Faculty Publications
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Item Understanding the initial stage oxidation and microstructural evolution of detonation sprayed NiCoCrAlY bond coat using in-situ high-temperature X-ray diffraction(Elsevier Ltd, 2022) Kala, V.; Santhy, K.; Govindarajan, G.; Rajasekaran, B.This study focuses on in-situ high-temperature X-ray diffraction (HT-XRD) investigation to understand the oxidation, microstructural evolution, and recrystallization of the NiCoCrAlY bond coat. HT-XRD analysis was carried out at a constant temperature of 1423 K for 3 h in a 10−4 Pa vacuum. The formation of α-Al2O3, Cr2O3, Co3O4, and NiCr2O4 oxides and microstructural evolution, such as homogenization of phases (γ and β) during in-situ HT-XRD, has been analyzed with FE-SEM (EDS), Density Functional Theory calculations and Rietveld refinement's support. β-(Ni,Co)Al phase depletion (by 77%) was found at 1423 K during the HT-XRD; however, no TGO formation was noticed. © 2022 Elsevier LtdItem Thermal expansion of Crofer 22 APU steel used for SOFC interconnect using in-situ high temperature X-ray diffraction(Elsevier Ltd, 2023) Manjunath, N.; Santhy, K.; Rajasekaran, B.Crofer 22 APU is ferritic stainless steel extensively used as metallic interconnect material in Solid Oxide Fuel Cell (SOFC) applications. The interconnects are exposed to both oxidizing and reducing atmospheres at high temperatures. As SOFCs are operated above 700 °C, understanding the thermal expansion behavior of the interconnect material with other components (anode, cathode, electrolyte) of the fuel cells is essential. Metallic interconnects should have a matchable thermal expansion to other ceramic materials such as anode, cathode, and solid electrolyte used in SOFCs. The present study evaluates the thermal expansion of Crofer 22 APU steel from 25 to 950 °C in a controlled atmosphere (10-4 mbar pressure) using in-situ high-temperature X-ray diffraction (XRD). The XRD patterns were analyzed using the ‘High Score Plus Software’ attached to the system, and the phases were identified using the standard Crystallographic Open Database (COD). The coefficient of thermal expansion (CTE) was determined based on the change in lattice parameter/peak shift to a lower 2θ value as a function of temperature. The normal XRD data showed no oxide formation on the Crofer steel after heating until 950 °C in in-situ high-temperature conditions. The peak shift to the lower 2θ degree observed in the XRD data was due to the relaxation of residual stress upon heating. The isothermal section and phase fraction of Crofer 22 APU alloys are analyzed with the help of thermo-calc with the iron database of TCFE7. The Fe-rich bcc phase was found to be stable up to high temperatures. The major phases are the Fe-rich bcc, Cr-rich BCC, and sigma phase in the solid state. The minor phases are FCC, M3P, TiC, Laves, and Ti4C2S2. The calculated lattice parameter of the Fe-rich BCC phase matches with the experimentally calculated data using XRD. The thermal expansion of Crofer 22 APU was found to be 11.9181 × 10-6 /°C at 950 °C. The in-situ high-temperature XRD technique has been an effective methodology for determining the thermal expansion behavior of the as-received Crofer steel. © 2023Item Thermal expansion and microstructure evolution of atmospheric plasma sprayed NiCrAlY bond coat using in-situ high temperature X-ray diffraction(Elsevier B.V., 2023) Abhijith Vijay, V.; Santhy, K.; Govindarajan, G.; Rajasekaran, B.The paper focuses on in-situ high-temperature X-ray diffraction (HT-XRD) study on atmospheric plasma sprayed NiCrAlY coating. The sample was in-situ heated from 25 °C to 1150 °C in a controlled atmosphere (3 × 10−4 bar), and the corresponding X-ray diffraction patterns for different temperatures were recorded. The effect of temperature on crystallite size, lattice strain, and coefficient of linear thermal expansion was studied. Major phases identified are γ-Ni, γ’-Ni3Al, β-NiAl, and α-Cr. The formation of stable α-Al2O3 and spinel was found above 1000 °C. The transformation of β to γ’ and γ phase was observed as a function of temperature. The equilibrium phases and the thermal expansion of disordered Face Centered Cubic (FCC) and Body Centered Cubic (BCC) phases were predicted and supported by Thermo-Calc prediction for the stable temperature range. Results showed that the non-equilibrium microstructure produced by thermal spray process did not alter the thermal expansion behaviour. In-situ treatment resulted in microstructure and elemental homogenization. The thermal expansion and mechanism of phase evolution were discussed. © 2022 Elsevier B.V.Item The effect of strain induced phase transformation on the thermal expansion compatibility of plasma sprayed spinel coating on SOFC metallic interconnect – A study using in-situ high temperature X-ray diffraction(Elsevier Ltd, 2023) N, M.; Santhy, K.; Rajasekaran, R.A new and novel approach has been adopted in this study to evaluate thermal mismatch induced by thermal expansion in substrate-coating contact pairs using in-situ high-temperature X-ray diffraction (HT-XRD). Atmospheric plasma sprayed (APS) Mn1.0Co1.9Fe0.1O4 (MCF) coating on Crofer 22 APU steel interconnect was investigated. In-situ HT-XRD was performed individually for substrate and coating from 25 °C to 900 °C. Diffraction data were recorded for different temperatures to obtain lattice parameters and strain as a function of temperature. The coefficient of thermal expansion (CTE) of MCF coating was slightly higher than steel substrate and showed no significant thermal expansion mismatch till 700 °C. The increasing lattice strain measured by Scherrer and Williamson-Hall methods indicates strain-induced phase transformation of MCF coating with temperature, supporting the phase transformation-induced self-healing phenomenon of MCF coating. The merit of in-situ HT-XRD as a tool for optimizing operating temperature and measuring thermal mismatch of solid oxide fuel cell (SOFC) stacks has been discussed. © 2023 Hydrogen Energy Publications LLCItem On the merit of solute segregation and low angle grain boundary for thermal stability and thermal expansion of cold-sprayed CuCrZr(Elsevier Ltd, 2025) Abhijith Vijay; Sreerag, M.P.; Varalakshmi, S.; Santhy, K.; Singh, R.; Kondás, J.; Makineni, S.K.; Rajasekaran, B.The precipitation hardenable CuCrZr alloy is a potential alternative to copper for inner liners in rocket thrust engines. Cold spray manufacturing has been seen as a promising processing route to manufacture bulk additive structure of CuCrZr. This work reveals that the cold-sprayed as-deposited Cu-Cr-Zr alloy, in its inherent non-equilibrium state. It is highly stable up to 950 °C and exhibits lower thermal expansion than the equilibrium Cu-Cr-Zr alloy, deduced using HT-XRD and Thermo-Calc. Atomic-scale compositional and diffraction analysis using Atom Probe Tomography (APT) and Electron Backscatter Diffraction (EBSD) support the Zener pinning effect of Cr segregation near the grain boundaries, along with a large fraction of low-angle grain boundaries (LAGBs), that contribute to the high thermal stability and controlled thermal expansion of the deposit. Cold spray deposition naturally yields microstructural features that are conducive to high thermal stability and controlled thermal expansion, features which are comparable to the self-organized microstructures observed in segregation engineering (SE). © 2025 Elsevier B.V.