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. 2026 Jan 27;4(5):599–611. doi: 10.1021/prechem.5c00203

Harnessing Visible Light: MXene/g‑C3N4/WO3/NiO Nanocomposite for Rapid Degradation of Tetracycline

Suganya Josephine Gali Anthoni †,*, Rubesh Ashok Kumar S †,‡, Vasvini Mary D †,‡, Vidhya Lakshmi N §, Mary Nisha U ∥
PMCID: PMC13217340  PMID: 42222713

Abstract

The ubiquity of antibiotics such as tetracycline (TC) in aquatic environments poses serious global health issues due to their persistence and ability to enhance antimicrobial resistance. This paper presents MXene/g-C3N4/WO3/NiO (MGWN), prepared by a simple hydrothermal route, which was evaluated for its performance as a photocatalyst in the photodegradation of TC under visible light. The coupling of metal oxides (WO3 and NiO) with carbon-based materials (MXene and g-C3N4) promotes photocatalytic activity through enhanced light absorption and charge separation. In-depth characterization using FT-IR, XRD, UV-DRS, FE-SEM, HR-TEM, and EDAX validated the development of textured nanostructure with particle sizes in the range 10–35 nm and a band gap of 2.84 eV. Photocatalytic activity tests demonstrated that MGWN exhibited a remarkable TC (5 ppm) removal rate of 99.35% within 120 min, adhering closely to pseudo-first-order kinetics. The apparent rate constant (k) was calculated to be 1.55 × 10–2 min–1 (R 2 0.9931), indicating a substantial rate of reaction. Further stability and reusability assessments revealed that the MGWN nanocomposite maintained over 90% photocatalytic efficiency after five consecutive cycles, reinforcing its potential for sustainable wastewater treatment applications. The findings highlight the MGWN nanocomposite as an effective and stable photocatalyst for removing persistent organic pollutants, paving the way for future advancements in environmental remediation technologies.

Keywords: antibiotic, heterogeneous photocatalysis, MXene/g-C3N4/WO3/NiO, persistent organic pollution, tetracycline

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1. Introduction

Persistent organic pollutants (POPs), such as antibiotics, are a major cause of antimicrobial resistance, posing a serious threat in the global arena. Antibiotics are a class of drugs that are used to act against bacteria by destroying them or retarding their growth. According to the WHO’s 2014 report, when these materials are present in the environment and continuously exposed to various infecting species, such as microbes, they can produce resistance to these microbes, posing a major public health concern as they hinder the treatment of infections. , Literature evidence shows a dramatic increase in the global use of antibiotics and predicts a 200% rise by 2030. Tetracycline (TC) is one of the most widely used antibiotics, first isolated from Streptomyces species in the early 1940s. Due to its potency, it has a broad spectrum of activity, suppressing many species of both Gram-positive and Gram-negative bacteria. Though the antibiotic is found to be active against most species, its overuse and lesser ability to degrade in environmental conditions have led to its existence as a POP and posed a threat to humanity. The presence of antibiotics in the environment may lead to their accumulation and residues, which are harmful and chronically toxic to all life forms. TC is capable of accumulating in the environment, entering the food chain, and spreading threats to mankind. Hence, the management/removal of antibiotics from the aquatic environment is a topic for discussion and is being worked on by various research groups around the globe.

In recent years, there has been a rising trend of interest in developing efficient treatment technologies for environmental pollutants. Processes like the advanced oxidation process, photocatalysis, adsorption, membrane separation, electrochemical process, reverse osmosis, biological process, and disinfection are generally practiced to treat different contaminant problems. Out of the various technologies mentioned above, the process of degradation by photocatalysis is found to be the most preferable technology as compared to other available methodologies. The process of photocatalysis uses the power of light to catalyze a catalyst to break down toxic contaminants into less toxic or harmless substances. There is more than one reason to prefer this technology to other available methodologies. This technology has been found to be highly effective in degrading various organic contaminants, regardless of their type or concentration. Additionally, this technology is practiced at low temperatures to minimize energy consumption. , Literature cites the efficient removal of antibiotics from the aqueous phase employing heterogeneous nanomaterials as photocatalysts. Titanium dioxide (TiO2) and ZnO-based nanomaterials were the initial forerunners in the field of heterogeneous photocatalysis under UV/visible light irradiation. , Materials such as ZnO, TiO2, and WO3 have been employed in their pristine phase or in combination with other metals or metal oxides, including doping, binary and ternary composites, or supported on carbon-based materials. −

