International Journal of Application or Innovation in Engineering & Management (IJAIEM) Web Site: www.ijaiem.org Email: editor@ijaiem.org Volume 4, Issue 4, April 2015 ISSN 2319 - 4847 Study The Structural and Optical Properties of Fe2O3 Thin Films Prepared by RF Magnetron sputtering Prof. Dr.Abdulhussein K.Elttayef1, Assist. Prof.Dr Muneer H.Jaduaa2 , Muthana A.Muhammed2 1 Ministry of Science and Technology 2 University of Wasit, College of Science ABSTRACT Fe2O3 thin films were deposited by reactive R.F. magnetron sputtering method on glass substrates with different thicknesses 50 and 100and 370 nm. The structure of Fe2O3 thin films was tested with the X-Ray diffraction and it was formed to be amorphous and after annealing becomes single crystal with recognized peak in (003). The surface morphology of the deposits materials have been studied by using atomic force microscope (AFM). The grain size of the nanoparticles observed in the range of (66.3), (72.37) and (79.23) nm for the thickness of 50, 100 and 370 nm respectively. The optical properties concerning the absorption and transmission spectra were studied for the prepared thin films. Keywords: Fe2O3: Thin Film; Nanostructure; Optical; Sputtering RF. 1. INTRODUCTION Sputtering simply is a term used to describe the mechanism in which atoms are ejected from the surface by energetic particles (almost ions A under high voltage acceleration ion). Two approaches can be followed to produce ions and sputter the target materials. The first is quite straightforward by using an ion source which is aimed toward the target Collecting the sputtered particles on a substrate enables the deposition of a thin film. However, ion beam sputtering is not widely used for industrial large scale applications. Ions guns are more often utilized in surface analytical techniques such as SIMS (secondary ion mass spectrometry) or to bombard the substrate during thin film deposition [1]. The sputtering process with the assistant of magnetron cathodes is called magnetron sputtering which is widely used in both scientific and industrial fields [2]. A magnetron uses a magnetic field to confine electrons close to the cathode, making it easier to sustain an electrical discharge at low pressure. There are various geometries but all magnets are arranged in such a way that the magnetic field lines are parallel to the cathode surface and perpendicular to the electric fielding lines. This causes the secondary electrons to drift in a closed path in the – E ×B direction, also known as the Hall Effect, trapping the electrons near the cathode surface. This arrangement results in enhanced ion bombardment and sputtering rates for both DC and RF discharges. Magnetron sputtering is particularly useful when high deposition rates and low substrate temperatures are required [3]. In RF magnetron sputtering, cathode and anode are changeable and for very short cycles, target functions as anode which cause the removal of insulating layer. By doing so, the process can continue [4, 5]. Due to the predicted half-metallic nature and high polarization (100%), Fe3O4 thin films have drawn a great deal of interest as promising candidates for application in tunneling magneto resistance (TMR) devices. Single crystalline thin films have been epitaxial grown on MgO (100) substrates, due to the good lattice match between the oxides. [6–8] Polycrystalline Fe3O4 thin films have also been deposited on Si substrates to study the properties. [9, 10] The deposition methods used to date include plasma assisted molecular-beam epitaxial (MBE) [6] pulsed laser deposition (PLD) from oxide targets [7, 9] and reactive sputter deposition from an Fe target with Ar–O2 mixture gas flow[8,10] Besides Fe3O4 , other iron oxides, Fe2O3 , FeO, and some nonstoichiometric oxides, have been reported to be present in the deposited films, depending on the deposition conditions.