The effect of Sn concentration on oxide texture and microstructure formation in zirconium alloys

AbstractThe development of oxide texture and microstructure formed on two zirconium alloys with differing Sn contents (Zr–1Nb–1Sn–0.1Fe, i.e. ZIRLO™ and Zr–1.0Nb–0.1Fe) has been investigated using transmission Kikuchi diffraction (TKD) in the scanning electron microscope (SEM) and automated crystal orientation mapping in the transmission electron microscope (TEM). Bulk texture measurements were also performed using electron backscatter diffraction (EBSD) in order to quantify and compare the oxide macrotexture development. The Sn-free alloy showed significantly improved corrosion performance by delay of the transition region and reduced levels of hydrogen pickup. The macroscopic texture and grain misorientation analysis of the oxide films showed that the improved corrosion performance and reduced hydrogen pick up can be correlated with increased oxide texture strength, the improved oxide grain alignment resulting in longer, more protective columnar grain growth. A lower tetragonal phase fraction is also observed in the Sn-free alloy. This results in less transformation to the stable monoclinic phase during oxide growth, which leads to reduced cracking and interconnected porosity and also to the formation of larger, well-aligned monoclinic grains. It is concluded that the Zr–1.0Nb–0.1Fe alloy is more resistant to hydrogen pickup due the formation of a denser oxide with a larger columnar grain structure

Strain localisation and failure at twin-boundary complexions in nickel-based superalloys

From Springer Nature via Jisc Publications RouterHistory: received 2020-06-22, accepted 2020-08-21, registration 2020-09-04, pub-electronic 2020-09-29, online 2020-09-29, collection 2020-12Publication status: PublishedAbstract: Twin boundaries (TBs) in Ni-based superalloys are vulnerable sites for failure in demanding environments, and a current lack of mechanistic understanding hampers the reliable lifetime prediction and performance optimisation of these alloys. Here we report the discovery of an unexpected γ″ precipitation mechanism at TBs that takes the responsibility for alloy failure in demanding environments. Using multiscale microstructural and mechanical characterisations (from millimetre down to atomic level) and DFT calculations, we demonstrate that abnormal γ″ precipitation along TBs accounts for the premature dislocation activities and pronounced strain localisation associated with TBs during mechanical loading, which serves as a precursor for crack initiation. We clarify the physical origin of the TBs-related cracking at the atomic level of γ″-strengthened Ni-based superalloys in a hydrogen containing environment, and provide practical methods to mitigate the adverse effect of TBs on the performance of these alloys

The effect of loading direction on strain localisation in wire arc additively manufactured Ti–6Al–4V

Ti–6Al–4V microstructures produced by high deposition rate Wire Arc Additive Manufacturing (WAAM) can be both heterogeneous and anisotropic. Key features of the as-built microstructures include; large columnar ß grains, an α transformation texture inherited from the β solidification texture, grain boundary (GB) α colonies, and Heat Affected Zone (HAZ) banding. The effect of this heterogeneity on the local strain distribution has been investigated using Digital Image Correlation (DIC) in samples loaded in tension; parallel (WD), perpendicular (ND) and at 45° (45ND) to the deposited layers. Full-field surface strain maps were correlated to the underlying local texture. It is shown that loading perpendicular to the columnar β grains leads to a diffuse heterogeneous deformation distribution, due to the presence of regions containing hard, and soft, α microtextures within different parent β grains. The ‘soft’ regions correlated to multi-variant α colonies that did not contain a hard α variant unfavourably orientated for basal or prismatic slip. Far more severe strain localisation was seen in 45° ND loading at ‘soft’ β grain boundaries, where single variant α GB colonies favourably orientated for slip had developed during transformation. In comparison, when loaded parallel to the columnar ß grains, the strain distribution was relatively homogeneous and the HAZ bands did not show any obvious influence on strain localisation at the deposit layer-scale. However, when using high-resolution DIC, as well as more intense shear bands being resolved at the β grain boundaries during 45° ND loading, microscale strain localisation was observed in HAZ bands below the yield point within the thin white-etching α colony layer

Best time to assess complete clinical response after chemoradiotherapy in squamous cell carcinoma of the anus (ACT II): a post-hoc analysis of randomised controlled phase 3 trial