MXene (Ti3C2) is a novel class of two-dimensional (2D) nanomaterials that exhibit a unique set of physical and chemical properties, − making them highly attractive for a wide range of applications. As members of the larger family of MXenes, Ti3C2 layers are composed of transition metal carbides, nitrides, or carbonitrides. − The shift from MAX phases to MXenes occurs through selective etching that removes the “A” element, resulting in the formation of 2D structures. MXenes retain the high electrical conductivity and layered structure of their MAX phase precursors but offer enhanced surface chemistry and hydrophilicity. MXene (Ti3C2) stands out due to its outstanding electrical conductivity, hydrophilic surface, and adaptable surface chemistry. In the context of photocatalytic activities, both MAX and MXene phases are preferred due to their excellent electronic properties and structural stability under light irradiation. The 2D nature of MXenes, such as Ti3C2, provides a high surface area that is advantageous for photocatalytic processes, as it enhances light absorption and facilitates the adsorption of reactants. − The flexible and conductive nature of Ti3C2 MXenes, combined with their ease of processing, opens up the horizons in the development of advanced materials for technological and environmental applications. −

In the quest to address the growing concern of antibiotic contaminants in aquatic environments, the use of carbon-based nanomaterials for photocatalytic degradation has emerged as a promising solution. The innovative application of MXene, integrated with graphitic carbon nitride (g-C3N4), complemented by metal oxides such as WO3 and NiO, spearheads a novel approach to water detoxification. This composite material, by harnessing the synergy between the unique properties of MXene and g-C3N4, alongside the catalytic prowess of added metal oxides, offers a significant enhancement in photocatalytic efficiency under visible light. The versatility and potent catalytic action of these carbon-based nanomaterials pave the way for the effective degradation of tetracycline, thus spotlighting a scalable and environmentally benign technology for purifying water from hazardous organic compounds. By optimizing the structural and compositional traits of these nanocomposites, this work aims to contribute a robust methodology for addressing one of the pressing environmental challenges of our time, the proliferation of antibiotic resistance and the preservation of aquatic ecosystems.

The current study introduces a novel photocatalyst, an MXene/g-C3N4/WO3/NiO (MGWN) nanomaterial, synthesized through a simple hydrothermal method aimed at addressing the challenge of TC degradation from aqueous phases. Through its innovative approach, this work seeks to contribute to the field of environmental remediation, highlighting the synergistic potential of combining carbon-based nanomaterials with metal oxides to enhance photocatalytic efficiency under visible light.

2. Experimental Section

2.1. Materials and Methods

The information about the material and chemicals used in this work and the detailed procedure of the photocatalytic degradation process are explained in the Supporting Information.

2.2. Preparation

2.2.1. MXene (Ti3C2)

The MXene material was prepared by a facile HF etching technique. Two g of MAX (Ti3AlC2) was taken in a 100 mL Teflon beaker, and it was dispersed in 70 mL of 49% HF. The solution mixture was then kept in the magnetic stirrer for 48 h at ambient temperature. After that, the etched black precipitate was filtered and washed with DI water and absolute ethanol (to reduce the pH). Then, the black precipitate was dried in a hot-air oven at 90 °C overnight. The dried MXene material was stored and sealed (Scheme ).

1. Synthesis of MXene (Ti3C2).

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2.2.2. Graphitic Carbon Nitride (gC3N4)

gC3N4 was prepared by a simple polymeric decomposition method. Five g of melamine was taken into the cleaned crucible and kept in the muffle furnace at 550 °C for 5 h. After 5 h, the sample was well-grounded and used for further studies (Scheme ).

2. Synthesis of gC3N4 .

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2.2.3. Tungsten Trioxide (WO3)

WO3 nanomaterial was synthesized using a simple precipitation method. A solution of 0.005 M sodium tungstate (Na2WO4·2H2O in 20 mL) was carefully poured into a beaker and placed on a magnetic stirrer rotating at approximately 400 rpm. The stirred mixture was maintained below 20 °C in an ice bath. Using a buret, 6 M of HCl solution was slowly added drop by drop to the beaker until the pH reached ∼2. After the complete addition, the solution was vigorously stirred for 60 min to allow for precipitate formation. Then the beaker was left to stand alone for 16 h, this process allows the growth of precipitate. The resulting pale-yellow precipitate was a result of the tungstic acid formation. The solution containing tungstic acid was then filtered and dried using a hot-air oven. The residue obtained after filtering was calcinated at 300 °C for 2 h. Once cooled, the resulting WO3 was ground thoroughly and stored in an airtight container.

