Biofabricated SnO2 Nanoparticles derived from Leaves Extract of Morinda citrifolia and Pandanus amaryllifolius for Photocatalytic Degradation

doi:10.21203/rs.3.rs-5088502/v1

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Biofabricated SnO₂ Nanoparticles derived from Leaves Extract of Morinda citrifolia and Pandanus amaryllifolius for Photocatalytic Degradation

https://doi.org/10.21203/rs.3.rs-5088502/v1

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This study investigates the biofabrication of SnO₂ nanoparticles (NPs) utilizing leaf extracts from Morinda citrifolia and Pandanus amaryllifolius for photocatalytic degradation of methylene blue (MB). The synthesis method integrates tin chloride pentahydrate with the leaf extracts, followed by calcination. Comprehensive characterization via FTIR, XRD, FESEM, EDX, HRTEM, and UV-Vis spectroscopy confirmed the successful formation of SnO₂ NPs, revealing distinct morphological and crystalline properties. Photocatalytic tests demonstrated that SnO₂ NPs derived from M. citrifolia achieved a superior degradation rate of 97%, compared to 80% from P. amaryllifolius, with optimal activity under neutral pH. Radical scavenger experiments identified electrons as the primary active species. Reusability tests indicated a gradual decline in efficiency over five cycles, demonstrating its stability. These findings underscore the potential of biofabricated SnO₂ NPs as sustainable and efficient solutions for dye-polluted water remediation, offering a promising avenue for environmental conservation and resource management.

Morinda citrifolia

Pandanus amaryllifolius

Methylene blue

Photocatalytic

The current rapid evolution of the economy and the continued depletion of natural resources owing to industrial pollution have an impact on the availability of water resources, which poses a serious danger to the sustainable development of both the environment and humans. According to the World Health Organization (WHO), approximately 25% of the diseases that afflict people today are caused by extended exposure to water pollution [1]. The majority of pollutants originate from industrial sources, with occasional contributions from home activities. This has resulted in the issue of dye-polluted water and efforts to develop a workable remedy. From an industrial perspective, the widespread use of dyes in several industries, including textiles, paint, cosmetics, plastics, paper, leather, and rubber, has caused a problem. This has led to the leakage of hazardous wastewater and large amounts of dye into the environment, which may eventually contaminate important water supplies [2]. considerable water consumption during the dyeing procedures in this instance was caused by large amounts of dye effluent discharge, which ultimately led to considerable water contamination. Approximately 10,000 different varieties of commercial dyes are constantly used, with an approximate yearly production of 7×10⁵ tons of dyes, according to statistical data [3].

Auxochrome and chromophore groups found in dye molecules are essential for determining color. In addition, salts, heavy metals, chemical compounds, and surfactants are included as additives to improve color adsorption [4]. Due to their sensitivity to molecular reagents and resistance to heat, dye molecules display complicated behavior. This means that finding a solution to the problem will be challenging and call for both inexpensive and efficient medical care. Numerous treatment methods are employed to remove colors, such as membrane separation, electrochemical oxidation, coagulation-flocculation, Fenton oxidation, chemical oxidation, ultrasonic, adsorption, chemical reduction, photocatalysis, and biological methods [5].

Because of their high energy and pressure requirements, cost, difficulty of use, color selectivity, chemical consumption, secondary pollutant creation, and time-consuming nature, these procedures are not advised. When there are significant health problems, dye-contaminated water can be dangerous and carcinogenic even at low quantitis (less than 1 ppm). Some of the health effects include rapid development of oedema, respiratory distress, human cancer, splenic sarcomas, hepatocarcinomas, human urinary bladder carcinogen and tumorigenicity, hypertension, intermittent fever, renal damage, and human cramps [6]. Furthermore, dyes prevent water bodies from reoxygenating, which halts the bulk of the biological processes that support aquatic life. Furthermore, colors reflect sunlight, which stops algae or water plants from photosynthesizing [7]. Heterogeneous approaches, such as photocatalytic processes, have shown promise in the remediation of a variety of hazardous compounds in response to these issues. They have benefits including quick cleanup and complete breakdown of organic pollutants into less harmful by-products (water and CO₂) without producing more dangerous materials [8].