Background: Guidelines for anal cancer recommend assessment of response at 6–12 weeks after starting treatment. Using data from the ACT II trial, we determined the optimum timepoint to assess clinical tumour response after chemoradiotherapy. Methods: The previously reported ACT II trial was a phase 3 randomised trial of patients of any age with newly diagnosed, histologically confirmed, squamous cell carcinoma of the anus without metastatic disease from 59 centres in the UK. We randomly assigned patients (by minimisation) to receive either intravenous mitomycin (one dose of 12 mg/m2 on day 1) or intravenous cisplatin (one dose of 60 mg/m2 on days 1 and 29), with intravenous fluorouracil (one dose of 1000 mg/m2 per day on days 1–4 and 29–32) and radiotherapy (50·4 Gy in 28 daily fractions); and also did a second randomisation after initial therapy to maintenance chemotherapy (fluorouracil and cisplatin) or no maintenance chemotherapy. The primary outcome was complete clinical response (the absence of primary and nodal tumour by clinical examination), in addition to overall survival and progression-free survival from time of randomisation. In this post-hoc analysis, we analysed complete clinical response at three timepoints: 11 weeks from the start of chemoradiotherapy (assessment 1), 18 weeks from the start of chemoradiotherapy (assessment 2), and 26 weeks from the start of chemoradiotherapy (assessment 3) as well as the overall and progression-free survival estimates of patients with complete clinical response or without complete clinical response at each assessment. We analysed both the overall trial population and a subgroup of patients who had attended each of the three assessments by modified intention-to-treat. This study is registered at controlled-trials.com, ISRCTN 26715889. Findings: We enrolled 940 patients from June 4, 2001, until Dec 16, 2008. Complete clinical response was achieved in 492 (52%) of 940 patients at assessment 1 (11 weeks), 665 (71%) of patients at assessment 2 (18 weeks), and 730 (78%) of patients at assessment 3 (26 weeks). 691 patients attended all three assessments and in this subgroup, complete clinical response was reported in 441 (64%) patients at assessment 1, 556 (80%) at assessment 2, and 590 (85%) at assessments 3. 151 (72%) of the 209 patients who had not had a complete clinical response at assessment 1 had a complete clinical response by assessment 3. In the overall trial population of 940 patients, 5 year overall survival in patients who had a clinical response at assessments 1, 2, 3 was 83% (95% CI 79–86), 84% (81–87), and 87% (84–89), respectively and was 72% (66–78), 59% (49–67), and 46% (37–55) for patients who did not have a complete clinical response at assessments 1, 2, 3, respectively. In the subgroup of 691 patients, 5 year overall survival in patients who had a clinical response at assessment 1, 2, 3 was 85% (81–88), 86% (82–88), and 87% (84–90), respectively, and was 75% (68–80), 61% (50–70), and 48% (36–58) for patients who did not have a complete clinical response at assessment 1, 2, 3, respectively. Similarly, progression-free survival in both the overall trial population and the subgroup was longer in patients who had a complete clinical response, compared with patients who did not have a complete clinical response, at all three assessments. Interpretation: Many patients who do not have a complete clinical response when assessed at 11 weeks after commencing chemoradiotherapy do in fact respond by 26 weeks, and the earlier assessment could lead to some patients having unnecessary surgery. Our data suggests that the optimum time for assessment of complete clinical response after chemoradiotherapy for patients with squamous cell carcinoma of the anus is 26 weeks from starting chemoradiotherapy. We suggest that guidelines should be revised to indicate that later assessment is acceptable. Funding: Cancer Research UK

The Effect of Iron on Dislocation Evolution in Model and Commercial Zirconium Alloys

Although the evolution of irradiation-induced dislocation loops has been well correlated with irradiation-induced growth phenomena, the effect of alloying elements on this evolution remains elusive, especially at low fluences. To develop a more mechanistic understanding of the role iron has on loop formation, we used state-of-the-art techniques to study a proton-irradiated Zr-0.1Fe alloy and proton- and neutron-irradiated Zircaloy-2. The two alloys were irradiated with 2-MeV protons up to 7 dpa at 350\ub0C and Zircaloy-2 up to 14.7 7 1025n • m-2, approximately 24 dpa, in a boiling water reactor at approximately 300\ub0C. Baseline transmission electron microscopy showed that the Zr3Fe secondary-phase particles in the binary system were larger and fewer in number than the Zr (Fe, Cr)2and Zr2(Fe, Ni) particles in Zircaloy-2. An analysis of the irradiated binary alloy revealed only limited dissolution of Ze3Fe, suggesting little dispersion of iron into the matrix, while at the same time a higher 〈a〉-loop density was observed compared with Zircaloy-2 at equivalent proton dose levels. We also found that the redistribution of iron during irradiation led to the formation of iron nanoclusters. A delay in the onset of 〈c〉-loop nucleation in proton-irradiated Zircaloy-2 compared with the binary alloy was observed. The effect of iron redistributed from secondary-phase particles because of dissolution on the density and morphology of 〈a〉 and 〈c〉 loops is described. The implication this may have on irradiation-induced growth of zirconium fuel cladding is also discussed