2.2.4. MXene/g-C3N4/WO3/NiO (MGWN)

Initially, the as-prepared MXene (50 mg), gC3N4 (350 mg), and WO3 (50 mg) were taken into a cleaned 100 mL beaker along with 186.2 mg of Ni (NO3)3. This solid mixture was dispersed with 20 mL of DI water. The above-prepared mixture was sonicated in the bath sonicator for 15 min and kept in the magnetic stirrer. Then, the buret was filled with freshly prepared Na2CO3 solution (66.18 mg in 20 mL of DI water) and placed above the beaker for the drop-by-drop addition (Scheme ). After the complete addition, again the solution mixture was sonicated for 15 min and transferred to a 250 mL Teflon-coated autoclave and placed in the furnace for 18 h at 180 °C. Finally, the precipitate was filtered and washed with DI water and absolute ethanol. Then, the collected sample was dried overnight in the hot-air oven at 90 °C. A series of MXene/g-C3N4/WO3/NiO was prepared with varying MXene loadings, resulting in nanomaterials labeled as MGWN 1 (0.25:5.75:0.75:0.25), MGWN 2 (0.5:5.5:0.75:0.25), MGWN 3 (0.75:5.25:0.75:0.25), MGWN 4 (1:5:0.75:0.25), and MGWN 5 (2:4:0.75:0.25).

3. Preparation of MGWN Nanomaterial.

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3. Results and Discussion

3.1. UV–Visible Analysis of MGWN

The UV–vis diffuse reflectance spectroscopy (DRS) results of MGWN, comprising MXene, g-C3N4, WO3, and NiO, provide a comprehensive insight into the optical properties of the nanomaterial. Figure shows the UV–vis DRS of MGWN and its bandgap analysis plot. The UV-DRS analysis of the MGWN reveals that the integration of MXene, g-C3N4, WO3, and NiO results in a material with a unique optical profile capable of absorbing light across a wide range of wavelengths. From the obtained results, the absorption edge of MGWN was found to be 460.2 nm (Figure a). This value suggests that the MGWN nanomaterial is active in both UV and visible light. The bandgap analysis was carried out by the traditional approach, “Tauc-Plot”. This method involves the plotting of (αhυ)2 as a y-axis versus hυ as an x-axis. The values were plotted as shown in Figure b, and the bandgap value was found to be 2.84 eV. This narrow bandgap indicates the material’s strong potential for application in areas requiring the harnessing of both UV and visible light, such as in advanced photocatalytic degradation processes or the development of solar light-driven systems. , The complementary absorption characteristics of the components within the MGWN suggest enhanced charge separation and transfer capabilities, critical for the efficiency of photocatalytic and solar energy conversion applications.

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(a, b) UV–vis DRS; (c) FT-IR; (d) XRD analysis of MGWN.

3.2. FT-IR Analysis of MGWN

The FT-IR analysis of the MGWN nanomaterial reveals distinct characteristic bands corresponding to each component, demonstrating successful integration within the nanomaterial (Figure (c)). The appearance of broad bands around 3380 cm–1 could be attributed to the O–H stretching vibrations, indicating the presence of surface −OH groups in the prepared nanomaterial. The band around 420 to 590 cm–1 could be assigned to the Ti–O–Ti stretching vibrations, suggesting the presence of MXene in MGWN. The characteristic peak of g-C3N4 is observed at around 1430 cm–1, corresponding to the stretching vibration modes of CN and C–N heterocycles, confirming the presence of graphitic carbon nitride in MGWN nanomaterial.

This is accompanied by a peak near 1233 cm–1, indicative of the tri-s-triazine units inherent to the g-C3N4 structure. WO3 is represented by bands around 810 and 714 cm–1, which could be attributed to the WO terminal stretching and W–O–W bridging stretching modes, respectively. These characteristic peaks confirm the successful incorporation of tungsten trioxide into the nanocomposite. The presence of NiO is confirmed by the absorption band observed around 400–600 cm–1, attributed to the Ni–O stretching vibrations, characteristic of nickel oxide’s vibrational modes. , The overlay of these characteristic bands in the FT-IR spectrum of the MGWN suggests a composite material where interfaces between MXene (Ti3C2), g-C3N4, WO3, and NiO are successfully formed. This heterojunction could facilitate charge separation and migration, improving the photocatalytic activity of the composite under visible light irradiation.

3.3. XRD Analysis of MGWN

The X-ray Diffraction (XRD) analysis was conducted on the synthesized MGWN nanomaterial, as shown in Figure d. This analysis was carried out to understand the crystallographic structure and phase purity of the composite material. The study revealed several distinct peaks corresponding to each component, indicating the successful synthesis of the compound and the presence of individual crystalline phases within the MGWN nanomaterial. The XRD pattern shows prominent peaks at 2θ values of approximately 12.5, 18.7, and 61.2°. These can be indexed to the (002), (004), and (110) planes of the hexagonal Ti3C2 phase, respectively, indicating a well-structured MXene phase within the nanomaterial.

