Defect structure and oxygen diffusion in PZT ceramics

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1 Defect structure and oxygen diffusion in PZT ceramics Adam Georg Balogh Institute of Materials Science Technische Universität Darmstadt A. G. Balogh Folie 1

2 Introduction Ferroelectrics are of great technical interest because of their sensing and actuator properties e.g.: smart materials (e.g. change of damping behavior) thin films for non-volatile memory applications However, the materials suffer from fatigue! (mechanically and electrically) electrical fatigue under polarization reversal is attributed to the hindrance of domain wall mobility with point defects and electrochemical degradation The exact fatigue mechanisms are still poorly understood Consequently, the investigation of point defects and their diffusion are of great interest A. G. Balogh Folie 2

3 Positron Annihilation Spectroscopy e + -Source β + -decay 22 Na 22 Ne 1275 kev Birth-γ Start e + TAC defect e + Diffusion typical diffusion length ~ λ 0.1 µm 2 Annihilation-γ s 511 kev PM Log N Stop PM MCA A. G. Balogh Folie 3

4 A. G. Balogh Folie 4 Trapping model defect Annihilation defect-free bulk e + λ b λ d κ d Thermalization Trapping e. g. for a single defect rate eq.: b d d d d b d b b b n n t d n d n n t d n d κ λ κ λ + = = ) exp( ) exp( ) ( τ τ t I t I t D + = ; 1 2 λ d τ = = = = d b d I I I C τ τ τ τ µ κ λ b κ d τ + = 1 1

5 Typical Lifetime Spectrum The lifetime spectrum is given by: N ( t) k + 1 = i= 1 I i t exp τ i τ i k defects yield to k+1 Lifetimecomponents τ k+1! H. S. Leipner, C. G. Hübner, T. E. M. Staab, R. Krause-Rehberg, Mater. Sci. Forum (2001), A. G. Balogh Folie 5

6 Ionic Radii Pauling 4- coordinate 6- coordinate 8- coordinate [pm] [pm] [pm] [pm] Pb La Zr Ti Nb [1] [2] R.D. Shannon, Acta Cryst., 1976, A32, 751. [3] R.D. Shannon and C.T. Prewitt, Acta Cryst., 1969, B25, 925. [4] R.D. Shannon and C.T. Prewitt, Acta Cryst., 1970, B26, [5] J.E. Huheey, E.A. Keiter, and R.L. Keiter in, 4th edition, HarperCollins, New York, USA, A. G. Balogh Folie 6

7 Effect of La +3 and Nb +5 -doping α a 0 : Å α,β,γ : Pb +2 -site ionic radii: r(la +3 )/r(pb +2 )~0.88 r(nb +5 )/r(pb +2 )~0.62 the dopant induces V Pb Zr +4 /Ti +4 -site ionic radii: r(nb +5 )/r([zr 60 Ti 40 ] +4 )~0.94 the dopant induces V Pb r(la +3 )/ r([zr 60 Ti 40 ] +4 )~1.38 dopant induces V O A. G. Balogh Folie 7

8 Cell metric from Rietveld refinement The lattice parameter a 0 as well as the cell volume monotonically decreases for both La +3 and Nb +5 doping. According to the ionic radii this suggests that La +3 occupies Pb-sites and Nb +5 Zr/Ti-sites exclusively. A. G. Balogh Folie 8

9 Cell volume cell volume [10-30 m 3 ] doped Pb(Zr 0.6 Ti 0.4 )O 3 La Nb dopant [mol. %] A. G. Balogh Folie 9

10 Defect Chemistry La 3+ on Pb 2+ site 2 La A V Pb Nb 5+ on Zr/Ti 4+ site 2 Nb B V Pb A. G. Balogh Folie 10

11 Calculated Positron Lifetimes DFT-pseudopotential, atomic superposition methods PbTiO 3 * LaCoO 3 * BaTiO 3 * PZT(60/40) τ / [ps] τ / [ps] τ / [ps] τ / [ps] bulk V A V B V O V O 160 V A V O *V.J. Ghosh, B. Nielsen and Th. Friessnegg, Phys. Rev. B Vol. 61 No. 1 (2000), This work with W. Puff and G. Bischoff, TU Graz A. G. Balogh Folie 11

