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Phyto-mediated synthesis of ZnO nanoparticles and their sunlight-driven photocatalytic degradation of cationic and anionic dyes

  • Naaser A. Y. Abduh , Abdullah Al-Kahtani and Abdel-Basit Al-Odayni EMAIL logo
Published/Copyright: October 9, 2024
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Open Chemistry
From the journal Open Chemistry Volume 22 Issue 1

Abstract

In this study, zinc oxide-based nanocatalysts were biosynthesized using Ocimum basilicum (OB) and Olea africana (OA) leaf aqueous extracts, termed OB-ZnO and OA-ZnO, as a simple, affordable, and environmentally friendly approach. Their characteristics and efficacy in photodegrading cationic dyes (crystal violet and methylene blue) and anionic dyes (methyl orange and naphthol blue black) were investigated. The catalyst’s properties were analyzed using various techniques, including Fourier transform infrared, X-ray diffraction, photoluminescence, thermogravimetric analysis, UV-Vis, transmission electron microscopy, energy-dispersive X-ray spectroscopy, and Brunauer–Emmett–Teller. Analysis revealed pure products having a hexagonal wurtzite structure, crystallite sizes of 15.04 and 21.46 nm, surface areas of 23.65 and 7.97 m2/g, particle sizes of 35 and 170 nm with spherical (uniform) and oval-like (non-uniform) shapes, and optical bandgaps of 3.15 and 3.05 eV, respectively. Photocatalytic applications under sunlight indicated excellent activity of both catalysts against targeted cationic and anionic dyes. Most notably, even though OA-ZnO has a lower surface area than OB-ZnO, it demonstrated greater efficiency. The variation in effectiveness is explained by the lower bandgap value of OA-ZnO and its ability to reduce electron–hole recombination due to its larger crystal size, which accelerates the degradation process. Additionally, both catalysts exhibited high stability after being used four times.

Keywords: biosynthesis; Ocimum basilicum extract; Olea africana extract; organic dyes; photodegradation; zinc oxide

1 Introduction

Water pollution caused by humans impacts present-day life and future generations, especially considering the recent increase in these pollutants brought on by waste from various industries [1]. Indeed, dyes are known to be among the worst water pollutants due to their widespread use in various industries, such as clothing, accessories, furniture, and plastics [2]. The textile industry is the major contributor to the contamination of natural water resources by discharging its dye-bearing waste directly into surrounding water bodies [3]. Dyes in wastewater can inhibit various processes, including normal physiological activity and photosynthesis in various aquatic plants and animals [4]. Thus, there was a strong desire among the scientific, environmental, and public health communities to tackle pollution and mitigate its effects. Several physical, chemical, and biological methods have been used to remove these pollutants, such as chlorination, reverse osmosis, adsorption, and electrochemical decomposition [5]. However, most of these methods are expensive, require multiple steps, introduce secondary pollutants, or are tedious [6]. More recently, advanced oxidation processes, such as ozonation, radiolysis, sonolysis, photocatalysis, Fenton chemistry, electrochemical oxidation, and wet air oxidation, have emerged as one of the most suitable strategies for water treatment because they are safer and have fewer limitations [7,8]. Among these, photocatalysis has attracted researchers due to its cost-effectiveness, simplicity, environmental friendliness, and its capability to completely eliminate target pollutants.

Photocatalysis using heterogeneous catalysts is a promising methodology and is highly recommended for treating wastewater to eliminate organic contaminants that cannot be removed by conventional methods due to their high chemical stability and limited biodegradability [9]. There are several metal oxide photocatalysts reported in the literature, such as TiO2, ZnO, SnO2, CeO2, MnO2, and Fe2O3 [10]. In addition, doped and mixed oxides were also synthesized and utilized [11]. For the photolysis process to be successful, a preferred photocatalyst must be selected based on its efficiency, economic viability, and environmental impact.

ZnO is a direct wide-bandgap semiconductor with a bandgap of 3.37 eV and an exciton binding energy of 60 meV. It has gained a lot of interest as a photocatalyst due to its high electron mobility, non-toxicity, photosensitivity, cost-effectiveness, ease of synthesis, and excellent stability [12]. ZnO NPs contain numerous active sites on their surface, allowing for the formation of numerous radicals [13,14,15]. This property makes them suitable for purification and disinfection applications. Furthermore, due to their peculiar physical and chemical properties, they have also been extensively used in applications related to the optical, chemical, sensing, and electrotechnology industries. Hence, various physical, chemical, and biological methods have been applied for the production of ZnO NPs of various sizes and shapes [16]. Chemical methods typically involve precipitation, sol–gel technology, solvothermal, hydrothermal, microwave techniques, and others [17]. Physical methods combine arc plasma, thermal evaporation, physical vapor deposition, ultrasonic, and laser ablation [18]. These approaches are quite costly and involve harmful chemicals that endanger humans and the environment [19]. Moreover, the use of harsh conditions, such as extended reaction times, high temperatures, and pressures, as well as the incorporation of catalysts during the preparation process, may lead to impure nanoproducts [20]. On the contrary, the biosynthetic route using plant extracts is a green, harmless, biocompatible, and environmentally sustainable method [21].

