Degree Type

Dissertation

Date of Award

2011

Degree Name

Doctor of Philosophy

Department

Materials Science and Engineering

First Advisor

Iver Anderson

Abstract

Gas atomization reaction synthesis (GARS) was employed as a simplified method for producing precursor powders for oxide dispersion strengthened (ODS) ferritic stainless steels (e.g., Fe-Cr-Y-(Ti,Hf)-O), departing from the conventional mechanical alloying (MA) process. During GARS processing a reactive atomization gas (i.e., Ar-O2) was used to oxidize the powder surfaces during primary break-up and rapid solidification of the molten alloy. This resulted in envelopment of the powders by an ultra-thin (t < 150 nm) metastable Cr-enriched oxide layer that was used as a vehicle for solid-state transport of O into the consolidated microstructure. In an attempt to better understand the kinetics of this GARS reaction, theoretical cooling curves for the atomized droplets were calculated and used to establish an oxidation model for this process. Subsequent elevated temperature heat treatments, which were derived from Rhines pack measurements using an internal oxidation model, were used to promote thermodynamically driven O exchange reactions between trapped films of the initial Cr-enriched surface oxide and internal Y-enriched intermetallic precipitates. This novel microstructural evolution process resulted in the successful formation of nano-metric Y-enriched dispersoids, as confirmed using high energy X-ray diffraction and transmission electron microscopy (TEM), equivalent to conventional ODS alloys from MA powders. The thermal stability of these Y-enriched dispersoids was evaluated using high temperature (1200yC) annealing treatments ranging from 2.5 to 1,000 hrs of exposure. In a further departure from current ODS practice, replacing Ti with additions of Hf appeared to improve the Y-enriched dispersoid thermal stability by means of crystal structure modification. Additionally, the spatial distribution of the dispersoids was found to depend strongly on the original rapidly solidified microstructure. To exploit this, ODS microstructures were engineered from different powder particle size ranges, illustrating microstructural control as a function of particle solidification rate. The consolidation of ultra-fine powders (dia. less than 5ym) resulted in a significant reduction in dispersoid size and spacing, consistent with initial scanning electron microscopy studies on as-atomized cross-sectioned particles that suggested that these powders solidified above the threshold velocity to effectively solute trap Y within the alpha-(Fe,Cr) matrix. Interestingly, when the solidification velocity as a function of particle size was extracted from the aforementioned theoretical particle cooling curves, it could be offered as supporting evidence for these microstructure observations. Thermal-mechanical treatments also were used to create and evaluate the stability of a dislocation substructure within these alloys, using microhardness and TEM analysis of the alloy sub-grain and grain structure. Moreover, elevated temperature tensile tests up to 800yC were used to assess the initial mechanical strength of the ODS microstructure.

Copyright Owner

Joel Rodney Rieken

Language

en

Date Available

2012-04-28

File Format

application/pdf

File Size

362 pages

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