12 260 Varying Zr/Ti ratio tetragonal morphotrop rhombohedral 90 Lifetime [ps] τ 2 τ 1 I Intensity I 2 [%] ,35 0,40 0,45 0,50 0,55 0,60 0,65 0,70 0,75 x Pb(Zr x Ti 1-x )O 3 A. G. Balogh Folie 12

13 Lifetime data of donor doped samples donor doping yields to the saturation of lifetime component τ 2 ~300ps (V Pb ) τ ps as τ 2 saturates, τ bulk disappears, sat. τ 1 can be attributed to V O τ~170 ps A. G. Balogh Folie 13

14 XPS Pb 4f N(E) [a.u.] XPS Mg Kα 6% La 1% La undoped 5/2 4.9 ev 7/2 Pb 4f N(E) [a.u.] XPS Al Kα 6% La La 3+ 2 kev Ar + V O 5/2 Pb 4f 7/2 1.5 ev O-plasma 4.8 ev 4.8 ev 1.5 ev BE [ev] BE [ev] A. G. Balogh Folie 14

15 About the defect structure of PZT - compensation mechanisms (i) Vacancy formation (e.g. for La 3+ -, Nb 5+ -doping): La 3+ on the A-site: 3 Pb(Zr /Ti)O 3 + La 2 O 3 3( La Pb ) 2 / 3 (V Pb ) 1 / 3 (Zr /Ti)O Pb O 3 Pb(Zr /Ti)O La 2 O 3 4 La Pb La 3+ on the B-site: 2 Pb(Zr /Ti)O 3 + La 2 O 3 2 Pb La (Zr /Ti ) (V O ) 1/ 2 O 5 / (Zr /Ti)O 2 Nb 5+ on the B-site: Pb(Zr /Ti)O 3 + Nb 2 O 5 2 Pb 1/ 2 (V Pb ) 1 / 2 Nb ( Zr /Ti ) O 3 + (Zr /Ti)O 2 5 Pb(Zr /Ti)O Nb 2 O 5 5 Pb(Nb (Zr /Ti ) Nb 5+ on the A-site: 5 Pb(Zr /Ti)O 3 + Nb 2 O 5 5 (Nb Pb ) 2 / 5 (V Pb ) 3 / 5 (Zr /Ti)O PbO Pb(Zr /Ti)O Nb 2 O 5 4 Nb Pb (V (Zr /Ti ) ) 1/ 4 (Zr /Ti) 3 / 4 O PbO ) 4 / 5 (V (Zr /Ti ) ) 1/ 5 O (Zr /Ti)O 2 ) 3 / 4 (Zr /Ti) 1/ 4 O 3 + PbO (V (Zr /Ti ) A. G. Balogh Folie 15

16 electrical compensation mechanisms (ii) Conduction states allow a fraction of free e - or h + in the material multiple charge states of the defects e.g. formation of Ti 3+ polaron states think of the FE oxide as a wide band gap SC Position of E F determines defect charge states and defect formation enthalpies A. G. Balogh Folie 16

17 The V Pb related lifetime τ 2 first principle total energy calculations predict [1] several stable charge states of V Pb The existance of V Pb -V O bound complexes is unlikely (endothermic, negative binding energies), However: [1] S. Pöykö and D.J. Chadi APL 76 (2000) 499 A. G. Balogh Folie 17

18 Vacuum annealing A. G. Balogh Folie 18

19 V O trapping coefficient (1) extremely high conc. k = µ C e.g.: µ für Si: µ(v si+ ): 6 x s -1 µ(v si0 ): 6 x s -1 µ(v si- ): 5 x s -1 (2) The charge is not 2+! Ti as a transition metal has empty 3d states charge compensation A. G. Balogh Folie 19

20 Temperature dependent trapping coefficient of positrons for different charge states Calculation for semiconductors A. G. Balogh Folie 20