Although the specific plant-based extract composition varies based on factors like plant type, growing conditions, part used, and extraction method, aqueous extracts are generally known to be lower in volatile compounds compared to their alcoholic counterparts. Ocimum basilicum (OB), commonly known as sweet basil, is a fragrant medicinal plant that is mostly used in traditional medicine [22] and as an ornamental plant. The leaf aqueous extract is rich in polyphenols like flavonoids, rosmarinic acid, luteolin, tannins, terpenoids, and glycosides [23]. Olea africana (OA) (Arabic name: zaitoon barri) has been reported to have antimalarial and antibacterial activities [24]. The aqueous extract of OA leaves contains flavonoids, biophenols, glycosides, steroids, and tannins [25]. These phytocompounds can potentially be used as reducing and stabilizing agents for NP production. The synthesis of ZnO NPs using plant extracts has sparked a lot of interest in nanotechnology. Plant parts, such as fruits, seeds, leaves, stems, and roots, have been used to manufacture various NPs due to the diverse phytochemicals present in their extracts, which act as stabilizing and reducing agents [26]. Hence, as the extracted chemicals vary depending on the source and the method of extraction, several NPs of various shapes, sizes, and optical properties can be synthesized [27,28,29].

To the best of our knowledge, no studies have utilized OA leaf aqueous extract for the bio-based synthesis of ZnO or compared its catalytic activity with that of an OB-induced ZnO nanocatalyst for the photodegradation of organic dye pollutants. In this study, ZnO-based nanocatalysts were biosynthesized using OB and OA aqueous extracts as an affordable and environmentally friendly approach. The synthesized catalysts were characterized for their structural, optical, and morphological properties using various techniques, including Fourier transform infrared (FTIR), X-ray diffraction (XRD), UV-Vis, transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), Brunauer–Emmett–Teller (BET), photoluminescence (PL), and thermogravimetric analysis (TGA). The photocatalytic activity of the synthesized photocatalysts was investigated against both cationic (crystal violet [CV] and methylene blue [MB]) and anionic (methyl orange [MO] and naphthol blue black [NBB]) dyes under sunlight.

2 Materials and methods

2.1 Materials

Leaves of OB and OA were collected from the Asir region, a province in the southern part of the Kingdom of Saudi Arabia. The following chemicals were utilized as supplied: MO from British Drug Houses Ltd (BDH) Chemicals Ltd. (Pool, England, UK); MB (95%), CV (≥90%), zinc nitrate hexahydrate (Zn(NO3)2·6H2O; 98%), and ammonium hydroxide (NH4OH; 25% in water) from Sigma-Aldrich (St. Louis, MO, USA); NBB from Riedel-de Haën (Seelze, Germany).

2.2 Preparation of aqueous leaf extract

The fresh leaves of OB and OA were sequentially washed with tap and deionized water and then allowed to dry for 3 weeks in the shade. To extract the water-soluble components, 10 g of the dry leaves were chopped into small pieces and immersed in 100 mL of deionized water. The mixture was then heated with stirring for 30 min at 50°C. After cooling, the aqueous leaf extract was filtered through Grade 4 Whatman filter paper and stored in a refrigerator (4–8°C) for later use [30,31].

2.3 Synthesis of ZnO catalysts

The photocatalysts were synthesized as follows: 5 g (0.017 mol) of Zn(NO3)2·6H2O was dissolved in 30 mL of OB- or OA-extract and heated at 75°C with stirring for 2 h. Then, drops of NH4OH (2 M) were added, and the resulting solution was heated for an additional 3 h. To minimize evaporation, the flask containing the mixture was loosely sealed with a glass sheet. After cooling, the resulting precipitate was filtered, washed thoroughly with a 33% ethanol-aqueous solution, and dried in a closed oven overnight at 80°C. The synthesized materials were calcined at 550°C under atmospheric pressure in an air environment, using a heating rate of 20°C/min for 3 h. After cooling (−20°C/min), the materials were stored in sealed vials for subsequent experiments. Under similar conditions, a reference ZnO catalyst was synthesized using deionized water in place of the plant extract (dw-ZnO) for activity comparison.

