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Page 1 of 43 RSC Advances RSC Advances This is an Accepted Manuscript, which has been through the Royal Society of Chemistry peer review process and has been accepted for publication. Accepted Manuscripts are published online shortly after acceptance, before technical editing, formatting and proof reading. Using this free service, authors can make their results available to the community, in citable form, before we publish the edited article. This Accepted Manuscript will be replaced by the edited, formatted and paginated article as soon as this is available. You can find more information about Accepted Manuscripts in the Information for Authors. Please note that technical editing may introduce minor changes to the text and/or graphics, which may alter content. The journal’s standard Terms & Conditions and the Ethical guidelines still apply. In no event shall the Royal Society of Chemistry be held responsible for any errors or omissions in this Accepted Manuscript or any consequences arising from the use of any information it contains. www.rsc.org/advances Page 1 of 43 RSC Advances Sol-gel based simonkolleite nanopetals with SnO2 nanoparticles in graphite-like amorphous carbon as efficient and reusable photocatalyst Moumita Pal, Susanta Bera and Sunirmal Jana* Sol-Gel Division CSIRCentral Glass and Ceramic Research Institute (CSIRCGCRI) 196 Raja S.C. Mullick Road, P.O. Jadavpur University, Kolkata 700032, India Abstract We report a new sol-gel nanocomposite (STC) having simonkolleite nanopetals (SC) and quasi-spherical tin oxide (SO) nanoparticles embedded in graphite-like amorphous carbon (C) as an efficient and reusable photocatalyst towards degradation of Rhodamine 6G (Rh 6G) dye under UV (, 254 nm) illumination. The STC was synthesized under vacuum curing (450oC) Manuscript of precursor gel derived from the sol (Zn : Sn, 2 : 1) in 2-methoxy ethanol with acetylacetone. Presence of tetragonal SO well decorated on rhombohedral SC forming nanoheterostructures in the carbon matrix was identified by X-ray diffraction, micro-Raman, X-ray photoelectron spectroscopy and electron microscopes (field emission scanning electron and transmission electron) studies. Carbon content and thermal weight loss behaviour in STC were studied by carbon determinator and thermogravimetry. The nanocomposite showed high photocatalytic Accepted activity (10-5M dye solution degraded completely in 32 min). Reusability test of the photocatalyst exhibited about 95% of the dye degradation after five successive recycles. In addition to accelerate photo-induced charge carrier separation and electron transport in the nanoheterostructures as revealed from electrochemical impedance spectroscopy response of the UV exposed nanocomposite, an active role of the carbon in an optimum content (~18%) was found for generating high BET specific surface area (~143 m2/g). This simple synthesis Advances strategy could open a new avenue to develop sol-gel nanocomposites as efficient and reusable photocatalysts from simonkolleite based different metal oxide semiconductors embedded in graphite-like amorphous carbon. RSC Key words: Sol-gel process, simonkolleite, tin oxide, graphite-like amorphous carbon, nanoheterostructures, photocatalysts *Corresponding author: Tel.: +91 33 23223303, Fax: +91 33 2473 0957 E-mail address: [email protected], [email protected] (S. Jana) 1 RSC Advances Page 2 of 43 1. Introduction Water pollution problem related to contamination of organic dyes is a serious global concern.1 In this regard, the synthetic wastewaters from different dye industries have posed a great threat to the water environment.2 The problem concerning the pollution could be mitigated cost effectively and economically by the use of nano metal oxide semiconductor (MOS) as photocatalyst under illumination of light.3 However, the fast recombination of photogenerated electrons and holes (charge carriers) could diminish the photocatalytic activity of the MOS.4 Thus, it is necessary to reduce the recombination rate of charge carrier that could enhance the lifetime of electrons and holes, resulting an improvement of the activity of semiconductors.2 Accordingly, several strategies could be adopted. One could be Manuscript an intentional creation of surface defects by incorporation of suitable doping element into the host crystal lattice.5 The defects could act as trap states that reside within the band gap of MOS. This strategy could result in the reduction of recombination rate of charge carrier. In the same vein, the existence of nano heterostructures from mixed oxide semiconductors could Accepted also be regarded as an effective strategy.3,6 These heterostructures could be constructed by different metal oxide semiconductors (such as ZnO, SnO2, TiO2) with wide band-gap energy.6,7-9 