PAUL SCHERRER INSTITUT Materials Science &Technology NANCER project partners: Rene Tölke, Barbara Scherrer, Henning Galinski, Thomas Ryll, Ludwig Gauckler, Nonmetallic Inorganic Materials, ETH Zurich Thomas Rudin, Antonio Tricoli, Karsten Wegner, Sotoris Pratsinis, Particle Technology Laboratory, ETH Zurich Sebastian Heiroth, Thomas Lippert, General Energy Research Department, PSI Villigen Ruggero Frison, Kazimir Conder, Laboratory for Development of Materials, PSI Villigen Nikolaos Karageorgakis, Andre Heeb, Thomas Graule, Institute of Materials Testing and Research, EMPA Dübendorf project contact: jennifer.rupp@mat.ethz.ch
Electroceramic Materials Ion conductors, MIECs, novel electrocatalysts (fluorite type solid solutions, cermets, perovskites ) Deposition Techniques Flame & Spray Pyrolysis, Sputtering, PLD, MOCVD, Combustion CVD Chip Capacitors Actuator Chips Thin Films Characterization Integration Sensors Battery Charger Chips Micro Fuel Cell Arrays
Spray Pyrolysis µ SOFC Flame Spray Pyrolysis Micro Gas Sensors Prof. Dr. S. Pratsinis Chemical Vapour Deposition Nanoparticle Synthesis Prof. Dr. Th. Graule Dr. Jennifer Rupp Prof. Dr. L. Gauckler Antonio Tricoli Thomas Rudin Dr. Karsten Wegner Dr. Andre Heel Nikolaos Karageorgakis Barbara Scherrer Thomas Ryll Rene Tölke Henning Galinski Pulsed Laser Deposition Thin Film Analytics Sputtering Solid State Chemistry Anna Evans PD Dr. Th. Lippert Sebastian Heiroth PD Dr. K. Conder Ruggero Frison
Goal: Operationable micro-solid Oxide Fuel Cell Membranes for Power in Portable Electronics 5 U.P. Muecke, D. Beckel, A. Bernard, A. Bieberle Hütter, S. Graf, A. Infortuna, P. Müller, J.L.M. Rupp, J. Schneider and L. J. Gauckler, Advanced Functional Materials, accepted 2008 L.J. Gauckler, D. Beckel, U. Mücke, P. Müller and J.L.M. Rupp, PCT patents: PCT /CH 2006/000573, PCT /CH 2006/000575, PCT /CH 2006/000605, 2006
)(24)(5(7)(6(7)8)(1)1)total electrical Conducivity [S/m] 10 1 0,1 0,01 1E-3 ((()0 (3at 500 C ))1E-4 20 40 60 80 100 120 140 Grain Size [nm] [1] Infortuna, A., A.S. Harvey, L.J. Gauckler, Advanced Functional Materials, 2008. 18: p. 127 135. [2] Hertz, J.L. and H.L. Tuller, Journal of Electroceramics, 2004. 13(1 3): p. 663 668. [3] Kosacki, I., et al., Solid State Ionics, 2000. 136 137: p. 1225 1233. [4] Garcia Sanchez, M.F., et al., Solid State Ionics, 2008. 179(7 8): p. 243 249. [5] J. H. Joo and G. M. Choi, Solid State Ionics, vol. 177, pp. 1053 1057, 2006. [6] T. Petrovsky, H. U. Anderson, and V. Petrovsky, Solid State Ionics 2002. Symposium (Mater. Res. Soc. Symposium Proceedings Vol.756), pp. 515 20 xvi+575, 2003. [7] S. Heiroth, Th. Lippert, A.Wokaun and M. Döbeli, Applied Physics A, [in press] [8] D. Perednis, PhD, ETH Zurich, Nr. 15190, 2003.
PLD R.f. sputtering Spray Pyrolysis amorphous nanocrystalline (brick type) nanocrystalline (columnar)??
PLD r.f. sputtered Spray Pyrolysis 400 nm 400 nm 400 nm Microstructure strongly dependent on thin film deposition on-going PhD thesis: Barbara Scherrer, ETH Zurich, Sebastian Heiroth, PSI Villigen, Ruggero Frison, PSI Villigen
PLD r.f. sputtered Spray Pyrolysis 400 nm 400 nm 400 nm cubic phase tetragonal phase Raman investigations: same material (ZrO 2 ) 0.92 (Y 2 O 3 ) 0.08 but different phase. strongly processing dependent on-going PhD thesis: Barbara Scherrer, ETH Zurich, Sebastian Heiroth, PSI Villigen, Ruggero Frison, PSI Villigen
Zirconia-based Films for micro-solid Oxide Fuel Cells Crystallographic density: with post-processing temperature on-going PhD thesis: Barbara Scherrer, ETH Zurich, Sebastian Heiroth, PSI Villigen, Ruggero Frison, PSI Villigen
Zirconia-based Films for micro-solid Oxide Fuel Cells fully nanocrystalline on-going crystallization I. Crystallographic density of thin films is larger compared to bulk. II. During crystallization material shows drastically lowered density. on-going PhD thesis: Barbara Scherrer, ETH Zurich, Sebastian Heiroth, PSI Villigen, Ruggero Frison, PSI Villigen
100 nm 20 C amorphous spray pyrolysis films at deposition on-going PhD thesis: Barbara Scherrer, Nonmetallic Inorganic Materials, ETH Zurich 12
100 nm 600 C nanocrystalline spray pyrolysis film after annealing on-going PhD thesis: Barbara Scherrer, Nonmetallic Inorganic Materials, ETH Zurich 13
100 µm cathode electrolyte anode Micro-SOFC membranes on Foturan substrates are feasible: 200 µm wide & < U.P. Muecke, D. Beckel, A. Bernard, A. Bieberle Hütter, S. Graf, A. Infortuna, P. Müller, J.L.M. Rupp, J. Schneider and L. J. Gauckler, Advanced Functional Materials, accepted 2008 L.J. Gauckler, D. Beckel, U. Mücke, P. Müller and J.L.M. Rupp, PCT patents: PCT /CH 2006/000573, PCT /CH 2006/000575, PCT /CH 2006/000605, 2006 14
100 µm Spray pyrolysis 200 nm PLD Spray pyrolysis PLD Micro-SOFC membranes on Foturan substrates are feasible: 200 µm wide & < U.P. Muecke, D. Beckel, A. Bernard, A. Bieberle Hütter, S. Graf, A. Infortuna, P. Müller, J.L.M. Rupp, J. Schneider and L. J. Gauckler, Advanced Functional Materials, accepted 2008 L.J. Gauckler, D. Beckel, U. Mücke, P. Müller and J.L.M. Rupp, PCT patents: PCT /CH 2006/000573, PCT /CH 2006/000575, PCT /CH 2006/000605, 2006 15
cell voltage [V] 0.50 0.45 0.40 0.35 0.30 0.25 0.20 0.15 0.10 550 C 500 C 450 C 300 250 200 150 100 50 power density [mw/cm 2 ] Spray pyrolysis PLD Spray pyrolysis PLD 200 nm 0.05 0.00 0 200 400 600 800 1000 1200 1400 1600 1800 current density [ma/cm 2 ] 0 Free-standing membrane operates with 237 mw/cm 2 at 550 C on-going PhD thesis: Anna Evans & Rene Tölke, Nonmetallic Inorganic Materials, ETH Zurich
Summary: NANCER Different ceramic thin film architectures can be engineered Test-chips for screening of electric and electrochemical properties of ceramic thin films were realized Ceramic thin film integration and operation in chip-sized devices such as micro-solid Oxide Fuel Cells or sensors