2.4 Photocatalytic experiments

The photocatalytic performance of the synthesized OB-ZnO, OA-ZnO, and dw-ZnO catalysts in the degradation of selected cationic (CV and MB) and anionic (MO and NBB) dyes was tested under sunlight (intensity = 835 W/m2) and atmospheric pressure on clear days in October with an average outdoor temperature of 40°C in Riyadh city, Saudi Arabia (24.7136° N, 46.6753° E). Basically, 10 mg of the obtained catalyst (OB-ZnO, OA-ZnO, and dw-ZnO) was added to 10 mL of the examined dye solution (10 mg/L). Before being exposed to sunlight, the suspension was magnetically stirred for 30 min in the dark to achieve an adsorption–desorption equilibrium. To ensure the effectiveness of the catalyst, a blank sample (without a catalyst) was treated in the same manner as the catalytic reaction system. At given time intervals, the mixture was centrifuged for 5 min at 5,000 rpm, and the clear solution was collected for UV-Vis spectrophotometric absorption analysis. The photodegradation efficiency (DE%) was assessed using equation (1):

(1) DE ( % ) = A 0 − A t A 0 100 ,

where A 0 and A t are the dye concentrations (mg/L) at initial and at time t of irradiation, respectively.

The reusability of the photocatalysts was tested over the course of four catalysis–recovery–reuse cycles. After each catalytic reaction cycle, the catalyst was recovered through centrifugation, washed three times with an acetone/ethanol mixture, dried overnight at 80°C, and then used for the subsequent cycle.

2.5 Characterization

The synthesized OB-ZnO and OA-ZnO NPs were characterized for their structures, morphologies, optical characteristics, compositions, and thermal stabilities using various techniques. The FTIR spectra were recorded using a KBr method in a Perkin Elmer BX spectrometer (Perkin Elmer, Waltham, MA, USA) from 400 to 4,000 cm−1. The XRD patterns were obtained using a Rigaku XtaLAB mini II benchtop X-ray 110 crystallography machine (The Woodlands, TX, USA) with a Cu Kα radiation (λ = 1.5418 Å), over a 2θ range of 10° to 80°, and a scanning rate of 3°/min. The optical properties were analyzed using a Shimadzu UV-2600 spectrophotometer. The TEM images were captured using a JEM-2100F field emission electron microscope (JEOL Ltd., Tokyo, Japan), operating at an 80 kV acceleration voltage. To achieve this, a drop of diluted nanocatalyst suspension in ethanol was deposited onto a lacey-carbon copper grid, dried, and then scanned. The surface area and pore characteristics were analyzed based on N2 adsorption–desorption isotherms recorded using a Micromeritics Tristar II 3020 (Micromeritics Instrument Corporation, GA, USA), following BET and BJH (Barrett–Joyner–Halenda) calculation methods. The elemental analysis of the target catalysts was confirmed using EDS (X-ray spectrometry) with an X-MaxN system (Oxford Instruments, Abingdon, UK). Thermal analysis was conducted using a Mettler Toledo TGA/DSC Star system (Columbus, OH, USA), performed in the temperature range of 25–700°C with a heating rate of 10°C/min under N2 gas.

3 Results and discussion

3.1 Synthesis approach

The properties of the synthesized nanophotocatalysts are primarily influenced by the synthesis protocol employed. Phyto-mediated synthesis of NPs offers a green, cost-effective, and straightforward approach. Consequently, the morphological, physical, and chemical properties of the biosynthesized material can be optimized by varying several factors affecting their final properties, including the reaction medium, conditions, and processing techniques. To evaluate the effect of the medium on the structural properties and catalytic activities of the ZnO nanocatalyst, two aqueous extracts (OB extract [OBE] and OS extract [OAE]) were prepared and utilized for the biosynthesis of ZnO. For comparative purposes, ZnO was also synthesized in an extract-free aqueous medium. During the extraction process [30,31], fresh leaves were thoroughly washed with water to remove dust and minimize microbial contamination. To achieve complete drying while preserving phytochemical integrity, the cleaned leaves were shade-dried at ambient temperature for 3 weeks. In this case, phytocompound transformation and degradation reported under certain storage conditions [32] can be avoided. The catalysts were prepared by heating 30 mL of 0.56 M Zn2+ in OBE, OAE, or deionized water for 2 h. To induce particle formation, the medium was alkalized by adding drops of NH4OH. Figure 1 illustrates a tentative mechanism for the biosynthesis of ZnO NPs facilitated by plant-based phytocompounds (with condensed tannins [CT] representing these compounds; such phytocompounds can function as mono-, bi-, or multidentate) derived from OB and OA.

Figure 1 Schematic illustration for the proposed mechanism of biosynthesis of ZnO nanophotocatalysts.
Figure 1

Schematic illustration for the proposed mechanism of biosynthesis of ZnO nanophotocatalysts.

