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Thermal analysis and microstructure of oxide dispersion strengthened ferritic steels produced by ball milling with different amounts of process control agent

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Abstract

Fe–14Cr–3 W–0.4Ti–0.25Y2O3 ferritic steels were produced by ball milling of initial mixture of elemental powders with various amounts of process control agent (PCA), ethanol (0.25 mass%, 2.5 mass%, 4 mass% and 20 mass%) under an Ar atmosphere and spark plasma sintering (SPS) consolidation at 1070 °C. The influence of the quantity of PCA on the properties (microstructure, density and Vickers hardness) of the as-milled powders and of the consolidated steels was investigated. X-ray diffraction shows a bcc–α-phase with fine crystallite size, 6.7–11 nm, for all powders. The particle size and the lattice constant of α-ferrite of the as-milled powders decrease as the amount of PCA increases. The powder milled with the highest amount of PCA, 20 mass%, contains carbides (M3C) and oxides ((Fe,Cr)2O3). The thermal analysis shows that as the amount of PCA increases, (1) the Curie temperature, Tc, increases, (2) the temperature of α → γ transition, Tα→γ, decreases, (3) the mass loss with CO/CO2 degassing increases, and (4) the milling with PCA hinders the nitrogen incorporation from milling media and air. The density and Vickers hardness of the SPS-consolidated and post-SPS annealed steels show an increasing trend with the increase in the amount of PCA. Carbides and oxides were detected in the post-SPS annealed steels derived from the powders milled with 2.5 mass% PCA and 4 mass% PCA (M23C6 and (Fe,Cr)2O3), and 20 mass% PCA (M3C and (Fe,Cr)2O3). The obtained results were discussed in terms of: (1) dissolution into the alloy matrix of carbon and oxygen released after the disintegration of PCA, (2) carbides and oxides precipitation during milling and/or upon heating and (3) promotion of thermally activated processes (such as carbothermal reaction) upon heating which can develop as well at the contact points/particle surfaces during SPS consolidation and can influence the process of densification.

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Acknowledgements

This work was supported by the CCDI-UEFISCDI PN-III-P1-1.2-PCCDI-2017-0871: Project 47PCCDI/2018 and Core Program PN19-03 (contract no. 21 N/08.02.2019) of Romanian Ministry of Research and Innovation and was partially supported by the European Community in the framework of the European Fusion Development Agreement (EFDA) under project WP13-MAT-01-ODSFS-01. The views and opinions expressed in this paper do not necessarily reflect those of the European Commission. The authors gratefully acknowledge N. Ordas (from Ceit-IK4 and TECNUN, University of Navarra, Spain) for her technical and experimental support.

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  1. National Institute of Materials Physics, PO Box MG 7, 77125, Magurele, Romania

    V. Mihalache, G. Aldica, I. Pasuk & I. Mercioniu

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  1. V. Mihalache
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Mihalache, V., Aldica, G., Pasuk, I. et al. Thermal analysis and microstructure of oxide dispersion strengthened ferritic steels produced by ball milling with different amounts of process control agent. J Therm Anal Calorim 138, 2515–2528 (2019). https://doi.org/10.1007/s10973-019-08593-y

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