Startseite Photoremediation of methylene blue by biosynthesized ZnO/Fe3O4 nanocomposites using Callistemon viminalis leaves aqueous extract: A comparative study
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Photoremediation of methylene blue by biosynthesized ZnO/Fe3O4 nanocomposites using Callistemon viminalis leaves aqueous extract: A comparative study

  • Poonam Dwivedi EMAIL logo , Indu Jatrana , Azhar U. Khan EMAIL logo , Azmat Ali Khan , Honey Satiya , Masudulla Khan , Il Soo Moon und Mahboob Alam EMAIL logo
Veröffentlicht/Copyright: 22. November 2021
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Nanotechnology Reviews
Aus der Zeitschrift Nanotechnology Reviews Band 10 Heft 1

Abstract

This article reports a simple, cost-effective, and eco-friendly biosynthesis of ZnO/Fe3O4 nanocomposites using Callistemon viminalis leaves’ water extract. For the first time, we used a green synthetic route via C. viminalis leaves’ extract to prepare ZnO/Fe3O4 nanocomposites (NCs) using zinc acetate and ferric chloride as precursor materials. Fourier transform infrared (FTIR) spectroscopic results revealed polyphenolic compounds mainly phenolic acids present in the plant extract acted as both reducing and stabilizing agents to synthesize ZnO/Fe3O4 NCs. Outcomes of XRD and X-ray photoelectron spectroscopy confirmed the formation of ZnO–Fe3O4 heterojunction in ZnO/Fe3O4 NCs, with crystallite sizes of 45, 35, and 60 nm, respectively, according to Debye–Scherrer’s formula. EDX confirmed Zn, Fe, and O in the ZnO/Fe3O4 nanocomposite. Scanning electron microscopy and transmission electron microscopy (TEM) analyses revealed the existence of both ZnO and Fe3O4 in the NCs with some agglomeration. The thermal stability of NCs was evaluated using thermogravimetric analysis (TGA) and differential thermal analysis (DTA) in a nitrogen atmosphere. In addition, as-prepared ZnO/Fe3O4 NCs along with biosynthesized ZnO and Fe3O4 (prepared by C. viminalis extract) nanoparticles were examined for photodegradation of methylene blue under visible light irradiation for 150 min. The result reveals that the photodegradation efficiency of ZnO/Fe3O4 NCs (99.09%) was higher compared to that of monometallic ZnO (84.7%) and Fe3O4 (37.1%) nanoparticles.

Keywords: ZnO/Fe3O4 nanocomposites; Callistemon viminalis ; XPS; photodegradation; methylene blue

1 Introduction

Industrialization and urbanization have increased water pollution to a great extent because of the direct disposal of organic and industrial waste into water bodies [1]. Among all, dying industries produce an enormous amount of wastewater containing unused dye along with other chemicals [2]. It reported that the majority of dyes are toxic and nonbiodegradable [3]. Hence, the dye effluent contaminates surface and underground water, which brings out adverse effects on flora and fauna [4,5]. Methylene blue (MB) is the most popular thiazine dye used in textile industries. The prolonged exposure to MB results in harmful effects, such as cyanosis, skin irritation, and gastrointestinal irritation, in living beings [6]. To solve this challenge, many physical and chemical techniques including flocculation–coagulation, surface adsorption, ion-exchange, chemical precipitation, and photocatalytic degradation have been used to remove the dye from waste water [7,8]. Because of the simple experimental procedure and decomposition of organic dye molecules into nontoxic simple products in the presence of semiconductors under proper light irradiation, the photodegradation process proves its superiority over other methods [9,10]. For semiconductor-assisted photocatalytic process, various materials, such as ZnO, CuO, TiO2, and more, have been widely used as photocatalysts previously [11,12,13]. Among different semiconductor materials, ZnO is a nontoxic, easily available, and cost-effective material with a bandgap of 3.2 and 60 MeV exciton binding energy [14]. That is why ZnO became the priority to many researchers working in the photocatalytic degradation of dyes using semiconductors. But ZnO semiconductor has a rapid tendency of recombination of photo-induced electron–hole pairs, which makes it difficult to gain the practical demand [15]. To overcome this problem, many metallic or nonmetallic materials, such as CdS, Ag2O, CuO, and g-C3N4, have doped with ZnO and showed improved efficiency toward photodegradation process [16,17,18,19].

However, the removal of nanocomposites (NCs) from the treated solution is very tedious and expensive, which is still a challenge. In this concern, magnetite nanoparticles (Fe3O4 NPs) play an effective role as they are easily separable from the solution by applying an external magnetic field [20]. Apart from this, doping of metallic NPs with magnetite NPs improves their functionality and recyclability and in turn cost effectiveness of the process [21,22]. Inspired by this, many researchers have synthesized and investigated the results of magnetite NCs [23]. After reviewing the literature, we observed that various approaches, such as sol–gel, hydrothermal synthesis, precipitation, and microemulsion, have been adopted for preparing magnetite composites [24,25,26,27]. But many of these methods have certain demerits, such as the use of expensive and hazardous chemicals and the formation of toxic byproducts, which makes it difficult to achieve the requirement of green synthesis. In recent decades, the use of bioproducts (including biomolecules, bacteria, fungi, or plant extracts) for the synthesis of NPs has attracted researchers as well [28]. Metals and metal oxide nanoparticles have also been used as homogeneous or heterogeneous nanocatalysts in various organic syntheses due to the large surface-to-volume ratio of nanoparticles compared to bulk materials [29,30]. This strategy provides a simple, cost-effective, and eco-friendly route for the fabrication of nanomaterials [31]. Although synthesis of ZnO/Fe3O4 NCs by different routes has been reported [32,33], a few reports on a green synthesis of ZnO/Fe3O4 NCs are available [34,35]. In our present study, we have synthesized ZnO/Fe3O4 NCs using Callistemon viminalis leaves’ extract as a green reducing and stabilizing agent. C. viminalis is a small tree that belongs to the family Myrtaceae with a characteristic brushlike flowers. It is a traditional medicine to treat hemorrhoids, gastroenteritis, diarrhea, and skin infection [36,37,38]. The phytochemical study reported that C. viminalis is rich in biomolecules, including viminadiones, quercetin, and betulinic acid, and can act as a green reducing and capping agent during the fabrication of nanomaterials.