For g-C3N4, a pronounced peak is observed at around 2θ = 27.4°, corresponding to the (002) plane, demonstrating a graphitic stacking structure typical of g-C3N4 (JCPDS #43-1035). This peak is indicative of the layered structure of the carbon nitride within the MGWN nanomaterial. The XRD pattern displays distinct peaks at 2θ values of 23.1, 23.6, 24.3, 34.2° assignable to the (002), (020), (200), (120), and (112) planes, respectively, of the monoclinic WO3 phase (JCPDS #87-1526). The sharp and well-defined peaks indicate a high degree of crystallinity. For NiO, characteristic peaks are noted at 2θ values of 35.3, 43.3, and 62.9°, which can be ascribed to the (111), (200), and (220) planes of the cubic phase of NiO. The presence of all these peaks confirms the successful synthesis of the MGWN nanomaterial, with each component maintaining its crystalline phase. The synergistic effect of these materials in the composite aims at enhancing the photocatalytic activity for the degradation of tetracycline under visible light irradiation.

3.4. FE-SEM Analysis MGWN

Figure shows the FE-SEM analysis for the primary gC3N4 (a, b) and MXene (Ti3C2) materials (c, d), signifying their disparate morphologies. In the gC3N4 structure (Figure a,b), it was observable that the material appeared to be loosely agglomerated with a fluffy morphology, consisting of highly thin nanosheets with a wrinkled appearance, having a sponge-like material structure. The high-magnification image shown in Figure b highlights the layered structure of the gC3N4 material that has irregular boundaries on a nanometric scale. On the other hand, for the MXene material (Figure c,d), it was observable that the material consisted of large platelets with well-defined layers characteristic of Ti3C2. These platelets were stacked on top of each other to form multilayered structures with an accordion-like appearance.

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FE-SEM analysis of (a, b) gC3N4 and (c, d) MXene.

Figure a shows a layered structure typical of MXene, with g-C3N4 layers interspersed, indicating the successful integration of these components. The WO3 and NiO particles were evenly distributed across the matrix, presenting as small, well-defined nodules adhered firmly to the surfaces of MXene and g-C3N4 layers (Figure b). This uniform dispersion suggests a strong interaction between the different constituents of the nanomaterials. The MGWN nanomaterial exhibited a textured surface pattern that enhances the surface area available for photocatalytic reactions. Furthermore, the detailed magnification revealed the porosity within the material, suggesting pathways for enhanced adsorption and accessibility of tetracycline molecules to the active sites. This structural complexity, as revealed by the FE-SEM analysis, supports the potential of MGWN for efficient photocatalytic degradation of tetracycline under visible light by providing ample reactive sites and facilitating charge separation and transfer processes.

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(a, b) FE-SEM images of MGWN and (c–i) EDAX analysis of MGWN.

3.5. EDAX and Elemental Analysis of MGWN

The Energy Dispersive X-ray Analysis (EDAX) results of MGWN composite, comprised of Ti3C2, g-C3N4, WO3, and NiO, indicated a highly heterogeneous material with a diverse elemental composition, as shown in Figure c. The Figure d–i revealed the presence of titanium (Ti), carbon (C), nitrogen (N), tungsten (W), nickel (Ni), and oxygen (O) peaks that align with the expected composition based on the starting materials (Figure d,e). The EDAX data showed a significant presence of titanium, confirming the existence of Ti3C2 layers. Titanium constituted approximately 0.2 wt % of the elemental composition. Carbon and nitrogen were both prominently featured in the spectrum. The g-C3N4 contributes primarily to these elements, with carbon also coming from the Ti3C2 layers. The analysis suggested around 32.4 wt % carbon and 45.6 wt % nitrogen in the composite, indicating a combined contribution from both Ti3C2 and g-C3N4. The WO3 phase accounted for the tungsten and a significant portion of the oxygen in the composite. Tungsten was found to be around 5.8 wt % of the composite, while oxygen, contributed from both NiO and WO3, was approximately 11.7 wt % as well. Nickel, originating from the NiO phase, was also detected and constituted about 4.3 wt % of the composite material. The elemental analysis provided insights into the complex composition of the MGWN composite, underscoring the multifaceted interactions between the different components (Ti3C2, g-C3N4, WO3, and NiO).

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(a) SAED; (b, c) HR-TEM; and (d, e) elemental mapping (EDS) analysis of MGWN.

3.6. HR-TEM Analysis MGWN

HR-TEM analysis was carried out to study the microscopic structure and morphology of the prepared MGWN nanomaterial (Figure ). The SAED pattern shown in Figure a reveals the presence of distinct concentric rings corresponding to the (002), (100), and (101) crystal planes of the crystalline gC3N4 layers, signifying the polymeric nature of the gC3N4 layers and the long-range crystalline order of the gC3N4 crystallites.