Metal oxide nanoparticles have found widespread use as photocatalysts because they are more effective than their bulk version. Among the numerous photoactive metal oxide nanoparticles that have been thoroughly investigated for these uses are SnO₂ nanoparticles (SnO₂ NPs). With a band gap energy of roughly 3.2 to 3.6 eV, SnO₂ NPs have shown outstanding photocatalytic activity. They have also shown improved electron mobility (100 to 200 cm²V^-1s^-1) [9][10][11]. Green synthesis, specifically the biofabrication process, has made it possible to replace the use of traditional methods that are known to be risky, costly, and occasionally require extended duration [12]. These methods include the sol-gel method [13], hydrothermal [14], mechanochemical [15], laser ablation [16] and electrolysis [17].

When it comes to the biofabrication process, prior research has documented the use of a number of plant extracts, including those from Aloe barbadensis miller [18], Pometia pinnata [19], Plectranthus amboinicus [20], Camellia sinensis [21], Aspalathus linearis [22], Delonix elata [23], Ziziphus jujuba [24], Cyphomandra betacea [25], Citrus aurantifolia [26], Litsea cubeba [27], Chromolaena odorata [28], soybean [29] and others, to mediate the preparation of pure SnO₂ NPs. In this context, the synthesis reaction employed phytochemicals, particularly the flavonoid group, which has the capacity to serve as capping and reducing agents [30][31]. In this research, the use of extracts from the leaves of Morinda citrifolia and Pandanus amaryllifolius to generate SnO₂ NPs is discussed using the biofabrication method. Figure 1 shows images of both plants. Fourier transform infrared (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), high resolution transmission electron microscopy (HRTEM), selected area diffraction (SAED), UV-Vis Diffuse Reflectance (UV-DRS), and Zeta potential analysis were used to discuss the morphologies and nanostructures based on the results of characterization processes. The degradation of organic dyes, specifically methylene blue (MB), was used to evaluate the photocatalytic activity of SnO₂ NPs.

2.1 Preparation of Morinda citrifolia and Pandanus amaryllifolius leaf extract

In this study, fresh leaves of M. citrifolia and P. amaryllifolius were collected from the Shah Alam district in Malaysia. The leaves underwent thorough cleaning using Milli-Q water to remove any impurities. The cleaned leaves were then dried in a conventional oven for 12 hours. After drying, 80 g of the leaf samples were blended using a vegetable blender to obtain a homogenized material. The blended leaf samples were subsequently boiled in an aqueous solution maintained at a temperature between 60-70°C. The extract was then filtered, and the resulting liquid was refrigerated at 4°C.

2.2 Preparation of SnO₂ NPs

M. citrifolia leaf extract was added dropwise to a stirring solution of tin chloride pentahydrate (SnCl₂.5H₂O) in a 1:1 ratio. The stirring was continued at room temperature for three hours to facilitate the reaction. The resulting colloidal mixture was then centrifuged to extract the gelatinous pellet. This pellet was left to dry overnight at 50 °C. Subsequently, the dried pellet underwent a calcination procedure at the optimized temperature of 600 °C for one hour. The reaction was repeated using different ratios of P. amaryllifolius leaf extract to tin chloride solution, specifically 3:1 and 5:1, following the parameters of a previous study [32][33].

2.3 Characterization process

In order to identify the functional group that is present in the final nanostructure of SnO₂ NPs, FTIR spectroscopic analysis was conducted using the Perkin Elmer Spectrum 400 and the attenuated total reflection (ATR) technique. The crystalline structure was confirmed using an X-ray diffractometer (Xpert Pro PAN) with CuKα radiation (λ=1.17545Å) at roughly 2θ = 5º to 90º with 45kV and a scan speed of 0.417782 */sec with 40mA. The morphological feature of SnO₂ NPs was examined using the FESEM (Jeol model JSM-7600F) at electron beam energy acceleration voltages of 5 kV. The shape feature of SnO₂ NPs was examined using the FESEM (Jeol model JSM-7600F). Following the SAED examination, the morphology of SnO₂ NPs was further examined using a HRTEM equipped with a 200 kV accelerating voltage-operated JEOL JEM-2100F electron microscope that was fitted with a LaB6 filament. In addition, the reflectance of solid SnO₂ NPs was measured using a UV-Vis spectrometer, brand name Varian model Carry 5000. Zeta potential analysis was conducted using Zetasizer 1600 model brand Malvern. For this analysis, 1 mg of optimized SnO₂ NPs was dissolved in 10 mL of distilled water and directly subjected to the operation at ± 500mV.

