Electron-hole recombination effect of SnO2 – CuO nanocomposite for improving methylene blue photocatalytic activity in wastewater treatment under visible light

V. Perumal; R. Uthrakumar; M. Chinnathambi; C. Inmozhi; R. Robert; M.E. Rajasaravanan; A. Raja; K. Kaviyarasu

doi:10.1016/j.jksus.2022.102388

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Original article

01 2022

:35;

102388

doi:

10.1016/j.jksus.2022.102388

Electron-hole recombination effect of SnO₂ – CuO nanocomposite for improving methylene blue photocatalytic activity in wastewater treatment under visible light

V. Perumal^{^a}, R. Uthrakumar^{^a,⁎}, M. Chinnathambi^{^b}, C. Inmozhi^{^c}, R. Robert^{^b}, M.E. Rajasaravanan^{^a}, A. Raja^{^d}, K. Kaviyarasu^{^e,^f,⁎}

a Department of Physics, Govt. Arts College (Autonomous), Salem 636007, Tamil Nadu, India

b Department of Physics, Govt. Arts College for Men, Krishnagiri 635001, Tamil Nadu, India

c Department of Physics, Govt. Arts College for Women, Salem 636008, Tamil Nadu, India

d Department of Chemistry, College of Natural Sciences, Yeungnam University, Gyeongsan, Republic of Korea

e UNESCO-UNISA Africa Chair in Nanosciences/Nanotechnology Laboratories, College of Graduate Studies, University of South Africa (UNISA), Muckleneuk Ridge, PO Box 392, Pretoria, South Africa

f Nanosciences African Network (NANOAFNET), Materials Research Group (MRG), iThemba LABS-National Research Foundation (NRF), 1 Old Faure Road, 7129, PO Box 722, Somerset West, Western Cape Province, South Africa

⁎Corresponding authors at: UNESCO-UNISA Africa Chair in Nanosciences/Nanotechnology Laboratories, College of Graduate Studies, University of South Africa (UNISA), Muckleneuk Ridge, PO Box 392, Pretoria, South Africa (K. Kaviyarasu). uthraloyola@yahoo.com (R. Uthrakumar), kavi@tlabs.ac.za (K. Kaviyarasu)

Received: 2022-6-11, Accepted: 2022-10-17,

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

Heterojunction photocatalysts have gained much attraction in pollutant degradation applications due to their unique good adsorption and photocatalytic decomposition capacity and more cycle durability. Tin oxide (SnO₂) doped with copper oxide (CuO) heterostructured photocatalyst was synthesized by a simple solution processes technique. X-ray diffraction and fluorescence spectroscopy were used to examine the structural properties of the SnO₂ - CuO heterostructure. Analyses of FE-SEM and TEM were performed on the samples to determine their surface morphology. The photodegradation property of SnO₂ - CuO heterostructure was studied using methylene blue (MB) model pollutant, where SnO₂ - CuO heterostructure (90.3 % at 180 min) was shown better than the SnO₂. Therefore, the n-p-junction (SnO₂ - CuO) heterostructure catalysis boosted the photodegradation of MB detailed studies on the electron-hole pair recombination were conducted on n-p-junctions to observe the effect of the interface on the recombination have been published.