After reviewing the literature, we understand that C. viminalis leaves’ extract-mediated biomimetic synthesis of ZnO/Fe3O4 has not been reported till date. In this study, we have attempted to understand the role of biomolecules present in leaves’ extract as a reducing and stabilizing agent for the fabrication of ZnO/Fe3O4 NCs. The novelty of this study is to show the efficacy of biosynthesized ZnO/Fe3O4 NCs as a photocatalyst in contrast to ZnO or Fe3O4 NPs for the degradation of MB solution under visible light irradiation.

2 Experimental methodology

2.1 Chemicals

All chemicals applied in this research study, including zinc acetate dihydrate (Thermo Fisher Scientific India Pvt. Ltd.), ferric chloride (Thermo Fisher Scientific India Pvt. Ltd.), sodium hydroxide (Merck Life Science India Pvt. Ltd.), and methylene blue (Merck Life Science India Pvt. Ltd.), were of analytical grade and used as received commercially without further purification. Deionised water was used throughout the experiment wherever required.

2.2 Preparation of C. viminalis leaves’ extract

Leaves of C. viminalis were collected from Jaipur National University campus, India. The collected leaves were thoroughly washed under tap water and finally washed using deionised water. After drying in shade, the leaves were powdered in an electrical grinder. About 25 g of the powdered leaves in 100 mL deionised water was refluxed in a Soxhlet apparatus (Sigma-Aldrich, India) for 2 h at 80°C on a magnetic stirrer. On cooling, the suspension was filtered through Whatmann’s filter paper, and the filtrate was collected as leaves’ extract and stored in a refrigerator at 2°C for further studies.

2.3 Biosynthesis of ZnO/Fe3O4 NCs

The ZnO/Fe3O4 NCs were prepared through an eco-friendly green route, and the synthesis procedure is briefly illustrated as follows: 30 mL of C. viminalis leaves’ extract was added slowly in a round-bottom flask containing 30 mL of zinc acetate solution (0.01 M) under stirring. After 10 min, 0.16 g of ferric chloride in 10 mL deionised water was introduced dropwise into the flask and heated to 60°C, followed by the addition of NaOH (0.1 M) to maintain pH 10. The color of the solution changes from black to blackish brown after 1 h stirring, which indicated the formation of ZnO/Fe3O4 NCs. Afterward, the solution was cooled to room temperature, centrifuged, collected in a China dish, washed several times with ethanol to remove unused extract and NaOH, dried in an oven at 80°C, and finally calcined at 300°C before storing for further studies. For comparison, monometallic nanoparticles (ZnO and Fe3O4) had also been synthesized using C. viminalis leaves’ extract. A schematic of aforementioned green synthesis is shown in Figure 1.

Figure 1 Schematic of green synthesis of ZnO NPs, Fe3O4 (NPs), and ZnO/Fe3O4 NCs.
Figure 1

Schematic of green synthesis of ZnO NPs, Fe3O4 (NPs), and ZnO/Fe3O4 NCs.

2.4 Characterization

FTIR spectral analysis in the range of 4,000–400 cm−1 was carried out to investigate the role of C. viminalis leaf extract in the fabrication of ZnO, Fe3O4, and ZnO/Fe3O4 nanoproducts using a PerkinElmer spectrophotometer (MNIT, Jaipur). A powder X-ray diffraction technique was performed to determine the crystallinity and particle size of biosynthesized product by PAN analytical (XPART PRO) diffractometer in the scattering range (2θ) of 20–80° using Cu Kα radiation (λ = 1.5406 Å). The surface morphology of green synthesized samples was determined by scanning electron microscopy (SEM) using Nova Nano SEM 450 (MNIT, Jaipur) and transmission electron microscopy (TEM) at IIT Roorkee. The elemental composition was investigated using EDX analysis. Chemical states of elements present in ZnO/Fe3O4 NCs were analyzed by X-ray photoelectron spectroscopic technique (XPS, PHI 5000 Versa Probe III, IIT Roorkee). The thermal stability of ZnO/Fe3O4 sample was recorded in a nitrogen atmosphere at a heating rate of 5°C min−1 by TGA/DTA analyzer (EXSTAR TG/DTA 6300, IIT Roorkee).

2.5 Designing of the photocatalytic activity experiment

The photocatalytic efficiency of biosynthesized ZnO, Fe3O4, and ZnO/Fe3O4 nanomaterials for the degradation of MB dye was evaluated under visible light at pH 7. For the photodegradation study, three experimental sets were prepared. Each set comprised seven beakers (100 mL) with 25 mL solution of MB (32 mg L−1) in each. The dose of biosynthesized ZnO, Fe3O4, or ZnO/Fe3O4 nanoproducts taken was 0.004 g in each beaker. After certain intervals of time (15, 30, 45, 60, 75, 90, and 150 min), one beaker from each set was removed from irradiation, and dye solutions were centrifuged at 8,000 rpm followed by filtration to remove the photocatalyst. MB degradation was examined by measuring the absorbance of the dye solution at λ max = 665 nm using a UV-Vis spectrophotometer. The percentage of MB degradation was determined by the following equation:

(1) η = A 0 − A t / A 0 × 100 .

In equation (1), η is the degradation percentage and A 0 and A t are the absorbances of MB dye solution at t = 0 and after time t, respectively.