The aqueous extracts of OB and OA leaves are rich in polyphenols, flavonoids, terpenoids, and tannins [23,25], which play a vital role in the synthesis of nanosized particles through complexation with metal ions. This intermediate step reduces aggregation and fosters the formation of smaller, nanosized particles. The resulting complexes (CT n @Zn(H2O) m /CT n @Zn(OH) m /CTn@Zn(OH) m x−, where n, m, and x are tentative numbers for simplicity) (Figure 1) may undergo decomplexation in basic media, leading to the precipitation of particles, typically in the form of M(OH) n . This process further facilitates the development of the desired nanostructures. To obtain the ready-to-use ZnO-based photocatalysts, the precipitates were subsequently subjected to calcination under air conditions at 550°C for 3 h. This calcination process ensured the production of pure materials by decomposing the zinc hydroxide and tracing extract-derived organic compounds into small, volatile fragments, such as organic gases, CO2, and H2O. The calcination temperature is one prominent influencer on the end properties of the photocatalyst [33]. For instance, Sharma et al. [34] have reported that the energy bandgap decreases with increasing calcination temperature from 400 to 600°C, likely due to an increase in the crystallite size. However, a study by Golsheikh et al. [35] reported better optical properties between 500 and 600°C. Accordingly, the calcination temperature in this work was carried out at 550°C, which was selected by different researchers [36,37].

3.2 Characterization

3.2.1 FTIR spectroscopy

Plant extracts generally contain a large number of phytochemicals, such as polyphenols, flavonoids, antibiotics, glycosides, antioxidants, and organic aggregates, which act as reducing and stabilizing agents in NP preparations [38]. Figure 2 shows the FTIR spectra of OB and OA extracts, as well as the corresponding synthesized OB-ZnO and OA-ZnO photocatalysts. As can be seen, the spectra of plant extracts show the presence of different organic functional groups. Hence, the peaks around 3,400 cm−1 were assigned to water, O–H, and N–H stretching vibrations, peaks in the range of 3,000–2,770 cm−1 to aliphatic C–H bonds, and strong peaks centered at 1,616 cm−1 (OB spectrum) and 1,625 cm−1 (OA spectrum) correspond to C═O/C═C stretching and N–H bending vibrational modes. According to the literature [39,40], OB leaf aqueous extract contains plenty of bioactive compounds, of which linalool, eugenol, methyl chavicol, and flavonoids are prominent. These compounds are characterized by alcoholic and phenolic OH and C═C bonds. Besides, the peaks for N–H may confirm the presence of amino acids [41]. Additionally, the peaks around 1,416, 1,080, and 600 cm−1 were assigned to C–C stretching, C–O stretching, and C–H bending of, e.g., terpenoids like linalool. The spectra of OB–ZnO and OA-ZnO catalysts contain the characteristic peaks of an adequately pure ZnO structure. Hence, the peaks at 3,420 and 1,630 cm−1 correspond to Zn–OH and adsorbed water stretching and bending vibrations, respectively. The Zn–O absorption band is clear at 424 and 436 cm−1 for OB-ZnO and OA-ZnO [42], respectively; the results are consistent with previous reports [43,44].

Figure 2 FTIR spectra of OB, OA, OB-ZnO, and OA-ZnO.
Figure 2

FTIR spectra of OB, OA, OB-ZnO, and OA-ZnO.

3.2.2 XRD analysis

Figure 3 displays the characteristic XRD diffraction peaks of the investigated catalysts, OB-ZnO, OA-ZnO, and dw-ZnO. The patterns exhibit the Bragg diffractions near 31.75°, 34.44°, 36.25°, 47.55°, 56.62°, 62.87°, 66.41°, 67.91°, 69.15°, 72.62°, and 77.03°, corresponding to planes 100, 002, 101, 102, 110, 103, 200, 112, 201, 004, and 202, confirming the hexagonal wurtzite structure of ZnO and matching the conventional data (JCPDS card no. 010800075) and reported results [45,46]. As can be seen, no shifts in the peak positions or new diffractions can be detected, confirming pure structures. Furthermore, the grain size can be calculated using the Scherrer equation, as follows (equation (2)):

(2) D = K λ β cos θ ,

where D is the average grain size, β is the full width at half-maximum (FWHM), K is a constant, and λ is the wavelength of the incidence X-ray (1.5406 nm).

Figure 3 XRD patterns of ZnO (JCPDS No. 0010800075), OB-ZnO, OA-ZnO, and dw-ZnO.
Figure 3

XRD patterns of ZnO (JCPDS No. 0010800075), OB-ZnO, OA-ZnO, and dw-ZnO.