Keywords

SnO2 – CuO heterostructure

Photodegradation

Electron-hole pair recombination

Electron microscopy

Heterojunction photocatalysts

Visible light irradiation

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1 Introduction

The fast industrialization and civilization process is creating the most hazardous pollution in the environment. Water pollution is one of the major concerns of eco-friendly environments (Kaviyarasu et al., 2012). Water pollution did not only create serious health impacts and have changed the lifestyle of water-living organisms (Perumal et al., 2022). Further, the premature deaths counts were increased day by day owing to the water pollution (Kasinathan et al., 2016). The recycling or purification of textiles, food, paint, and leather industries wastes (organic pollutant) are challenging task, because are it easily mixed with water resource (Chandrasekar et al., 2021). Research communities are much interested to develop the fast, highly efficient, and low-cost degradation method (physical, chemical, and biological). Among them, solar-driven semiconductor - based photocatalysis technology have gained much attention owing to the simple, eco-friendly, and can decomposed the organic pollutants without secondary products (Arularasu et al., 2018; Panimalar et al., 2020; Amal George et al., 2022 ). The different semiconductor materials were used for photocatalysts process such as metal oxide (Geetha et al., 2018; Panimalar et al., 2022; Raja et al., 2019; Perumal et al., 2022 ), transition metal sulfide (Panimalar et al., 2022; Chandrasekar et al., 2022; Manjula et al., 2018; Amanulla et al., 2021 ), carbon-based materials (Thirupathy et al., 2020; Kayalvizhi et al., 2022; Subbareddy et al., 2020; Alhaji et al., 2019 ), and metal-organic frameworks (MOFs). Among them, metal oxide widely investigated for photocatalytic field, which owing to the high chemical stability, low toxic nature, wide bandgap, and large exaction biding energy. Most of semiconductors metal oxide only absorbs UV lights only, which limited the practical application. The combination of two metal oxides was not only cover the visible and UV spectra, also boosted the photocatalytic properties.

The use of metal oxide nanostructures in electronics, optics, and photonics systems has gained wide attention because of their wide bandgaps (3.7 eV) and large exciton binding energies (60 meV) (Kennedy et al., 2017; Fang et al., 2014; Murmu et al., 2021 ). Among them, SnO₂ and CuO heterojunction were formed the n-p-junction, which was boosted the photocatalytic properties due to their high photosensitivity, reduce the recombination rate, non-toxic nature, and large bandgap. SnO₂ is wide bandgap n-type semiconductor (3.7 eV) and CuO is a p-type semiconductor (1.5 eV). In n-p-heterojunction, CuO was acts as a sink, where it helps to sperate the electron-hole pair (reduced the recombination) and the photogenerated electrons-holes pair move in the opposite direction, get gather in the valence band of SnO₂ and efficiently pairs of electrons and holes recombine less frequently. Due to the low recombination of (high movement of electron in the opposite direction) SnO₂ - CuO heterostructure, the photocatalytic property of SnO₂ - CuO heterostructure will be improved (George et al., 2022; Kumar et al., 2016). In this study, SnO₂ - CuO heterostructured photocatalyst was synthesized by a simple solution processes method. The as structural, optical, morphology were thoroughly characterized by XRD, UV–vis spectroscopy, FESEM and EDX. As MB dye degradation was illuminated with UV light, the catalysts were measured for their activity. The photocatalytic activities in the degradation of high concentrated malachite green dyes have been investigated in detailed.

2 Experimental

2.1

2.1 Materials

Copper acetate tetrahydrate (Cu(CO₂CH₃)₂·4H₂O), tin chloride pentahydrate (SnCl₄·5H₂O), sodium hydroxide (NaOH), Polyvinylpyrrolidone (PVP), Ethanol (C₂H₅OH) purchasing was done through Sisco Research Laboratories Pvt. ltd, India. No further purification was performed on the chemicals.

2.2

2.2 Synthesis method of SnO₂ - CuO heterostructured photocatalyst

SnO₂ - CuO heterostructured photocatalyst was synthesized by a simple solution processes method. Initially, 1:1 ratio of copper acetate tetrahydrate and tin chloride pentahydrate were added in 100 mL deionized (DI) water and stirrer 1 h. In addition to the clear solution, PVP was added in 0.1 g and stirred for 15 min. Then, 1.5 g of sodium hydroxide was dissolved 50 mL and sodium hydroxide solution gradually added the above homogeneous solution. Several times, DI water and ethanol were used to wash the precipitate. A final annealing at 400 °C for 3 hrs in an air atmosphere was followed by a drying at 80 °C overnight. The product was noted as SnO₂ - CuO. For comparison, SnO₂ and CuO were also synthesized under the same reaction condition without copper acetate tetrahydrate and tin chloride pentahydrate, respectively.