3 Results and discussion

3.1 FTIR analysis

The involvement of biomolecules present in C. viminalis leaves’ extract, for the fabrication of nanomaterials, was screened by FTIR spectroscopic analysis. Figure 2 depicts the FTIR spectra of C. viminalis leaves’ extract as well as biosynthesized ZnO, Fe3O4, and ZnO/Fe3O4 nanomaterials. The FTIR spectrum of C. viminalis leaves’ extract (Figure 2a) showed some major absorption bands at 3,419, 2921.76, 1718.16, 1451.86, 1368.87, and 1180.95 cm−1 were assigned to O–H stretching of phenolic acids and phenols, C–H stretching in CH3 and CH2, C═O groups in phenolic acids and flavonoids, C═C stretching of the aromatic ring, and C–H deformation in CH3 and C–OH stretching in phenolic acids, respectively, as reported in various literature [39,40,41].

Figure 2 FTIR spectra of (a) C. viminalis leaf extract, (b) ZnO, (c) Fe3O4, and (d) ZnO/Fe3O4 NCs.
Figure 2

FTIR spectra of (a) C. viminalis leaf extract, (b) ZnO, (c) Fe3O4, and (d) ZnO/Fe3O4 NCs.

However, after the reduction of metal precursors into their respective metal nanoparticles, a remarkable difference in intensity, position, and shape of absorption peaks had been observed, which showed the participation of biomolecules (present in leaves’ extract) in the reduction and capping of nanomaterials. The additional peaks in the spectra of monometallic NPs at 466.53 cm−1 (Figure 2(b)) and 612 cm−1 (Figure 2(c)) were allocated to Zn–O and Fe–O stretching vibrations, respectively, confirming the formation of ZnO and Fe3O4 NPs [42]. Moreover, shifting in absorption peak values of Zn–O (452.93 cm−1) and Fe–O (591.63 cm−1) towards lower wave numbers in ZnO/Fe3O4 (Figure 2(d)) indicated the formation of bimetallic nanocomposite. Furthermore, shrinkage/shifting of peaks corresponding to C═O, C═C, and C–OH groups (1718.16, 1451.86, and 1180.95 cm−1) in the spectra of nanoproducts suggests that polyphenolic compounds mainly phenolic acids are responsible for the bioreduction of metal ions and capping of as-prepared nanoproducts.

3.1.1 Mechanism of biosynthesis

On the basis of FTIR results, a possible mechanism for the C. viminalis leaves’ extract-mediated synthesis of ZnO, Fe3O4, and ZnO/Fe3O4 has been proposed.

In short, betulinic acid present in leaves’ extract undergoes oxidation according to the free radical mechanism, that is, betulinic acid to dehydro betulinic acid (Scheme 1). Zn+2/Fe+3 ions (present in solution) form complex with dehydro betulinic acid via transfer of electrons from anionic dehydro betulinic acid to metal ions. On calcination, the resulting complex is converted into respective metal oxide nanoparticles because of the capping effect of biomolecules [43].

Scheme 1 Proposed mechanism for the biosynthesis of ZnO, Fe3O4, and ZnO/Fe3O4 NCs.
Scheme 1

Proposed mechanism for the biosynthesis of ZnO, Fe3O4, and ZnO/Fe3O4 NCs.

3.2 XRD analysis

The phase and crystal structure of biosynthesized ZnO, Fe3O4, and ZnO/Fe3O4 nanomaterials were examined by powder X-ray diffraction analysis. Figure 3 depicts the X-ray patterns of ZnO (a), Fe3O4 (b), and ZnO/Fe3O4 (c). In Figure 3(a), XRD peaks at 2θ values = 32.03°, 34.73°, 36.66°, 48.03°, 57.05°, 68.32°, and 69.49° were indexed to the respective (100), (002), (101), (102), (110), (112), and (201) crystalline planes of hexagonal wurtzite phase of ZnO (JCPDS Card No. 36-1451), whereas in Figure 3(b), diffraction peaks at 2θ values = 30.16°, 35.29°, 43.12°, 56.83°, and 62.59° correspond to the miller indices (220), (311), (400), (511), and (440), respectively (JCPDS Card No. 19-0629), which confirm the face-centered cubic structure of Fe3O4 [44]. For ZnO/Fe3O4 NCs (Figure 3c), peaks at 32.56°, 34.87°, 36.07°, 57.28°, 68.92°, and 69.58° corresponding to (100), (002), (101), (110), (112), and (201) planes infer the presence of ZnO in hexagonal wurtzite phase, whereas peaks at 2θ = 30.10°, 35.65°, 43.15°, and 62.86° represent (220), (311), (400), and (440) planes of face-centered cubic structure of iron. The identification of a dual phase with shifting of the respective peak values in the XRD pattern of NCs indicates the formation of Zn–Fe heterojunction. Moreover, the crystallite size (D) of as-prepared nanoproducts is calculated using Debye–Scherrer’s formula (D = kλ/β cos θ) and at maximum intense peaks, the size of ZnO, Fe3O4, and ZnO/Fe3O4 is found to be 45, 35, and 60 nm, respectively.

Figure 3 Powder XRD pattern of biosynthesized NPs: (a) ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs.
Figure 3

Powder XRD pattern of biosynthesized NPs: (a) ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs.

3.3 SEM and TEM analysis

Morphology and nanoscale of the biosynthesized samples were analyzed using SEM and TEM. An overview of SEM images of Zn, Fe3O4, and ZnO/Fe3O4 samples is shown in Figure 4(a–c). As observed from images, the morphology of ZnO/Fe3O4 differs from ZnO or Fe3O4, which suggested the formation of ZnO/Fe3O4 NCs. Furthermore, in the SEM image of ZnO/Fe3O4, rod-shaped particles of ZnO and cubic-shaped structures of Fe3O4 are clearly visible, which interprets the interaction of Fe3O4 with ZnO. Morphological differences among as-prepared samples were also identified by TEM micrographs (Figure 4(d–f)). The spherical shape of ZnO NPs with a particle size of ∼45 nm can be seen in Figure 4(d), whereas Fe3O4 NPs have an irregular shape (Figure 4(e)) with a particle size of ∼35 nm. The coexistence of ZnO and Fe3O4 can be clearly identified in the TEM micrograph of NCs (Figure 4(f)), wherein Fe3O4 can identify as dark particles with some agglomeration because of its highly magnetic nature and ZnO as bright particles surrounding Fe3O4. Moreover, selected area electron diffraction (SAED) image of ZnO/Fe3O4 NCs (Figure 4(g)) also interprets the incorporation of Fe3O4 in the crystalline lattice of ZnO NPs, which resulted in a comparatively less crystalline and large-sized ZnO/Fe3O4 NCs. Thus, the results obtained from SEM and TEM analyses were in close agreement with XRD results.

