K. Nagasawa1), O. Mentré2), S. Daviero-Minaud2),

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Presentation transcript:

The Electrochemical and thermal performances of Ca3Co4O9-δ as a cathode material for IT-SOFCs K. Nagasawa1), O. Mentré2), S. Daviero-Minaud2), N. Preux2), A. Rolle2) and H. Nakatsugawa1) 1) Graduate School of Engineering, Yokohama National University, 79-5 Tokiwadai, Hodogaya Word, Yokohama, Kanagawa, 240-8501, Japan 2) UCCS - Unite de Catalyse et de Chimie du Solide – UMR CNRS 8181, Ecole Nationale Superieure de Chimie de Lille, Batiment C7a – BP.90, 108, 59652, Villeneuve d'Ascq cedex, France GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009 Outline Background Disposition for Ca3Co4O9-δ Cell Manufacturing Thermal Dilatometory Chemical Compatibility Electrode Deposition Preliminary Electrochemical Tests Conclusions GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009 Back ground Cobalt Oxide in Cathode materials for IT-SOFC 3D Perovskite 2D Perovskite Sm0.5Sr0.5CoO3 La1-xSrxCoO3 Ba0.5Sr0.5Co1-xFexO3 　　　・ YBaCo4O7 GdBaCo2O5 showing promising cathode performances. 　mechanical incompatibility with electrolyte in TEC 　chemical incompatibility reactivity with zirconia ( IT) GDR ITSOFC-PACTE Tours 8-10 juin 2009

Crystal structure and oxygen vacancy in Ca3Co4O9-δ 2D misfit layered structure X2/m(0 p 0)s0 CoO2 Hexagonal layer High electrical conduction layer Co valence 3+/4+ Cf. NaxCoO2-yH2O  Ca3Co4O9 σ > 100 S/cm Ca2CoO3 Rock salt layer Co valence 2+/ 3+ Oxygen Vacancy δ ～ 0 – 0.15 Possible ionic conduction O [Ca2CoO3]pCoO2 GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009 Thermal dilatometry Temperature (ºC) . ΔL/L0 (-) Thermal expansion coefficient (10-6 ºC-1) CGO → TEC = 11-12 x 10-6 (ºC-1) Experimental Value Ca3Co4O9 → TEC = 9-10 x 10-6 (ºC-1) 30CGO-Ca3Co4O9 → TEC = 10-11 x 10-6 (ºC-1) Caliculated Theoretical Value from HT-XRD → TEC = 13 x 10-6 (ºC-1) GDR ITSOFC-PACTE Tours 8-10 juin 2009

Optimizing grain size by ball milling times initial condition (0 hour) 9 hours 12 hours 24 hours Mean grain size 0～12 h →1.5-4 m 24 h → 0.5-1 m GDR ITSOFC-PACTE Tours 8-10 juin 2009

Reaction test with electrolyte YSZ(a) 750℃ 100 hours Ca3Co4O9 + or CGO(b) YSZ CGO GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009 Experimental Test Cell preparation CaCO3 Ball milling Calcination 880℃　12h Sintering 880℃ 24h + 30 wt% CGO Ball milling Co3O4 + dispersant + acetone Deposit CGO pellet Heat treating 700℃ ink Drying in air + binder + acetone <Cell size> 10-11 mm in diameter 1.5-2 mm thick ・XRD ・Thermal dilatometry ・SEM ・Impedance measurement GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009 SEM image Cross section of the cell Cell surface <Ca3Co4O9-δ electrode cell> 50.0 μm resin Ca3Co4O9 CGO 20.0 μm resin 70%Ca3Co4O9-30%CGO CGO GDR ITSOFC-PACTE Tours 8-10 juin 2009

Impedance spectra of Ca3Co4O9-δ -1 1 2 6 [ in air ] [ at 700 ºC ] <HF> <LF> [ 700 ºC in air ] ASR = 4.00 Ω.cm2 GDR ITSOFC-PACTE Tours 8-10 juin 2009

Impedance spectra of 30CGO-Ca3Co4O9-δ -1 1 2 6 [ in air ] [ at 700 ºC ] <HF> <LF> [ 760 ºC in air ] ASR = 1.05 Ω.cm2 [ 700 ºC in air ] ASR = 1.42 Ω.cm2 GDR ITSOFC-PACTE Tours 8-10 juin 2009

Activation energy →Improve low activation energy by added 30% CGO GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009 Conclusions Good chemical compatibility with CGO (TEC, Chemical reactivity). Good adherence between electrode and electrolyte, no crack surface. Relatively Low ASR value of Ca3Co4O9 and 30CGO-Ca3Co4O9 cell. the limiting stage is the ionic conductivity for Ca3Co4O9  Necessity for optimization of the microstructure. (grain size optimization, use of cellulose for porosity)  Optimization of the Oxygen conductivity (doping, … measurement of the permittivity under investigation (SPS- Toulouse, France) GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009

GDR ITSOFC-PACTE Tours 8-10 juin 2009