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Optical Studies of Ni and Fe Doped Tin Oxide Nanoparticles by Co-Precipitation Method
1.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 293 Optical Studies of Ni and Fe doped Tin Oxide Nanoparticles by Co- precipitation Method Amutha.T1, P. Lavanya1, M.Rameshbabu2 and K.Prabha1* 1 Department of Physics, Mother Teresa Women’s University, Kodaikanal. Tamilnadu, India 2Department of Physics, Arulmigu Palaniandavar College of Arts and Culture, Palani, Tamilnadu, India ---------------------------------------------------------------------***--------------------------------------------------------------------- Abstract – Pure, Ni and Fe doped Tin Oxide (SnO2) nanoparticles were synthesized by simple co-precipitation method. The structural, chemical and optical properties of the samples were analyzed using X-ray diffraction (XRD), UV–visible spectroscopy, FT-IR and Photo Luminescence Studies. SnO2 crystallites were found to exhibit Tetragonal Rutile structure. Ni and Fe doped SnO2 nanoparticles revealed that the metal ions substituted in the Sn lattice. A significant red shift in the UV absorbing band edge was observed with the doped Ni and Fe contents. The FT-IR analyses confirmed the incorporation of Ni and Fe in the synthesized powder. Key Words: Tin Oxide, XRD, UV-Vis Absorption, FT-IR, PL Studies 1. INTRODUCTION Among the various important categories of the functional materials like, polymers, magnetic, dielectric and semiconductors, the ferromagnetic semiconductors are emerged as attracting materials and driven a considerable attention in the recent years [1-2]. Tin oxide (SnO2) is one of the most intriguing materials to be investigated today. This is because SnO2 is a well-known n-type semiconductor with a wide band gap of 3.6-3.8 eV [3-5], and for its potential application in transparent conductive electrode for solar cells, a gas sensing material for gas sensors, transparent conducting oxide electrodes, photochemical and photoconductive devices in liquid crystal display, gas discharge display, lithium-ion batteries, etc.,[6-10]. Co-precipitation [11] is a suitable chemical method in a nanoparticles synthesis because it does not require high pressure and temperature, impure materials are eliminated by filtration and repeated washing and cost effective method. In the present study, SnO2 nanoparticles were synthesized by co-precipitation method and ultrasonic wave agitation was used to homogenize nanoparticles size. 2. EXPERIMENTAL ANALYSIS 2.1 Synthesis For the preparation of pure, Ni and Fe doped SnO2 nanoparticles, co-precipitation method have been adopted. The following analar grade precursors, 1.5 mM of NiCl2.6H2O, 1.5 mM of FeCl2.6H2O and 1.5 M of SnCl2.2H2O were taken to release Ni, Fe and Sn respectively. The aqueous solutions were taken in atomic weight percentage ratio to prepare doped SnO2 nanoparticles. De‐ionized water was taken as solvent for the preparation electrolyte. The solution was stirred for 2 hours using hot plate with a magnetic stirrer. Then, ammonium hydroxide (NH4OH) was added into the solution (drop by drop), with stirring, until pH 9 was reached. The each doped solutions were then kept at room temperature for one day to complete the aging process. The resultant solution was washed several times with ethanol and double distilled water and dried in oven keeping the temperature at 100○C for 6 hrs. These precursors were ground in an agate mortar and pestle for 30 minutes to obtain fine powder. These powders were placed in an alumina crucible at sintering temperature as 500 °C for 2 hrs in a furnace and brought the furnace to room temperature at the rate of 50°C per hour to get the annealed powder sample of pure and doped SnO2.