Figure 4 SEM images: (a): ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs. TEM images: (d) ZnO, (e) Fe3O4, (f) ZnO/Fe3O4 NCs, and (g) SAED pattern of ZnO/Fe3O4 NCs.
Figure 4

SEM images: (a): ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs. TEM images: (d) ZnO, (e) Fe3O4, (f) ZnO/Fe3O4 NCs, and (g) SAED pattern of ZnO/Fe3O4 NCs.

3.4 EDX analysis

To determine the chemical composition of ZnO, Fe3O4, and ZnO/Fe3O4 nanoproducts, EDX analysis was carried out and results are displayed in Figure 5(a–c). It can be seen in Figure 5(a) that the EDX spectrum consists of strong peaks for Zn and O, whereas Figure 5(b) shows Fe and O elemental peaks. In case of ZnO/Fe3O4 NCs (Figure 5(c)), strong signals for Zn, Fe, and O elements were well recognized, which further confirmed the coexistence of ZnO and Fe3O4. The appearance of carbon in all three spectra may be due to biomolecular capping on the surface of nanoproducts [45]. Based on EDX outcomes, the weight percentage of elements in ZnO/Fe3O4 NCs was 32.56, 38.67, and 28.77% for Zn, Fe, and O, respectively.

Figure 5 EDX spectrum of (a) ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs.
Figure 5

EDX spectrum of (a) ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs.

3.5 XPS analysis

XPS analysis was carried out to demonstrate the chemical nature of the surface of biosynthesized ZnO/Fe3O4 NCs. Figure 6(a) depicts the full scan spectrum of ZnO/Fe3O4 and the appearance of major peaks at binding energies of 1,021 eV (Zn2p), 725 eV (Fe2p), 530 eV (O1s), and 284 eV (C1s) confirms the fabrication of ZnO/Fe3O4 NCs. High-resolution XPS spectra of Fe2p, Zn2p, O1s, and C1s are shown in Figure 6(b–e). In Figure 6(b), a doublet for Fe2p at 711.94 and 726.93 eV was assigned to respective binding energies of Fe2p3/2 and Fe2p1/2 of Fe3O4 [46,47]. In the Zn2p spectra (Figure 6(c)), the spin-orbit doublet Zn2p3/2 and Zn2p1/2 peaks were centered at binding energies of 1021.7 and 1044.65 eV, respectively [48]. It is evident from the literature that Zn2p3/2 and Zn2p1/2 peaks are separated by 23 eV in pure ZnO. From the XPS results, peaks of Zn2p in NCs were separated by 21 eV, which strongly manifests the synergistic effect between ZnO and Fe3O4 NPs, contributing to the enhancement in photocatalytic activity of NCs [49]. XPS spectrum of C1s (Figure 6(d)), consists of three peaks at 283 eV (C–C) [50], 284 eV (C═C) [46,51], and 285 eV (C═O) [52], attributed to the polyphenolic compounds of leaves’ extract acting as a stabilizing agent for ZnO/Fe3O4 NCs [53]. In the O1s spectrum shown in Figure 6(e), the peak position at 529.89 eV was assigned to oxygen in Fe–O of ZnO/Fe3O4, corresponding to ferro–ferric oxide. The deconvolution of O1s signals revealed the presence of Zn–O of ZnO at a binding energy of 530.89 eV. The peak at 531.89 eV may be due to the hydroxyl group of biomolecular capping and oxygen chemisorbed onto the surface of ZnO/Fe3O4 NCs [54]. Under visible light irradiation, these active oxygen species on the surface of NCs may contribute to MB degradation via oxygen ions, such as O−1 and O−2, which in turn improves the photocatalytic activity of ZnO/Fe3O4 NCs [55].

Figure 6 XPS spectra of ZnO/Fe3O4 NCs: (a) survey spectrum, (b) Fe2p, (c) Zn2p, (d) C1s, and (e) O1s.
Figure 6

XPS spectra of ZnO/Fe3O4 NCs: (a) survey spectrum, (b) Fe2p, (c) Zn2p, (d) C1s, and (e) O1s.

3.6 Thermal analysis

Thermal characteristics of ZnO/Fe3O4 NCs were determined simultaneously in a single run by using TGA and DTA (Figure 7). TGA results showed that the thermal decomposition of ZnO/Fe3O4 NCs occurred in four steps. Initially, up to 100°C, the weight loss of 5.2% was due to the loss of adsorbed water on the surface of NCs. The weight loss observed in the second step (200–400°C) was 17.3%, which might be due to the dismissal of biomolecules capped on the surface of NCs. The loss in weight observed in between 400 and 600°C (third step) was assigned to the adsorbed oxygen species [56]. In the last step, a loss of 7.5% in weight was observed up to 800°C. DTA thermogram (Figure 7) displayed energy changes irrespective of change in weight. The peaks observed at 328 and 599°C were associated with the release of bioactive molecules and adsorbed oxygen, respectively. A peak at 927°C in DTA thermogram probably infers a crystalline transition of ZnO/Fe3O4 NCs.

Figure 7 Thermograms of ZnO/Fe3O4 NCs.
Figure 7

Thermograms of ZnO/Fe3O4 NCs.