21 Temperature dependant positron lifetimes 1,12000 relative rise 1, , , , ,02000 Fe O(V) charge transfer above 150 K Positive charge state Fe 0 % Fe 0,5 % Fe 1,0 % Neutral charge state 1, , Temperature [K] A. G. Balogh Folie 21

22 Mössbauer spectra of 57 Fe (0.5%):Pb 1 (Zr 54 Ti 46 ) 1 O 3 at different temperatures Intensity (arbitrary units) a b 300 K 80 K Doublet: Fe O v dipoles Isomery shift: charge state Fe 3+ (in agreement with ESR) c 4.2 K Velocity (mm/s) Sextet: low spin relaxation No magnetic intereaction because the large avarage distance between Fe atoms: distribution is homogenous A. G. Balogh Folie 22

23 Interpreting the donor doping effects τ 2 is clearly associated to V Pb τ 2 gradually increases from 255 to 305 ps with the dopant concentration for high donor concentrations the position of E F, which energetically favours associated V O -V Pb vacancy complexes defect concentrations are generally so high that saturation occurs τ 1 is stable at ~170 ps which corresponds to single V O further evidence that τ 1 is not the bulk lifetime but associated with V O comes from vacuum annealing experiments (defect formation enthalpy is about E~ 1eV) the charge state of V O is probably not 2+ A. G. Balogh Folie 23

24 Microstructural Effects undoped 2 Nb 1 Nb 4 Nb SEM images provided by H. Kungl A. G. Balogh Folie 24

25 18 O Thermal indiffusion Oxygen Tracer Diffusion 18 O Ion Implantation 18 O Annealing of the samples / Electrical fatigueing depth profiling of the 18 O Tracer by means of SIMS or NRA 18 O(p,γ) 19 N E res :151.2 ± 0.05 kev However using poly samples GB contributions are apparent! A. G. Balogh Folie 25

26 18 O-tracer Diffusion Experiments Thermal indiffusion of 18 O is possible However, limited temperature range ( ºC) Alternative: 18 O ion implantation Depth profiles include several fast diffusive components D ranges from 7 x x cm 2 /sec Seperation of the components Electric cycling mediated diffusion is in progress A. G. Balogh Folie 26

27 18 Oxygen Tracer Diffusion thermal 18 O exchange indiffusion 400ºC for 3 hrs. 2psi 18 O A. G. Balogh Folie 27

28 Principle of SIMS measurement primery ions (O or Cs) SIMS crater secondary ions to analyse optic sputtering sample A. G. Balogh Folie 28

29 SIMS 18 O depth profiles in PZT (Pb-Zr-Ti-O) ferroelectric samples A. G. Balogh Folie 29

30 Activation enthalpies and chemical surface reaction for O in PZT A. G. Balogh Folie 30

31 Implant. Depth [Å] O Conc. [arb. units] depth Oxygen Implantation 18 O in PZT 5 kev 10 kev F W H M : 14 nm F W H M : 25 nm x 0 : 9 nm x 0 : 15 nm 15 kev 20 kev F W H M : 33 nm F W H M : 44 nm x 0 : 22 nm x 0 : 28 nm nuclear de/dx elec. 30 de/dx kev F W H M : 64 nm x 0 : 41 nm de/dx [ev/å] Im plantation D epth [nm ] 18 O Implant. Energy [kev] A. G. Balogh Folie 31

32 Summary and Conclusions PAS clearly shows that La as well as Nb doping yields to the saturation of lifetime component τ 2, suppossedly belonging to τ(v Pb ) ~300ps both dopants produce single Pb vacancies we suggest the existance of associated V Pb V O vacancies in undoped samples, However τ(v Pb V O ) 0 < τ(v Pb ) 2- as τ 2 saturates, τ bulk disappears, and I 2 drops, τ 1 can be attributed to τ(v O ) ~155 ps consequently the dopant also creates V O Surprisingly V O 2+ are easily detectable with PAS A. G. Balogh Folie 32

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