Morphological controlled synthesis of ceo2 sno2 nanocomposites and its structural and optical properties

Accepted Manuscript Morphological controlled synthesis of CeO2/SnO2 nanocomposites and its structural and optical properties S Usharani, V Rajendran PII: S2468-2179(17)30109-0 DOI: 10.1016/j.jsamd.2017.08.001 Reference: JSAMD 115 To appear in: Journal of Science: Advanced Materials and Devices Received Date: 28 June 2017 Revised Date: 30 July 2017 Accepted Date: August 2017 Please cite this article as: S Usharani, V Rajendran, Morphological controlled synthesis of CeO2/SnO2 nanocomposites and its structural and optical properties, Journal of Science: Advanced Materials and Devices (2017), doi: 10.1016/j.jsamd.2017.08.001 This is a PDF file of an unedited manuscript that has been accepted for publication As a service to our customers we are providing this early version of the manuscript The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain ACCEPTED MANUSCRIPT Morphological controlled synthesis of CeO2/SnO2 nanocomposites and its structural and optical properties S Usharani* and V Rajendran Department of Physics, Presidency College, Chennai-05, Tamilnadu, India RI PT Corresponding author Email address: sushamoorthy15@gmail.com Abstract CeO2/SnO2 nanocomposites with different dimensional nanostructures were synthesized by the wet chemical method, using various surfactants such as SDS, CTAB and Triton X-100 infrared (FTIR), Transmission electron SC The prepared CeO2/SnO2 samples were analyzed by X-ray diffraction (XRD), Fourier transform microscopy (TEM), UV-Diffuse Reflectance Spectroscopy (UV-DRS) and Photoluminescence (PL) spectroscopy The XRD patterns reveal M AN U the presence of a mixed phase of SnO2 and CeO2; The TEM analysis showed the mixed morphology of uniformly dispersed spherical with ellipsoidal shape observed at SDS assisted CeO2/SnO2 nanocomposites; whereas spherical with hexagonal shape nanostructure was observed at Triton X-100 assisted CeO2/SnO2 nanocomposites The one dimensional (1D) nanorod like structure observed for the CTAB assisted CeO2/SnO2 nanocomposites shows CTAB acting as a face-specific capping agent to form rod-shaped micelles The room temperature TE D photoluminescence emission studies of CeO2/SnO2 nanocomposites showed strong peaks in the UV region, and several peaks in the visible region, which are likely to have originated from the oxygen vacancies and are potential material for optoelectronic device applications The UV EP results show the absorption edges shifted to a high energy region and the blue shifts that had occurred in all the samples Keywords: CeO2/SnO2; Surfactants; Mixed morphology; Nanorods; Optical properties AC C Introduction Nanomaterials with various morphologies are a pillar of today’s nanoscience and bioscience, considerably used as biomarkers, therapeutics, catalysts and structural reinforcements [1] Recent research groups synthesised zero dimensional (0D), one dimensional (1D), two dimensional (2D) and three dimensional (3D) nanostructured materials and reported their potential for varied applications, such as electrocatalysts, gas sensing and photocatalysts [2-6] The ability to enhance the properties by controlling the particle size and morphology may lead to potentially useful technological applications [2] In recent years great efforts have been made in ACCEPTED MANUSCRIPT developing an easy process to prepare size and shape controlled nanomaterials Various research groups reported, using various solvents, surfactants and pH, which strongly influenced the shape and size of the nanomaterials [7-10], in particular, using various surfactants which may play an important role in synthesizing size and morphology controlled nanomaterials [11] RI PT The shape and size dependent optical and electronic properties of semiconducting nanomaterials, such as CdS/SnO2, TiO2, ZnO, CeO2, CeO2/ZrO2, CuO/CeO2, CeO2/TiO2, SnO2 have various applications such as gas sensors, detectors for infrared light and lasers, solar cells, optical materials, luminescence devices, and optoelectronic devices [12-17] SnO2 and CeO2 SC nanomaterials reveal that they are promising materials