1 TNA user feedback Advanced microscopy characterization of - PowerPoint Presentation

1. 1TNA user feedbackAdvanced microscopy characterization of innovative ceramic coatings for hydrogen technologies 31st May 2023ESTEEM3 – Final event – Paris, FRTHIS PROJECT HAS RECEIVED FUNDING FROM THE EUROPEAN UNION’S HORIZON 2020 RESEARCH AND INNOVATION PROGRAMME UNDER GRANT AGREEMENT NO 823717Elisa ZanchiPolitecnico di Torino, Italy

2. 231st May 2023OutlineNetwork and collaborations around ESTEEM3 project The CeramECS project: “Glass-ceramic and ceramic materials for energy conversion and storage” Motivation: Solid Oxide Cell technologies for hydrogen energyCeramic protective coatingsElectrophoretic deposition (EPD)Advanced TEM characterization Further activities: the GlaMater projectConcluding remarksESTEEM3 – Final event – Paris, FRElisa Zanchi, Politecnico di Torino

3. 331st May 2023ESTEEM3 – Final event – Paris, FRInternational Centre of Electron Microscopy for Materials Science at the AGH-UST, Krakow, PolandElectrophoretic deposition expertiseA.R. BoccacciniEPD processingF. Smeacetto, E. ZanchiAdvanced microscopy characterizationG. CempuraDepartment of Applied science and Technology, Institute of Physics, GLANCE Group, Turin, ItalyTesting & characterisationS. Molin, J. Ignaczak EPD upscalingA.G. SabatoIndustrial partnerfor EU projectsStack testingH. JavedDresden, GermanyErlangen, GermanyBarcelona, SpainGdansk, PolandGA # 700300GA # 874577Elisa Zanchi, Politecnico di TorinoNetwork and collaborations

4. 431st May 2023Motivation: H2 technologiesESTEEM3 – Final event – Paris, FRInterconnectSolid oxide cells (SOCs) are electrochemical energy conversiondevices operating at temperatures in the range of 600–850 °CWhy SOCs?Efficient energy conversion technologyClean: Low GHGs emissionsReduction of CO2 fingerprintSOEC: Electrical energy  Chemical energy (H2)SOFC: Chemical energy (H2) Electrical energy rSOC: integration in renewable energy systems30 cells stack, Sunfire GmbH Elisa Zanchi, Politecnico di Torino

5. 531st May 2023SOC stackESTEEM3 – Final event – Paris, FRGrant # 874577 - NewSOCHT corrosionProgressive oxidation limits the electric conductivityVolatile Cr-compounds degrade the cell performance I) Deposition of a ceramic protective coatingGas tightnessNeed to completely avoid gas leakageSuppress undesired reactionsII) Design of innovative interface conceptsFerritic stainless-steels are widely used as interconnects SOC stacksElectrical connectionSeparation between oxidizing/reducing atmosphere CeramECS Elisa Zanchi, Politecnico di TorinoInterconnect

6. 631st May 2023HT corrosionESTEEM3 – Final event – Paris, FRThe coating must:Reduce the oxidation rate of the steelReduce Cr-evaporationEnsure high electrical conductivityCompatible thermal expansion coefficient (11-13 10-6 K-1)Applying a protective coating on the steel is a promising approach to extend the interconnect life and avoid cathode poisoningThe Mn-Co spinel family (MCO) has been shown to be particularly promising The functional properties can be improved by Modifications with additional elements – dopingOptimized deposition and sinteringCoMnXu et al, Science 21 (2019) 19E. Zanchi et al., J. Power Sources. 455 (2020) 227910. Elisa Zanchi, Politecnico di Torino

7. 731st May 2023Electrophoretic depositionESTEEM3 – Final event – Paris, FRElisa Zanchi, Politecnico di TorinoElectrophoresis : motion of charged particles in a suspension under the influence of an electric field Deposition: coagulation of particles to a dense massm= mass deposited at time t on surface SCs = concentration in the suspensionµ = electrophoretic mobilityE = electric field appliedE. Zanchi, et al., Mater. Lett. 286 (2021) 129229 e = dielectric constant of the liquid.h = viscosity of the liquid.ζ = Zeta potential.v = particle velocity.Hamaker’s equation:  Experimental challenges: Stability of the suspensionDeposition parametersSintering process1) Upscale of the electrophoretic deposition set-up2) Modification of the spinel by electrophoretic co-depositionCompared to other techniques, EPD Has a simple and adaptable set-upIs a fast and versatile techniqueReduces processing time and costEPD set-up @ POLITO

8. 831st May 2023CeramECSESTEEM3 – Final event – Paris, FRGA # 700300EPD adapted to a 3-electrode set-up ̴20x20 cm surface successfully deposited The EPD deposited Mn–Co spinel coating showed improved stability…to validate EPD for real dimension devicesSOC Stack test: 850 °C, 3000 hElisa Zanchi, Politecnico di TorinoGlass-ceramic and ceramic materials for energy conversion and storageEPD apparatus upscale

9. 931st May 2023Mn-Co spinel coatingESTEEM3 – Final event – Paris, FRAdvanced TEM post-mortem characterizationCrofer22APUCrofer22APUMCO EPD coatingElisa Zanchi, Politecnico di TorinoFib lamella: to investigate reactions at the steel-coating interface and developed phasesOverview of the FIB lamella Magnification of oxide scale-coatinginterfaceCrofer22APUOxide ScaleOxide scaleMCO coatingCoating

