a degradation rate of 50%. This suggests that while the photocatalyst is effective in degrading diclofenac, the presence of tetracycline may have a slight inhibitory effect on its degradation efficiency for diclofenac.\u003c/p\u003e\n \u003cp\u003eOverall, the simultaneous photodegradation of diclofenac and tetracycline demonstrates the potential of the photocatalyst for the efficient removal of these emerging contaminants from water sources. Further optimization of the photocatalytic process may enhance the degradation efficiency for diclofenac and other pharmaceutical compounds, contributing to the development of advanced water treatment technologies.\u003c/p\u003e\n\u003c/div\u003e"},{"header":"4. Conclusion","content":"\u003cp\u003eThis study demonstrates the effective utilization of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites as photocatalysts for the degradation of organic pollutants, particularly tetracycline (TC) and diclofenac. The synthesized nanocomposites exhibited superior photocatalytic activity, outperforming pristine Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e counterparts. The enhanced performance of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites can be attributed to the synergistic effects of Ag and CuS, which improve the charge carrier separation and extend the light absorption range, leading to increased photocatalytic efficiency. The presence of Ag also contributes to lowering the bandgap energy, making the nanocomposites more active under visible light. EDX analysis confirmed the successful doping of Ag and CuS into the Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e lattice, which was further supported by XRD analysis showing distinct diffraction peaks corresponding to the different phases. FESEM images revealed the morphological characteristics of the nanocomposites, indicating the formation of well-defined structures with enhanced surface areas. UV-Vis and FTIR spectroscopy provided insights into the optical and chemical properties of the nanocomposites, highlighting the shifts in absorption peaks and the presence of functional groups associated with photocatalytic activity. The photocatalytic activity of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites was evaluated through the degradation of tetracycline under visible light irradiation. The nanocomposites exhibited excellent performance, achieving a degradation efficiency of 100% within 30 minutes, compared to lower efficiencies observed for Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e and CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e. Furthermore, the effect of catalyst dosage, pH, and scavengers on the photocatalytic activity was investigated. The results showed that higher catalyst dosages and alkaline pH conditions significantly enhanced the degradation efficiency, while scavengers initially reduced the efficiency but had minimal impact in the later stages of the reaction. Additionally, the simultaneous photodegradation of diclofenac and tetracycline revealed the versatility of Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites in treating multiple pollutants, with promising degradation efficiencies observed for both compounds. In conclusion, Ag/CuS/Fe\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocomposites show great potential for environmental remediation applications, particularly in the treatment of wastewater contaminated with organic pollutants. Further studies could focus on optimizing the synthesis parameters and exploring the recyclability and long-term stability of the nanocomposites for practical applications.\u003c/p\u003e"},{"header":"Declarations","content":"\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eR.Mohammadzadeh kakhki wrote the mail text and lead the project. H.Bolandhemmat cooperated with doing the experiments.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eAdil M, Rahman A, Zulifqar S, et al. Facile synthesis of binary metal-substituted copper oxide as a solar light-driven photocatalyst and antibacterial substitute. Advanced Powder Technology. 2021;32:940\u0026ndash;950.\u003c/li\u003e\n\u003cli\u003eBashir S, Jamil A, Amin R, et al. Hydrothermally synthesized Gd-doped BiSbO4 nanoparticles and their graphene-based composite: A novel photocatalytic material. Journal of Solid State Chemistry. 2022;312:123217.\u003c/li\u003e\n\u003cli\u003eAli H, Khan E. 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Journal of Photochemistry and Photobiology A: Chemistry, 385, 112040. doi: 10.1016/j.jphotochem.2019.112040\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true},"keywords":"Ag@CuS-doped magnetite nanocomposite, Photocatalytic activity, Tetracycline, Diclofenac, visible light","lastPublishedDoi":"10.21203/rs.3.rs-4642539/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-4642539/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThe contamination of water sources by pharmaceutical pollutants presents significant environmental and health hazards, making the development of effective photocatalytic materials crucial for their removal. This research focuses on the synthesis of a novel Ag@CuS-doped magnetite nanocomposite and its photocatalytic efficiency against tetracycline and diclofenac contaminants. The nanocomposite was created through a straightforward and scalable precipitation method, integrating silver nanoparticles (Ag NPs) and copper sulfide (CuS) into a magnetite framework. Various analytical techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and energy-dispersive X-ray spectroscopy (EDS), were employed to characterize the structural and morphological properties of the synthesized material. The photocatalytic activity was tested by degrading tetracycline and diclofenac under visible light. Results indicated a marked improvement in the photocatalytic performance of the Ag@CuS-doped magnetite nanocomposite compared to both pure magnetite and CuS-doped magnetite. The enhanced photocatalytic efficiency is attributed to the synergistic interaction between Ag NPs, CuS, and Fe3O4, which improves light absorption and charge separation, thereby increasing the generation of reactive oxygen species (ROS) and promoting the degradation of the pollutants. This study highlights the potential of the Ag@CuS-doped magnetite nanocomposite as an efficient and reusable photocatalyst for eliminating pharmaceutical pollutants from water.\u003c/p\u003e","manuscriptTitle":"Synthesis of Ag@ CuS doped mineral magnetite nanocomposite with improved photocatalytic activity against tetracycline and diclofenac pollutants","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-07-19 20:33:37","doi":"10.21203/rs.3.rs-4642539/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2024-07-10T06:36:24+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-07-09T05:34:11+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-07-04T06:15:04+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"304368330602983559739419737328563331604","date":"2024-06-28T14:17:58+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"201607363760544181814712285450190342756","date":"2024-06-28T03:01:40+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-06-28T02:01:02+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2024-06-28T01:54:24+00:00","index":"","fulltext":""},{"type":"editorInvited","content":"","date":"2024-06-27T17:52:44+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2024-06-27T17:50:09+00:00","index":"","fulltext":""},{"type":"submitted","content":"Scientific Reports","date":"2024-06-26T11:53:37+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"1ccd50a4-36e9-46ac-adab-5ec3a3ea8c6f","owner":[],"postedDate":"July 19th, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2024-08-22T19:26:34+00:00","versionOfRecord":{"articleIdentity":"rs-4642539","link":"https://doi.org/10.1038/s41598-024-69644-5","journal":{"identity":"scientific-reports","isVorOnly":false,"title":"Scientific Reports"},"publishedOn":"2024-08-16 15:56:52","publishedOnDateReadable":"August 16th, 2024"},"versionCreatedAt":"2024-07-19 20:33:37","video":"","vorDoi":"10.1038/s41598-024-69644-5","vorDoiUrl":"https://doi.org/10.1038/s41598-024-69644-5","workflowStages":[]},"version":"v1","identity":"rs-4642539","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-4642539","identity":"rs-4642539","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}