3.1 Mechanism for biofabrication of SnO₂ NPs

The mechanism for the fabrication of SnO₂ NPs is illustrated in figure 2. The leaves extract dissolved in water is thoroughly mixed with the dissociated tin cations. The hydroxyl groups attached to the aromatic compounds provide active sites, making them prone to form tetravalent bonds. Concurrently, water molecules interact with this tetravalent complex, generating hydrogen bonds. Additionally, the presence of organic components stabilizes the intermediate product and prevents aggregation. Finally, calcination is performed as the last step, decomposing the organic residues and yielding SnO₂ NPs [34][35].

For the leaves utilized in this study, the most likely phytochemical compounds involved in the reaction process are identified as flavonoids. These compounds are shown in figure 3. These flavonoid compounds are known as quercetin 3-O-β-D-glucopyranoside (L-epicatechin) and 2-(3,4-dihydroxyphenyl)-3,4-dihydro-2H-chromene-3,5,7-triol (catechin) from M. citrifolia [36] and P. amaryllifolius [37], respectively. Based on the proposed mechanism, it is suggested that the hydroxyl groups located at the para- and meta-positions of the aromatic rings make these compounds susceptible to and compatible with the reaction, given their significant presence in the leaves. Another aspect supporting this proposal, besides the suggested mechanism, is the well-documented evidence in prior literature that flavonoids possess strong chelating abilities, especially in the adsorption of metal ions [38][39][40][41]. Consequently, this characteristic facilitates the formation of coordination bonds between the tin cations and hydroxyl molecules, enhancing the overall efficacy of the process. By examining the proposed molecular structure, comparisons were made to previous research on the biosynthesis of SnO₂ NPs. It was found that nearly all the proposed phytochemical compounds were polyphenolic flavonoids or compounds heavily bonded with hydroxyl groups [42].

3.2 Fourier transform infrared (FTIR) analysis

The absorption bands of the synthesized SnO₂ NPs from M. citrifolia and P. amaryllifolius employing various extract to precursor salt ratios are visible in the infrared spectra shown in figures 4. The purpose of this investigation was to investigate the existence of relevant functional groups for the SnO₂ synthesis. The results indicate that there are two primary sets of absorption peaks present in all examined samples: the stretching vibration of Sn-OH and the anti-symmetry vibration of Sn-O, which are located in the 600 to1000 cm^-1 range, respectively [43][44][45].

The findings indicate that Sn-O anti-symmetrical vibration peaks are uniformly distributed in the same area and show almost the same strength throughout the proposed ratio range. On the other hand, the Sn-OH peaks show up regardless of the fluctuation in the applied extract concentration. This may be explained by the competing hydrogen bonding that occurs between the phytochemicals and the OH group of water molecules, which produces distinct capping volumes on the surface of Sn⁴⁺ and, in turn, diverse Sn-OH vibrational or stretching patterns. Furthermore, CO₂ absorption peaks have been found in the vicinity of 3000 cm^-1[46], which has led to some spectrometer tuning fluctuation about 2200 cm^-1. Nevertheless, these peaks are negligible. Overall, it is feasible to produce SnO₂ NPs sustainably by using these ratios.

3.3 X-ray diffraction (XRD) analysis

The XRD spectra of the synthesized SnO₂ NPs derived from M. citrifolia and P. amaryllifolius are shown in figure 5, using JCPDS card no. 01-077-0452. The collected peaks at 2θ values of 26^o, 33^o, 37^o, 51^o, 54^o, 57^o, 61^o, 64^o, 65^o, 70^o, 78^o and 83^o can be indexed as (110), (10 1), (200), (211), (220), (002), (310), (112), (301), (202), (321) and (222) planes. In addition, high intensity peak attributed from tetragonal shape and crystalline in nature was observed at 26^o, 33^o and 51^o, that belongs to Braggs reflections of (110), (101) and (211) set of lattice plane. The XRD patterns acquired corroborate with the past works of literature [47][48][49]. By using the Scherrer formula, D= kλ/β cos θ, the average nanocrystalline size was calculated based on the plane with the highest atomic density in SnO₂ NPs, which is (110) [50]. Regarding this formula, D is particle diameter size, k is Cu Ka (1.54 Å) X-ray wavelength of the X-ray source, β is the full width at half maximum (FWHM), θ is the diffraction angle and k is the unknown shape factor [51].