The crystallite sizes of OB-ZnO, OA-ZnO, and dw-ZnO were found to be 15.04, 21.46, and 25.58 nm, respectively. These findings underscore the potential of the plant extracts to influence the synthesis of smaller ZnO crystallites (OB-ZnO and OA-ZnO) compared to those produced in water (dw-ZnO). As illustrated in Figure 1, the aqueous extracts from the leaves of OB and OA are rich in polyphenols and flavonoids, including tannins, which effectively cap and stabilize metal ions through complex formation. This interaction facilitates the nucleation of crystallites and minimizes aggregation. Furthermore, it is well-established that the specific phytocompounds present in a plant extract can vary depending on the plant species and its part. Although phytocompounds from various plants may share similar functionalities – such as those found in polyphenols and flavonoids – their types and concentrations can differ markedly. This variability contributes to the differences in the sizes of synthesized ZnO nanoparticles [47]. Consequently, the phytocompounds derived from OB appear to inhibit ZnO crystal growth more effectively than those from OA, resulting in the formation of smaller crystallites.

3.2.3 TGA

Figure 4 depicts TGA curves for the as-synthesized catalysts, OB-ZnO and OA-ZnO. On the thermograms, three types of water molecules could be detected: adsorption, crystallization, and constitutional water, as further confirmed by FTIR analysis (see Section 3.2.1). The loss of absorbed and crystallized water occurred below 300°C [48,49], observed at derivative-TGA (deriv.-TGA) of 115 and 291°C in the OB–ZnO curve, and 160 and 293°C in the OA–ZnO curve, with a total mass loss of 1.2 and 1.0 wt%, respectively. Above 300°C, the thermograms show peaks for constitutional water – in which the protons attached to the outer oxygens of the polyanions – evaporation [50], i.e., at deriv.-TGA of 355 and 365°C. These results confirm the stability and purity of the as-synthesized catalysts.

Figure 4 TGA curves of (a) OB-ZnO and (b) OA-ZnO.
Figure 4

TGA curves of (a) OB-ZnO and (b) OA-ZnO.

3.2.4 Nitrogen adsorption–desorption isotherms

The quantity of adsorbed gas depends on both the adsorption conditions (the relative pressure (P/P 0) and temperature) and the morphology of the solid/gas interface [51]. The adsorption/desorption isotherm can be used to study the surface characteristics. The type of isotherm and desorption hysteresis can offer more information about the material surface, which is valuable for surface area and porosity analysis. The catalyst’s morphology typically affects its performance in the photodegradation of organic dyes. Hence, a higher surface area provides more active sites available for organic molecules to adsorb. Furthermore, the higher the number of active sites, the greater the harvested incident light and the better the rate of photodegradation [52]. As shown in Figure 5, OB-ZnO and OA-ZnO catalysts exhibit type IV isotherms. Moreover, the desorption curves indicated type H4 hysteresis loops, as classified by the IUPAC [53]. As can be seen in Table 1, the calculated BET-specific surface area is higher for the OB-ZnO (23.65 m2/g) than for the OA-ZnO (7.97 m2/g) NPs; the surface area decreases as crystallite size increases, a result supported by TEM and XRD results.

Figure 5 Nitrogen adsorption–desorption isotherms of (a) OB-ZnO and (b) OA-ZnO.
Figure 5

Nitrogen adsorption–desorption isotherms of (a) OB-ZnO and (b) OA-ZnO.

Table 1

BET-surface areas, pore volumes, and pore diameters of OB-ZnO and OA-ZnO

Catalyst Specific surface area (m²/g) Pore volume (cm³/g) Pore size (nm) Crystallite size (XRD; nm) Particle size (TEM; nm) Optical bandgap (eV)
OB-ZnO 23.65 0.248 2.75 15.04 35 3.15
OA-ZnO 7.97 0.021 12.06 21.46 170 3.05

3.2.5 TEM analysis

Figure 6 shows the TEM micrographs of the biosynthesized OB-ZnO and OA-ZnO catalysts. As can be seen, the OB-ZnO NPs are regular, mostly spherical in shape, while the OA-ZnO particles are more irregular and tend to be longer on one side than the other, resulting in oval- and rod-like shapes. Moreover, the particle size of the OB-ZnO catalyst (average 35 nm) is evidently smaller than that of the OA-ZnO (about 170 nm), which definitely reflects the impact of the extract type on the final properties of the NPs, such as their morphology and, subsequently, their catalytic performance. These results are consistent with the XRD data and demonstrate the ability of the OB extract to inhibit crystal growth more effectively than the OA extract [54]. The particle size determined using XRD is smaller than that measured by an electron microscope (e.g., TEM) due to, on the one hand, the aggregation events observed using the microscope and, on the other hand, reasons related to the Scherer formula, which was originally developed for cubic structures and deviated when applied to other structures [55].