for optoelectronic devices such as solar cells, conductive layers, and transistors due to its excellent electrical and optical properties [17- M AN U 20] Significantly, the mixed metal oxide nanocomposites of SnO2/CeO2 have received much attention, because of their excellent physicochemical properties and their potential applications [21-24] Our work shows the synthesis of CeO2/SnO2 nanocomposites by the wet chemical method using anionic-Sodium Dodecyl Sulphate (SDS), cationic-cetyl trimethyl ammonium bromide (CTAB) and nonionic-Triton X-100 surfactants, and investigates the influence of the surfactants on their crystalline nature, size, morphology and optical properties The synthesis of TE D CeO2/SnO2 nanocomposites with different morphologies has been reported in earlier literature [25,26]; however, to the best of our knowledge, there is no report in literature regarding the morphological controlled synthesis of CeO2/SnO2 nanocomposites with different surfactants such as SDS, CTAB and Triton X-100 In this paper, we investigate the synthesis of CeO2/SnO2 EP nanocomposites with nanorod, hexagonal and spherical with ellipsoidal morphology, and their structural and optical properties AC C Experimental 2.1 Materials Analytical grade Cerrous chloride (CeCl3), tin (II) chloride dihydrate (SnCl2.2H2O), ammonium hydroxide (NH4OH), SDS, CTAB and Triton X-100 were purchased from Aldrich and used without any further purification Double distilled water was used as a solvent to prepare the CeO2/SnO2 nanocomposites 2.2 Preparation of CeO2/SnO2 nanocomposites In a typical synthesis, 0.1 M of cerrous chloride (CeCl3) was mixed with 100 ml of water and stirred for 15 Similarly, 0.1 M of tin (II) chloride dehydrate (SnCl2.2H2O) was mixed ACCEPTED MANUSCRIPT with 100 ml of water and stirred for 15 These two aqueous solutions were mixed together with constant stirring for 30 at room temperature and then g of anionic surfactant SDS was added and the stirring was continued for h After h the aqueous ammonium hydroxide (NH4OH) solution was added dropwise to attain the pH value of 6.5 under vigorous stirring The RI PT stirring was continued overnight at room temperature and the resulting milky white colloidal gel product was obtained The prepared sample was initially dried at 100oC for 12 hrs, and later the dried sample was transferred into the alumina crucible and calcined in a muffle furnace at 600oC for hrs The same procedure was repeated to prepare the CeO2/SnO2 nanocomposites of SC cationic and non-ionic surfactants, such as CTAB and Triton X-100 2.3 Characterization details M AN U The structure of the prepared sample was analyzed using X-ray diffraction (XRD) analysis The XRD pattern of the nanopowders was recorded using a powder X-ray diffractometer (Schimadzu model: XRD 6000), using CuKα (λ=1.5417 Å) radiation The operating conditions were 40 kV and 30 mA in the scanning range 20-70˚ at the rate of deg/min The crystallite size of the nanocomposites was calculated using Debye Scherrer’s formula D = 0.89λ/βcosθ, where λ represents the wavelength of the X-ray, θ indicates Bragg’s TE D angle, and β is the FWHM of the characteristic peaks Fourier transform infrared (FTIR) spectra were taken using an FTIR model Bruker IFS 66 V spectrometer, using the KBr-pellet technique The EDX studies were carried out by the Philips model CM 20 High- resolution images and selected area electron diffraction patterns were observed with a JEOL JEM-2200FS transmission EP electron microscope (TEM) operating at 200 kV using a copper grid For TEM imaging, a small amount of the sample was dispersed in acetone and sonicated for min, after which the solution AC C was drop-casted onto carbon coated copper-grids Diffuse reflectance UV-vis spectra were recorded in Nujol mode on a CARY 5E UV–vis–NIR spectrophotometer The photoluminescence emission spectra were carried out on a Fluoromax-4 spectrofluorometer with a Xe lamp as the excitation light source Results and discussion The XRD patterns of the CeO2/SnO2 nanocomposite prepared with different surfactants are shown in Fig 1(a-c) The diffractogram indicates the formation of the cubic fluorite structure of