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1.
Sci Rep ; 10(1): 17019, 2020 Oct 07.
Article in English | MEDLINE | ID: mdl-33028967

ABSTRACT

An amendment to this paper has been published and can be accessed via a link at the top of the paper.

2.
J Appl Crystallogr ; 53(Pt 5): 1181-1194, 2020 Oct 01.
Article in English | MEDLINE | ID: mdl-33117107

ABSTRACT

This paper describes in detail two neutron diffraction residual stress measurements, performed on the ENGIN-X neutron scattering instrument at the ISIS facility in the UK and on the SALSA instrument at the Institut Laue-Langevin in Grenoble, France. The measurements were conducted as part of the NeT Task Group 6 (TG6) international measurement round robin on an Alloy 600/82 multi-pass weldment - a slot in an Alloy 600 plate filled with three Alloy 82 weld beads, simulating a repair weld. This alloy/weld combination is considered challenging to measure, due to the large grain size and texture in the weld, and large gradients in the stress-free lattice parameter between the parent and weld metal. The basic principles of the neutron diffraction technique are introduced and issues affecting the reliability of residual stress characterization are highlighted. Two different analysis strategies are used for estimation of residual stresses from the raw data. Chemical composition studies are used to measure the mixing of parent and weld metal and highlight the steep lattice parameter gradients that arise as a consequence. The inferred residual stresses are then compared with three sets of measurements performed on the same plate by other NeT partners on E3 at the HZB in Berlin, STRESS-SPEC at the FRM II in Munich and KOWARI in Sydney. A robust Bayesian estimation average is calculated from the combined five-instrument data set, allowing reliable best estimates of the residual stress distribution in the vicinity of the weldment. The systematic uncertainties associated with the residual stress measurements are determined separately in the weld and parent materials, and compared with those in the NeT TG4 benchmark. This is a three-pass slot-welded plate fabricated from American Iron and Steel Institute AISI 316L(N) austenitic stainless steel, and is normally considered less challenging to measure using diffraction techniques than all nickel welds. The uncertainties in the stress measurements by neutron diffraction for these two weldments seem to be comparable.

3.
Sci Rep ; 10(1): 13536, 2020 Aug 11.
Article in English | MEDLINE | ID: mdl-32782253

ABSTRACT

By time-of-flight (TOF) neutron diffraction experiments, the influence of segregation-induced microstructure bands of austenite (γ) and martensite (α' ) phases on the partitioning of stress and strain between these phases was investigated. Initially, tensile specimens of a Co-added stainless steel were heat treated by quenching and partitioning (Q&P) processing. Tensile specimens were subsequently loaded at 350 °C parallel to the length of the bands within the apparent elastic limit of the phase mixture. Lattice parameters in both axial and transverse directions were simultaneously measured for both phases. The observation of a lattice expansion for the γ phase in the transverse direction indicated a constraint on the free transverse straining of γ arising from the banded microstructure. The lateral contraction of α' imposed an interphase tensile microstress in the transverse direction of the γ phase. The multiaxial stress state developed in the γ phase resulted in a large deviation from the level of plastic strain expected for uniaxial loading of single phase γ. Since segregation-induced banded microstructures commonly occur in many engineering alloys, the analysis of stress and strain partitioning with the present Q&P steel can be used to interpret the observations made for further engineering alloys with two-phase microstructures.

4.
Inorg Chem ; 58(9): 6143-6154, 2019 May 06.
Article in English | MEDLINE | ID: mdl-30964275

ABSTRACT

In situ synchrotron powder X-ray diffraction measurements have demonstrated that the isostructural AUO4- x ( A = alkaline earth metal cation) oxides CaUO4- x and α-Sr0.4Ca0.6UO4- x undergo a reversible phase transformation under reducing conditions at high temperatures associated with the ordering of in-plane oxygen vacancies resulting in the lowering of symmetry. When rhombohedral (space group R3̅ m) CaUO4- x and α-Sr0.4Ca0.6UO4- x are heated to 450 and 400 °C, respectively, in a hydrogen atmosphere, they undergo a first-order phase transformation to a single phase structure which can be refined against a triclinic model in space group P1̅, δ-CaUO4- x and δ-Sr0.4Ca0.6UO4- x, where the oxygen vacancies are disordered initially. Continued heating results in the appearance of superlattice reflections, indicating the ordering of in-plane oxygen vacancies. Cooling ordered δ-CaUO4- x and δ-Sr0.4Ca0.6UO4- x to near room temperature results in the reformation of the disordered rhombohedral phases. Essential to the transformation is the generation of a critical amount of oxygen vacancies. Once these are formed, the transformation can be accessed continuously through thermal cycling, showing that the transformations are purely thermodynamic in origin. Stoichiometric structures of both oxides can be recovered by heating oxygen deficient CaUO4- x and α-Sr0.4Ca0.6UO4- x under pure oxygen to high temperatures. When heated in air, the amount of oxygen vacancy defects that form in CaUO4- x and α-Sr0.4Ca0.6UO4- x are found to correlate with the A site composition. The inclusion of the larger Sr2+ cation on the A site reduces defect-defect interactions, which increases the amount of defects that can form and lowers their formation temperature. The relative difference in the amount of defects that form can be understood on the basis of oxygen vacancy and U5+ disordering as shown by both ab initio calculations and estimated oxygen vacancy formation energies based on thermodynamic considerations. This difference in defect-defect interactions consequently introduces variations in the long-range ordered anionic lattice of the δ phases despite the isostructural relationship of the α structures of CaUO4- x and Sr0.4Ca0.6UO4- x. These results are discussed with respect to the influence the A site cation has upon anion defect formation and ordering and are also compared to δ-SrUO4- x, the only other material known to be able to undergo a reversible symmetry lowering and disorder-to-order transformation with increasing temperature.

5.
Materials (Basel) ; 10(4)2017 Apr 06.
Article in English | MEDLINE | ID: mdl-28772747

ABSTRACT

A new generation of alloys, which rely on a combination of various strengthening mechanisms, has been developed for application in molten salt nuclear reactors. In the current study, a battery of dispersion and precipitation-strengthened (DPS) NiMo-based alloys containing varying amounts of SiC (0.5-2.5 wt %) were prepared from Ni-Mo-SiC powder mixture via a mechanical alloying (MA) route followed by spark plasma sintering (SPS) and rapid cooling. Neutron Powder Diffraction (NPD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the characterization of the microstructural properties of these in-house prepared NiMo-SiC DPS alloys. The study showed that uniformly-dispersed SiC particles provide dispersion strengthening, the precipitation of nano-scale Ni3Si particles provides precipitation strengthening, and the solid-solution of Mo in the Ni matrix provides solid-solution strengthening. It was further shown that the milling time has significant effects on the microstructural characteristics of these alloys. Increased milling time seems to limit the grain growth of the NiMo matrix by producing well-dispersed Mo2C particles during sintering. The amount of grain boundaries greatly increases the Hall-Petch strengthening, resulting in significantly higher strength in the case of 48-h-milled NiMo-SiC DPS alloys compared with the 8-h-milled alloys. However, it was also shown that the total elongation is considerably reduced in the 48-h-milled NiMo-SiC DPS alloy due to high porosity. The porosity is a result of cold welding of the powder mixture during the extended milling process.

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