Figure 6 TEM images of (a) OB-ZnO and (b) OA-ZnO.
Figure 6

TEM images of (a) OB-ZnO and (b) OA-ZnO.

3.2.6 Optical analysis

The electronic structure of the photocatalyst has a substantial impact on its performance [56], which is generally enhanced by reducing the bandgap. Hence, to compute the optical bandgap of the synthesized ZnO NPs, equation (3) was used:

(3) ( α h ν ) n = A ( h v − E g ) ,

where α is the absorption coefficient, h is Planck’s constant, ν is the photon frequency, A is a photonic energy-independent constant, hν is the photon energy, E g is the optical bandgap, and n is the semiconductor charge transition (n = 2 or 0.5 for direct and indirect transitions, respectively).

A plot of (αhν)2 vs hν is displayed in Figure 7, and tangential lines intercepting the abscissa were used to assess the bandgap. Accordingly, the E g values of OB-ZnO and OA-ZnO were determined to be 3.15 and 3.05 eV, respectively. Such a finding is a classic example of the quantum size effect, where the bandgap energy increases with a decrease in the crystallite size [57]. When particle size decreases, the bandgap widens as electrons and holes are closer together, causing higher kinetic energy due to Coulombic interactions between them [58].

Figure 7 UV-Vis Tauc’s plot and (inset) UV-Vis absorption spectra of OB-ZnO and OA-ZnO.
Figure 7

UV-Vis Tauc’s plot and (inset) UV-Vis absorption spectra of OB-ZnO and OA-ZnO.

3.2.7 EDS analysis

An EDS test was carried out to determine the elemental composition of the synthesized nanocatalysts, OB-ZnO and OA-ZnO. The EDX spectra, shown in Figure 8, confirm the purity of the produced NPs, as no impurity peaks were detected. Within the accuracy tolerance of the EDS method, the spectra showed a very close Zn-to-O ratio (atomic difference <4.5%) to that theoretically expected, supporting the nominal structures.

Figure 8 EDS spectra of OB-ZnO and OA-ZnO.
Figure 8

EDS spectra of OB-ZnO and OA-ZnO.

3.2.8 PL analysis

PL enables the investigation of the electronic structure and optical properties of semiconductor materials by providing information on surface oxygen vacancies defects, as well as the separation and recombination of photoinduced charge carriers. The intensity of the PL peak is directly related to the rate of electron–hole recombination, i.e., a fast recombination rate results in an intense peak, while a low rate recombination rate (indicating better charge separation) leads to a broader emission peak [59]. The PL spectra shown in Figure 9 demonstrate multi-emission peaks in the range of 350–500 nm. Hence, three emission peaks are more prominent and centered at 406 and 467 nm (blue bands) and 488 nm (green bands). The blue bands in the UV region are assigned to the near band edge, originating from the direct recombination of free excitons through an exciton–exciton collision process [60]. The green band can be attributed to the charge carrier transitions, e.g., between the oxygen vacancy and interstitial oxygen [61,62]. Despite both spectra having a similar emission pattern, the intensity of the emission peaks of OB-ZnO is higher than that of the OA-ZnO nanocatalyst, which is consistent with the literature [63].

Figure 9 PL spectra of OB-ZnO and OA-ZnO.
Figure 9

PL spectra of OB-ZnO and OA-ZnO.

3.2.9 Photocatalytic activity of ZnO NPs

The as-synthesized OB-ZnO and OA-ZnO nanocatalysts were evaluated for their photocatalytic activity against cationic dyes (CV, MB) and anionic dyes (MO, NBB) under sunlight irradiation. The photodegradation efficiency of OB-ZnO and OA-ZnO was compared to that of blank (no catalyst) and control (dw-ZnO) samples, as shown in Figure 10. Hence, throughout the degradation period under catalyst-free conditions, a negligible quantity (∼3%) of the test dyes was degraded, suggesting the high stability of organic dyes (under experimental conditions). Furthermore, dw-ZnO-catalyzed photodegradation of CV, MB, MO, and NBB was insufficient, reaching only 32, 46, 22 and 28%, respectively. Generally, the efficiency of dye degradation under sunlight increases with the contact time. However, the photocatalytic activity of OA-ZnO is higher than that of OB-ZnO, reflecting the influence of the source type of the phytocompounds used for NP production.

Figure 10 Degradation profile of CV, MB, MO, and NBB under sunlight irradiation in the absence of catalyst (blank) and the presence of OB-ZnO, OA-ZnO, and dw-ZnO photocatalysts.
Figure 10

Degradation profile of CV, MB, MO, and NBB under sunlight irradiation in the absence of catalyst (blank) and the presence of OB-ZnO, OA-ZnO, and dw-ZnO photocatalysts.