2.3

2.3 Characterization techniques

The crystalline structure of as-synthesized sample was characterized by X-ray diffractometer (XRD) (AERIS high-resolution bench top) with CuK_α radiation. The morphology and energy dispersive X-ray spectroscopy (EDX) of SnO₂ - CuO was investigated by FE-SEM (Thermo scientific Apreo S) with an acceleration voltage of 20 kV and TEM (JEOL Japan, JEM-2100 Plus) with an acceleration voltage of 200 kV. μ-Raman vibration modes of as synthesized samples were examined by Raman spectrometer (HORIBA France, LABRAM HR Evolution) at green (532 nm) laser light. The optical absorption properties of the samples were performed by UV–vis-DRS SHIMADZU, UV 3600 PLUS analysis, to evaluate the optical properties of the samples.

2.4

2.4 Photocatalytic studies

By degrading organic pollutants under visible light, SnO₂ - CuO heterostructured catalysts were evaluated for their photocatalytic properties. We stirred 50 mL of DI water for 15 min with 10 ppm of methylene blue (MB) dye and 10 ppm of magnesium blue (MB) dye. Then, 50 mg of SnO₂ - CuO heterostructured catalyst was added the above solution and stirred 20 min under the dark condition. An under visible light irradiated 10 cm away from the surface of the solution was then used to expose the model pollutant with catalyst. The organic pollutant solution was collected each 30 min and studied the UV–vis absorption spectrum. The decomposition rate of each catalyst was studied by following equation (Abinaya et al., 2018).

(1)

D (%) = \frac{C_{0} - C_{t}}{C_{0}} \times 100

3 Results and discussion

3.1

3.1 XRD pattern

The SnO₂ sample (Fig. 1) shows the diffraction peaks at 25.38°, 33.81°, 38.91°, 51.55°, 54.37°, 57.93°, 61.46°, 64.75° and 65.61° are assigned to (1 1 0), (1 0 1), (2 0 0), (2 1 0), (2 1 1), (2 2 0), (0 0 2), (3 1 0), (1 1 2) and (3 0 1) planes, respectively. It was matched with tetragonal rutile structure (JCPDS card no. 41–1445). It appears that CuO diffraction peaks are located at 32.51°, 35.55°, 38.72°, 48.75°, 53.48°, 58.25°, 61.51°, 66.21°, and 68.07°, which correspond to planes as follows: (1 1 0), (0 0 2), (1 1 1), ( −2 0 2), (0 2 0), (2 0 2), ( −1 1 3), ( −3 1 1), and (2 2 0). All the peaks are well-matched with the monoclinic CuO (JCPDS card no. 48–1548). Further composite the SnO₂ and CuO, there was no significant changes in the diffraction pattern, which could be attributed to the formation SnO₂ - CuO nanocomposite (Mariammal et al., 2012).

XRD pattern of samples containing SnO2, CuO, and SnO2 - CuO nanocomposites.

3.2

3.2 μ-Raman spectrum

The vibration mode of SnO₂ - CuO composite was analyzed by μ-Raman analysis as shown in Fig. 2. The peaks located at 633 cm⁻¹ and 779 cm⁻¹ could be assigned to the (A_1g) symmetric and (B_2g) asymmetric stretching of Sn-O bonds, respectively. The peak at ∼ 569 cm⁻¹ represent (E_g) doubly degenerate mode of oxygen ions in SnO₂. In CuO sample was observed with three peaks at 295, 345, and 625 cm⁻¹, which are assigned to the A_g mode (oxygen vibrations along the crystallographic b-axis), B_1g mode (a-axis vibrations of oxygen), and B_2g mode (oxygen vibrations perpendicular to the b-axes). Thus, the presence of SnO₂ and CuO in the composites were confirmed from the μ-Raman spectroscopy (Kumar et al., 2021).

μ-Raman spectrum of SnO2, CuO, and SnO2 - CuO nanocomposite samples.

3.3

3.3 FTIR analysis

The functional properties of SnO₂, CuO and SnO₂ - CuO heterostructure sample were studied by FTIR analysis as shown in Fig. 3. At 3433 cm⁻¹, a broad band was observed; it was attributed to the stretching vibration of water molecules in the O—H direction. Due to the presence of PVP in the SnO₂ - CuO heterostructure, two more-absorption bands were observed at 2927 cm⁻¹ and 1388 cm⁻¹, which correspond to N—H and C—H vibrations. There are two peaks at 620 cm⁻¹ and 580 cm⁻¹ corresponding to Sn-O and Cu–O vibrations, respectively. The most inorganic metal–oxygen (M−O) stretching modes were observed 700 cm⁻¹ to 400 cm⁻¹. From the FTIR analysis, the presence and formation of SnO₂ - CuO heterostructure were confirmed (Joshi et al., 2016; Wang et al., 2018).