Given that the most crystalline SnO₂ NPs are representative of peak intensity, altitude, and narrowness, 3:1 is the preferred ratio for M. citrifolia for these reasons. The nanoscale dimension of the crystallite was determined to be 29.19 nm using the Scherrer formula. It is thought that the hydroxyl group of phytochemicals participates in Sn⁴⁺ reduction during the capping action, which requires less energy to weaken the bonding of the O-H bonds and increases its susceptibility to carrying out the capping action [52]. This process is assumed to reach saturation at a ratio of 3:1, at which point highly dense polyphenolic phytochemicals bind to Sn⁴⁺ with steric hindrance, causing uncapped Sn⁴⁺ to agglomerate. This increases the likelihood that agglomeration will be prevented, leading to large crystallite size.

For the case of P. amaryllifolius work-based, when the extract ratio was increased, the XRD peaks for the P. amaryllifolius work-based example show dependency. Lower extract concentrations provide XRD peaks that are sharp and intense, giving a preferred ratio of 1:1 results in a crystallite size of 9.02 nm. A comparable phenomenon of a reduction in peak intensity was also noted while employing Citrus aurantifolia [26], Tradescantia spathacea [43], Camellia sinensis [53], Lycopersicon esculentum [54], Tilia cordata [55] whenever the extract's concentration rises. The phytochemicals in the extract are probably what cause this phenomena because they disrupt the SnO₂ NPs' crystallinity, which causes a less organized arrangement of atoms on the surface [53]. Another explanation can be related to the synergistic impact of the hydroxyl groups, which allows them to do two tasks whenever possible: they can operate as dispersants because of the C=O bond, as well as a reducing and capping agent. Consequently, the dispersion activity of SnO₂ NPs reduces the clumping problem when ratios between 1:1 and 5:1 are used.

Table 1. The crystallite size of SnO₂ NPs derived from M. citrifolia and P. amaryllifolius.

Ratio of extract to precursor salt	M. citrifolia		P. amaryllifolius
Ratio of extract to precursor salt	Crystallite size D (nm)	FWHM (^oC)	Crystallite size D (nm)	FWHM (^oC)
1:1	13.25	0.67	9.02	1.03
3:1	29.19	0.25	6.92	1.31
5:1	12.32	0.75	6.10	1.50

3.4 Field emission scanning electron microscopy (FESEM) and energy dispersive X-ray spectroscopy (EDX) analysis

FESEM and EDX analyses were conducted using SnO₂ NPs with a ratio of 3:1 for M. citrifolia-based sample and a ratio of 1:1 for P. amaryllifolius-based sample. Figure 6 demonstrates the morphological images of SnO₂ NPs with tinny spherical SnO₂ NPs with rigid agglomeration are produced when M. citrifolia extract concentration is applied in an equivalent proportion to a precursor salt solution. This is consistent with earlier research on biosynthesized SnO₂ NPs, which showed morphological results that were either spherical or quasi/semi-quasi forms [56][57][58]. The homogeneity of the nanospheres, which lowers agglomeration, is thought to be caused by the hydroxylated flavonoid contained in the leaf extract consistently having stabilizing activity [59]. When compared to the two succeeding samples, the spherical morphology shown in SnO₂ NPs derived from P. amaryllifolius shows that incredibly small nanoparticles was produced. These nanoparticles appear as a spherical sponge-like shape upon examination. It may be deduced that increased electrostatic contacts are the outcome of the capping action carried out on the Sn⁴⁺ surface by the relevant phytochemicals. Subsequently, it causes a progressive adjustment of thermodynamics, which results in a marginal variation in the orientations of atomic groupings. This ocassion is in line to the author's view in Tilia cordata work-based, where the author suggests that limited nucleation of nanoparticles due to significant phytochemical interference could lead to a variety of forms in nanoparticles [55]. Since tiny nanoparticles are present in SnO₂ NPs, it is doubtful that the nanoscale measurements for both samples will be obtained.