CeO2 (JCPDS card No 43-1002) at 2θ values 28.5, 33.0, 47.4, 56.4, 59.1 and 69.5, that correspond to (111), (200), (220), (311), (222) and (400) crystal planes, respectively [19] ACCEPTED MANUSCRIPT Similarly, the diffraction peaks indicate that the formation of cassiterite type tetragonal structure of SnO2 (JCPDS card No.41-1445) at 2θ values 26.6, 33.7, 37.7, 51.7, 54.7, 61.9, 64.6 and 66.1 correspond to (110), (101), (200), (211), (220), (310), (112), and (300) crystal planes, respectively [27] The XRD results show that the prepared CeO2/SnO2 nanocomposites exhibit a RI PT good crystalline nature [9,26,28], due to the influence of the anionic (SDS), cationic (CTAB) and nonionic (Triton X) surfactants and no other peaks were found, which indicates that the formation of nanocomposites is of high purity The crystallite sizes of the CeO2/SnO2 nanocomposite are calculated by using the Debye-Scherrer equation (Equation 1) from full width D = 0.89λ/βcosθ SC at half maximum (FWHM) values of the CeO2 and SnO2 planes (1) M AN U where λ represents the wavelength of the X-ray, θ indicates Bragg’s angle, and β is the FWHM of the characteristic peaks It was found to be 34.1, 32.0 and 30.8 nm for the CeO2/SnO2 nanocomposites for the surfactants of SDS, CTAB and Triton X respectively The XRD results show that the peak intensity of the Triton X assisted CeO2/SnO2 nanocomposite shown in Fig 1(c), was notably lower than that of the other two surfactants such as SDS and CTAB assisted CeO2/SnO2 nanocomposites (Fig 1.(a,b)), which may be due to the smaller particle size TE D The FTIR spectra of the prepared CeO2/SnO2 nanocomposites with three different surfactants are shown in Fig 2(a-c) In the spectra, the peaks observed at 3422 and 1637 cm-1 are ascribed to the presence of the –OH and H2O functional groups The overlapped absorption band in the region 549-691 cm-1 is due to the Sn-O-Sn and Ce-O stretching vibrations and is in close EP agreement with the reported values [29,30] The absorption band centered at 2918 cm-1 is assigned to the C-H stretching vibrations from the SDS, CTAB and Triton X [11] AC C Fig 3(a-c) is the TEM image of the CeO2/SnO2 nanopowder for three different surfactants such as SDS, CTAB and Triton X Figure 3(a) shows the formation of the uniformly distributed mixed morphology such as spherical with ellipsoidal shaped nanoparticles in the SDS assisted CeO2/SnO2 nanocomposite Baljinder Singh et al reported that a less polar anionic surfactant (due to a long hydrophobic chain) may adsorb on the ZnO surface, thus leading to the formation of small nanorods [31] Samaele et al reported that SDS assisted nanomaterials produce a mixed morphology such as nanorods with sphere like particles [32] During the nanostructure formation, the anionic surfactant SDS acts as a transporter of the particle, and leads to control the growth direction that is adsorbed on to the intermediate colloidal species ACCEPTED MANUSCRIPT surface In the presence of SDS, the products are capped by the surface modifier and the restriction of the particle growth in a definite direction leads to the formation of a spherical with ellipsoidal structure, as well as to prevent the agglomeration and produce the dispersible morphology [32] As shown in Figure 3(b), the CTAB assisted sample shows the rod like RI PT structure The CTAB plays an important role in the formation of nanorods [33] Leonardo Scarabelli et al reported the synthesis of a gold nanorod, using CTAB as a surfactant CTAB act as a face- specific capping agent to form rod-shaped micelles, which are expected to induce anisotropic growth on spherical seeds In the presence of CTAB, the chloride ions (Cl-) from the SC precursor will be eventually replaced by bromide ions (Br-) from the surfactant, leading to a complex formation that will influence their redox potential, which is cathodically shifted In this, M AN U the redox potential will influence the growth kinetics to form the nanorods [34] In Fig 3(c), the Triton X assisted CeO2/SnO2 nanocomposite shows the spherical with hexagonal morphology The surfactant plays an important role in controlling the morphology of the sample In the crystallization