FTIR spectrum of SnO2, CuO, and SnO2 - CuO nanocomposite samples.

3.4

3.4 UV–vis analysis

The optical absorption and optical bandgap of SnO₂, CuO and SnO₂ - CuO heterostructure samples as shown in Fig. 4(a-c). Within the 200 nm to 800 nm wavelength range of pure SnO₂, CuO, and SnO₂ - CuO samples were studied for their optical absorption spectra. The SnO₂ and CuO samples exhibited an absorption edge around ∼400 and 800 nm, respectively. When combination with SnO₂ and CuO (heterostructure), the intermediate absorption edge was observed at 500 nm. The shift indicates that the introduction of a new energy level presence in the bandgap. The energy bandgap values have been calculated by Kubelka-Munk. At any wavelength, the Kubelka-Munk function is given by equation 2 and 3.

(2)

\frac{α}{S} = F (R) = \frac{{(1 - R)}^{2}}{2 R}

(3)

R = \frac{R_{Sample}}{R_{Standard}}

(a-c) UV–vis absorption spectrum of SnO2, CuO, and SnO2 - CuO samples and; (d-f) bandgap energy of SnO2, CuO, and SnO2 - CuO samples.

‘α’ is the absorption coefficient, ‘S’ is the scattering coefficient, and F(R) is the (K-M) Kubelka Munk function. The bandgap of SnO₂, CuO and SnO₂ - CuO samples were found to be 3.36 eV, 1.51 eV, and 2.3 eV, respectively as shown in inset Fig. 4(d-f). This new energy level was increasing the photocatalytic properties (Harish et al., 2016).

3.5

3.5 Morphology analysis

The morphology of SnO₂ - CuO heterostructures were analyzed by FESEM techniques. As shown in Fig. 5(a-f), SnO₂, CuO and SnO₂ - CuO heterostructure samples exhibit different morphologies. The FESEM image of SnO₂ in Fig. 5(a-b) shows rock-like morphology and it agglomerated. In Fig. 5(c-d) shows the FESEM image of CuO, which was nanoparticles matrix. In fact, the FESEM images of SnO₂ - CuO heterostructures revealed that the sample was rock-like, and nanoparticles morphology was bunch of rock-like and nanoparticles aggregated together to form an irregular morphology as shown in Fig. 5(e-f) respectively.

(a-b) FESEM images of SnO2; (c-d) CuO; and (e-f) SnO2 - CuO nanocomposite samples.

The illustration shows TEM images of Fig. 6(a-b) SnO₂ - CuO heterostructure, the TEM results were in good agreement with FESEM (rock-like and nanoparticles morphology). Based on the TEM images of SnO₂ - CuO, the clear lattice fringes were observed, which is due to the good crystalline nature of SnO₂ - CuO nanocomposite. Nevertheless, smaller particles contain grain boundaries, which work as barriers to the passage of free carriers and traps for carriers. Furthermore, the elemental distribution mapping of SnO₂ - CuO was characterized by FESEM analysis with EDX mapping as shown in Fig. 7(a-d). The Sn, Cu and O elements were uniform distribution of rock-like SnO₂ - CuO heterostructure, where it confirmed SnO₂ - CuO in (rock-like and nanoparticles morphology structure) (Panimalar et al., 2022; Magdalane et al., 2021; Subash et al., 2022 ).

(a-b). TEM images of SnO2 - CuO nanocomposite sample.

(a-d). FESEM and EDX mapping of SnO2 - CuO nanocomposite sample.

