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Ion Implantation and Annealing of Crystalline Oxides and Ceramic Materials C.W. WHITE, L.A. BOATNER, P.S. SKLAD, C.J. McHARGUE, J. RANKIN , G.C. FARLOW and M.J. AZIZ  Oak Ridge Natronal Laboratory, Oak Ridge, TN 37831, USA By : Younes Sina & Uk Huh The University of Tennessee, Knoxville
The unit cell of SrTiO3 consists of a central Ti4+-ion, which is octahedrallycoordinated by 6 O2--ions. At the corners of the cube Sr2+-ions are situated O SrTiO3 Ti Sr
Space group:             Pm-3mNumber:                        221Pearson symbol:         cP5 Unit cell dimensions: a = 3.795 Å Atomic positions: Ti  at (0, 0, 0) Ca  at (1/2, 1/2, 1/2) O  at (1/2, 0, 0)  Orthorhombic structure CaTiO3 a≈c
Al2O3 O Al
CaTiO3 Crystal Damage Annealing in air @ 270- 550 ⁰C Pb (540 keV, 1x1015 /cm2) Rutherford Back  Scattering(RBS) 2 Mev He+ TEM
SrTiO3 100 110 111 Crystal Damage Annealing in air @ 270- 550 ⁰C From few minutes to many hours Pb (540 keV, 1x1015 /cm2) Rutherford Back  Scattering(RBS) 2 Mev He+
Al2O3 Crystal Damage Annealing in air @ 800- 1200 ⁰C 2Al (90 keV, 4x1016 /cm2)&  3 O(55 keV, 6x1016 /cm2) Rutherford Back  Scattering(RBS) 2 Mev He+ TEM
Al2O3 Crystal Damage Annealing in Ar @ 800 & 960 ⁰C Fe (160 keV, 4x1016 /cm2 ,L N2) Rutherford Back  Scattering(RBS) 2 Mev He+ TEM
SrTiO3             implanted by:  Pb (540 keV, 1x1015 /cm2) Liquid Nitrogen 100 Ion channeling before annealing Depth of the amorphous region: 1800 Å Ion channeling after annealing (400 ° C/30 min) Implanted Pb is substitutional  in the lattice after annealing Epitaxial Recrystallization
(100) SrTiO3             implanted by:  Pb (540 keV, 1x1015 /cm2) Ion channeling after annealing 302 ° C/45 min Epitaxial Recrystallization Depth of the amorphous region  after annealing: 800 Å
Crystallized depth vs. annealing time (100) SrTiO3             implanted by:  Pb (540 keV, 1x1015 /cm2) 302 ° C Slope 0.91 Å/s Induction period
(100) SrTiO3             implanted by:  Pb (540 keV, 1x1015 /cm2) 3 Å/s Increasing T  Increasing Slope 1.48 Å/s 350 ° C 325 ° C 0.91 Å/s 302 ° C The induction period decreases markedly as  the annealing temperature increases.
Crystallization of amorphous SrTiO3 Amorphous ->Crystal Transformation V(T)=V0e-Q/RT V00.05 cm/s & Q0.77 eV Q0.77 eV Kinetics of crystallization of Pb- implanted (100) SrTiO3
SrTiO3 100 110 111 Pb (540 keV, 1x1015 /cm2) Growth in the (110) direction almost is the same of (100) Growth in the (111) direction is not linear with time Crystallization kinetics are not strongly affected by Pb concentration
CaTiO3-High symmetry face             implanted by:  Pb (540 keV, 1x1015 /cm2)            Ion channeling spectra after annealing at 425 ° C/15 h in air
Cross section micrograph of Pb (250 keV, 4x1015 /cm2) implanted CaTiO3
CaTiO3   (High symmetry face)             implanted by:  Pb (250 keV, 4x1015 /cm2)             Ion channeling spectra after annealing at 500 ° C/h in air Ion channeling spectra in the as-implanted state
Recrystallization of amorphous CaTiO3 Amorphous ->Crystal Transformation Q1.3 eV Q3.76 eV Kinetics of crystallization of Pb- implanted CaTiO3
Crystallization of amorphous  Al2O3 Amorphous ->Crystal Transformation 1600Å A few minutes at 800 ° C for 1600 Å      γ->α 100 hr at 800 ° C  For 800 Å      γ->α γ->α stops before reaching the surface
Annealing at 960 ° C/ 90 min TEM  cross section of ->α transition in Al2O3
Crystallization of amorphous Al2O3 Amorphous ->Crystal Transformation implanted by:  2  Al (90 keV, 4x1016 /cm2) & 3 O (55 keV, 6x1016 /cm2)  at liquid nitrogen           960 ° C/45 min
Kinetics of ->α transition in Al2O3 Temperature dependence of the ->α interface velocity in Al2O3
A micrograph of Fe- implanted Al2O3 (LN2) after annealing at 960 ° C/45 min
Annealing of Fe (160 keV, 4x1016 /cm2 ,L N2) implanted α- Al2O3 As implanted Al2O3 Fe 960 ° C/45 min
1500 Å Fe toward the surface Annealing Crystal Damage Crystallization behavior (amorphous ->->α ) remains the same but the kinetics of /α transformation increase by the presence of Fe  Fe The presence of Fe in the amorphous film increases the crystallization kinetics at least by a factor of 4
Thank you

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Younes Sina, Uk Huh, Ion Implantation

  • 1. Ion Implantation and Annealing of Crystalline Oxides and Ceramic Materials C.W. WHITE, L.A. BOATNER, P.S. SKLAD, C.J. McHARGUE, J. RANKIN , G.C. FARLOW and M.J. AZIZ Oak Ridge Natronal Laboratory, Oak Ridge, TN 37831, USA By : Younes Sina & Uk Huh The University of Tennessee, Knoxville
  • 2.