Typically, several factors affect the photocatalytic performance of ZnO, such as the crystallite size, bandgap, carrier recombination, surface area, photon absorption, and the concentration of defects [64]. By closely investigating the degradation profiles, it was noticeable that the amount adsorbed in the first 30 min (conducted in the dark) was significantly greater in the case of OB-ZnO compared to OA-ZnO. In addition, the adsorption of cationic dyes (CV and MB) was found to be higher than that of anionic ones (MO and NBB), possibly due to the abundance of negatively charged active sites on the catalyst surface. Moreover, the detected variation is consistent with the BET data, which suggests a higher surface area of OB-ZnO compared to OA-ZnO, consequently providing more opportunities for dye adsorption. Bandgap and PL analysis also revealed favorable optical properties for the OA-ZnO catalyst over the OB-ZnO catalyst. However, it is reported that the position of the conduction band (CB) and valence band (VB) affects the photocatalytic activity more than the surface area [65]. Moreover, the photocatalytic activity is evidently enhanced for larger crystal sizes. The larger the semiconductor crystal surface, the longer the lifetime of the carrier movement and the lesser the electron–hole recombination [66]. Herein, even though the surface area of the OA-ZnO catalyst is smaller, its improved photocatalytic performance depends on its bandgap, recombination rate, and grain size values, as previously observed [67]. More importantly, the as-synthesized OB-ZnO and OA-ZnO nanocatalysts can be applied for the photodegradation of both cationic and anionic dyes with outstanding efficiency. This demonstrates their utility for colorant removal and water treatment. In general, morphology-controlled ZnO NPs can be obtained by using plant extract-based phytochemicals as reducing and stabilizing agents. Hence, the size, shape, and optical characteristics of ZnO NPs, as well as their photocatalytic activity, are significantly influenced by the source of phytocompounds [68].

As shown in Figure 10, complete photodegradation of the tested dyes in the presence of plant-based ZnO was achieved between 50 and 90 min. The catalytic performance of OA-ZnO is higher than that of OB-ZnO, with nearly 100% degradation efficiency at about 80, 60, 60, and 50 min for OA-ZnO, in contrast to 100, 90, 80, and 60 min for OB-ZnO against CV, MB, MO, and NBB, respectively. Furthermore, the degradation rates of the dyes followed the order of anionic (NBB > MO) > cationic (MB > CV) dyes. Notably, the observed higher degradation rates for the anionic dyes (MO and NBB) relative to their cationic counterparts (CV and MB) can be attributed to their differing acid–base behaviors in solution. Anionic dyes, such as MO and NBB, function as weak acids when dissolved in water [69], releasing H+ ions and consequently lowering the pH more than the cationic dyes (CV and MB). This reduction in pH negatively impacts the generation of hydroxyl radicals (˙OH), which are crucial for the photodegradation process. Therefore, the lesser photodegradation observed for the cationic dyes compared to the anionic ones may be related to this mechanism [70].

Figure 11 illustrates a proposed photocatalytic degradation mechanism of the investigated organic dyes, CV, MB, MO, and NBB, using ZnO nanophotocatalysts. When ZnO is irradiated with photonic energy equal to or higher than its bandgap, the electrons absorb the light energy and photoexcite from the VB to the CB, thereby generating electron–hole pairs (e−/h+). The e−/h+ pairs transfer to the ZnO surface and are involved in redox reactions. Basically, the photodegradation depends on the photocatalyst’s ability to inhibit recombination of the excitons so that they can transit alternatively to produce reactive oxygen species (ROS). As can be seen, the conduction band electrons (e−) react with dissolved oxygen species (O2) to produce superoxide radical ions (˙O2 −) and then hydrogen peroxide (H2O2), which is able to either initiate dye degradation or further react with water (H2O) to produce hydroxyl radicals (˙OH). On the other hand, h+ can react with water or hydroxyl ions (OH−) to produce hydroxyl radicals. These radicals are critical in the degradation reaction toward water treatment. They react with the adsorbed dyes on the ZnO surface to form intermediate compounds that can degrade to green compounds such as carbon dioxide (CO2), H2O, and inorganic compounds [71]. The wide bandgap of ZnO (3.37 eV, corresponding to a wavelength of 368 nm in the UV region), limits its potential use under sunlight irradiation, as only approximately 5% of the solar light can excite ZnO electrons. This low excitation efficiency inadequately inhibits the recombination rate of the generated electron–hole pairs (e⁻/h⁺). Consequently, enhancing the photocatalytic activity of ZnO requires strategies to broaden its light absorption into the visible region, improve carrier mobility, and increase charge separation. In this study, the observed differences in performance between OB-ZnO and OA-ZnO can be attributed to their distinct properties, which arise from the biosynthesis methods employed, specifically the use of different plant extract sources.