3.7 Assessment of the photocatalytic activity

The photodegradation of MB in the presence of as-prepared nanoproducts was examined under visible light, and the extent of degradation was measured in terms of absorbance of MB solution using a UV-Vis spectrophotometer after certain intervals of time for 150 min. The results of degradation studies are showcased in (Figures 8 and (9, and Table 1, which revealed that the degradation of MB increases with an increasing irradiation time. From the absorbance spectra of MB (Figure 8 and Table 1), it can be seen clearly that initially, 15 min of exposure to sunlight, MB solution was degraded by 6.14, 2.27, and 28.03% and after 90 min, MB solution was degraded by 48.3, 29.94, and 63.25% in the presence of biosynthesized ZnO, Fe3O4, and ZnO/Fe3O4 samples, respectively.

Figure 8 UV-Vis absorbance spectra of MB solution during the photocatalytic process with biosynthesized: (a) ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs.
Figure 8

UV-Vis absorbance spectra of MB solution during the photocatalytic process with biosynthesized: (a) ZnO, (b) Fe3O4, and (c) ZnO/Fe3O4 NCs.

Figure 9 Graphical portrayal of percentage removal of MB at 15, 90, and 150 min in the presence of as-prepared ZnO, Fe3O4, and ZnO/Fe3O4.
Figure 9

Graphical portrayal of percentage removal of MB at 15, 90, and 150 min in the presence of as-prepared ZnO, Fe3O4, and ZnO/Fe3O4.

Table 1

Comparative analysis on the photoremediation of MB in the presence of biosynthesized ZnO, Fe3O4, and ZnO/Fe3O4 NCs for a period of 150 min

Sr. no. Time (min) ZnO (E max) Fe3O4 (E max) ZnO/Fe3O4 (E max)
1 Initially 1.32 1.32 1.32
2 15 1.239 1.29 0.956
3 30 0.987 1.19 0.854
4 45 0.914 1.12 0.806
5 60 0.865 1.023 0.772
6 75 0.722 0.992 0.578
7 90 0.682 0.93 0.485
8 150 0.202 0.829 0.012

As shown in Figure 8, MB dye was almost completely degraded (99.09%) by ZnO/Fe3O4 NCs in 150 min, whereas ZnO and Fe3O4 NPs degraded it by 84.7 and 37.1%, respectively. These outcomes of MB absorbance spectra revealed that the degradation efficiency of ZnO NPs was increased in the presence of Fe3O4 NPs. The enhancement in MB removal by ZnO/Fe3O4 NCs compared to ZnO NPs indicated the synergistic effect between ZnO and Fe3O4, assigning to the degradation of MB.

Moreover, the degradation efficiency of ZnO/Fe3O4 NCs was examined for three consecutive runs, and the results are shown in Figure 10.

Figure 10 Reutilizing performance of ZnO/Fe3O4 up to three cycles.
Figure 10

Reutilizing performance of ZnO/Fe3O4 up to three cycles.

From the results, it is clear that the composites were active up to three cycles. Although in the third cycle, the degradation efficiency was decreased (90.1%). This decrement may be due to the adsorbance of some MB on the surface of photocatalyst, which perhaps blocks some active sites of NCs and can also be due to some loss of NCs during the recovery process.

The possible mechanism for the photodegradation of MB dye over biosynthesized ZnO/Fe3O4 NCs under visible light is shown in Figure 11.

Figure 11 Possible mechanism of photocatalytic degradation of MB in the presence of C. viminalis leaves’ extract-mediated biosynthesized ZnO/Fe3O4 NCs.
Figure 11

Possible mechanism of photocatalytic degradation of MB in the presence of C. viminalis leaves’ extract-mediated biosynthesized ZnO/Fe3O4 NCs.

The phenomenon of photodegradation of MB takes place when visible light is irradiated on the photocatalyst (ZnO, Fe3O4, or ZnO/Fe3O4), which leads to the generation of electron–hole pairs in conduction/valence bands (VBs) simultaneously on the surface of the photocatalyst (equation (2)). In the conduction band (CB), oxygen on the surface of the photocatalyst combines with the excited electron and forms ˙ O 2 − (superoxide radical; equation (3)). This radical checks the recombination of e−/h+ pairs by converting into ˙OH radicals through hydroperoxyl radicals (HOO˙) and H2O2 intermediates (equation (4)). Simultaneously, holes produced in VB react with the surface water to produce hydroxyl radicals (˙OH; equation (5)). The hydroxyl radicals produced in CB and VB, on the surface of photocatalyst, act as a strong oxidizing agent, which in turn degrade MB molecules into simple inorganic molecules, such as water, carbon dioxide, and inorganic ions (equation (6)). The survey of the previous literature also reveals that ˙ O 2 − (superoxide) radicals and hydroxyl radicals (˙OH) are the leading reactive species for the photodegradation of MB dye [57].

As shown in Figure 8 and Table 1, the absorption intensity of dye gradually decreases with an increasing irradiation time and finally diminished in case of ZnO/Fe3O4. This is because of a breakdown of the heterocyclic conjugated structure of MB molecule into simple molecules, such as water, carbon dioxide, and inorganic ions. Apart from this, the photocatalytic efficiency of ZnO/Fe3O4 NCs was greater compared to ZnO NPs, and this can be summarized as follows: Fe3O4 NPs possess a narrow bandgap, and hence, e−/h+ pairs produced in it under irradiation recombines fastly, as a result charge carriers could not survive for a long time for the photocatalysis process [58]. In ZnO/Fe3O4 NCs, the energy level of CB and VB of ZnO differs from that of Fe3O4. During irradiation, some photogenerated electrons from ZnO are captured by Fe3O4 NPs at the composite’s interface, where they react with the surface oxygen to form superoxide radicals. However, some holes transfer to VB of Fe3O4 from ZnO and react with the surface water to produce hydroxyl radicals (˙OH). This phenomenon at the interface restricts an electron–hole recombination in ZnO. As a resultant, the generation of reactive species increases at the junction of ZnO–Fe3O4, which accelerates the degradation of dye molecules [59]. Hence, the efficient charge transfer separation at heterojunction of two different semiconductor materials attributes to an enhanced photo-catalytic activity of ZnO/Fe3O4 NCs to degrade MB solution. However, a comparison data for photodegradation of MB dye solution by ZnO/Fe3O4 NCs synthesized by different routes are displayed in Table 2. The results show considerable proficiency for the current study of MB degradation by C. viminalis-synthesized ZnO/Fe3O4 NCs.

