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The Role of Bi/Material Interface in Integrity of Layered Metal/Ceramic
Masini, Alessia ; Černý, Martin (referee) ; Bermejo, Raul (referee) ; Chlup, Zdeněk (advisor)
The present doctoral thesis summarises results of investigation focused on the characterisation of materials involved in Solid Oxide Cell technology. The main topic of investigation was the ceramic cell, also known as MEA. Particular attention was given to the role that bi-material interfaces, co-sintering effects and residual stresses play in the resulting mechanical response. The first main goal was to investigate the effects of the manufacturing process (i.e. layer by layer deposition) on the mechanical response; to enable this investigation, electrode layers were screen-printed one by one on the electrolyte support and experimental tests were performed after every layer deposition. The experimental activity started with the measurement of the elastic characteristics. Both elastic and shear moduli were measured via three different techniques at room and high temperature. Then, uniaxial and biaxial flexural strengths were determined via two loading configurations. The analysis of the elastic and fracture behaviours of the MEA revealed that the addition of layers to the electrolyte has a detrimental effect on the final mechanical response. Elastic characteristics and flexural strength of the electrolyte on the MEA level are sensibly reduced. The reasons behind the weakening effect can be ascribed to the presence and redistribution of residual stresses, changes in the crack initiation site, porosity of layers and pre-cracks formation in the electrode layers. Finally, the coefficients of thermal expansion were evaluated via dilatometry on bulk materials serving as inputs for finite elements analyses supporting experiments and results interpretation. The second most important goal was to assess the influence of operating conditions on the integrity of the MEA. Here interactions of ceramic–metal interfaces within the repetition unit operating at high temperatures and as well at both oxidative and reductive atmospheres were investigated. The elastic and fracture responses of MEA extracted from SOC stacks after several hours of service were analysed. Layer delamination and loss of mechanical strength were observed with increasing operational time. Moreover, SEM observations helped to detect significant microstructural changes of the electrodes (e.g. demixing, coarsening, elemental migration and depletion), which might be responsible for decreased electrochemical performances. All the materials presented in this work are part of SOC stacks produced and commercialised by Sunfire GmbH, which is one of the world leading companies in the field.
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The Role of Bi/Material Interface in Integrity of Layered Metal/Ceramic
Masini, Alessia ; Černý, Martin (referee) ; Bermejo, Raul (referee) ; Chlup, Zdeněk (advisor)
The present doctoral thesis summarises results of investigation focused on the characterisation of materials involved in Solid Oxide Cell technology. The main topic of investigation was the ceramic cell, also known as MEA. Particular attention was given to the role that bi-material interfaces, co-sintering effects and residual stresses play in the resulting mechanical response. The first main goal was to investigate the effects of the manufacturing process (i.e. layer by layer deposition) on the mechanical response; to enable this investigation, electrode layers were screen-printed one by one on the electrolyte support and experimental tests were performed after every layer deposition. The experimental activity started with the measurement of the elastic characteristics. Both elastic and shear moduli were measured via three different techniques at room and high temperature. Then, uniaxial and biaxial flexural strengths were determined via two loading configurations. The analysis of the elastic and fracture behaviours of the MEA revealed that the addition of layers to the electrolyte has a detrimental effect on the final mechanical response. Elastic characteristics and flexural strength of the electrolyte on the MEA level are sensibly reduced. The reasons behind the weakening effect can be ascribed to the presence and redistribution of residual stresses, changes in the crack initiation site, porosity of layers and pre-cracks formation in the electrode layers. Finally, the coefficients of thermal expansion were evaluated via dilatometry on bulk materials serving as inputs for finite elements analyses supporting experiments and results interpretation. The second most important goal was to assess the influence of operating conditions on the integrity of the MEA. Here interactions of ceramic–metal interfaces within the repetition unit operating at high temperatures and as well at both oxidative and reductive atmospheres were investigated. The elastic and fracture responses of MEA extracted from SOC stacks after several hours of service were analysed. Layer delamination and loss of mechanical strength were observed with increasing operational time. Moreover, SEM observations helped to detect significant microstructural changes of the electrodes (e.g. demixing, coarsening, elemental migration and depletion), which might be responsible for decreased electrochemical performances. All the materials presented in this work are part of SOC stacks produced and commercialised by Sunfire GmbH, which is one of the world leading companies in the field.
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