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David M. Collins

Publications and source records attributed to David M. Collins.

15 recordsLinked to original sources

Revealing 3D Strain and Carbide Architectures in Additively Manufactured Ni Superalloys

Fast directional solidification during Laser Additive Manufacturing (LAM) produces a complex microstructure in nickel-based superalloys, comprising columnar grains with cellular sub-grain structures and carbides. Using non-destructive Scanning 3D X-ray Diffraction (S3DXRD), we reveal spatially complex orientation and intergranular strain relationships that couple strongly to processing-induced cellular sub-grain networks and a primary cubic metal carbide (MC) phase. We have examined 3D orientation and elastic strain tensor fields across 82 $\gamma$ grains together with the spatial distribution of over 37,000 MC carbides in an ABD-900AM alloy sample manufactured by the Directed Energy Deposition (DED) LAM process. Carbides are spatially associated with the cellular sub-grain network with a weak but present orientation relationship with their parent $\gamma$ grains. The MC carbides, known to be Ti, Ta and Nb rich, form in regions of high solute segregation, resulting in a significant volumetric lattice parameter patterning in the associated $\gamma$ phase regions. These chemically distinct solute-rich regions possess a higher associated elastic modulus compared to intercellular regions and determine the local residual stress patterning. These results provide the first non-destructive 3D study of the relationship between rapid solidification-induced segregation, deformation heterogeneity and carbide architectures in an additively manufactured Ni-based superalloy. The insights provide crucial detail to rationalise LAM process parameter optimisation and the coupled spatially governed structural performance.

cond-mat.mtrl-sci

The influence of dislocations on R-phase transformations in a NiTi shape memory alloy

The ability to control the stress-induced phase transformation of the shape memory alloy, NiTi, is an important technological challenge that must be understood for their wide application in devices that can exploit their reversible strain properties. This study elucidates the direct relationship between dislocation density and the \textit{R}-phase transformation, including its formation temperature from interrupted annealing of rolled NiTi samples. Deformation is shown to determine the enthalpy change required for the B2$\rightarrow$\textit{R}-phase transformation, with associated transformation temperatures being modifiable via dislocation density and recovery processes. Recovery is shown to be rapid, highly heterogeneous and sensitive to crystal orientation. Grains with a $\langle100\rangle$ direction close to the macroscopic rolling direction recover more rapidly than $\langle110\rangle$ and $\langle111\rangle$ orientated grains. Considered to be governed by processing induced residual stresses and resultant crystallographic dependent annihilation/slip pathways, there are opportunities to tune B2$\rightarrow$\textit{R}-phase transformation on either a grain-averaged or an orientation dependant per-grain basis.

cond-mat.mtrl-sci

A micromechanical study of heat treatment induced hardening in α-brass

The mechanisms that govern a previously unexplained hardening effect of a single phase Cu-30wt%Zn α-brass after heating have been investigated. After cold-work, the alloy possesses an increased yield strength and hardening rate only when heat treated to temperatures close to 220{^\circ}C, and is otherwise softer. Crystallographic texture and microstructure, explored using electron backscatter diffraction (EBSD), describe the deformation heterogeneity including twin development, as a function of heat treatment. When heated, an increased area fraction of deformation twins is observed, with dimensions reaching a critical size that maximises the resistance to dislocation slip in the parent grains. The effect is shown to dominate over other alloy characteristics including short range order, giving serrated yielding during tensile testing which is mostly eliminated after heating. In-situ X-ray diffraction during tensile testing corroborates these findings; dislocation-related line broadening and lattice strain development between as worked and heated α-brass is directly related to the interaction between the dislocations and the population of deformation twins. The experiments unambiguously disprove that other thermally-induced microstructure features contribute to thermal hardening. Specifically, the presence of recrystallised grains or second phases do not play a role. As these heat treatments match annealing conditions subjected to α-brass during deformation-related manufacturing processes, the results here are considered critical to understand, predict and exploit, where appropriate, any beneficial process-induced structural behaviour.

cond-mat.mtrl-sci

Microscale stress-geometry interactions in an additively manufactured NiTi cardiovascular stent: A synchrotron dual imaging tomography and diffraction study