3.6

3.6 Photocatalytic activity

The photocatalytic property of SnO₂ - CuO heterostructures were analyzed using MB model pollutant. The UV absorption spectrum of model pollutant was revealed in the Fig. 8(a-d). The degradation rate of MB was calculated from the UV–vis absorption spectra and the calculated percentage of SnO₂, CuO, and SnO₂ - CuO was 58 %, 62.2 %, and 90.3 %, respectively as shown in Fig. 8(a). In the dark condition, a negligible amount of decomposition was observed, and it as shown in Fig. 8(b). The SnO₂ - CuO heterostructure shows much better performance under light irradiation when compared with other samples, which is owing to heterojunction as shown in Fig. 8(c). The optimum concentration of Cu has formed the heterojunction, which increases the trap state in the heterojunction and reduced the recombination rate of electrons (e^-) and holes (h⁺). The Fig. 8(d) (energy band diagram of the SnO₂ - CuO heterostructure) shows possible photodegradation mechanism of MB. From photodegradation mechanism scheme, the SnO₂ - CuO heterostructure absorbed the photons from the electromagnetic radiation and electron - hole (e^-/h⁺) pair create in the heterojunction. The electrons generated by photogeneration were transferred from the CB of CuO to the CB of SnO₂. It is important for dye solution degradation to produce highly reactive radical ions, including hydroxyl radicals (OH^–) and superoxide radical ions (^•O₂). $H_{2} O + h^{+} \to H^{+} + {OH}^{+} (Oxidation)$ $O_{2} + e^{-} \to O_{2}^{-} (Reduction)$

Absorption spectrum of SnO2 - CuO heterostructure samples as a function of MB dye degradation efficiency.

Degradation efficiency of C/Co vs time (different concentration) of SnO2, CuO, and SnO2 - CuO heterostructure samples.

Reusability of SnO2 - CuO photocatalyst under light irradiation

A schematic illustration of the photocatalytic mechanism for the heterojunction SnO2 - CuO nanoparticles

These defect levels operate as active sites for the photocatalytic response because photo-generated electrons and holes can be trapped by oxygen and surface hydroxyl species. In CuO, electron-hole pairs were separated after the hole was transferred from the VB of SnO₂. Hydroxide radicals (OH^•) were formed from OH^• as OH^• was being reduced. In this reaction, the super radicals reacted with each other and gave off H₂O as a yield. These highly active species ultimately oxidize CO₂ and H₂O by generating either photogenerated electrons or holes from reactive hydroxide radicals with high oxidation abilities (Roguai and Djelloul, 2022; Begum et al., 2022).

4 Conclusion

The SnO₂ - CuO heterostructure was synthesized by a simple solution processes technique. The physical properties of SnO₂ - CuO heterostructure were deliberate by XRD and μ-Raman analysis, where the exhibits of SnO₂ and CuO were confirmed. The presences of SnO₂ and CuO in heterojunction were confirmed from the FESEM with EDX analysis. In fact, the photodegradation activity of SnO₂ - CuO heterostructure were studied by using MB model pollutant, where SnO₂ - CuO heterostructure was degrades 90.3 % amount of highly reactive with MB in 180 min and convert into inactive some other radicals. Though, the degradation percentage of SnO₂ - CuO heterostructure was high when compared with other sample due to the high catalytic and low recombination rate of n-p-heterojunctions was calculated to be 90.3 %. Water and wastewater treatment can utilize the SnO₂ - CuO heterostructure to decompose emerging pollutants using visible light.

Acknowledgements

In their acknowledgement, the authors express their gratitude to the management team. The authors also appreciate the support and encouragement of Yeungnam University, Gyeongsan, Republic of Korea.

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.

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Thirupathy C., Lims S.C., Sundaram S.J., Mahmoud A.H., Kaviyarasu K., . Equilibrium synthesis and magnetic properties of BaFe₁₂O₁₉/NiFe₂O₄ nanocomposite prepared by co precipitation method. Journal of King Saud University-Science. 2020;32(2):1612-1618.
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Wang, K., Zhang, W., Lou, F., Wei, T., Qian, Z., Guo, W. J. Solid State Electrochem. Preparation of electrospun heterostructured hollow SnO₂/CuO nanofibers and their enhanced visible light photocatalytic performance 22, (2018) 2413.

Introduction

Experimental

Materials
Synthesis method of SnO2 - CuO heterostructured photocatalyst
Characterization techniques
Photocatalytic studies

Results and discussion

XRD pattern
μ-Raman spectrum
FTIR analysis
UV–vis analysis
Morphology analysis
Photocatalytic activity

Conclusion

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