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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

Chemical Vapor Deposition of NiFe2O4 using Nickelocene and N-butylferrocene

Mark Kimbell

Prof. Takoudis

Manish Singh

Yi Yang

project
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
background
Background
  • The magnetoelectric (ME) effect
    • Ferroelectric and ferromagnetic coupling
      • Magnetic switching by an applied electric field
      • Electric polarity switching by an applied magnetic field
magnetoelectric materials
Magnetoelectric Materials
  • Uses
    • Memory storage devices
    • Tunable microwave devices
    • Sensors
    • Transducers

C Israel, ND Mathur & JF Scott, Nature Materials 7 (2008) 93

magnetoelectric composites
Magnetoelectric Composites
  • Magnetoelectric composites
    • Made up of a piezoelectric layer and a magnetostrictive layer

NiFe2O4

chemical vapor deposition cvd
Chemical Vapor Deposition (CVD)

Argongas

Heater

Oxygen gas

Substrate

Quartz tube

Vacuum pump

precursors
Precursors
  • Source of the vapor which is fed into the reaction chamber
  • N-BUTYLFERROCENE
  • NICKELOCENE
  • C14H18Fe
  • Ni(C5H5)2
nickel oxide data
Nickel Oxide Data

Nickel Oxide Growth Rate

(Reactor = 400 oC)

Temperature of Nickelocene (oC)

slide9

Iron Oxide Data

Iron Oxide Growth Rate

(Reactor = 500 oC)

Growth Rate (nm/min)

Temperature of N-Butylferrocene (oC)

important results
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

x ray photoelectron spectroscopy xps
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

xps results
XPS Results
  • Longer cycles (5 cycles, 90 seconds each)

Ni 2p

Fe 2p

O 1s

C 1s

xps results1
XPS Results
  • Shorter cycles (20 cycles, 18 seconds each)

Ni 2p

Fe 2p

O 1s

C 1s

xps results2
XPS Results
  • Co-Deposition

Ni 2p

Fe 2p

O 1s

C 1s

xps results3
XPS Results
  • Co-Deposition

Ni 2p

Fe 2p

O 1s

C 1s

xps results iron
XPS Results – Iron

*

Peaks correspond to Fe(III) oxidation state

* S. A. Chambers, Y. J. Kim, and Y. GaoSurf. Sci. Spectra 5 219 (1998)

xps results nickel
XPS Results – Nickel

*

Peaks correspond to Ni(II) oxidation state

* A. N. Mansour, Surf. Sci. Spectra 3 231 (1994)

xps results4
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
summary
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
future work
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
references
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
acknowledgements
Acknowledgements
  • EEC-NSF Grant # 0755115
  • Dr. Christos Takoudis
  • Graduate students: Yi Yang, Manish Singh, Qian Tao
cycling
Cycling

Argongas

Heater

Oxygen gas

Substrate

Quartz tube

Vacuum pump

Cycling

co deposition
Co-Deposition

Argongas

Heater

Oxygen gas

Substrate

Quartz tube

Vacuum pump

Co-Deposition

experiment setup
Experiment – Setup

Temperature

controllers

Precursor

containers

  • nickelocene
  • n-butylferrocene

Cold trap

Reaction chamber

Vacuum pump

ellipsometer
Ellipsometer
  • Used to measure film thickness

Light source

Θ

Analyzer

Polarizer

Sample

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