Figure b clearly reveals a uniformly distributed multicomponent system with Ti3C2 MXene layers represented as thin sheets of characteristic accordion-like morphology, indicating efficient delamination of MXene during the synthesis process. In the Figure, the gC3N4 layers were represented as the light-colored sheet-like structures uniformly distributed between the MXene layers to facilitate efficient interaction between the two carbon nanomaterials. Figure c clearly reveals the highly magnified image of the WO3 and NiO nanoparticles, uniformly distributed between the MXene and gC3N4 sheets, with spherical and quasi-spherical morphologies and a size range of 10–35 nm. The lattice fringes were clearly distinguishable, indicating the crystalline nature of both oxide components. Figure d,e present the EDS analysis conducted for a representative composite particle, revealing major elemental peaks corresponding to Ti, C, N, W, O, and Ni, confirming the successful incorporation of all four constituents within the MGWN nanocomposite.

3.7. Plausible Photocatalytic Degradation Mechanism

The photocatalytic degradation of tetracycline (TC) by MGWN nanomaterial under visible light irradiation could be explained (Figure ) through a proposed mechanism that involves multiple steps, capitalizing on the synergistic effects of the constituents in the nanomaterial. Each component plays a vital role in enhancing the photocatalytic performance toward TC degradation. Upon irradiation with visible light, both WO3 and g-C3N4 would be excited due to their suitable bandgap energies, leading to the generation of electrons and holes (e– and h+) in their respective conduction and valence bands. Meanwhile, MXene (Ti3C2), with its metallic conductivity, would as an excellent electron conductor, facilitating the transfer of photogenerated electrons. The strategic assembly of MXene with g-C3N4 and WO3 facilitates efficient separation and transfer of photogenerated e–/h+ pairs. The electrons in the conduction band of g-C3N4 transfer to the conduction band of MXene with ease due to its excellent electrical conductivity. Similarly, electrons from WO3 also migrate to MXene, whereas NiO, with its p-type semiconductor properties, accepts the holes from the valence band of g-C3N4 and WO3, enhancing charge separation efficiency and reducing recombination.

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Plausible photocatalytic degradation mechanism of tetracycline.

The separated electrons on the MXene surface interact with oxygen molecules (O2) present in water to produce superoxide radicals (O2 •–), while the holes in the NiO react with water (H2O) or hydroxide ions (OH–) to generate hydroxyl radicals (•OH). These reactive oxygen species (•OH and O2 •–) possess strong oxidizing power capable of degrading TC molecules adsorbed on the catalyst’s surface into smaller nontoxic molecules, CO2, and water. The unique heterostructured MGWN nanocomposite utilizes its components’ synergistic properties for effective charge generation, separation, and transfer, along with an efficient generation of reactive oxygen species under visible light, leading to the enhanced photocatalytic degradation of tetracycline. The presence of MXene enhances electron transfer, reducing recombination, g-C3N4 expands the visible light absorption range, WO3 facilitates charge separation, and NiO assists in hole transfer, altogether providing a high-performance platform for the efficient photocatalytic degradation of TC under visible light irradiation.

4. Photocatalytic Studies

The photocatalytic degradation studies of tetracycline (TC) demonstrated notable variations in degradation efficiency among the different catalysts tested. Figure a presents the initial testing results of the pristine material. The degradation percentages for the various catalysts were as follows, Blank (no catalyst) showed 18%, g-C3N4 achieved 55%, NiO exhibited 38%, WO3 recorded 25%, and MXene 30%. The control experiment, referred to as Blank, indicated an 18% degradation efficiency of TC, suggesting that some degree of degradation occurred due to photolysis under visible light conditions. In Figure b, when g-C3N4 was used as the catalyst, the degradation efficiency improved to 42.2%, demonstrating the photocatalytic capability of g-C3N4 in degrading TC under visible light irradiation. The performance of MXene/g-C3N4/WO3/NiO nanomaterials with different stoichiometric ratios (labeled as MGWN 1 to MGWN 5) varied significantly, which showcased the impact of composition on photocatalytic activity. MGWN 1 exhibited a notably high degradation efficiency of 88.06%, indicating superior photocatalytic activity in the degradation of TC. The efficiency slightly decreased with MGWN 2 at 62.89% and MGWN 3 at 52.2%, suggesting that the specific stoichiometric ratios of these variants might be less optimal for TC degradation compared to MGWN 1. Remarkably, MGWN 4 achieved the highest degradation efficiency among all tested nanomaterials at 99.35%. This result suggests that the stoichiometric ratio and structure of MGWN 4 are highly conducive to the photocatalytic degradation of TC under visible light, possibly due to an optimal synergy between the constituents of the nanomaterial.

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(a, b) Photocatalytic degradation of TC by MGWN series; (c) variation of MGWN; (d) variation of TC; and (e) variation of aq. pH.

On the other hand, MGWN 5 showed a degradation efficiency of 69.3%, which, while lower than MGWN 4, still represents a substantial improvement over the blank and g-C3N4 counterparts. These results highlight the effectiveness of MXene/g-C3N4/WO3/NiO nanomaterial in degrading TC from aqueous solutions, with particular emphasis on the remarkably high efficiency of MGWN 4. This set of data underscores the potential of tailored nanomaterials in addressing persistent organic pollutants like antibiotics in environmental remediation applications.