(2) Photocatalyst surface + h ν → e CB −   + h VB + ,

(3) 2 e CB − + 2 O 2 → 2 O 2 ⋅ ,

(4) 2 ⋅ O 2 − + 2 H + → 2 HOO ⋅ → H 2 O 2 → 2 O ⋅ H ( oxidizing agent ) ,

(5) h VB + + H 2 O → H + + O ⋅ H ( oxidizing agent ) ,

(6) O ⋅ H + MB → Degradation products ( CO 2 + H 2 O + Simple inorganic ions ) .

Table 2

A comparable study of MB dye removal by ZnO/Fe3O4 NCs (from the literature) with present study

S. no. ZnO/Fe3O4 (ppm) MB (ppm) Synthesis method Degradation time (min) Degradation efficiency (%) Ref.
1 50 10 Hydrothermal 180 89.2 [29]
2 500 20 One-pot synthesis 90 98.9 [37]
3 2,500 20 Microwave reactor 60 63.02 [60]
4 160 32 Biosynthesis 150 99.09 Present study

4 Conclusion

In this study, ZnO/Fe3O4 NCs as well as ZnO and Fe3O4 NPs were successfully synthesized via eco-friendly route using C. viminalis leaves’ extract without using any toxic additives. FTIR study indicated that the leaves’ extract played a key role in the reduction and stabilization of ZnO/Fe3O4 NCs, ZnO NPs, and Fe3O4 NPs, through the interaction of O–H, C═O, and C═C groups of phytochemicals present in C. viminalis leaves’ extract. Nanosize and the presence of pure phase in the crystal structure of biosynthesized products without major impurities, were confirmed by XRD analysis. XRD results were supported by XPS outcomes and revealed the formation of Zn–Fe hetero-junction in ZnO/Fe3O4 NCs. Evidence of SEM, TEM, and EDX analyses also confirms the existence of Zn and Fe in composite nanoparticles. In addition, the photodegradation of MB under visible light irradiation was carried out using synthesized ZnO, Fe3O4, and ZnO/Fe3O4 as a photocatalyst. The results obtained in this study demonstrate that compared to monometallic (ZnO and Fe3O4) NPs, bimetallic NCs of Zn and Fe (ZnO/Fe3O4) accelerated the degradation of MB. The enhanced photocatalytic activity was attributed to the synergistic effect between ZnO and Fe3O4 nanoparticles in ZnO/Fe3O4 NCs. Moreover, ZnO/Fe3O4 NCs can be reused for three successive runs. Therefore, these findings suggest that ZnO/Fe3O4 NCs synthesized via C. viminalis leaves’ extract have a potential as an efficient photocatalyst for water purification.

Acknowledgements

The authors would like to thank the Chancellor, Jaipur National University, Jaipur of India for providing laboratory facilities for this study.

  1. Funding information: This study was funded by the Researchers Supporting Project Number (RSP-2021/339) King Saud University, Riyadh, Saudi Arabia.

  2. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

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

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Received: 2021-09-07
Revised: 2021-10-11
Accepted: 2021-10-26
Published Online: 2021-11-22

© 2021 Poonam Dwivedi et al., published by De Gruyter

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

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  108. Application of antiviral materials in textiles: A review
  109. Phase transformation and strengthening mechanisms of nanostructured high-entropy alloys
  110. Research progress on individual effect of graphene oxide in cement-based materials and its synergistic effect with other nanomaterials
  111. Catalytic defense against fungal pathogens using nanozymes
  112. A mini-review of three-dimensional network topological structure nanocomposites: Preparation and mechanical properties
  113. Mechanical properties and structural health monitoring performance of carbon nanotube-modified FRP composites: A review
  114. Nano-scale delivery: A comprehensive review of nano-structured devices, preparative techniques, site-specificity designs, biomedical applications, commercial products, and references to safety, cellular uptake, and organ toxicity
  115. Effects of alloying, heat treatment and nanoreinforcement on mechanical properties and damping performances of Cu–Al-based alloys: A review
  116. Recent progress in the synthesis and applications of vertically aligned carbon nanotube materials
  117. Thermal conductivity and dynamic viscosity of mono and hybrid organic- and synthetic-based nanofluids: A critical review
  118. Recent advances in waste-recycled nanomaterials for biomedical applications: Waste-to-wealth
  119. Layup sequence and interfacial bonding of additively manufactured polymeric composite: A brief review
  120. Quantum dots synthetization and future prospect applications
  121. Approved and marketed nanoparticles for disease targeting and applications in COVID-19
  122. Strategies for improving rechargeable lithium-ion batteries: From active materials to CO2 emissions
https://doi.org/10.1515/ntrev-2021-0117
Schlagwörter für diesen Artikel
ZnO/Fe3O4 nanocomposites; Callistemon viminalis; XPS; photodegradation; methylene blue
Creative Commons
BY 4.0