2.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 294 3. RESULTS AND DISCUSSION 3.1 X-Ray Diffraction Analysis Fig.1: XRD patterns of (a) Pure (b) Fe and (c) Ni doped SnO2 nanoparticles. Table 1: Crystallite size and lattice parameters of pure, Ni and Fe doped SnO2 nanoparticles. Fig.1 shows the XRD patterns of pure, Ni and Fe doped SnO2 nanoparticles calcinated at 500°C for 2 hrs. The XRD patterns revealed that all the samples possess tetragonal rutile structure (JCPD File. Nos. 00-041-1445 and 01-070- 6995) and the crystallographic space group (P42/mnm) 136. The broadening of the Bragg peak is due to the occurrence of smaller in crystallite size. The decrease in the crystallite size of doped samples when compared to pure is due to the decrease in the crystallinity of the doped samples [12]. A slight shift is observed in the unit cell parameters which indeed indicate that the doped atoms might be substituted into the lattice sites of parent atoms [13]. The crystallite size of the Ni and Fe co-doped SnO2 samples were calculated by the Debye-Scherrer’s equation which is given by d = kλ/(β cosθ), where ‘k’ is the shape factor, ‘λ’ is the wavelength of x-rays used, β is the full width at half maximum of the prominent Bragg peak and θ is the Bragg angle. Crystallite size and lattice parameters of pure, Ni and Fe doped SnO2 nanoparticles are shown in the Table 1. 3.2 UV-Vis. Analysis Fig.2: Tauc’s plot of (a) Pure (b) Ni and (c) Fe doped SnO2 nanoparticles. Name of the Sample Crystallite Size (nm) Lattice parameters (Å) a = b c SnO2 35 4.7371 3.1905 Ni doped SnO2 21 4.6246 3.1363 Fe doped SnO2 17 4.6279 3.1379 (a) (b) (c)
3.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 295 Fig. 2 shows that the direct optical energy band gap (Eg) of the samples can be determined by the X-axis intercept of the straight-line portion of (h)2 versus the photon energy (h). The estimated band gap energy of pure SnO2 is ~ 3.64 eV, while, the band gap energy of the Ni and Fe doped compound found as 3.19 and 3.12 eV. The observed band gap energy of pure SnO2 nanoparticles is quite higher than the band gap energy of bulk SnO2 (3.6 eV). The optical absorption edge of the spectrum of pure is sifted to blue wavelength and for doped sample is shifted to red wavelength with respect to the bulk (3.6 eV). The broad blue emission is due to the electron transition mediated by defect levels in the band gap. A significant decrease in band gap is observed with respect to doped samples. The decrease in the band gap energy may be due to the accumulation of donor energy levels of TM ions in the actual band gap of SnO2. 3.3 FT-IR Analysis Fig -3: FT-IR spectra of (a) Pure (b) Ni and (c) Fe doped SnO2 nanoparticles. Figure 3 shows the FTIR spectrum of pure and Ni and Fe co-doped SnO2 nanoparticles. At 1641 cm-1 and 3438 cm-1 indicates the presence of C=O and OH functional groups respectively [14]. The absorption band at 643 cm-1 is associated with the antisymmetric O–Sn-O stretching mode of the surface bridging oxide formed by the condensation of the adjacent surface hydroxyl groups, which is in close agreement with the reported literatures [14, 15]. The peak at 1066 cm-1 is attributed to the NH deformation of ammonia [15, 16]. The above studies confirmed the formation of the tin oxide powder. 3.4 PL Analysis Fig.4: PL spectrum of (a) pure SnO2 (b) Ni and (c) Fe doped SnO2 nanoparticles.
4.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 296 The fig. 4 shows the PL spectra of pure SnO2 nano emission bands at 370 nm, 418 nm, 435 nm, 467 nm and for Ni doped SnO2 emission bands at 369 nm, 421 nm, 448 nm, 467 nm and for Fe doped SnO2 emission bands at 370 nm, 422 nm, 450 nm, 467 nm. The blue emission peak at 467 nm is possibly attributed to the electron transition, mediated by defect levels in band gap, such oxygen vacancies or tin interstitials [17, 18]. The luminescence for doped samples is associated with the recombination of many more electrons and holes trapped at the surface of the SnO2 nanoparticles. 3.5 SEM and EDX Analysis Fig.5: (a) SEM image and (b) EDX spectrum of pure SnO2 nanoparticles, (c) SEM image (d) EDX spectrum of Ni doped SnO2 nanoparticles, (e) SEM image (f) EDX spectrum of Fe doped SnO2 nanoparticles Table 2: Atomic Weight % of pure SnO2 nanoparticles. Eleme nt AN Series unn.C [wt.% ] Norm.C [wt.%] Atom.C [at.%] (1 Sigma) [wt.