The atomic percentages of Sn and O in SnO₂ NPs derived from M. citrifolia are 34.39% and 65.61%, respectively as shown in table 2. Meanwhile,the atomic percentages of Sn and O for P. amaryllifolius are 69.31% and 30.69%, respectively. The composition of Sn and O levels are within an acceptable range and are in line with earlier research, confirming the elements purity [60][61].

Table 2. The atomic percentages of SnO₂ NPs.

Work-based	Ratio of extract to precursor salt	Atomic (%)
Work-based	Ratio of extract to precursor salt	Sn	O
M. citrifolia	3:1	34.39	65.61
P. amaryllifolius	1:1	30.69	69.31

3.5 High Resolution transmission electron microscopy (HRTEM) and selected area diffraction (SAED) analysis

The HRTEM reaults reveal that the sample consists of well-crystallized nanoparticles with varying particle sizes. The consists visibility of lattice fringes across different regions indicates high crystaallinity throughout the sample. This might be due to different synthesis conditions of post-synthesis treatments. Figure 7a and b depict aggregated nanoparticles with a roughly spherical shape for M. citrifolia experimental, while significant spherical shape with a highly polycrystalline structure and some minor agglomerates for P. amaryllifolius work-based. These morphological findings are consistent with FESEM images, which show spherical formations of SnO₂ NPs derived from P. amaryllifolius and not to M. citrifolia work-based. The particle size distribution appears to vary within different regions of the sample, as indicated by the inset histograms in Figure 4a and 4c. The mean particle sizes give values of 3.24 nm for M. citrifolia and to 7.63 nm for P. amaryllifolius. This finding is believed within the optimal range for producing finely tuned nanoparticles for photocatalytic testing.

The interplanar distances for all samples shown in figure 7b and d are comparable to those obtained from XRD analysis, as tabulated in Table 3. Notably, P. amaryllifolius work-based obtained values of d indicate a correlation for the (101) plane, unlike the (110) planes obtained from M. citrifolia experimental or other reports. Following the principle of lowest energy, active sites of the nuclei might encourage nanoparticles to grow along the most stable crystal face, indicating that the preferential growth lattice plane is (101) rather than the conventional (110) plane. Consequently, the surface energy in various crystallographic orientations follows to the order (101) > (110) [62]. Additionally, the SAED spectra exhibits multiple rings consistent with XRD diffraction peaks (Figure 7e and f). As expected, the highly crystalline nature of SnO₂ NPs provides prominent diffraction rings corresponding to reflections (110), (101), (200) and (211) [54][63]. The pattern displays distinct diffraction spots arranged in rings, which is characteristic of polycrystalline materials. The presence of these indexed planes indicates the materials’s crystallographic orientations and confirm its prolycrystalline nature. The pattern suggest the presence of multiple crystallinedomains oriented in different directions, contributing to the ring-like appearance of the diffraction spots. The distinct diffraction spots in the SAED patterns confirm the high crystallinity of the sample. The sharpness and clarity of these spots indicate well-ordered crystaalline regions within the material. The indexed planes correspond to known crystallographic planes of specific phases, providing insights into the phase composition of the sample. The consistent indentification of (110), (101), (200) and (211) planes suggests a common phase throughout the sample. The ring-like arrangement of diffraction spots in both patterns is typical of polycrystalline samples. This indicates that the sample consists of numerous small crystallites with random orientations. The SAED results are conssistent with the HRTEM findings, where lattice fringes corresponding to specific planes were observed. This corelations strengthens the overall analysis, confirming the materials crystalinity and phase purity.

Table 3. The comparable d values of SnO₂ NPs obtained via TEM and XRD

Work-based	TEM d value (Å)	XRD d value (Å)	Plane hkl
M. citrifolia	3.25	3.28	(110)
P. amaryllifolius	2.55	2.36	(101)

3.5 UV-Vis Diffuse Reflectance (UV-DRS) analysis

The reflectance characteristics of SnO₂ NPs derived from M. citrifolia and P. amaryllifolius using a variation of extract to precursor ratio are illustrated in Figure 8 (left). The reflectance edges for all samples of SnO₂ NPs fall within the visible region. SnO₂ NPs obtained from M. citrifolia demonstrate a reflectance edge at 511 nm with a corresponding reflection of 51%, while from the result of P. amaryllifolius experimental, the reflectance values were recorded as 59% and fall at 527 nm, accordingly. The reflectance values are employed to compute energy band gap, using the Kubelka-Munk formula F(R) = (1-R)²/ 2R = k/s, where F(R) is the Kubelka-Munk functions, and k, s are the K-M scattering and absorption coefficients, respectively [64]. The energy band gap spectrum is constructed by plotting the square of the Kubelka-Munk function against energy and extending the linear portion of the curve, as illustrated in the depicted in figure 8 (right).