  • 3. The unit cell of SrTiO3 consists of a central Ti4+-ion, which is octahedrallycoordinated by 6 O2--ions. At the corners of the cube Sr2+-ions are situated O SrTiO3 Ti Sr
  • 4. Space group: Pm-3mNumber: 221Pearson symbol: cP5 Unit cell dimensions: a = 3.795 Å Atomic positions: Ti  at (0, 0, 0) Ca  at (1/2, 1/2, 1/2) O  at (1/2, 0, 0) Orthorhombic structure CaTiO3 a≈c
  • 6. CaTiO3 Crystal Damage Annealing in air @ 270- 550 ⁰C Pb (540 keV, 1x1015 /cm2) Rutherford Back Scattering(RBS) 2 Mev He+ TEM
  • 7. SrTiO3 100 110 111 Crystal Damage Annealing in air @ 270- 550 ⁰C From few minutes to many hours Pb (540 keV, 1x1015 /cm2) Rutherford Back Scattering(RBS) 2 Mev He+
  • 8. Al2O3 Crystal Damage Annealing in air @ 800- 1200 ⁰C 2Al (90 keV, 4x1016 /cm2)& 3 O(55 keV, 6x1016 /cm2) Rutherford Back Scattering(RBS) 2 Mev He+ TEM
  • 9. Al2O3 Crystal Damage Annealing in Ar @ 800 & 960 ⁰C Fe (160 keV, 4x1016 /cm2 ,L N2) Rutherford Back Scattering(RBS) 2 Mev He+ TEM
  • 10. SrTiO3 implanted by: Pb (540 keV, 1x1015 /cm2) Liquid Nitrogen 100 Ion channeling before annealing Depth of the amorphous region: 1800 Å Ion channeling after annealing (400 ° C/30 min) Implanted Pb is substitutional in the lattice after annealing Epitaxial Recrystallization
  • 11. (100) SrTiO3 implanted by: Pb (540 keV, 1x1015 /cm2) Ion channeling after annealing 302 ° C/45 min Epitaxial Recrystallization Depth of the amorphous region after annealing: 800 Å
  • 12. Crystallized depth vs. annealing time (100) SrTiO3 implanted by: Pb (540 keV, 1x1015 /cm2) 302 ° C Slope 0.91 Å/s Induction period
  • 13. (100) SrTiO3 implanted by: Pb (540 keV, 1x1015 /cm2) 3 Å/s Increasing T Increasing Slope 1.48 Å/s 350 ° C 325 ° C 0.91 Å/s 302 ° C The induction period decreases markedly as the annealing temperature increases.
  • 14. Crystallization of amorphous SrTiO3 Amorphous ->Crystal Transformation V(T)=V0e-Q/RT V00.05 cm/s & Q0.77 eV Q0.77 eV Kinetics of crystallization of Pb- implanted (100) SrTiO3
  • 15. SrTiO3 100 110 111 Pb (540 keV, 1x1015 /cm2) Growth in the (110) direction almost is the same of (100) Growth in the (111) direction is not linear with time Crystallization kinetics are not strongly affected by Pb concentration
  • 16. CaTiO3-High symmetry face implanted by: Pb (540 keV, 1x1015 /cm2) Ion channeling spectra after annealing at 425 ° C/15 h in air
  • 17. Cross section micrograph of Pb (250 keV, 4x1015 /cm2) implanted CaTiO3
  • 18. CaTiO3 (High symmetry face) implanted by: Pb (250 keV, 4x1015 /cm2) Ion channeling spectra after annealing at 500 ° C/h in air Ion channeling spectra in the as-implanted state
  • 19. Recrystallization of amorphous CaTiO3 Amorphous ->Crystal Transformation Q1.3 eV Q3.76 eV Kinetics of crystallization of Pb- implanted CaTiO3
  • 20. Crystallization of amorphous Al2O3 Amorphous ->Crystal Transformation 1600Å A few minutes at 800 ° C for 1600 Å γ->α 100 hr at 800 ° C For 800 Å γ->α γ->α stops before reaching the surface
  • 21. Annealing at 960 ° C/ 90 min TEM cross section of ->α transition in Al2O3
  • 22. Crystallization of amorphous Al2O3 Amorphous ->Crystal Transformation implanted by: 2 Al (90 keV, 4x1016 /cm2) & 3 O (55 keV, 6x1016 /cm2) at liquid nitrogen 960 ° C/45 min
  • 23. Kinetics of ->α transition in Al2O3 Temperature dependence of the ->α interface velocity in Al2O3
  • 24.
  • 25. A micrograph of Fe- implanted Al2O3 (LN2) after annealing at 960 ° C/45 min
  • 26. Annealing of Fe (160 keV, 4x1016 /cm2 ,L N2) implanted α- Al2O3 As implanted Al2O3 Fe 960 ° C/45 min
  • 27. 1500 Å Fe toward the surface Annealing Crystal Damage Crystallization behavior (amorphous ->->α ) remains the same but the kinetics of /α transformation increase by the presence of Fe Fe The presence of Fe in the amorphous film increases the crystallization kinetics at least by a factor of 4
  • 28.