Experimental investigation and thermodynamic modelling of ZrO 2 -based systems
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1 Experimental investigation and thermodynamic modelling of ZrO 2 -based systems O.B. Fabrichnaya,G.B. Savinykh, G. Schreiber H.J. Seifert Institute for Materials Science, Technical University of Freiberg, Germany Experimental studies and thermodynamic modelling of the ZrO 2 -La 2 O 3 -Y 2 O 3 system Experimental study and thermodynamic modelling of the ZrO 2 -Nd 2 O 3 -Y 2 O 3 system Preliminary results for the ZrO 2 -Sm 2 O 3 -Y 2 O 3 system This work was financially supported by DFG grant SE 647/9-2 Porto, TOFA-meeting, September 14, 2010
2 Thermal barrier coating (TBC) TBC: YSZ (tetragonal t ZrO 2 stabilised by Y 2 O 3 ) New candidates: YSZ co-stabilised by other RE 2 O 3, pyrochlore structure RE 2 Zr 2 O 7 (RE=Gd-La) TGO (thermally grown oxide): α-al 2 O 3 forming during thermal cycling BC (bond coat): Ni-Cr-Al-Y or Pt modified aluminide Ni-based alloy Aim of the project: Thermodynamic database development for the ZrO 2 -RE 2 O 3 -Y 2 O 3 -Al 2 O 3 system (RE = La, Nd, Sm, Gd, Yb) Methods: CALPHAD and experimental studies (co-precipitation, phase equilibria, XRD, SEM/EDX, DTA) Other applications: Solid Oxide Fuel Cell, Oxygen Sensors, Nuclear Materials, Refractory Materials, Directionally Solidified Eutectic Composites Al 2 O 3 -Y 3 Al 5 O 12 (ZrO 2 )
3 Thermodynamic modelling Phase Model Fluorite (F) (Zr +4,RE +3,Y +3 ) 1 (O -2,Va) 2 Tetragonal (T) Monoclinic (M) A (RE +3, Y +3,Zr +4 ) 2 (Va,O -2 ) 1 (O -2 ) 3 H X C B Pyrochlore (Pyr) (RE +3,Y +3,Zr +4 ) 2 (Zr +4,Y +3,RE +3 ) 2 (O -2,Va) 6 (O -2 ) 1 (Va,O -2 ) 1 Perovskite (LaYP) (La +3,Y +3 ) 1 (Y +3,La +3 ) 1 (O -2 ) 3 δ-zr 3 Y 4 O 12 (Y +3 ) 4 (Zr +4 ) 3 (O -2 ) 12 Liquid (L) (RE +3,Y +3,Zr +4 ) P (O -2 ) Q
4 Scheme of co-precipitation and following treatments
5 System ZrO 2 -Y 2 O 3 b a c Phase diagram (a), enthalpy of mixing in fluorite phase along with solution calorimetry data (b), activity in fluorite phase along with vapour pressure data (c)
6 Phase diagrams for binary systems ZrO 2 -La 2 O 3 and La 2 O 3 -Y 2 O 3 Accepted from [2008Fab] [2010Fab_2]
7 Experimental studies of the ZrO2-La2O3-Y2O3 system
8 Experimental study of sample #2 ZrO La 2 O Y 2 O C First transformation occurs at 1503 C (Pyr Flu) second at 1572 C (LaYO 3 B) 1600 C
9 Experimental studies of the ZrO 2 -La 2 O 3 -Y 2 O 3 system Composition #8 ZrO La 2 O Y 2 O C 1600 C Pyr+C F
10 Thermodynamic modelling of the ZrO 2 -La 2 O 3 -Y 2 O 3 system Fabrichnaya et al. 2010, J. Alloys Comp.
11 Phase diagrams for binary systems ZrO 2 -Nd 2 O 3 and Nd 2 O 3 -Y 2 O 3 Calculated in [Fabrichnaya 2010] Calculated in [Fabrichnaya 2010]
12 Calculations based on binary approximation T=1523 K Experimental data are from [1986Hin]
13 Isothermal section of the ZrO 2 -Nd 2 O 3 -Y 2 O 3 system at 1250 C and XRD pattern for sample #7 (ZrO Nd 2 O 3-5.4Y 2 O 3 ) and sample #23 (ZrO Nd 2 O Y 2 O 3 ) 23 7
14 Isothermal section of the ZrO 2 -Nd 2 O 3 -Y 2 O 3 system at 1400 C and XRD pattern for sample #7 (ZrO Nd 2 O 3-5.4Y 2 O 3 ) and sample #23 (ZrO Nd 2 O Y 2 O 3 ) 23 7
15 Isothermal section of the ZrO 2 -Nd 2 O 3 -Y 2 O 3 system at 1600 C and XRD pattern for sample #7 (ZrO Nd 2 O 3-5.4Y 2 O 3 ) and sample #23 (ZrO Nd 2 O Y 2 O 3 ) 7 23
16 DTA investigation of sample #7 ZrO Nd 2 O 3-5.4Y 2 O 3 Transformation B+Pyr F 1459 C
17 Technische Universität Bergakademie Freiberg DTA investigation of sample #23 ZrO Nd2O3-2.73Y2O3 # C # C Transformations: Pyr F 1471 C B A 1608 C
18 Isothermal section at 1600 C and SEM for samples #2, 4, 23 #2 B F 23 #23 F A 2 4 #4 F B C
19 Phase diagrams of ZrO 2 -Sm 2 O 3 and Sm 2 O 3 -Y 2 O 3 systems
20 Isothermal sections of the ZrO 2 -Sm 2 O 3 -Y 2 O 3 system at 1250, 1400 and 1600 C
21 Conclusions 1. Phase relations are experimentally studied in the system ZrO 2 -La 2 O 3 -Y 2 O 3 at C by XRD and SEM/EDX. DTA investigation confirmed reaction Pyrochlore + Y 2 O 3 _C Fluorite occuring at ~1440 C. The obtained data were used for thermodynamic modelling of the system. 2. Phase relations of the ZrO 2 -Nd 2 O 3 -Y 2 O 3 system are experimentally studied at C by XRD and SEM/EDX. DTA investigation of sample with composition ZrO Nd 2 O Y 2 O 3 confirmed reaction Pyrochlore + (Nd,Y) 2 O 3 _B Fluorite occuring ~1460 C. DTA investigation of sample ZrO Nd 2 O Y 2 O 3 indicated two transformations confirmed by XRD: Pyr F at 1442 C and B A 1604 C 3. The thermodynamic parameters of the ZrO 2 -Nd 2 O 3 -Y 2 O 3 system are assessed based on obtained experimental results. 4. The isothermal sections of the ZrO 2 -Sm 2 O 3 -Y 2 O 3 system are calculated based on binary extrapolation. The first experiments revealed several differences with calculations
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