The energy band gaps 3.70 and 3.51 eV are observed for M. citrifolia and P. amaryllifolius-based, respectively. By having these values, it is indicated that they require low energy for photoactivation and the application of the photocatalyst to the visible region is said to be compatible [65]. This finding is also very much in agreement with the optimal ratio suggested by the sharpness and intense peak in XRD analysis.

3.6 Analysis of Zeta Potential

In this study, the ZP values for SnO₂ NPs derived from M. citrifolia and P. amaryllifolius were found to be -51.1 and -30.7 mV, respectively. These values indicate good electrical stability and suggest a well-dispersed colloidal system with minimal agglomeration [66].

Table 4. Zeta potential of SnO₂ NPs

Work-based	ZP (mV)
M. citrifolia	-51.1
P. amaryllifolius	-30.7

3.6 Photocatalytic activities

The photocatalytic activity of the SnO₂ NPs was evaluated through experiments using different catalytic loadings and pH levels, with measurements taken at 10-minute intervals. All samples were stirred in the dark for 30 minutes prior to irradiation to achieve an adsorption-desorption equilibrium [67]. The following formula is used to compute the percentage of dye degradation, where C₀ is the dye's initial concentration prior to illumination and C_t is its concentration following time t [68].

Degradation % = (C₀ - C_t) /C₀ x 100

The results are shown in figure 9. It was found that the degradation of methylene blue (MB) using SnO₂ nanoparticles from both photocatalysts exhibited a turbidity effect. The highest degradation rates were 97% and 80% with a 200 mg loading (Fig. 9a and 9b). It is presumed that the generation of O₂^-• and OH• radicals were diminished, leading to a decrease in degradation efficiency, and that catalyst particle accumulation occurs when the catalyst amount exceeds the optimal level. The higher photodegradation performance of SnO₂ NPs derived from M. citrifolia may be due to their smaller particle size, as indicated by HRTEM results, which show a nanoscale size of 3.24 nm compared to 7.63 nm for P. amaryllifolius-derived SnO₂. The smaller particle size may facilitate easier agglomeration, thereby increasing the turbidity of the solution and making part of the catalyst surface unavailable for photon absorption [69]. A previous study described a similar scenario during the removal of rose bengal (RB) under UV irradiation, where degradation initially increased due to enhanced active sites and particle density but later encountered interference from agglomeration with increased photocatalyst loading [70].

The photocatalytic reaction was proceeded using the optimal catalyst loading of 200 mg for SnO₂ NPs derived from M. citrifolia and P. amaryllifolius under three different pH levels: 3, 7, and 11. During the reaction setup, the pH was carefully adjusted to 3 using 0.1 M of HCl and to 11 using 0.1 M of NaOH, added dropwise into the solution. From the results, methylene blue (MB) was optimally photodegraded at rates of 97% and 80% using SnO₂ NPs derived from M. citrifolia and P. amaryllifolius, respectively, as illustrated in figures 9c and d. The photodegradation of MB with all samples of SnO₂ NPs followed a similar pattern, with the highest degradation observed under neutral conditions (pH 7). This suggests that the breakdown of MB molecules is not favoured by these SnO₂ NPs photocatalysts at lower or higher pH levels. Under acidic conditions, the attraction of MB molecules to the surface of SnO₂ nanoparticles is diminished due to the competitive forces exerted by H⁺ ions, resulting in lower degradation rates. In alkaline conditions, the increased concentration of hydroxyl ions leads to more reactions with holes, generating more OH• radicals. However, this results in the desorption of OH• along with dye molecules on the surface of the SnO₂ NPs, inhibiting MB degradation. Optimal degradation occurs under neutral conditions, where the negatively charged surface of SnO₂ NPs enhances the electrostatic attraction with MB molecules. This increases the photo-oxidation rate with minimal recombination of electron-hole pairs, leading to efficient degradation of MB molecules. This behaviour contrasts with the degradation of rhodamine B by SnO₂ NPs prepared from C. ternatea flowers, which was rapid under both acidic and basic conditions [71]. However, it is consistent with the degradation of methyl orange reported in experiments using C. gigantea, which showed a preference for nearly neutral conditions (pH 6.5) [32].