Figure 11 Schematic diagram of the possible mechanism for the photocatalytic degradation of organic dyes on ZnO NPs.
Figure 11

Schematic diagram of the possible mechanism for the photocatalytic degradation of organic dyes on ZnO NPs.

3.2.10 Reusability

The recovery and reusability of the test catalysts were analyzed for four cycles. The reusability of the catalyst is a crucial factor in evaluating its applicability in real applications; thus, the catalyst’s integrity after multiple cycles is essential for its continued use in practical applications. To minimize waste generation and production costs, the catalyst needs to be easily extracted and recycled after the catalytic reaction. Therefore, recycling studies were conducted under similar conditions to the initial photocatalytic experiment. The data acquired from the four cycles are summarized in Table 2, which supports a highly stable catalyst with no significant activity loss for up to four cycles. The decrease in activity after four cycles (lost activity (%), the variance in photodegradation efficiency between the first and fourth cycles) of OB-ZnO nanocatalyst reuse against CV, MB, MO, and NBB was found to be 4.20, 5.85, 4.92, and 7.53%, compared to that of OA-ZnO (4.10, 6.12, 5.52, and 6.15, respectively).

Table 2

Recycling efficiency of OB-ZnO and OA-ZnO in the degradation of CV, MB, MO, and NBB under sunlight irradiation

Catalyst Dye Cycle 1 Cycle 2 Cycle 3 Cycle 4 Lost activity (%)
OB-ZnO CV 95.35 94.04 93.50 91.25 4.20
MB 98.29 96.35 95.23 92.54 5.85
MO 94.91 93.58 91.23 90.24 4.92
NBB 98.30 95.10 94.40 90.89 7.53
OA-ZnO CV 95.16 94.65 91.87 91.25 4.10
MB 97.32 94.60 93.69 91.36 6.12
MO 94.85 92.27 90.58 89.61 5.52
NBB 94.02 91.82 90.64 88.23 6.15

4 Conclusion

In this study, phytochemicals from aqueous extracts of OB and OA plant leaves were used to synthesize ZnO nanocatalysts, known as OB- and OA-ZnO. The obtained ZnO crystals were crystallized in a hexagonal wurtzite structure, exhibiting two distinct morphologies. ZnO induced by OB displayed uniform-sized spherical particles, whereas OA-ZnO resulted in irregular shapes and sizes. The photocatalytic activity of OA-ZnO was higher than that of OB-ZnO NPs against the tested cationic dyes (CV and MB) and anionic dyes (MO and NBB) in a polluted aqueous environment, while all were higher than that of dw-ZnO. It is evident that the surface area was not as critical as the bandgap or recombination rate in determining degradation efficacy. The named catalysts exhibited good stability and activity even after four cycles of reuse. Hence, the method used for synthesis, the feasibility of morphology control, and potential applications in water treatment against certain types of colorants that can be efficiently removed may deserve further studies in the future.

Acknowledgements

The authors thank the Researchers Supporting Project (number RSP2024R266), King Saud University, Riyadh, Saudi Arabia, for their financial support.

  1. Funding information: The research was supported by the Researchers Supporting Project (RSP2024R266), King Saud University, Riyadh, Saudi Arabia.

  2. Author contributions: Conceptualization, Naaser A. Y. Abduh, Abdullah Al-Kahtani, and Abdel-Basit Al-Odayni; formal analysis, Naaser A. Y. Abduh and Abdel-Basit Al-Odayni; investigation, Naaser A. Y. Abduh, Abdullah Al-Kahtani, and Abdel-Basit Al-Odayni; methodology, Naaser A. Y. Abduh, and Abdel-Basit Al-Odayni; writing – original draft, Naaser A. Y. Abduh and Abdel-Basit Al-Odayni; writing – review and editing, Naaser A. Y. Abduh, Abdullah Al-Kahtani, and Abdel-Basit Al-Odayni.

  3. Conflict of interest: The authors declare no conflict of interest.

  4. Data availability statement: The data that support the findings of this study are reported in the manuscript.

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Received: 2024-06-04
Revised: 2024-08-30
Accepted: 2024-09-12
Published Online: 2024-10-09

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  136. Green synthesis of silver nanoparticles from Olea europaea L. extracted polysaccharides, characterization, and its assessment as an antimicrobial agent against multiple pathogenic microbes
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  149. Phytochemical screening, antioxidant properties, and photo-protective activities of Salvia balansae de Noé ex Coss
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  151. Phyto-fabrication and characterization of gold nanoparticles by using Timur (Zanthoxylum armatum DC) and their effect on wound healing
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https://doi.org/10.1515/chem-2024-0093
Keywords for this article
biosynthesis; Ocimum basilicum extract; Olea africana extract; organic dyes; photodegradation; zinc oxide
Creative Commons
BY 4.0

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