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Chemical Vapor Deposition of NiFe 2 O 4 using Nickelocene and N-butylferrocene

Chemical Vapor Deposition of NiFe 2 O 4 using Nickelocene and N-butylferrocene. Mark Kimbell. Prof. Takoudis Manish Singh Yi Yang. Project. Chemical Vapor Deposition Nickel Oxide ( NiO ) using Ni(C 5 H 5 ) 2 Iron Oxide (Fe 2 O 3 ) using FeC 14 H 18 Nickel Ferrite (NiFe 2 O 4 )

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Chemical Vapor Deposition of NiFe 2 O 4 using Nickelocene and N-butylferrocene

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  1. Chemical Vapor Deposition of NiFe2O4 using Nickelocene and N-butylferrocene Mark Kimbell Prof. Takoudis Manish Singh Yi Yang

  2. Project • Chemical Vapor Deposition • Nickel Oxide (NiO) using Ni(C5H5)2 • Iron Oxide (Fe2O3) using FeC14H18 • Nickel Ferrite (NiFe2O4) • Choose appropriate conditions based on NiO and Fe2O3 growth rates • XPS to analyze chemical composition • XRD to analyze crystalline structure

  3. Background • The magnetoelectric (ME) effect • Ferroelectric and ferromagnetic coupling • Magnetic switching by an applied electric field • Electric polarity switching by an applied magnetic field

  4. Magnetoelectric Materials • Uses • Memory storage devices • Tunable microwave devices • Sensors • Transducers C Israel, ND Mathur & JF Scott, Nature Materials 7 (2008) 93

  5. Magnetoelectric Composites • Magnetoelectric composites • Made up of a piezoelectric layer and a magnetostrictive layer NiFe2O4

  6. Chemical Vapor Deposition (CVD) Argongas Heater Oxygen gas Substrate Quartz tube Vacuum pump

  7. Precursors • Source of the vapor which is fed into the reaction chamber • N-BUTYLFERROCENE • NICKELOCENE • C14H18Fe • Ni(C5H5)2

  8. Nickel Oxide Data Nickel Oxide Growth Rate (Reactor = 400 oC) Temperature of Nickelocene (oC)

  9. Iron Oxide Data Iron Oxide Growth Rate (Reactor = 500 oC) Growth Rate (nm/min) Temperature of N-Butylferrocene (oC)

  10. Important Results • Treactor = 400oC • Tnickelocene = 60oC • Treactor = 400oC • Tn-butylferrocene = 65oC NiO growth rate = 4.6 nm/min Fe2O3 growth rate = 8.5 – 9 nm/min

  11. The Plan

  12. X-Ray Photoelectron Spectroscopy (XPS) • Uses x-rays to knock electrons free from surface • Measures kinetic energy of electrons to determine chemical composition http://www.sckcen.be/microstructure/Infrastructure/XPS/Infrastructure_XPS.htm

  13. XPS Results • Longer cycles (5 cycles, 90 seconds each) Ni 2p Fe 2p O 1s C 1s

  14. XPS Results • Shorter cycles (20 cycles, 18 seconds each) Ni 2p Fe 2p O 1s C 1s

  15. XPS Results • Co-Deposition Ni 2p Fe 2p O 1s C 1s

  16. XPS Results • Co-Deposition Ni 2p Fe 2p O 1s C 1s

  17. XPS Results – Iron * Peaks correspond to Fe(III) oxidation state * S. A. Chambers, Y. J. Kim, and Y. GaoSurf. Sci. Spectra 5 219 (1998)

  18. XPS Results – Nickel * Peaks correspond to Ni(II) oxidation state * A. N. Mansour, Surf. Sci. Spectra 3 231 (1994)

  19. XPS Results • Do not indicate the presence of NiFe2O4 • Probably due to interactions between the two gases • Presence of carbon • From atmosphere • Argon sputtering • From unreacted precursor • Due to relatively low deposition temperature

  20. Summary • XPS revealed the presence of both Ni(II) and Fe(III) • The ratio of Ni to Fe did not indicate NiFe2O4 • Different deposition conditions must be used in order to achieve the correct ratios • Higher reactor temperature • Higher iron precursor temperature • Lower nickel precursor temperature

  21. Future Work • Try different deposition conditions to deposit NiFe2O4 thin films • X-ray diffraction (XRD) on NiFe2O4 thin films to determine crystalline structure • Anneal to reduce carbon contamination, correct defects / change crystal structure

  22. References • E. Ascher, H. Rieder, H. Schmid, and H. Stössel, J. Appl. Phys. 37 (1966) 1404 • W. Eerenstein, N. D. Mathur and J. F. Scott, Nature 442, (2006) 759-765 • A.M.J.G. Van Run, D.R. Terrell, and J.H. Scholing, Journal of Materials Science 9 (1974) 1710-1714 • W. Yeh and M. Matsumura, Jpn. J. Appl. Phys. Vol. 36 (1997) Pt. 1, No. 11 • M. Singh, Y. Yang, and C.G. Takoudis, Journal of The Electrochemical Society, 155 (9) (2008) D618-D623 • S.A. Chambers, Y.J. Kim, and Y. Gao, Surf. Sci. Spectra 5 (1998) 219 • S. Oswald and W. Bruckner, Surf. Interface Anal. 36 (2004) 17–22 • http://www.sckcen.be/microstructure/Infrastructure/XPS/Infrastructure_XPS.htm

  23. Acknowledgements • EEC-NSF Grant # 0755115 • Dr. Christos Takoudis • Graduate students: Yi Yang, Manish Singh, Qian Tao

  24. Questions?

  25. Cycling Argongas Heater Oxygen gas Substrate Quartz tube Vacuum pump Cycling

  26. Co-Deposition Argongas Heater Oxygen gas Substrate Quartz tube Vacuum pump Co-Deposition

  27. Experiment – Setup Temperature controllers Precursor containers • nickelocene • n-butylferrocene Cold trap Reaction chamber Vacuum pump

  28. Ellipsometer • Used to measure film thickness Light source Θ Analyzer Polarizer Sample

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