Figure 10 is a schematic representation of the general photocatalytic degradation process of MB using SnO₂ NPs. Three phases are hypothesized for the degradation process: adsorption (i), oxidative species production (ii) , and final MB molecule breakdown (iii to v) [54][72][73]. SnO₂ NPs capacity to draw MB molecules more strongly to their surface is necessary for the adsorption of MB molecules on their surface. Subsequently, the light-induced oxidative species formation in SnO₂ produces holes (h⁺) in the valence band (VB) and electrons (e^-) in the conduction band (CB). At this time, photogenerated e^- will reside in CB and photogenerated h⁺ will reside in VB after being sent in the opposite direction. Later, at the surface of SnO₂ NPs, e^- reacts with dissolved oxygen (O₂) to oxidize it and produce superoxide radicals (O₂^-•), and h⁺ oxidizes H₂O molecules to produce hydroxyl radicals (OH•). These two species break down MB molecules because they are strong oxidizers. Here, S-Cl, N-CH₃, CS, CN, and C-O bonds were broken during the degradation process, resulting in fragments of 4-(N,N-dimethyl)-aniline and 3-(dimethylamino)benzenesulfonate. As a result, a series of intermediate products degrade, causing the MB rings to open and smaller organic molecules to form [72]. This process continues until total mineralization is reached, producing the reaction known non-hazardous by-products, H₂O and CO₂. The transition from blue to colorless is a powerful sign of the SnO₂ surface great adsorption capability, which is caused by the MB molecule π-π interactions [74].

The primary oxidative species involved in the photodegradation of MB are identified by radical trapping experiments, referred to as scavenger tests, in order to further elucidate the potential reaction mechanism of MB photodegradation by biosynthesized SnO₂ NPs. The purpose of this experiment was to identify the particular reactive species that cause MB degradation. The MB solution containing the optimized SnO₂ NPs was supplemented with approximately 1 mL of 2 mM of different scavenger reagents in this study. The optimized photodegradation parameters were then employed in the process. These reagents were isopropanol (IPA) for hydroxyl radicals (OH•), EDTA for photogenerated holes (h⁺), benzoquinone (BQ) for superoxide radicals (O₂^-•), and AgNO₃ for electrons (e^-) [75]. The result shows in figure 11 indicates that AgNO₃ inhibits the photocatalytic degradation efficiency of MB by SnO₂ NPs produced from both plant sources, meanwhile the kinetic momentum for degradation activity is retained by BQ, EDTA, and IPA. These findings imply that superoxide anion (O₂^-•), hydroxyl radical (OH•), and photogenerated hole (h⁺) have a negligible inhibitory effect on the photocatalytic process, however the introduction of electrons (e^-) from AgNO₃ inhibits the photocatalytic activity. The removal rate of MB dramatically decreased to 55% and 15% for M. citrifolia and P. amaryllifolius experimental, respectively, remarkably with the addition of AgNO₃. This suggests that the active species involved in the elimination of MB are e^-[76]. EDTA acts as a scavenger for h⁺ to prevent the recombination of electrons and holes, but no discernible inhibition was seen [77]. Moreover, it is discovered that O₂^-• from BQ is less successful in preventing the breakdown of O₂. Furthermore, O₂^-• from BQ is found to be less effective in inhibiting the dissolution of O₂ [78]. This finding contradicts previous scavenging experiments using SnO₂ NPs from T. cordifolia [77] , P. pinnata [19] and C. ternatea [71], which indicated that the main reactive species are OH• from IPA. The scavenging activity was explained by the radical ability to be trapped by surface and photonic contacts, which in turn decreased the production of further oxidation.

Because it aligns with practicality and cost considerations while performing dye-polluted water, photocatalyst stability is important for practical applications [79][80]. As a result, five repetitions of the photocatalytic evaluation were carried out utilizing optimized SnO₂ NPs that were extracted from the methylene blue (MB) dye following the ideal degradation condition. Water, methanol, and acetone were used to thoroughly wash the SnO₂ NPs until all traces of blue staining were completely removed from their surface. Before being utilized again for more catalytic cycles, the recovered SnO₂ NPs were dried in a drying cabinet. The weight of the SnO₂ NPs catalyst was changed in relation to the MB volume for every cycle.