%] O 8 K-series 21.41 28.60 74.82 4.20 Sn 50 L-series 53.45 71.40 25.18 1.64 Total : 100.00 100.00 Table 3: Atomic Weight % of Fe doped SnO2 nanoparticles. Element AN Series unn.C [wt.%] Norm.C [wt.%] Atom.C [at.%] (1 Sigma) [wt.%] Sn 50 L-Series 72.50 89.39 54.60 2.22 O 8 K-Series 7.93 9.78 44.33 2.60 Fe 26 K-Series 0.67 0.82 1.07 0.07 Total: 81.00 100.00 100.00 Table 4: Atomic Weight % of Ni doped SnO2 nanoparticles. Element AN Series unn.C [wt.%] Norm.C [wt.%] Atom.C [at.%] (1 Sigma) [wt.%] O 8 K-Series 9.29 13.67 53.93 3.76 Sn 50 L-Series 58.47 86.02 45.74 1.86 Ni 28 K-Series 0.21 0.31 0.33 0.06 Total 67.97 100.00 100.00 Figure 5 shows the typical morphology and Table 2, Table 3 and Table 4 shows the composition of Pure, Ni and Fe doped Tin Oxide nano particles. Fig.5 (a) shows the SEM morphology showing the presence of large spherical aggregates of small individual nanoparticles. In Fig.5(c), Ni and Fe co-doped SnO2 SEM morphology shows spherical and nano rod aggregates of small individual nano particles. The presence of Sn, Ni and Fe is confirmed from the selective area EDX analysis. It can be verified from the results of change in cell dimension of XRD data and EDX shows that the Ni and Fe is successfully doped in the SnO2. 4. CONCLUSIONS Pure, Ni and Fe doped SnO2 powders in nanometric dimensions were found by the co-precipitation method. The XRD pattern reveals the phase, structure and lattice parameters. The band gap energy of SnO2 is promising for the application in optical device. The FT-IR studies confirm the presence of the Sn–O bond. The PL emission spectrum of the Pure and Ni & Fe co- doped SnO2 nanostructures were observed in the strong visible region. It was attributed to the surfaced effects related to the oxygen vacancies. The SEM study confirms the presence of uniform
5.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 04 Special Issue: 09 | Sep -2017 www.irjet.net p-ISSN: 2395-0072 One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India © 2017, IRJET | Impact Factor value: 5.181 | ISO 9001:2008 Certified Journal | Page 297 grains in the synthesized powder. EDX reveals the presence of the elements, Sn, Co, Fe and O2. ACKNOWLEDGEMENT The author thanked DST_SERB, New Delhi for the financial support under the DST-SERB major research project (Reference No. SERB/4496/2016-17 dated 24.09.2016). We are thankful to Prof.C.SANJEEVIRAJA, (Formerly Professor, Dean Science Alagappa University) Emeritus Scientist, Department of Physics Alagappa Chettiar College of Engineering & Technology, Karaikudi for his valuable suggestions during this research work. REFERENCES [1] G.A. Prinz, Science, 282 (1998) 1660. [2] S.A. Wolf, D.D. Awschalom, R.A.Buhrman,J.M. Daughton,S.V.Molnar,M.L.Roukes, A.Y. Chtcheljanova and D.M.Treger, Science, 294 (2001) 1488. [3] Ganesh E Patil, D D Kajale, D N Chavan, N K Pawar, P T Ahire, S D Shinde,V B Gaikwad and G H Jain, Bull. Mater. Sci., 34 (2011)1. [4] L. C. Nehru, V. Swaminathan, C. Sanjeeviraja, American Journal of Materials Science, 2 (2012) 6. [5] S. Gnanam, V. Rajendran, Digest Journal of Nanomaterials and Biostructures, 5 (2010) 699. [6] A. Kay, M. Gratzel, Chem. Mater., 14 (2002)2930. [7] Sipra Choudhury, C. A. Betty, K. G. Girija, and S. K. Kulshreshtha, Appl. Phys. Lett., 89 (2006) 071914. [8] R. Triantafyllopoulou, X. Illa, O. Casals, S. Chatzandroulis, C. Tsamis, A. Romano-Rodriguez, J.R. Morante, Microelectronic Engineering, 85 (2008)1116. [9] Huiyong Liu, V. Avrutin, N. Izyumskaya, Ü. Özgür, H. Morkoç, Super Lattices and Microstructures, 48 (2010) 458. [10] Chunjoong Kim, Mijung Noh, Myungsuk Choi, Jaephil Cho,and Byungwoo Park, Chem. Mater. 17(2005)3297. [11] Hidalgo, P.,R.H.R. Castro, A.C.V. Coelbo and D. Gouvea, Chemistry of Materials Journal , 17(2005)4149. [12] R.N.Mariammal, N.Rajamanickam, K.Ramachandran, J.Nano.Electron.Phy.3(2011) 92. [13] S.Kesava Pandian, K.Karthik, K.Sureshkumar and N.Victor Jaya, Materials and Manufacturing process, 27(2012)130. [14] Shen E, Wang C, Wang E, Kang Z, Gao L, Hu C, etal. PEG-assisted synthesis of SnO2 nanoparticles. Mater Lett 2004; 58:3761–4. [15] Krishnakumar T, Pinna N, Prasnna Kumari K, Perumal K, Jayaprakash R., Mater. Lett., 62(2008) 3437. [16] Aziz M, Abbas S S, Baharom W R W, Mater. Lett.,91(2013)31. [17] Tawale J S, Gupta G, Mohan A, Kumar A, Srivastava A K., Sens. Actuators B 201(2014)369. [18] Gu F, Wang S F, Lu M K, Zhou G J, Xu D, Yuan D R, J.Phys. Chem.B;108 (200) 8119.
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