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We present a dynamic implementation of the beam-tracking x-ray imaging method providing absorption, phase, and ultrasmall angle scattering signals with microscopic resolution and high frame rate. We demonstrate the method's ability to capture dynamic processes with 22-ms time resolution by investigating the melting of metals in laser additive manufacturing, which has so far been limited to single-modality synchrotron radiography. The simultaneous availability of three contrast channels enables earlier segmentation of droplets, tracking of powder dynamic, and estimation of unfused powder amounts, demonstrating that the method can provide additional information on melting processes.

Ti-containing micro-alloyed steels are often alloyed with molybdenum (Mo) to reduce nano-precipitate coarsening, although the mechanism is still disputed. Using small angle neutron scattering we characterised the precipitate composition and coarsening of Ti-alloyed and Ti-Mo-alloyed steels. The results demonstrate ~25 at.% of Ti is substituted by Mo in the (Ti, Mo)C precipitates, increasing both the precipitate volume percent and average size. Mo alloying did not retard precipitation coarsening, but improved lattice misfit between precipitate and matrix, contributing to better ageing resistance of the Ti-Mo-alloyed steel. This new understanding opens opportunities for designing ageing-resistant micro-alloyed steels with lean alloying elements.

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 DAE-AM process replicator, real-space imaging enables quantification of the melt-pool boundary and flow dynamics during solidification. This imaging knowledge was also used to informed precise diffraction measurements of temporally resolved microstructural phases during transformation and stress development with a spatial resolution of 100 µm. 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 the large solidification range of IN718 suggests that the accumulated plasticity exhausts the ductility of the alloy, causing liquation cracking. This study has revealed additional fundamental mechanisms governing the formation of highly non-equilibrium microstructures during DED-AM.

The Directed Energy Deposition Additive Manufacturing (DED-AM) of SS316L was studied using in situ and operando synchrotron X-ray imaging to quantitively understand the effect of processing parameters on the melt-pool morphology and surface quality. It was found that surface roughness of DED-AM builds can result from melt pool surface perturbations caused by changes in the melt flow and build stage motion perturbations. Process maps are developed that quantitatively correlate build quality to process parameters including powder feed rate, laser power and traverse speed. How the AM process parameters control build efficacy is clarified, and the processing conditions required to dampen surface perturbations leading to roughness were determined.

Porosity and high surface roughness can be detrimental to the mechanical performance of laser powder bed fusion (LPBF) additive manufactured components, potentially resulting in reduced component life. However, the link between powder layer thickness on pore formation and surface undulations in the LPBF parts remains unclear. In this paper, the influence of processing parameters on Ti-6Al-4 V additive manufactured thin-wall components are investigated for multilayer builds, using a custom-built process replicator and in situ high-speed synchrotron X-ray imaging. In addition to the formation of initial keyhole pores, the results reveal three pore phenomena in multilayer builds resulting from keyhole melting: (i) healing of the previous layers' pores via liquid filling during remelting; (ii) insufficient laser penetration depth to remelt and heal pores; and (iii) pores formed by keyholing which merge with existing pores, increasing the pore size. The results also show that the variation of powder layer thickness influences which pore formation mechanisms take place in multilayer builds. High-resolution microcomputed tomography images reveal that clusters of pores form at the ends of tracks, and variations in the layer thickness and melt flow cause irregular remelting and track height undulations. Extreme variations in height were found to lead to lack of fusion pores in the trough regions. It is hypothesised that the end of track pores were augmented by soluble gas which is partitioned into the melt pool and swept to track ends, supersaturating during end of track solidification and diffusing into pores increasing their size.

Nano-sized interphase precipitates, which form in ordered rows, are critical for HSLA (High Strength Low Alloy) steels, in achieving the desired strength needed for downgauging for light-weighting automotive structures. The occurrence of interphase precipitation (as opposed to random, heterogeneous precipitation inside grains) is dependent on a number of inter-connected parameters such as alloy chemistry, ferrite-growth rate, temperature, crystallography and precipitate shape and size. In this study, we employ data analysis based on the Machine Learning algorithms: Decision Tree and Random Forrest to predict when interphase precipitation occurs. The results show that Decision Tree could not provide an accurate prediction, even as the depth was increased, whereas Random Forrest was able to, after up-sampling the minority class, a score of 98% for Accuracy, Recall, Precision and F1, which is adequate for predicting the occurrences of interfacial precipitates. The importance of individual features on the artificial classification task was evaluated and the precipitate chemistry and morphology were recognised by algorithms as the most informative features for decision making. Because our final goal was to predict the interphase precipitation for samples outside our training set we used receiver operating characteristic curve (ROC) and we found a strong classification prediction as the area under the curve was 0.98. In addition, particles containing Mo with disk shape were predicted to be very likely to form interphase precipitates. The alloy composition range for Ti, Mo and Mn was derived through Gaussian kernel estimate distribution and 0.18 Ti, 0.44 Mo and 1.5 Mn (all in wt.%) had the highest peaks.

A mechanism for modelling the growth of faceted primary M7C3 needles during solidification of chromium carbide overlays is presented for the first time. In contrast with existing models that consider diffusion-controlled growth over the length of the needle, this work disaggregates the flow of solute at the tip (diffusion-controlled) and the faceted sides (interface-controlled). The proposed solution predicts an initial transient followed by a steady state longitudinal growth. The outward growth of the needle prism faces is linear and slow, consistent with interface-dominated kinetics. Abrupt decreases in longitudinal growth rate was observed when the tip of the carbides approached other carbides, consistent a soft-impingement effect when the diffusion field of two carbides a overlap. The model was compared to in-situ visualisation of the solidification of an alloy with primary chromium carbide needles, and was found to match closely to observations.