After achieving a 97% efficiency in the first dye degradation cycle, the degradation efficiencies of SnO₂ NPs obtained from M. citrifolia decreased gradually to 75% and 74% in the second and third cycles, 52% in the fourth cycle, and 29% in the fifth cycle (Figure 12a). In contrast, the first degradation efficiency of 80% in the experimental setting with P. amaryllifolius dropped to 46% in the second cycle as shown in figure 12b. This was followed by a progressive reduction, with degradation rates stabilizing at roughly 46%, 43%, 40%, and 38%, respectively, by the fifth cycle. The observed drop can be attributed to the ultimate decline in activity and reaction rate, indicating a limitation in the photocatalyst efficiency [81]. For all samples, the SnO₂ NPs photocatalyst's degradation efficiency generally drops over the course of five consecutive cycles. Agglomeration of SnO₂ NPs may have caused this decrease by lowering the overall volume of specific surface area [82]. Nevertheless, in completing the photodegradation of MB, the SnO₂ NPs photocatalyst demonstrates commendable recyclability. The fascinating findings demonstrate that the SnO₂ NPs photocatalyst could be recycled up to five times with only a slight decline in degrading efficiency. This confirms that the SnO₂ NPs photocatalyst exhibits remarkable stability and reusability, making it a useful catalyst for the ecologically benign degradation of dyes and organic contaminants.

This study has demonstrated the efficacy of biofabricated SnO₂ NPs synthesized from the leaf extracts of M. citrifolia and P. amaryllifolius in the photocatalytic degradation of methylene blue, a common dye pollutant. The synthesis process, which employed tin chloride pentahydrate in conjunction with the respective leaf extracts, followed by calcination, yielded SnO₂ NPs with distinct morphological and crystalline properties, as confirmed through extensive characterization techniques including FTIR, XRD, FESEM, EDX, HRTEM, and UV-DRS spectroscopy. While XRD analysis revealed a prominent plane of (110) similar to the previous report, FTIR research revealed the presence of two important absorption peaks belonging to the Sn-OH and Sn-O groups. Tiny spherical nanoparticles were seen in the FESEM morphological result, which was consistent with the HRTEM observation. Furthermore, the produced SnO₂ NPs were found to be suitable for photocatalytic testing based on the band gap value measured by UV-DRS, which was 3.70 eV for M. citrifolia and 3.51 eV for P. amaryllifolius. The photocatalytic performance of SnO₂ NPs was evaluated under various conditions, with SnO₂ NPs derived from M. citrifolia exhibiting a superior degradation rate of 97%, compared to 80% from P. amaryllifolius, with optimal activity observed under neutral pH conditions. Radical scavenger tests identified electrons as the primary active species in the degradation process, providing crucial insights into the mechanistic aspects of photocatalysis.

Furthermore, recyclability tests revealed a gradual decline in efficiency over five cycles, indicating its stability and potential for reuse, even though with diminishing returns. This gradual loss of activity underscores the need for further optimization to enhance the long-term performance and durability of these photocatalysts. In summary, the biofabrication of SnO₂ NPs using plant extracts presents a sustainable and environmentally friendly approach to water remediation, leveraging the natural reducing and capping agents found in M. citrifolia and P. amaryllifolius. These findings offer significant implications for the development of green nanotechnology applications in environmental conservation, particularly in the treatment of dye-polluted wastewater. Future research should focus on improving the stability and efficiency of these biofabricated NPs, as well as exploring their applicability in the degradation of a broader range of pollutants, to fully harness their potential in advancing sustainable environmental technologies.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgments

The authors wish to extend their sincere appreciation to the Ministry of Higher Education Malaysia, the Research Management Centre (RMC), and the Institute of Science (IOS) at Universiti Teknologi MARA (UiTM).

Ethical Approval Not applicable

This research was funded by the Research Management Centre (RMC) UiTM through the GIP grants, grant number 600-RMC/GIP 5/3 (001/2023).

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Biofabricated SnO₂ Nanoparticles derived from Leaves Extract of Morinda citrifolia and Pandanus amaryllifolius for Photocatalytic Degradation

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