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Item Synthesis of Praseodymium-Doped Ceria-Based Electrolyte Material by Hydrothermal Method(Springer Science and Business Media Deutschland GmbH, 2022) Rao, R.; Kamath, K.; Priyanka, R.; Shajahan, I.; Prasad Dasari, H.P.Praseodymium-doped ceria (PDC)-based electrolyte powder was synthesised by the hydrothermal method. The as-synthesised powder was studied by various powder characterisations such as X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM) analysis to find out the crystallinity, phase, nature and structural morphology. The shrinkage behaviour (linear shrinkage and shrinkage rate) of PDC powder at high temperatures was performed by dilatometer studies. The crystallographic parameters including the crystallite size, lattice strain and lattice parameter were calculated from XRD analysis. Raman spectroscopy analysis revealed the characteristic peak at 460 cm−1 which corresponds to the F2g peak of the cubic phase of ceria and the peak at 550 cm−1 is attributed to intrinsic oxygen vacancies that confirmed the formation of ceria praseodymium solid solution. © 2022, The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd.Item Praseodymium doped ceria as electrolyte material for IT-SOFC applications(Elsevier Ltd, 2018) Shajahan, I.; Ahn, J.; Nair, P.; Medisetti, S.; Patil, S.; Niveditha, V.; Uday Bhaskar Babu, G.; Prasad Dasari, H.P.; Lee, J.-H.Praseodymium-doped ceria (PDC, Ce0.9Pr0.1O2) electrolyte material for intermediate temperature solid oxide fuel cells (IT-SOFCs) has been successfully synthesised by EDTA-citrate method. From X-Ray diffraction (XRD), fluorite structure along with a crystallite size of 5.4 nm is obtained for PDC nanopowder calcined at 350 °C/24 h. Raman spectroscopy confirmed the structure, presence of oxygen vacancies with the manifestation of the main peak at 457 cm?1 and with a secondary peak at 550 cm?1. From Transmission Electron Microscopy (TEM) analysis, the average particle size is around 7–10 nm and selected area electron diffraction (SAED) patterns further confirmed the fluorite structure of PDC nanopowder. The PDC nanopowder displayed a BET surface area of 65 m2/g with a primary particle size of ?13 nm (calculated from BET surface area). Dilatometer studies revealed a multi-step shrinkage behaviour with the multiple peaks at 522, 1171 and 1461 °C which may be originated due to the presence of multiple size hard agglomerates. The PDC electrolyte pellet sintered at 1500 °C displayed an ionic conductivity of 1.213E-03 S cm?1 along with an activation energy of 1.28eV. Instead of a single fluorite structure, XRD of sintered PDC pellet showed multiple structures (Fluorite structure (CeO2) and cubic structure (PrO2). © 2018 Elsevier B.V.Item Dilatometer studies of praseodymium doped ceria: Effect of synthesis methods on sintering behaviour(Elsevier Ltd, 2020) Shajahan, I.; Prasad Dasari, H.P.; Govardhan, P.Praseodymium-doped ceria (Ce0.9Pr0.1O2, PDC), as an electrolyte material for IT-SOFCs, is investigated with respect to the effect of synthesis method and a detailed analysis was carried out to understand the effect on crystallite size, morphology, specific surface area and sintering behaviour. The various synthesis routes such as microwave assisted co-precipitation method, room temperature co-precipitation method and EDTA-citrate complexing method was adopted for the synthesis of praseodymium doped ceria-based nano-materials. XRD pattern confirms the fluorite-type crystal structure of ceria and Raman spectroscopy analysis confirms the structure with the presence of oxygen vacancies. PDC synthesised by microwave assisted co-precipitation method using isopropyl alcohol as solvent exhibited better sintering activity, reduced the sintering temperature and promoted the densification rate when compared to other synthesis methods with uni-model shrinkage behaviour with shrinkage maxima at 765 °C. Based on two