4.1. Preliminary Studies

4.1.1. Variation of Catalyst

The efficiency of TC degradation using the MGWN 4 catalyst is significantly influenced by the amount of catalyst used (Figure c). Initially, employing 3 mg of the MGWN 4 catalyst resulted in a 51.27% degradation efficiency for tetracycline. Increasing the catalyst amount to 5 mg led to a notable improvement in efficiency, reaching 64.5%. This trend of increasing degradation efficiency with higher catalyst quantities persisted, with 7 mg of the catalyst achieving a 76.12% degradation rate. Upon increasing the catalyst quantity to 10 mg, a notable enhancement in efficiency was observed, resulting in a 97.07% degradation efficiency. This improvement is likely attributable to the presence of a larger number of active sites and increased surface area, enabling more effective interaction with the tetracycline molecules.

The degradation of tetracycline showed a notable improvement with the addition of more catalysts. Using 15 mg of the catalyst resulted in a 97.74% degradation rate, and this efficiency marginally increased to 98.06% when 20 mg of the catalyst was used. This marginal increase suggests that (15 and 20 mg) beyond a certain point, the addition of more catalyst does not proportionally enhance the degradation process, possibly because the reaction dynamics reach a point of saturation where most of the tetracycline molecules have been efficiently interacted with, and an additional catalyst does not significantly contribute to the reaction efficiency.

4.1.2. Variation of Concentration

The influence of varying concentrations of tetracycline on photocatalytic degradation under visible light irradiation was systematically investigated and shown in Figure d. The performance of the MGWN 4 nanomaterial in degrading tetracycline from the aqueous phase was assessed across different initial concentrations, ranging from 5 to 50 ppm. The results showcase a significant dependency of the photocatalytic efficiency on the initial antibiotic concentration. At a lower concentration of 5 ppm, the degradation efficiency was notably high, reaching 98.06%, suggesting an optimal interaction between the tetracycline molecules and the photocatalyst under visible light irradiation. When the concentration was doubled to 10 ppm, a slight dip in performance was observed, yielding a 97.41% degradation efficiency, which indicates a marginal impact of increased contaminant load on photocatalytic activity.

However, as the concentration further escalated to 15 ppm, a pronounced decrease in efficiency was observed, with only 59.98% of the TC being degraded. This trend continued for higher concentrations; at 20 ppm, the efficiency further decreased to 43.85%, and a significant drop was observed at 25 ppm, with the efficiency plummeting to 23.3%. When the TC concentration reached 50 ppm, the degradation efficiency hit a low of 20.68%, highlighting a substantial decline in photocatalytic performance at high contaminant levels. These results elucidate the critical influence of antibiotic concentration on the degradation process, revealing that higher concentrations of tetracycline pose a challenge to the photocatalytic system, possibly due to the saturation of active sites on the catalyst surface or the attenuation of visible light penetration through the solution.

4.1.3. Variation of pH

The influence of variations in aqueous pH on TC degradation using MGWN 4 nanomaterial significantly impacts photocatalytic activity (Figure e). The results indicate that at a very acidic pH of 1.2, the degradation efficiency was remarkably high at 99.35%, demonstrating nearly complete TC removal. As the pH increases, slight decreases in efficiency are noted, with degradation efficiencies of 98.7% at pH 2.21 and 97.74% at pH 3.3, which still shows the catalyst’s high effectiveness within this acidic range. In the range from slightly acidic to neutral, the results show subtle changes in efficiencies. At pH 4.02, the efficiency is 98.06%, and it slightly increases to 98.38% at pH 5. The efficiency matches the earlier level at pH 6.02, with 97.74%. As the pH becomes slightly alkaline at 7.1, the efficiency decreases to 95.48%, indicating reduced photocatalytic activity under neutral to alkaline conditions.

In the alkaline range, decreasing efficiency becomes more pronounced, with significant drops recorded at 86.12 to 67.4% (pH 8 to 11), which illustrates a substantial decrease in photocatalytic degradation of TC under strongly alkaline conditions. The MGWN 4 nanomaterial has been shown to have its peak photocatalytic performance in highly acidic environments, with a diminishing efficiency as the conditions move toward neutral and alkaline. The superior performance in acidic conditions is likely due to the increased generation of reactive species under acidic pH. On the other hand, the decline in alkaline conditions may result from a combination of factors, including reduced generation of reactive species and potential recombination of photogenerated electron–hole pairs. Hence, the neutral pH was fixed as an optimum condition for the photocatalytic degradation of TC.