Artikel in diesem Heft

  1. Research Articles
  2. Improved impedance matching by multi-componential metal-hybridized rGO toward high performance of microwave absorption
  3. Pure-silk fibroin hydrogel with stable aligned micropattern toward peripheral nerve regeneration
  4. Effective ion pathways and 3D conductive carbon networks in bentonite host enable stable and high-rate lithium–sulfur batteries
  5. Fabrication and characterization of 3D-printed gellan gum/starch composite scaffold for Schwann cells growth
  6. Synergistic strengthening mechanism of copper matrix composite reinforced with nano-Al2O3 particles and micro-SiC whiskers
  7. Deformation mechanisms and plasticity of ultrafine-grained Al under complex stress state revealed by digital image correlation technique
  8. On the deformation-induced grain rotations in gradient nano-grained copper based on molecular dynamics simulations
  9. Removal of sulfate from aqueous solution using Mg–Al nano-layered double hydroxides synthesized under different dual solvent systems
  10. Microwave-assisted sol–gel synthesis of TiO2-mixed metal oxide nanocatalyst for degradation of organic pollutant
  11. Electrophoretic deposition of graphene on basalt fiber for composite applications
  12. Polyphenylene sulfide-coated wrench composites by nanopinning effect
  13. Thermal conductivity and thermoelectric properties in 3D macroscopic pure carbon nanotube materials
  14. An effective thermal conductivity and thermomechanical homogenization scheme for a multiscale Nb3Sn filaments
  15. Friction stir spot welding of AA5052 with additional carbon fiber-reinforced polymer composite interlayer
  16. Improvement of long-term cycling performance of high-nickel cathode materials by ZnO coating
  17. Quantum effects of gas flow in nanochannels
  18. An approach to effectively improve the interfacial bonding of nano-perfused composites by in situ growth of CNTs
  19. Effects of nano-modified polymer cement-based materials on the bending behavior of repaired concrete beams
  20. Effects of the combined usage of nanomaterials and steel fibres on the workability, compressive strength, and microstructure of ultra-high performance concrete
  21. One-pot solvothermal synthesis and characterization of highly stable nickel nanoparticles
  22. Comparative study on mechanisms for improving mechanical properties and microstructure of cement paste modified by different types of nanomaterials
  23. Effect of in situ graphene-doped nano-CeO2 on microstructure and electrical contact properties of Cu30Cr10W contacts
  24. The experimental study of CFRP interlayer of dissimilar joint AA7075-T651/Ti-6Al-4V alloys by friction stir spot welding on mechanical and microstructural properties
  25. Vibration analysis of a sandwich cylindrical shell in hygrothermal environment
  26. Water barrier and mechanical properties of sugar palm crystalline nanocellulose reinforced thermoplastic sugar palm starch (TPS)/poly(lactic acid) (PLA) blend bionanocomposites
  27. Strong quadratic acousto-optic coupling in 1D multilayer phoxonic crystal cavity
  28. Three-dimensional shape analysis of peripapillary retinal pigment epithelium-basement membrane layer based on OCT radial images
  29. Solvent regulation synthesis of single-component white emission carbon quantum dots for white light-emitting diodes
  30. Xanthate-modified nanoTiO2 as a novel vulcanization accelerator enhancing mechanical and antibacterial properties of natural rubber
  31. Effect of steel fiber on impact resistance and durability of concrete containing nano-SiO2
  32. Ultrasound-enhanced biosynthesis of uniform ZnO nanorice using Swietenia macrophylla seed extract and its in vitro anticancer activity
  33. Temperature dependence of hardness prediction for high-temperature structural ceramics and their composites
  34. Study on the frequency of acoustic emission signal during crystal growth of salicylic acid
  35. Controllable modification of helical carbon nanotubes for high-performance microwave absorption
  36. Role of dry ozonization of basalt fibers on interfacial properties and fracture toughness of epoxy matrix composites
  37. Nanosystem’s density functional theory study of the chlorine adsorption on the Fe(100) surface
  38. A rapid nanobiosensing platform based on herceptin-conjugated graphene for ultrasensitive detection of circulating tumor cells in early breast cancer
  39. Improving flexural strength of UHPC with sustainably synthesized graphene oxide
  40. The role of graphene/graphene oxide in cement hydration
  41. Structural characterization of microcrystalline and nanocrystalline cellulose from Ananas comosus L. leaves: Cytocompatibility and molecular docking studies
  42. Evaluation of the nanostructure of calcium silicate hydrate based on atomic force microscopy-infrared spectroscopy experiments
  43. Combined effects of nano-silica and silica fume on the mechanical behavior of recycled aggregate concrete
  44. Safety study of malapposition of the bio-corrodible nitrided iron stent in vivo
  45. Triethanolamine interface modification of crystallized ZnO nanospheres enabling fast photocatalytic hazard-free treatment of Cr(vi) ions
  46. Novel electrodes for precise and accurate droplet dispensing and splitting in digital microfluidics
  47. Construction of Chi(Zn/BMP2)/HA composite coating on AZ31B magnesium alloy surface to improve the corrosion resistance and biocompatibility
  48. Experimental and multiscale numerical investigations on low-velocity impact responses of syntactic foam composites reinforced with modified MWCNTs
  49. Comprehensive performance analysis and optimal design of smart light pole for cooperative vehicle infrastructure system
  50. Room temperature growth of ZnO with highly active exposed facets for photocatalytic application
  51. Influences of poling temperature and elongation ratio on PVDF-HFP piezoelectric films
  52. Large strain hardening of magnesium containing in situ nanoparticles
  53. Super stable water-based magnetic fluid as a dual-mode contrast agent
  54. Photocatalytic activity of biogenic zinc oxide nanoparticles: In vitro antimicrobial, biocompatibility, and molecular docking studies
  55. Hygrothermal environment effect on the critical buckling load of FGP microbeams with initial curvature integrated by CNT-reinforced skins considering the influence of thickness stretching
  56. Thermal aging behavior characteristics of asphalt binder modified by nano-stabilizer based on DSR and AFM
  57. Building effective core/shell polymer nanoparticles for epoxy composite toughening based on Hansen solubility parameters
  58. Structural characterization and nanoscale strain field analysis of α/β interface layer of a near α titanium alloy
  59. Optimization of thermal and hydrophobic properties of GO-doped epoxy nanocomposite coatings
  60. The properties of nano-CaCO3/nano-ZnO/SBR composite-modified asphalt
  61. Three-dimensional metallic carbon allotropes with superhardness
  62. Physical stability and rheological behavior of Pickering emulsions stabilized by protein–polysaccharide hybrid nanoconjugates