[11,12] Fe2O3 is brown or reddish brown and hence can be easily distinguished from the other oxides, FeO and Fe3O4 , which are black. The crystal structure of both of the later oxides are based on the fcc Bravias Lattice with lattice parameters a50.8936 nm for Fe3O4 and 0.4307 nm for FeO. It has been reported that Fe3O4 can be obtained in polycrystalline thin films only after a certain critical thickness has been deposited [13] which is not ideal for practical device applications. Here we report our investigations of the deposition of Fe2O3 thin films RF sputtered from an iron oxide target. Volume 4, Issue 4, April 2015 Page 99 International Journal of Application or Innovation in Engineering & Management (IJAIEM) Web Site: www.ijaiem.org Email: editor@ijaiem.org Volume 4, Issue 4, April 2015 ISSN 2319 - 4847 2. EXPERIMENTAL DETAILS (Fe2O3) thin films were prepared on glass substrates via reactive radio frequency (RF) magnetron sputtering system using pure iron oxide (Fe2O3) target with purity of 99.99%. The glass substrates were cleaned chemically and ultrasonically, the glass substrate was cleaned by ethanol followed by distilled water rinse, subsequently samples are placed in beaker contain distilled water inside ultrasonic device for 2 hour at 353K The substrates and target were fixed in the chamber of magnetron sputtering system . The base pressure of the deposition chamber was kept at 6 × 10−5 Torr, 3. Results and discussion: 3.1 Structural Properties The X-Ray diffraction (XRD) analysis is conducted to determine the Phases and the grain size. The XRD patterns for the investigated Fe2O3 samples prepared at room temperatures and constant deposition time as well as those deposited at different thicknesses are shown in Fig.(1 a,b,c).And after annealing at 500oC the XRD pattern are shown in Fig.(2,a,b,c). Fig. (1-a, b, c) XRD of Fe2O3 thin films (50,100 and 370 nm) before annealing. Volume 4, Issue 4, April 2015 Page 100 International Journal of Application or Innovation in Engineering & Management (IJAIEM) Web Site: www.ijaiem.org Email: editor@ijaiem.org Volume 4, Issue 4, April 2015 ISSN 2319 - 4847 Fig. (2-a, b, c) XRD of Fe2O3 thin films (50,100 and 370 nm) after annealing. The structure of Fe2O3 thin films were formed to be amorphous and after annealing becomes single crystal with recognized peak in (003) at 31.2o. These results in agreement with the standard Fe2O3 X-ray diffraction data file [N 1997 JCPDS prevalent]. The mean crystallite size has been obtained with Scherer relation: D = kλ / (βCosθ) (1) where D is the crystallite size, k is a fixed number of 0.9, λ is the X-ray Wavelength, θ is the Bragg’s angle in degrees, and β is the full-width-at-half maximum (FWHM) of the chosen peak. The mean size of crystallization calculated for 50,100 nm and 370 nm thin films of Fe2O3 is found to be1.63 nm ,0.87nm and 1.05 nm respectively. 3.2.Morphology Morphological information of these thin film surfaces was analyzed by the AFM as shown in fig. (3) and fig. (4). From the topographic images, it can be seen that the films deposited with thickness of 50 and 100 nm appear to be more uniform that the topography of the sample deposited with thickness of 370 nm. The grain size of the nanoparticles observed in the range of (66.3), (72.37) and (79.23) nm for the thickness of 50, 100 and 370 nm respectively. Volume 4, Issue 4, April 2015 Page 101 International Journal of Application or Innovation in Engineering & Management (IJAIEM) Web Site: www.ijaiem.org Email: editor@ijaiem.org Volume 4, Issue 4, April 2015 ISSN 2319 - 4847 Fig. (3):AFM images for Fe2O3 thin films before annealing: a) 50nm b) 100nm c) 370 nm. Fig.4.AFM images for Fe2O3 thin films after annealing: a) 50nm b) 100 nm c) 370 nm. 3.3 Optical Properties Figure (5) illustrates transmittance spectrum of Fe2O3 films for different thickness (50,100,370 nm.). It is observed that maximum transmittance of 85% at (50 nm) thickness for wavelength range (600-1100 nm).After annealing the transmittance decrease to 75% for the same thickness as shown in figure(6) Volume 4, Issue 4, April 2015 Page 102 International Journal of Application or Innovation in Engineering & Management (IJAIEM) Web Site: www.ijaiem.org Email: editor@ijaiem.org Volume 4, Issue 4, April 2015 ISSN 2319 - 4847 Fig. (5) Transmittance spectrum of Fe2O3 films for different thickness before annealing. Fig. (6) Transmittance spectrum of Fe2O3 thin films after annealing temperature of 500 oC. 3.4 The Energy gap The energy gap can be calculated from equation: ( α h)1/2 = B ( h – Egopt. )1/2 (2) Where :( α )Absorption coefficient, (h) Planck's constant, ( ν) The frequency of the photon , (hν) photon energy, (B ) Constant depends on the probability of the transfer of electronic. The relations are drawn between (α hν)2 and photon energy ( hν) before and after annealing ,as shown in figures (7.a,b and c) and figure (8,a,b and c) respectively . a Eg=3.72eV Volume 4, Issue 4, April 2015 b Page 103 International Journal of Application or Innovation in Engineering & Management (IJAIEM) Web Site: www.ijaiem.org Email: editor@ijaiem.org Volume 4, Issue 4, April 2015 ISSN 2319 - 4847 c Eg=3.81eV Fig. (7, a, b, c) allowed direct transition electronic for Fe2O3 thin films before annealing: a) t=50 nm, b) t=100 nm, c) t= 370 nm Fig. (4-13) allowed direct transition electronic for Fe2O3 thin films after annealing: a) t=50 nm, b) t=100 nm, c) t= 370 nm Volume 4, Issue 4, April 2015 Page 104 International Journal of Application or Innovation in Engineering & Management (IJAIEM) Web Site: www.ijaiem.org Email: editor@ijaiem.org Volume 4, Issue 4, April 2015 Thickness (nm.) ISSN 2319 - 4847 Allowed photon energy Eg (eV) before annealing Allowed photon energy Eg(eV) after annealing 50 3.68 3.70 100 3.72 3.75 370 3.81 3.85 4.Conclusion We have successfully prepared Fe2O3 films by reactive R.F. magnetron sputtering method on glass substrates with different thicknesses. The resulting Fe2O3 films were characterized by XRD measurement and AFM. The optical properties concerning the absorption and transmission spectra were studied for the prepared thin films. References [1] [2] [3] [4] [5] A. Anders Surface & Coatings Technology 200 (2005) 1893 – 1906. P. J. Kelly and R. D. Arnell, Vacuum 56 (3), 159 (2000). F.L.Akkad, APunnose, J.Prabu, J.Appl.Phys A 71(2000)157A magnetron uses a magnetic J. L. Vossen, and W. Kern, “Thin film processes II”, Academic press (1st edition, 1991), pp. 24-32. P. M. Martin, “Handbook of deposition technologies for films and coatings”, Elsevier (3rd edition, 2010), pp. 277278. [6] D. M. Lind, S. M. Berry, G. Chern, H. Mathias, and L. R. Testardi, Phys. Rev. B 45, 1838 (1992). [7] C. A. Klient, H. C. Semmelhack, M. Lorenz, and M. K. Krause, J. Magn. Mater. 140–144, 725 (1995). [8] D. T. Margulies, F. T. Parker, F. E. Spada, R. S. Goldman, J. Li, R. Sinclair, and A. E. Berkowitz, Phys. Rev. B 53, 9175 (1996). [9] W. L. Zhou, K.-Y. Wang, C. J. O’Connor, and J. Tang, J. Appl. Phys. 89, 7398 (2001). [10] J. M. D. Coey, A. E. Berkowitz, L. I. Balcells, F. F. Putris, and F. T. Parker, Appl. Phys. Lett. 72, 734 (1998). [11] E. Lochner, K. A. Shaw, R. C. DiBari, W. Portwine, P. Stoyonov, S. D.Berry, and D. M. Lind, IEEE Trans. Magn. 30, 4912 (1994). [12] F. C. Voogt, T. Fujii, P. J. M. Smulders, L. Niesen, M. A. James, and T.Hibma, Phys. Rev. B 60, 11193 (1999). [13] T. S. Chin and N. C. Chiang, J. Appl. Phys. 81, 5250 (1997). Author AbdulhusseinK.Elttayef, is currently a professor of physics At the Applied physics center, Baghdad, Iraq. He received his Ph.D Degree from Heriot –Watt University (U.K) in 1990. His currently research Interests include the preparation of nano films (semiconductors and polymers) by different methods for applications of gas sensors, solar cells and optical detectors. He has written 40 scientific publications in this area Muthana A.Muhammed M.SC student in physics department, college of science, Wasit University. His research interest includes the preparation of nano films and applications . Muneer H.Jaduaa, He is Assistant Proff. ,at physics dept., college of science, Wasit university. He is leading research group in the field of solid state and material Science. Volume 4, Issue 4, April 2015 Page 105