This study explores cardiovascular stents fabricated using laser powder bed fusion (LPBF); an emerging method to offer patient-specific customisable parts. Here, the shape memory alloy NiTi, in a near equiatomic composition, was investigated to deconvolve the material response from macroscopic component effects. Specifically, stress-geometry interactions were revealed, in-situ, for a minaturised cardiovascular stent subjected to an externally applied cylindrical stress whilst acquiring synchrotron X-ray imaging and diffraction data. The approach enabled the collection of spatially resolved micromechanical deformation data; the formation of stress-induced martensite and R-phase was evident, occurring in locations near junctions between stent ligaments where stress concentrations exist. In the as-fabricated condition, hardness maps were obtained through nanoindentation, demonstrating that the localised deformation and deformation patterning is further controlled by porosity and microstructural heterogeneity. Electron backscatter diffraction (EBSD) supported these observations, showing a finer grain structure near stent junctions with higher associated lattice curvature. These features, combined with stress concentrations when loaded will initiate localised phase transformations. If the stent was subjected to repeated loading, representing in-vivo conditions, these regions would be susceptible to cyclic damage through transformation memory loss, leading to premature component failure. This study highlights the challenges that must be addressed for the post-processing treatment of LABF-processed stents for healthcare-related applications.

cond-mat.mtrl-sci

Grain-level effects on in-situ deformation-induced phase transformations in a complex-phase steel using 3DXRD and EBSD

A novel complex-phase steel alloy is conceived with a deliberately unstable austenite, $γ$, phase that enables the deformation-induced martensitic transformations (DIMT) to be explored at low levels of plastic strain. The DIMT was thus explored, in-situ and non-destructively, using both far-field Three-Dimensional X-Ray Diffraction (3DXRD) and Electron Back-Scatter Diffraction (EBSD). Substantial $α'$ martensite formation was observed under 10% applied strain with EBSD, and many $\varepsilon$ grain formation events were captured with 3DXRD, indicative of the indirect transformation of martensite via the reaction $γ\rightarrow \varepsilon \rightarrow α'$. Using $\varepsilon$ grain formation as a direct measurement of $γ$ grain stability, the influence of several microstructural properties, such as grain size, orientation and neighbourhood configuration, on $γ$ stability have been identified. Larger $γ$ grains were found to be less stable than smaller grains. Any $γ$ grains oriented with {100} parallel to the loading direction preferentially transformed with lower stresses. Parent $\varepsilon$-forming $γ$ grains possessed a neighbourhood with increased ferritic/martensitic volume fraction. This finding shows, unambiguously, that $α$/$α'$ promotes $\varepsilon$ formation in neighbouring grains. The minimum strain work criterion model for $\varepsilon$ variant prediction was also evaluated, which worked well for most grains. However, $\varepsilon$-forming grains with a lower stress were less well predicted by the model, indicating crystal-level behaviour must be considered for accurate $\varepsilon$ formation. The findings from this work are considered key for the future design of alloys where the deformation response can be controlled by tailoring microstructure and local or macroscopic crystal orientations.

cond-mat.mtrl-sci

Registration between DCT and EBSD datasets for multiphase microstructures

The ability to characterise the three-dimensional microstructure of multiphase materials is essential for understanding the interaction between phases and associated materials properties. Here, laboratory-based diffraction-contrast tomography (DCT), a recently-established materials characterization technique that can determine grain phases, morphologies, positions and orientations in a voxel-based reconstruction method, was used to map part of a dual-phase steel alloy sample. To assess the resulting microstructures that were produced by the DCT technique, an EBSD map was collected within the same sample volume. To identify the 2D slice of the 3D DCT reconstruction that best corresponded to the EBSD map, a novel registration technique based solely on grain-averaged orientations was developed -- this registration technique requires very little a priori knowledge of dataset alignment and can be extended to other techniques that only recover grain-averaged orientation data such as far-field 3D X-ray diffraction microscopy. Once the corresponding 2D slice was identified in the DCT dataset, comparisons of phase balance, grain size, shape and texture were performed between DCT and EBSD techniques. More complicated aspects of the microstructural morphology such as grain boundary shape and grains less than a critical size were poorly reproduced by the DCT reconstruction, primarily due to the difference in resolutions of the technique compared with EBSD. However, lab-based DCT is shown to accurately determine the centre-of-mass position, orientation, and size of the large grains for each phase present, austenite and martensitic ferrite. The results reveals a complex ferrite grain network of similar crystal orientations that are absent from the EBSD dataset. Such detail demonstrates that lab-based DCT, as a technique, shows great promise in the field of multi-phase material characterization.

cond-mat.mtrl-sci

Per-grain and neighbourhood stress interactions during deformation of a ferritic steel obtained using three-dimensional X-ray diffraction