process, the surfactant Triton X-100 which might be attributed to the steric repulsions among surface molecules leads to hindering the growth and form agglomerated spherical with hexagonal shape nanomaterials [31,32] The high resolution and low resolution TE D images of SDS, CTAB and Triton X assisisted CeO2/SnO2 nanocomposites are shown in the supplementary material (S1) The selected area electron diffraction (SAED) patterns of the samples are shown in an inset of Fig 3(a-c), which reveals that all the samples were polycrystalline in nature Fig 3(d-f) shows the EDX spectra of the CeO2/SnO2 nanocomposites EP for the three different surfactants, such as SDS, CTAB and Triton X-100 It confirms that Sn, Ce and O are the only elements present in the CeO2/SnO2 nanocomposite which demonstrated the AC C purity of the prepared catalyst with different surfactants The UV absorption spectra of the prepared samples with three different surfactants are shown in Fig 4(a-c) The absorption edges are observed at 458, 424 and 371 nm for the SDS, CTAB and Triton X-100 assisted CeO2/SnO2 nanocomposite As observed from the spectra, the absorption edges are shifted to a high energy region and the blue shifts occurred in all the samples Considering the blue shift of the absorption positions of the bulk SnO2, the absorption onset of the present samples is assigned to the direct transition of the electrons in the SnO2 nano crystals [35] The absorption spectra showed strong absorption below 400 nm It is noted that the absorption of ceria in the UV region originates from the charge transfer transition between the ACCEPTED MANUSCRIPT O2- (2p) and Ce4+ (4f) orbit in CeO2 [36] Further, the optical band gap energy of all the prepared samples was calculated using the following equation (αhυ) = C (hυ–Eg)n (2) RI PT Here α is the absorption coefficient, hυ is the photon energy, C is the constant, and n = 1/2 for a directly allowed transition The optical absorption coefficient α was calculated according to the equation α = (2.303x103 Aρ)/lc, where A is the absorbance of the sample CeO2/SnO2, ρ is the real density of, l is the path length, and c is the concentration of the CeO2/SnO2 suspensions For SC the indirect transitions, the plots of (αhυ)2 versus photon energy for the different surfactants assisted CeO2/SnO2 nanocomposites, are shown in Fig 5(a-c) The band gap energies of the M AN U samples prepared with different surfactants obtained by the (αhυ)2 versus (hυ) curve are 2.7, 2.92 and 3.3 eV respectively The band gap energy suggests that the CeO2/SnO2 nanocomposite is a potential material for opto-electronic devices [9] The crystallite size (D), morphology and band gap values of CeO2/SnO2 nanocomposite with different surfactants-SDS, CTAB and Triton X are shown in Table.1 Fig 6(a-c) shows the room temperature PL emission spectra of the CeO2/SnO2 TE D nanocomposites for different surfactants The strong UV emission peak at 324 nm is ascribed to the nearest band edge emission of the excitons [37] In addition to this, strong blue green emission peaks at 463 and 477 nm were observed Similarly, the weak emission peaks appearing in the spectra at 415, 434, 447, 486 and 519 nm are due to the transition in the defect states In EP the cubic structure of CeO2, the oxygen ions are not closely packed for which ceria produce many oxygen vacancies When an oxygen atom was lost from CeO2, an electron pair was trapped AC C in the oxygen vacancy cavity, which gives F centres In ceria, the oxygen defect states were present just below the Ce 4f level Thus the emission peak that appeared in CeO2 can be assigned to the oxygen related defects [36] The emission peaks that appeared at 463, 477, 415, 434, 447, 486 nm are observed due to F centres in CeO2 CeO2 has some percentage of Ce3+ which is present in the grain boundary The presence of Ce3+ in the CeO2 material acts as a hole trap and the oxygen vacancy as an electron trap These two undergo radiative recombination resulting in the 519 nm emission peak [36] The PL intensity was observed to be high in SDS assisted CeO2/SnO2 nanocomposites compared to CTAB and Triton X assisted CeO2/SnO2 nanocomposites The high