Establishing a Scientific Basis for Optimizing Compositions, Process Paths and Fabrication Methods for Nanostructured Ferritic Alloys for Use in Advanced Fission Energy Systems

Odette, G Robert ; Cunningham, Nicholas J., Wu, Yuan ; Etienne, Auriane ; Stergar, Erich ; Yamamoto, Takuya

关键词: nanostructured ferritic alloys;    friction stir welding;    small angle neutron scattering;    TEM;    atom probe tomography;    mechanical alloying;   

DOI  :  10.2172/1035173
RP-ID  :  DOE/07ID14825
PID  :  OSTI ID: 1035173

美国|英语

来源: SciTech Connect

【 摘 要 】

The broad objective of this NEUP was to further develop a class of 12-15Cr ferritic alloys that are dispersion strengthened and made radiation tolerant by an ultrahigh density of Y-Ti-O nanofeatures (NFs) in the size range of less than 5 nm. We call these potentially transformable materials nanostructured ferritic alloys (NFAs). NFAs are typically processed by ball milling pre-alloyed rapidly solidified powders and yttria (Y2O3) powders. Proper milling effectively dissolves the Ti, Y and O solutes that precipitate as NFs during hot consolidation. The tasks in the present study included examining alternative processing paths, characterizing and optimizing the NFs and investigating solid state joining. Alternative processing paths involved rapid solidification by gas atomization of Fe, 14% Cr, 3% W, and 0.4% Ti powders that are also pre-alloyed with 0.2% Y (14YWT), where the compositions are in wt.%. The focus is on exploring the possibility of minimizing, or even eliminating, the milling time, as well as producing alloys with more homogeneous distributions of NFs and a more uniform, fine grain size. Three atomization environments were explored: Ar, Ar plus O (Ar/O) and He. The characterization of powders and alloys occurred through each processing step: powder production by gas atomization; powder milling; and powder annealing or hot consolidation by hot isostatic pressing (HIPing) or hot extrusion. The characterization studies of the materials described here include various combinations of: a) bulk chemistry; b) electron probe microanalysis (EPMA); c) atom probe tomography (APT); d) small angle neutron scattering (SANS); e) various types of scanning and transmission electron microscopy (SEM and TEM); and f) microhardness testing. The bulk chemistry measurements show that preliminary batches of gas-atomized powders could be produced within specified composition ranges. However, EPMA and TEM showed that the Y is heterogeneously distributed and phase separated, but TEM, SANS and APT show that attritor milling for 20 to 40 h sufficiently mixes the Y. TEM, SANS and APT showed that subsequent powder annealing treatments result in the precipitation of a high density of NFs. All the annealed powder variants and HIP consolidated alloys had a bimodal distribution of grain sizes; however, APT and TEM show the presence of NFs in both large and small grains. Alloys extruded at 850?��C contain a unimodal distribution of fine grains. The initial milling procedures in this study added a significant quantity of O as well as contaminant N to the powders. An improved milling procedure effectively eliminated the contamination resulting in lower O content that was insufficient to produce Y-Ti-O NFs in the size range below 3 nm. TEM showed that the low O resulted in fewer and larger oxide phases that are more highly enriched in Y, resulting in low Vicker's hardness values 250 kg/mm^2 compared to 443 kg/mm^2 in an alloy consolidated from the preliminary powders with higher O content. In order to overcome the problem of O deficiency, FeO additions during 40 h attritor milling were made to increase the O content to a nominal value of 0.135%. The annealed powder and corresponding 1150?��C HIP and 850?��C extrusion consolidated alloy showed a very uniform distribution of fine scale NFs. The HIP consolidated alloy had promising high temperature creep strength, but low toughness and a high ductile to brittle transition temperature (DBTT). An extruded and cross-rolled alloy processed at 850??C, however, exhibited a lower DBTT. Also investigated were the effects of Ti and Y content on the NFs in alloys produced from conventionally milled powders that varied Y2O3 from 0.2 to 0.5 wt.% while maintaining Ti/Y atom ratios of 1.6, 2.4, and 3.1. SANS showed the volume fraction and number density of the NFs increases with Y and to a lesser extent Ti. Notably, the NF size and composition are relatively independent of the alloy Y and Ti content, except at the lowest Y2O3 concentration of 0.2 wt.%. An APT characterization of MA957 joined by friction stir welding (FSW) showed that this solid sate joining procedure had only a modest effect on the NF number density (N) and average diameter () compared to an as extruded sample. FSW appears to rearrange the NFs, which become highly aligned with sub-boundary and dislocation structures to an extent that are not observed in the as extruded case. The aligned NF structures are less apparent, but seem to persist after post weld annealing at 1150??C for 3 h following which reduces N, consistent with a significant reduction in hardness. Lastly, several NFA materials, including MA957 and various 14YWT alloys, have been included in irradiation experiments performed at the Advanced Test Reactor, the JOYO sodium cooled fast reactor, the High Flux Isotope Reactor, and the SINQ spallation neut