Three-dimensional X-ray diffraction (3DXRD) has been used to measure, in-situ, the evolution of $\sim 1800$ grains in a single phase low carbon ferritic steel sample during uniaxial deformation. The distribution of initial residual grain stresses in the material was observed to prevail as plasticity builds, though became less pronounced, and therefore less influential as strain increased. The initial Schmid factor of a grain was found to be strongly correlated to the intergranular stress change and the range of stresses that are permissible; a grain well aligned for easy slip is more likely to exhibit a range of stresses than those orientated poorly for dislocation motion. The orientation path of a grain, however, is not only dependent on its initial orientation, but hypothesised to be influenced by its stress state and the stress state of its grain environment. A grain neighbourhood effect is observed: the Schmid factor of serial adjoining grains influences the stress state of a grain of interest, whereas parallel neighbours are much less influential. This phenomenon is strongest at low plastic strains only, with the effect diminishing as plasticity builds. The influence of initial residual stresses becomes less evident, and grains rotate to eliminate any orientation dependent load shedding. The ability of the BCC ferrite to exhaust such neighbourhood interactions, which would otherwise be detrimental in crystal structures with lower symmetric and fewer slip systems, is considered key to the high ductility possessed by these materials.

cond-mat.mtrl-sci

Implementing and evaluating far-field 3D X-ray diffraction at the I12 JEEP beamline, Diamond Light Source

Three-dimensional X-ray diffraction (3DXRD) is shown to be feasible at the I12 Joint Engineering, Environmental and Processing (JEEP) beamline of Diamond Light Source. As a demonstration, a microstructually simple low-carbon ferritic steel was studied in a highly textured and annealed state. A processing pipeline suited to this beamline was created, using software already established in the 3DXRD user community, enabling grain centre-of-mass positions, orientations and strain tensor elements to be determined. Orientations, with texture measurements independently validated from electron backscatter diffraction (EBSD) data, possessed a $\sim 0.1^\circ$ uncertainty, comparable with other 3DXRD instruments. The spatial resolution was limited by the far-field detector pixel size; the average of the grain centre of mass position errors was determined as $\pm \sim 80 μ$m. An average per-grain error of $\sim 1 \times 10^{-3}$ for the elastic strains was also measured; this could be reduced in future experiments by improving sample preparation, data collection and analysis techniques. Application of 3DXRD onto I12 shows great potential, where its implementation is highly desirable due the flexible, open architecture of the beamline. User-owned or designed sample environments can be used, thus 3DXRD could be applied to previously unexplored scientific areas.

cond-mat.mtrl-sci

Macroscopic analysis of time dependent plasticity in Ti alloys

Component failure due to cold dwell fatigue of titanium and its alloys is a long-standing problem which has significant safety and economic implications to the aviation industry. This can be addressed by understanding the governing mechanisms of time dependent plasticity behaviour of Ti at low temperatures. Here, stress relaxation tests were performed at four different temperatures on three major alloy systems: commercially pure titanium (two alloys with different oxygen content), Ti-6Al-4V (two microstructures with differing beta phase fractions) and Ti-6Al-2Sn-4Zr-xMo (two alloys with different Mo content x= 2 or 6, and portion of beta phase). Key parameters controlling the time dependent plasticity were determined as a function of temperature. Both activation volume and energy were found to increase with temperature in all six alloys. It was found that the dwell fatigue effect is more significant by oxygen alloying but is suppressed by the addition of Mo. The presence of the beta phase did not strongly affect the dwell fatigue, however, it was suppressed at high temperature due to the low strain rate and strain rate sensitivity.

cond-mat.mtrl-sci

Weighted ellipse fitting routine for spotty or incomplete Debye-Scherrer rings on a 2D detector

We introduce a weighted ellipse fitting routine to measure Debye Scherrer rings acquired on 2D area detectors and demonstrate its use in strain determination. The method is relatively robust against incomplete rings due to low number of grains in the diffraction volume (spotty rings), or strong texture (intensity depletion in some azimuths). The method works by applying an annular mask around each diffraction ring and fitting an ellipse, using all pixel positions and their diffracted intensity as weights in the minimisation. We compare this method to the more popular cake integration method, and show that the weighted ellipse method works when the cake integration method fails or works poorly. The lattice strain sensitivity from spotty diffraction rings is in the order or 2E-5 or better. The algorithm has been made available for public use and works with 2D diffraction patterns acquired in a laboratory scale XRD equipment, TEM or a synchrotron.

physics.app-ph

An in-situ synchrotron diffraction study of stress relaxation in titanium: Effect of temperature and oxygen on cold dwell fatigue

There is a long-standing technological problem in which a stress dwell during cyclic loading at room temperature in Ti causes a significant fatigue life reduction. It is thought that localised time dependent plasticity in soft grains favourably oriented for easy plastic slip leads to load shedding and an increase in stress within a neighbouring hard grain poorly oriented for easy slip. Quantifying this time dependent plasticity process is key to understand the complex cold dwell fatigue problem. Knowing the effect of operating temperature and oxygen content on cold dwell fatigue will be beneficial for future alloy design to address this problem. In this work, synchrotron X-ray diffraction during stress relaxation experiments was used to characterise the time dependent plastic behaviour of two commercially pure titanium samples (grade 1 and grade 4) with different oxygen content at 4 different temperatures (room temperature, 75C, 145C and 250C). Lattice strains were measured by tracking the diffraction peak shift from multiple crystallographic plane families (21 diffraction rings) as a function of their orientation with respect to the loading direction. Critical resolved shear stress, activation energy and activation volume were established for both prismatic and basal slip as a function of temperature and oxygen content by fitting a crystal plasticity finite element model to the lattice strain relaxation responses measured along the loading axis for five strong reflections. Higher strain rate sensitivity was found to lead to higher plasticity during cold dwell.