sintering models (CHR/Dorn method), the initial stage sintering mechanism was investigated in the present study and confirmed that the grain boundary diffusion (m = 2) as the dominant mechanism and the activation energy was found to be 116 kJ/mol (CHR model) and 176 kJ/mol (Dorn Method) for initial stages of sintering for PDC material synthesised by microwave assisted co-precipitation method using isopropyl alcohol as solvent. © 2019 Elsevier B.V.Item Effect of sintering aids on sintering kinetic behavior of praseodymium doped ceria based electrolyte material for solid oxide cells(Elsevier Ltd, 2020) Shajahan, I.; Prasad Dasari, H.P.; Saidutta, M.B.The present study investigates the effect of sintering additives (Li, Co, Fe, and Mg) on the sintering kinetic behavior of the praseodymium-doped-ceria (PDC) electrolyte of solid oxide electrolyzer cell. 3Li-PDC, 3Co-PDC, 3Fe-PDC, and 3 Mg-PDC pellets were obtained from the synthesis of PDC nano-powder by microwave-assisted co-precipitation method using isopropyl alcohol as a solvent and followed by sintering additive wetness impregnation method. Linear shrinkage and shrinkage rate data suggest a positive sintering effect for 3Li-PDC and 3Co-PDC pellets and a negative sintering effect for 3 Mg-PDC and 3Fe-PDC pellets than compared to PDC pellets alone. The addition of lithium as a sintering additive (3Li-PDC) had reduced the sintering temperature of PDC from 1100 °C to 850 °C. For PDC, 3Li-PDC, 3Co-PDC, 3Fe-PDC and 3 Mg-PDC pellets sintered at 1100 °C, 850 °C, 1000 °C, 1200 °C, 1100 °C for 2 h resulted in a relative density of 93.6 ± 0.25, 95.8 ± 0.45, 95.0 ± 0.20, 92.7 ± 0.10, and 94.5 ± 0.10%, respectively. The XRD patterns of the sintered PDC pellets suggested a secondary phase formation (PrO2) in 3Co-PDC, 3Fe-PDC, and 3 Mg-PDC pellets indicating that the addition of these sintering aids results in poor solubility limit of Pr in CeO2. On the other hand, XRD patterns of PDC and Li-PDC sintered pellets displayed no secondary peak indicating good solid-solution formation. The activation energy of the 3Li-PDC pellet is obtained from CHR and Dorn methods and was found to be 182 kJ/mol and 196 kJ/mol. From the CHR method, for the 3Li-PDC pellet, the initial sintering behavior is by the grain boundary diffusion mechanism (m = ~2). © 2020 Hydrogen Energy Publications LLCItem Dilatometer studies on LAMOX based electrolyte materials for solid oxide fuel cells(Elsevier Ltd, 2021) Das, A.; Lakhanlal, u.; Shajahan, I.; Prasad Dasari, H.P.; Saidutta, M.B.; Harshini, H.The present study deals with the citrate complexion synthesis of LAMOX-based Solid Oxide Fuel Cell (SOFC) electrolyte materials (La1.8Dy0.2Mo2-xWxO9 (x = 0, 0.1, 0.2, 0.5, and 1), La1.8Dy0.2Mo2-xGaxO9 (x = 0.1 and 0.2), and La1.8Dy0.2Mo2-xVxO9 (x = 0.025, 0.05, 0.1, and 0.2)) and their characterization to understand the sintering behaviour and phase stability. From the dilatometer studies, the linear shrinkage and shrinkage rate of the LDMW (x = 0, and 0.1) showed better shrinkage than LM and LDM. Gallium addition (LDMG) and Vanadium addition (LDMV) showed a negative impact on shrinkage behaviour. In the temperature range of 500–580 °C, the abrupt change in shrinkage rate showed the transition of phase from ? to ? for the LM. The modification of LM to LDM, LDMW, and LDMV suppressed the formation of the ? phase. During thermal expansion behaviour study in the temperature range of 100–500 °C and 550–800 °C, the LM sintered pellet showed the coefficient of thermal expansion (CTE) values of 13.3 ? 10?6/°C and 21.6 ? 10?6/°C respectively. The LDM and LDMW sintered pellets showed the CTE values in the range of 14–15 ? 10?6/°C and 16–19 ? 10?6/°C, respectively. The relative density of the sintered pellets (1100 °C/5 h in air) (LM, LDM, LDMW, and LDMG (x = 0.1)) is found to be >90%. It provides the suitability of these materials for further investigation as electrolytes of SOFCs/SOECs. © 2020 Elsevier B.V.