4.2. Kinetics

The kinetic studies for the photocatalytic degradation of TC by MGWN 4 nanomaterial were systematically conducted under visible light irradiation at various initial concentrations (TC). The photocatalytic activity of MGWN 4 was evaluated over different periods, showing its efficiency in degrading TC from an aqueous solution, as shown in Figure a. The concentrations of TC examined were 5, 10, 15, and 20 ppm, with observation periods spanning up to 600 min. At an initial concentration of 5 ppm and 240 min of visible light irradiation, the degradation percentage of TC achieved was 99.35%. This result indicates that even at lower concentrations, MGWN 4 exhibits significant photocatalytic activity, initiating a rapid degradation process. For a concentration of 10 ppm with an extended period of 300 min, the degradation efficiency was observed to be 99.67%.

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(a) Kinetic studies of MGWN 4 at various TC concentrations; (b) reusability studies; and (c) scavenger analysis.

This demonstrates that MGWN 4 maintains its photocatalytic effectiveness, promoting TC degradation even as the concentration increases. With a further increase in the concentration of TC to 15 ppm and extending the irradiation time to 540 min, the degradation percentage noted was 98.70%. The sustained photocatalytic activity over longer periods underscores the stability and durability of MGWN 4 in degrading higher concentrations of TC. The highest concentration studied, 20 ppm over a time frame of 600 min, showed a degradation percentage of 98.22%. This outcome reveals that MGWN 4 is capable of handling higher pollutant loads, albeit with a slight reduction in efficiency, which is expected due to the proportional increase in TC concentration to catalyst active sites.

These kinetic study results elucidate the photocatalytic prowess of MGWN 4 under visible light for the degradation of TC across different concentrations and exposure times. Table shows the pseudo-first-order rate constants and reaction rates for the photocatalytic degradation of TC at different concentrations. The reaction kinetics, predominantly following a pseudo-first-order model (Figure S1), further corroborated the efficiency of MGWN 4 in the photodegradation process. The MGWN 4 nanomaterial proves to be a potent candidate for alleviating the concern of antibiotic persistence in water bodies.

1. Pseudo-First Order Rate Constants for the Photocatalytic Degradation of TC under Visible Light Irradiation for MGWN 4 Nanomaterial.

  visible light
concentration (ppm) rate constant min –1 R 2
5 1.55 × 10–2 0.9931
10 5.95 × 10–3 0.9946
15 6.31 × 10–3 0.9865
20 6.41 × 10–3 0.9812
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Zhang et al. investigate a CeO2–WO3 nanocomposite for the degradation of tetracycline, achieving a removal rate of 94.28% under optimal conditions (Table ). However, the study does not examine CeO2/MXene/gC3N4/WO3 composites and lacks a literature review on their antibiotic degradation capabilities. Akbari et al. explained that MXene-based ternary nanophoto composites were synthesized for the efficient removal of tetracycline from water, demonstrating a superior degradation efficiency of 98% under optimized conditions, which is attributed to improved light absorption and enhanced separation capabilities of photogenerated carriers. Chen et al. focus on a CeO2@WO3 nanocomposite for the degradation of cephalexin, rather than on CeO2/MXene/gC3N4/WO3. The study highlights the synthesis, optimization, and photocatalytic performance of the CeO2@WO3 heterojunction, achieving a degradation efficiency of 98.8% under visible light. Rokesh et al. examine hybrid photocatalysts, specifically CeO2/MXene/WO3 nanocomposites, emphasizing their impressive structural and interfacial characteristics. These features improve photoabsorbance and charge separation, resulting in the effective degradation of antibiotics in water through photocatalytic methods powered by solar energy. Suyana et al. focus on g-C3N4-based systems for photocatalytic antibiotic degradation, discussing heterostructures, doping, and porous structures. However, it does not specifically address the degradation of antibiotics using CeO2/MXene nanocomposites. Madona et al. examine a CeO2/MXene for the purpose of antibiotic degradation. The research particularly highlights a C-CeO2/g-C3N4 heterojunction, which accomplished an impressive 87.5% degradation of Amoxicillin when exposed to sunlight. This finding underscores the material’s photocatalytic efficiency and its effective bactericidal properties against various pathogens. Pushpa et al. observed a significant degradation of 92% for Cefixime over five consecutive runs. This degradation occurred under the most favorable conditions, which included a pH of 6, a photocatalyst concentration of 0.30 g/L, and a 10% Sm2O3 content in the nanocomposites.