cond-mat.mtrl-sci

Correlative Synchrotron X-ray Imaging and Diffraction of Directed Energy Deposition Additive Manufacturing

The governing mechanistic behaviour of Directed Energy Deposition Additive Manufacturing (DED-AM) is revealed by a combined in situ and operando synchrotron X-ray imaging and diffraction study of a nickel-base superalloy, IN718. Using a unique process replicator, real-space phase-contrast imaging enables quantification of the melt-pool boundary and flow dynamics during solidification. This imaging knowledge informed precise diffraction measurements of temporally resolved microstructural phases during transformation and stress development with a spatial resolution of 100 $μ$m. The diffraction quantified thermal gradient enabled a dendritic solidification microstructure to be predicted and coupled to the stress orientation and magnitude. The fast cooling rate entirely suppressed the formation of secondary phases or recrystallisation in the solid-state. Upon solidification, the stresses rapidly increase to the yield strength during cooling. This insight, combined with IN718 $'$s large solidification range suggests that the accumulated plasticity exhausts the alloy$'$s ductility, causing liquation cracking. This study has revealed additional fundamental mechanisms governing the formation of highly non-equilibrium microstructures during DED-AM.

physics.app-ph

Ultra high-temperature deformation in a single crystal superalloy: Meso-scale process simulation and micro-mechanisms

A mesoscale study of a single crystal nickel-base superalloy subjected to an industrially relevant process simulation has revealed the complex interplay between microstructural development and the micromechanical behaviour. As sample gauge volumes were smaller than the length scale of the highly cored structure of the parent material from which they were produced, their subtle composition differences gave rise to differing work hardening rates, influenced by varying secondary dendrite arm spacings, gamma-prime phase solvus temperatures and a topologically inverted gamma/gamma-prime microstructure. The gamma-prime precipitates possessed a characteristic `X' morphology, resulting from the simultaneously active solute transport mechanisms of thermally favoured octodendritic growth and N-type rafting, indicating creep-type mechanisms were prevalent. High resolution-electron backscatter diffraction (HR-EBSD) characterisation reveals deformation patterning that follows the gamma/gamma-prime microstructure, with high geometrically necessary dislocation density fields localised to the gamma/gamma-prime interfaces; Orowan looping is evidently the mechanism that mediated plasticity. Examination of the residual elastic stresses indicated the `X' gamma-prime precipitate morphology had significantly enhanced the deformation heterogeneity, resulting in stress states within the gamma channels that favour slip, and that encourage further growth of gamma-prime precipitate protrusions. The combination of such localised plasticity and residual stresses are considered to be critical in the formation of the recrystallisation defect in subsequent post-casting homogenisation heat treatments.

cond-mat.mtrl-sci

Dislocation density distribution at slip band-grain boundary intersections

We study the mechanisms of slip transfer at a grain boundary, in titanium, using Differential Aperture X-ray Laue Micro-diffraction (DAXM). This 3D characterization tool enables measurement of the full (9-component) Nye lattice curvature tensor and calculation of the density of geometrically necessary dislocations (GNDs). We observe dislocation pile-ups at a grain boundary, as the neighbor grain prohibits easy passage for dislocation transmission. This incompatibility results in local micro-plasticity within the slipping grain, near to where the slip planes intersect the grain boundary, and we observe bands of GNDs lying near the grain boundary. We observe that the distribution of GNDs can be significantly influenced by the formation of grain boundary ledges that serve as secondary dislocation sources. This observation highlights the non-continuum nature of polycrystal deformation and helps us understand the higher order complexity of grain boundary characteristics.

cond-mat.mtrl-sci

Warren-Averbach line broadening analysis from a time of flight neutron diffractometer

The well known Warren-Averbach theory of diffraction line profile broadening is shown to be applicable to time of flight data obtained from a neutron spallation source. Without modification, the method is applied to two very different examples; a cold worked ferritic steel and a thermally stressed alumina-30% SiC composite. Values of root mean square strains averaged over a range of lengths for the ferritic steel were used to estimate dislocation densities; values were found to be in good agreement with geometrically necessary dislocation densities independently measured from similarly orientated grains measured from electron backscatter diffraction analysis. An analytical model for the ceramic is described to validate the estimate of root mean square strain.

cond-mat.mtrl-sci