intensity PL emission peaks were due to the uniformly distributed ACCEPTED MANUSCRIPT spherical with ellipsoidal mixed morphology of CeO2/SnO2 nanocomposites The strong photoluminescence of the CeO2/SnO2 nanocomposites in the UV region suggests that they may find uses as luminescent labels and light-emitting molecular substances in nanoscale materials in optical memory systems in the future [38] Conclusion RI PT photoluminescent or nano-optoelectronic devices, photonic applications and as optical memory CeO2/SnO2 nanocomposites were successfully synthesized by the wet chemical method with various surfactants such as SDS, CTAB and Triton X-100 The XRD patterns reveal the SC presence of a mixed phase of SnO2 and CeO2; and possess good crystalline nature in all the surfactants assisted CeO2/SnO2 nanocomposites Furthermore, the Triton X assisted CeO2/SnO2 M AN U nanocomposites possess low intensity peaks which reveal the lower particle size The FTIR results confirmed the formation of the Ce–O and Sn–O bond The EDX studies revealed the chemical compositions of the CeO2/SnO2 sample The TEM studies revealed the decrease in particle agglomeration and the various morphologies with respect to the addition of different surfactants In particular, the CTAB assisted CeO2/SnO2 nanocomposites show the 1D nanorod like structure The UV and photoluminescence property of the CeO2/SnO2 nanocomposites TE D shows that it could be used for optoelectronic device applications The size and morphological controlled nanocomposite materials make them promising candidates for future optoelectronic devices, spintronic devices, gas sensing and visible light photocatalytic performance Acknowledgement EP Authors are grateful to the Department of Science and Technology (DST), India for financial support to carry this work [1] AC C References H Heinz, C Pramanik, O Heinz, Y Ding, R.K Mishra, D Marchon, R.J Flatt, I.ELopis, J Llop, S Moya, R.F Ziolo, Nanoparticle decoration with surfactants: Molecular interactions, assembly, and applications, Surf Sci Rep 72 (2017) 1-58 [2] B Ahmed, S Kumar, S 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nanocomposite: (d) SDS, (e) CTAB and (f) Triton X AC C Fig UV-vis absorption spectra of different surfactants assisted CeO2/SnO2 nanocomposite: (a) SDS, (b) CTAB and (c) Triton X Fig Tauc plots of (αhυ)2 versus photon energy for the different surfactants assisted CeO2/SnO2 nanocomposite: (a) SDS, (b) CTAB and (c) Triton X Fig PL emission spectra of different surfactants effect on CeO2/SnO2 nanocomposite: (a) SDS, (b) CTAB and (c) Triton X 11 M AN U SC RI PT ACCEPTED MANUSCRIPT AC C EP TE D Fig Fig 12 AC C EP TE D M AN U SC RI PT ACCEPTED MANUSCRIPT Fig 13 AC C EP TE D M AN U SC RI PT ACCEPTED MANUSCRIPT Fig 14 AC C EP TE D M AN U SC RI PT ACCEPTED MANUSCRIPT Fig 15 M AN U SC RI PT ACCEPTED MANUSCRIPT TE D Fig Table The crystallite size (D), morphology and band gap values of CeO2/SnO2 AC C Surfactants EP nanocomposite with different surfactants-SDS, CTAB and Triton X Crystallite Size (nm) (XRD) Morphology (TEM) Band gap energy (eV) SDS 34.1 Spherical with ellipsoidal 2.7 CTAB 32.0 Nanorods 2.92 Triton X 30.8 Spherical with hexagonal 3.3 16 ACCEPTED MANUSCRIPT Highlights Synthesis of low dimensional nanostructures • 1D nanorod like structure observed for the CTAB assisted CeO2/SnO2 nanocomposites • Mixed morphology nanostructures are formed by SDS and Triton X-100 assisted RI PT • nanocomposites RTPL studies revealed the strong emission in UV and visible region due to excitons and EP TE D M AN U SC F centers AC C • ...ACCEPTED MANUSCRIPT Morphological controlled synthesis of CeO2/ SnO2 nanocomposites and its structural and optical properties S Usharani* and V Rajendran Department of Physics, Presidency College,... paper, we investigate the synthesis of CeO2/ SnO2 EP nanocomposites with nanorod, hexagonal and spherical with ellipsoidal morphology, and their structural and optical properties AC C Experimental... nonionic-Triton X-100 surfactants, and investigates the influence of the surfactants on their crystalline nature, size, morphology and optical properties The synthesis of TE D CeO2/ SnO2 nanocomposites with