Now-a-days, the nano heterostructures attracts the materials scientists due to their remarkable properties and several applications10 including photocatalysis. With respect to the activity, the large specific surface areas as well as unique spatial architectures of the Advances heterostructures could make them highly efficient photocatalysts. It could improve the efficiency of photocatalytic activity by reducing the recombination rate of photogenerated RSC charge carrier and accelerates the reduction-oxidation reactions for degradation of organic pollutants (e.g. organic dyes). It is worthy to note11-13 that the carbon (e.g. graphene, carbon nano tube, amorphous carbon) could couple with several basic materials (such as oxides, metals, polymers) to 2 Page 3 of 43 RSC Advances advance their functional properties including their optoelectronic property. Therefore, for enhancement of photocatalytic activity of a semiconductor, major works had already been reported on carbon (C) coupled single metal oxide semiconductor (such as ZnO/C, SnO2/C, 11-13 TiO2/C) nanocomposites. Also, very recently, carbon coupled mixed metal oxide semiconductors (e.g. -Fe2O3/Mn3O4/graphene), which showed excellent charge transfer performance towards photocatalytic water oxidation had also been reported.14 In the carbon- coupled nanocomposite, the photogenerated electrons would accumulate on the surface of carbon to convert O2 to O2 and the holes could remain on the semiconductor surface – – 15 transforming H2O / OH to OH for fast degradation of organics. On the other hand, the carbon could enhance the textural property (particularly surface area and porosity) that could Manuscript necessary for effective contact of photodegradable organic dyes. Simonkolleite (Zn5(OH)8Cl2.H2O, SC) synthesized mostly by hydrothermal, sonochemical and sol-gel processes is known as common corrosion product for zinc bearing materials.16,17 It can also enhance the performance of photoelectrochemical cells.17 The SC Accepted could be transformed into ZnO by thermal heating at relatively lower temperatures.16 Moreover, simonkolleite is now recognized as one of the wide band gap semiconductors having electronic band structure similar to ZnO (bulk band gap energy, 3.3 eV).17 As a semiconductor, the SC could also be able to decompose organic dye (e.g. methyl orange). It is also known that the electrochemical/photochemical property of SC could improve by Advances 18 coupling with TiO2. This would form heterostructures, SC/TiO2. On the other hand, SnO2 is a well-known MOS having widespread applications (e.g. Li-ion batteries, gas sensing, RSC 11 19 photovoltaic conversion etc.). However, the photocatalytic activity of SnO2 is low. To the best of our knowledge, no report is yet available on carbon coupled simonkolleite based heterostructure semiconductors nanocomposite that would act as carbon coupled mixed semiconductors. With this aspect, we considered SC/SnO2 as a new heterostructure system. In addition, due to ability of 3 RSC Advances Page 4 of 43 carbon to couple easily with several materials even with heterostructures, we attempted to synthesize in-situ a nanocomposite of carbon coupled SC/SnO2 heterostructures. In this system, it could be expected that the photogenerated electrons of SC would transfer to SnO2 as the electronic band structure of SC is similar to ZnO.17 This would result the wide separation vis-à-vis reduction in recombination rate of charge carrier. Moreover, the carbon in the nanocomposite could further enhance the photogenerated charge separation in the photo-responsive materials through accelerating electron transport and improvement of the textural property that could be a favourable factor for enhancement of photocatalytic activity of the material towards degradation of organic dye under light illumination.20 In this respect, we should mention that -Fe2O3/Mn3O4/graphene composite has very recently been reported for Manuscript photocatalytic water oxidation.14 The reported work is a motivation of this work. Sol-gel is a facile technique especially for preparation of thin films and nanomaterials. In this technique, the properties of a material (such as microstructural, optical, electronic, optoelectronic) primarily depend upon several parameters such as precursor composition and Accepted chemistry, doping etc.5 Moreover, the curing treatments (e.g. vacuum curing, controlled- atmosphere curing) could also influence significantly upon the properties. This is because various chemisorptions and desorption processes and oxygen diffusion mechanisms are highly involved during the curing treatments.5 However, among different curing treatments, the vacuum curing could found to be a very important one as carbon based nanocomposite Advances sol-gel material
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