10. 1031st May 2023ESTEEM3 – Final event – Paris, FROverview of the FIB lamella from coated interconnectElisa Zanchi, Politecnico di TorinoEDS map of the lamella: Different Mn and Co distribution in the coatingCr confined in the oxide scale and absence of “reaction layer”Mn-rich sub scale oxidationCrofer22APUScaleCoatingMn-Co spinel coating

11. 1131st May 2023ESTEEM3 – Final event – Paris, FRElisa Zanchi, Politecnico di TorinoExperimental HAADF –STEM and Simulated HAADF STEM Simulated SAED of Cr2MnO4, superimposed on experimental oneMn-rich oxide scale grainRemarkable diffusion of Mn leading to Cr-Mn spinel formationIncreased the electric conductivity and lower Cr evaporation compared to pure chromia scaleOCrMnFe59.230.410.00.2EDS compositionOxide scaleCoatingMn-Co spinel coatingAdvanced TEM characterisation of oxide scale–coating interface

12. 1231st May 2023ESTEEM3 – Final event – Paris, FRElisa Zanchi, Politecnico di TorinoAt.%OCrMnCoFe153.50.617.627.80.6254.51.329.114.80.3Oxide scaleCoating12Dual phase structure of the Mn-Co spinel coatingCobalt-rich grains: MnCo2O4 cubic structure Mn-rich elongated grains: Mn2CoO4 tetragonal structureSimulated SAED of Mn2CoO4 superimposed on exp. one [ZA 301]Advanced TEM characterisation of oxide scale–coating interfaceMn-Co spinel coating

13. 1331st May 2023Fe-Cu co-doping of the Mn-Co spinel coating…to improve the functional properties of the Mn-Co spinel by addition of transition metalsESTEEM3 – Final event – Paris, FRTwo-step Reactive sintering:ReductionRe-oxidationElectrophoretic co-deposition of 3 precursors: cathodic depositionSuccessful in-situ doping: Stabilization of the cubic spinel structureWater-ethanol suspensionDeposited on Crofer22APUOptimised deposition at 50 V for 30 sFour different spinel compositionsElisa Zanchi, Politecnico di TorinoCeramECSGlass-ceramic and ceramic materials for energy conversion and storage

14. 1431st May 2023ESTEEM3 – Final event – Paris, FRDoped spinel coatingsBetter oxidation resistance of Fe-Cu doped coatings compared to base Mn-Co spinelImproved spinel stabilitySynergic effect of Cu and FeCharacterization of Mn-Co spinel coatings with Fe-Cu additionCu addition boosts densificationNo Cr diffusion during agingAssessment of dilatometric properties of Fe-Cu doped spinels Elisa Zanchi, Politecnico di TorinoFe additionFe+Cu addition

15. 1531st May 2023ESTEEM3 – Final event – Paris, FRAdvanced TEM characterization of doped coatings Fe and Cu homogeneously distributed in the coating10Fe10Cu sample: Highest amount of dopantsThin oxide scaleSteelCoatingHigh coating densificationElisa Zanchi, Politecnico di TorinoDoped spinel coatingsPoint c3:Solution with CrMnCoO4 Zone axis 101Point c2:Solution with MnCo2O4 Zone axis 112Point b1:Solution with MnCo2O4 Zone axis 112

16. 1631st May 2023ESTEEM3 – Final event – Paris, FR5Fe5Cu sample: lowest amount of dopantsHomogeneous distribution of Fe and Cu in the Mn-Co spinelFe+Cu addition: synergic effect in suppressing the double-phase spinel formationElisa Zanchi, Politecnico di TorinoView of the lamella from the outer coating sideDoped spinel coatingsAdvanced TEM characterization of doped coatings Point 1:Solution with MnCo2O4 Zone axis 1141SteelCoating

17. 1731st May 2023ESTEEM3 – Final event – Paris, FRGas tightnessII) Design of innovative interface conceptsCrofer22APU.. To minimize reactions between steel and the sealantImprove thermo-mechanical properties of the jointGlaMater (March 2023)HT (air)Alumina layer with enhanced surface roughnessGlass ceramic sealantCrofer22APUAluminaSuccessful EPD modification:Elisa Zanchi, Politecnico di Torino“Advanced glass and ceramic materials for energy applications” GlaMaterFurther activities in ESTEEM3

18. 1831st May 2023ESTEEM3 – Final event – Paris, FRThe Transnational Access provided by ESTEEM3 Project enabled: Elisa Zanchi, Politecnico di TorinoThe consolidation of fruitful networkingStrengthening of AGH-POLITO collaboration Publications on high-impact journalsTraining on TEM characterization techniques Professional (and personal!) experience for PhD activity Results and publications on the CeramECS projects provided:A first in-depth characterization of Mn-Co dual spinel structure and oxide scale evolution after stack test at relevant conditionsA first comprehensive assessment of synergic effect of Fe-Cu addition into the Mn–Co spinel structure Better understanding of coating degradation phenomena …to improve the performance and durability of SOC devices and boost hydrogen technologiesKrakow, 2019Krakow, 2023Concluding remarks

19. 1931st May 2023ESTEEM3 – Final event – Paris, FRAcknowledgmentsThis project has received funding from the Fuel Cells and Hydrogen 2 Joint Undertaking (now Clean Hydrogen Partnership) under Grant Agreement No 874577-NewSOC. This Joint Undertaking receives support from the European Union’s Horizon 2020 Research and Innovation program, Hydrogen Europe and Hydrogen Europe Research.Thank you for the attentionelisa.zanchi@polito.itElectrophoretic deposition, FAU, Erlangen, Germany,