2. A Comparison of the Photocatalytic Efficiency of the Prepared MGWN with the Reported Literature.

s. no material light source target pollutant degradation percentage refs
1 CeO2–WO3 visible light tetracycline 94.28
2 Fe2O3–SiO2/MXene visible light tetracycline 98
3 CeO2@WO3 visible light cephalexin 98.8
4 CeO2/MXene/WO3 xenon lamp tetracycline 83
5 gC3N4 vis-sun light tetracycline, amoxicillin 80.5
6 CeO2/MXene sunlight amoxicillin 87.5
7 Sm2O3/MXene/g-C3N4 visible light cefixime 92
8 MGWN 4 visible light tetracycline 99.5 present work
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4.3. Reusability Studies

The studies on the reusability and stability of photocatalytic degradation of tetracycline (TC) are essential for assessing the practical application of the catalyst over multiple cycles. The results indicate a gradual decrease in degradation efficiency over six consecutive cycles (see Figure b), beginning with a high of 99.35% in the first cycle. Although there is a gradual decrease in performance, the catalyst remains highly efficient, with the following degradation efficiencies recorded: 96.74% in the second cycle, 90.3% in the third cycle, 87.1% in the fourth cycle, a slight decline to 85.7% in the fifth cycle, and finally reaching 83.9% in the sixth cycle. During each degradation cycle (from the second to the sixth), the degradation percentage approaches approximately 99% with increased irradiation time. These results indicate that, despite the reduction in efficiency over time, the catalyst retains a significant portion of its initial activity, underscoring its durability and potential for repeated use in the photodegradation of TC.

4.4. Scavenger Analysis

To clarify the crucial active agent involved in the photocatalytic degradation of antibiotics using MGWN (Figure c), radical scavenging experiments were performed. In these studies, a different scavenger was added to the media, namely blank (without scavenger, 99.35%) degradation, EDTA (electron/hole scavenger, 80.4%) degradation, BQ (superoxide anion scavenger, 86.5%) degradation, and IPA (hydroxyl scavenger, 17.4%) degradation. However, it can be seen from these studies that, due to the addition of IPA, the efficiency fell drastically to 17.4%, which is a strong indication that hydroxyl radicals (−OH) were the primary active agent in the photocatalytic degradation mechanism of the MGWN system. This shows that the addition of BQ resulted in a minor loss of efficiency to 86.5%, implying that the superoxide anion radical was a minor constituent, whereas the addition of EDTA resulted in a loss of efficiency to 80.4%, implying that both electrons and hole pairs make a minor contribution to the overall photocatalytic reaction mechanism, but to a lesser extent than −OH groups. These experimental results have definitively proven that the leading degradation pathway is the −OH radical-driven process, which is very likely produced by the oxidation of surface-adsorbed water molecules and hydroxide ions by the photogenerated holes at the heterojunction interface in the composite, which is collectively promoted by the multicomponent structure of the resulting MGWN nanocomposite.

5. Conclusions

The study on the photocatalytic degradation of tetracycline (TC) using the MGWN nanomaterial under visible light irradiation demonstrates its significant potential for environmental remediation, particularly in removing antibiotics from water. The MXene/g-C3N4/WO3/NiO (MGWN) nanomaterial was synthesized using a simple hydrothermal technique. Various analytical methods, including FT-IR, XRD, UV-DRS, FE-SEM, HR-TEM, EDAX, and AFM, were employed to characterize the material. The results revealed that MGWN has a textured surface, with particle sizes ranging from 10 to 35 nm. XRD analysis confirmed its crystalline structure, and the band gap of MGWN was measured at 2.84 eV. Composed of Ti3C2, g-C3N4, WO3, and NiO, this nanomaterial exhibits a synergistic effect that enhances the photocatalytic process. This synergy facilitates efficient electron transfer, charge separation, and the generation of reactive oxygen species, leading to the effective degradation of TC into nontoxic byproducts. Experimental results indicated that degradation efficiency varies with the stoichiometric ratio of the components, with MGWN 4 achieving the highest efficiency at 99.35%. Kinetic studies further supported these findings, showing the effective degradation of TC by the MGWN 4 nanomaterial across various concentrations and time frames, with notable efficiency even at lower concentrations after 240 min of irradiation. These results highlight the importance of component ratios and material structure in maximizing photocatalytic activity. Overall, the MGWN nanomaterial presents a promising solution for the photocatalytic degradation of persistent organic pollutants in aquatic environments.

Supplementary Material

pc5c00203_si_001.pdf (213.8KB, pdf)

Acknowledgments

The authors gratefully acknowledge VMRF – AVIT for providing infrastructure and lab facilities. The authors would also like to thank Dr. S.A.V. Satyamurthy, Director Research, Vinayaka Mission’s Research Foundation for his valuable support.

Data will be made available on request.

The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/prechem.5c00203.

  • Detailed descriptions of the materials and methods, visible photoreactor, and procedures for photocatalytic degradation (PDF)

S.J.G.A.: Investigation, methodology, supervision, writing – original draft. R.A.K.S.: Data curation, software, validation, writing – review and editing. V.M.D.: Data curation, software, writing – review and editing. V.L.N.: Writing – review and editing. M.N.U.: Data curation, formal analysis.

The authors declare no competing financial interest.

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Associated Data

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Supplementary Materials

pc5c00203_si_001.pdf (213.8KB, pdf)

Data Availability Statement

Data will be made available on request.

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