  63. Optimization of volume fraction and microstructure evolution during thermal deformation of nano-SiCp/Al–7Si composites
  64. Phase analysis and corrosion behavior of brazing Cu/Al dissimilar metal joint with BAl88Si filler metal
  65. High-efficiency nano polishing of steel materials
  66. On the rheological properties of multi-walled carbon nano-polyvinylpyrrolidone/silicon-based shear thickening fluid
  67. Fabrication of Ag/ZnO hollow nanospheres and cubic TiO2/ZnO heterojunction photocatalysts for RhB degradation
  68. Fabrication and properties of PLA/nano-HA composite scaffolds with balanced mechanical properties and biological functions for bone tissue engineering application
  69. Investigation of the early-age performance and microstructure of nano-C–S–H blended cement-based materials
  70. Reduced graphene oxide coating on basalt fabric using electrophoretic deposition and its role in the mechanical and tribological performance of epoxy/basalt fiber composites
  71. Effect of nano-silica as cementitious materials-reducing admixtures on the workability, mechanical properties and durability of concrete
  72. Machine-learning-assisted microstructure–property linkages of carbon nanotube-reinforced aluminum matrix nanocomposites produced by laser powder bed fusion
  73. Physical, thermal, and mechanical properties of highly porous polylactic acid/cellulose nanofibre scaffolds prepared by salt leaching technique
  74. A comparative study on characterizations and synthesis of pure lead sulfide (PbS) and Ag-doped PbS for photovoltaic applications
  75. Clean preparation of washable antibacterial polyester fibers by high temperature and high pressure hydrothermal self-assembly
  76. Al 5251-based hybrid nanocomposite by FSP reinforced with graphene nanoplates and boron nitride nanoparticles: Microstructure, wear, and mechanical characterization
  77. Interlaminar fracture toughness properties of hybrid glass fiber-reinforced composite interlayered with carbon nanotube using electrospray deposition
  78. Microstructure and life prediction model of steel slag concrete under freezing-thawing environment
  79. Synthesis of biogenic silver nanoparticles from the seed coat waste of pistachio (Pistacia vera) and their effect on the growth of eggplant
  80. Study on adaptability of rheological index of nano-PUA-modified asphalt based on geometric parameters of parallel plate
  81. Preparation and adsorption properties of nano-graphene oxide/tourmaline composites
  82. A study on interfacial behaviors of epoxy/graphene oxide derived from pitch-based graphite fibers
  83. Multiresponsive carboxylated graphene oxide-grafted aptamer as a multifunctional nanocarrier for targeted delivery of chemotherapeutics and bioactive compounds in cancer therapy
  84. Piezoresistive/piezoelectric intrinsic sensing properties of carbon nanotube cement-based smart composite and its electromechanical sensing mechanisms: A review
  85. Smart stimuli-responsive biofunctionalized niosomal nanocarriers for programmed release of bioactive compounds into cancer cells in vitro and in vivo
  86. Photoremediation of methylene blue by biosynthesized ZnO/Fe3O4 nanocomposites using Callistemon viminalis leaves aqueous extract: A comparative study
  87. Study of gold nanoparticles’ preparation through ultrasonic spray pyrolysis and lyophilisation for possible use as markers in LFIA tests
  88. Review Articles
  89. Advance on the dispersion treatment of graphene oxide and the graphene oxide modified cement-based materials
  90. Development of ionic liquid-based electroactive polymer composites using nanotechnology
  91. Nanostructured multifunctional electrocatalysts for efficient energy conversion systems: Recent perspectives
  92. Recent advances on the fabrication methods of nanocomposite yarn-based strain sensor
  93. Review on nanocomposites based on aerospace applications
  94. Overview of nanocellulose as additives in paper processing and paper products
  95. The frontiers of functionalized graphene-based nanocomposites as chemical sensors
  96. Material advancement in tissue-engineered nerve conduit
  97. Carbon nanostructure-based superhydrophobic surfaces and coatings
  98. Functionalized graphene-based nanocomposites for smart optoelectronic applications
  99. Interfacial technology for enhancement in steel fiber reinforced cementitious composite from nano to macroscale
  100. Metal nanoparticles and biomaterials: The multipronged approach for potential diabetic wound therapy
  101. Review on resistive switching mechanisms of bio-organic thin film for non-volatile memory application
  102. Nanotechnology-enabled biomedical engineering: Current trends, future scopes, and perspectives
  103. Research progress on key problems of nanomaterials-modified geopolymer concrete
  104. Smart stimuli-responsive nanocarriers for the cancer therapy – nanomedicine
  105. An overview of methods for production and detection of silver nanoparticles, with emphasis on their fate and toxicological effects on human, soil, and aquatic environment
  106. Effects of chemical modification and nanotechnology on wood properties
  107. Mechanisms, influencing factors, and applications of electrohydrodynamic jet printing
  108. Application of antiviral materials in textiles: A review
  109. Phase transformation and strengthening mechanisms of nanostructured high-entropy alloys
  110. Research progress on individual effect of graphene oxide in cement-based materials and its synergistic effect with other nanomaterials
  111. Catalytic defense against fungal pathogens using nanozymes
  112. A mini-review of three-dimensional network topological structure nanocomposites: Preparation and mechanical properties
  113. Mechanical properties and structural health monitoring performance of carbon nanotube-modified FRP composites: A review
  114. Nano-scale delivery: A comprehensive review of nano-structured devices, preparative techniques, site-specificity designs, biomedical applications, commercial products, and references to safety, cellular uptake, and organ toxicity
  115. Effects of alloying, heat treatment and nanoreinforcement on mechanical properties and damping performances of Cu–Al-based alloys: A review
  116. Recent progress in the synthesis and applications of vertically aligned carbon nanotube materials
  117. Thermal conductivity and dynamic viscosity of mono and hybrid organic- and synthetic-based nanofluids: A critical review
  118. Recent advances in waste-recycled nanomaterials for biomedical applications: Waste-to-wealth
  119. Layup sequence and interfacial bonding of additively manufactured polymeric composite: A brief review
  120. Quantum dots synthetization and future prospect applications
  121. Approved and marketed nanoparticles for disease targeting and applications in COVID-19
  122. Strategies for improving rechargeable lithium-ion batteries: From active materials to CO2 emissions
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Heruntergeladen am 11.10.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ntrev-2021-0117/html?lang=de
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