High Al Low-density steels could have a transformative effect on the light-weighting of steel structures for transportation. They can achieve the desired properties with the minimum amount of Ni, and thus are of great interest from an economic perspective. In this study, the mechanical properties of two duplex low-density steels, Fe-15Mn-10Al-0.8C-5Ni and Fe-15Mn-10Al-0.8 C (wt.%) were investigated through nano-indentation and simulation through utilization of ab-initio formalisms in Density Functional Theory (DFT) in order to establish the hardness resulting from two critical structural features (κ-carbides and B2 intermetallic) as a function of annealing temperature (500–1050 °C) and the addition of Ni. In the Ni-free sample, the calculated elastic properties of κ-carbides were compared with those of the B2 intermetallic Fe3Al−L12 and the role of Mn in the κ structure and its elastic properties were studied. The Ni-containing samples were found to have a higher hardness due to the B2 phase composition being NiAl rather than FeAl, with Ni-Al bonds reported to be stronger than the Fe-Al bonds. In both samples, at temperatures of 900 °C and above, the ferrite phase contained nano-sized discs of B2 phase, wherein the Ni-containing samples exhibited higher hardness, attributed again to the stronger Ni-Al bonds in the B2 phase. At 700 °C and below, the nano-sized B2 discs were replaced by micrometre sized needles of κ in the Ni-free sample resulting in a lowering of the hardness. In the Ni-containing sample, the entire α phase was replaced by B2 stringers, which had a lower hardness than the Ni-Al nano-discs due to a lower Ni content in B2 stringer bands formed at 700 °C and below. In addition, the hardness of needle-like κ-carbides formed in α phase was found to be a function of Mn content. Although it was impossible to measure the hardness of cuboid κ particles in γ phase because of their nano-size, the hardness value of composite phases, e.g. γ + κ was measured and reported. All the hardness values were compared and rationalized by bonding energy between different atoms.

A multi-phase field method is developed to investigate the effects of transformation strain on the transformation kinetics, thermodynamic stability and pairing of interphase precipitates in micro-alloyed steels. The model conserves homogeneity of stress in the diffuse interface between elastically inhomogeneous phases and provides an explanation of the mechanism resulting in the pairing of two adjacent interphase precipitates. Several scenarios of inhomogeneous elastic conditions have been considered. The simulations for a situation where only the interfacial energy is considered to contribute to the transformation show that this energy can lead to the establishment of a neck between two neighbouring precipitates. However, if sufficient time is given, one of the precipitates will completely dissolve into its neighbouring particle. On the other hand, when both strain and interfacial energies act on the system, the bridge between the particles becomes stabilised leading to the pairing of the particles. This is a result of the particles tendency to minimise the strain energy due to the excessive strain field generated by the neck between the two particles.

A multi-component phase field model was developed based on CALPHAD method and directly coupled with the CALPHAD thermodynamic database using a four-sublattice model. Interphase carbide precipitation at the γ/α interface is simulated and the predictions are tested against reported experimental results for a medium carbon, vanadium micro-alloyed steel during an isothermal γ→α+MC transformation at 973 K. The model is found to be able to accurately predict: interphase precipitate composition, morphology and size of the precipitates. Furthermore, the tip-to-tip pairing of interphase precipitates in γ/α interphase boundaries is elucidated and found to be attributable to the minimisation of interfacial energy.

Directed Energy Deposition Additive Manufacturing (DED-AM) is one of the principal AM techniques being explored for both the repair of high value components in the aerospace industry as well as freeform fabrication of large metallic components. However, the lack of fundamental understanding of the underlying process-structure-property relationships hinders the utilisation of DED-AM for the production or repair of safety-critical components. This study uses in situ and operando synchrotron X-ray imaging to provide an improved fundamental understanding of laser-matter interactions and their influence on the melt pool geometry. Coupled with process modelling, these unique observations illustrate how process parameters can influence the DED-AM melt pool geometry. The calibrated simulation can be used for guidance in an industrial additive manufacturing process for microstructure and quality control.

Directed Energy Deposition Additive Manufacturing (DED-AM) is transformative for the production of larger, geometrically complex metallic components. However, the mechanical properties of titanium alloy DED-AM components do not always reach their full potential due to microstructural features including porosity and regions of lack of fusion. Using in situ and operando synchrotron X-ray imaging we gain insights into key laser-matter interaction and microstructural feature formation mechanisms during DED-AM of Ti-6242. Analysis of the process conditions reveals that laser power is dominant for build efficiency while higher traverse speed can effectively reduce lack of fusion regions. We also elucidate the mechanisms underlying several physical phenomena occurring during the deposition of titanium alloys, including the formation of a saddle-shaped melt pool and pore pushing. The findings of this work clarify the transient kinetics behind the DED-AM of titanium alloys and can be used as a guide for optimising industrial additive manufacturing processes.

In-situ characterization techniques have been applied to elucidate the influence of γ/α transformation upon the extent of interphase precipitation in a low-carbon, vanadium-HSLA steel. Electron Back-scattered diffraction analyses of the γ/α orientation relationship with continuous cooling at 2 and 10 K/s suggest that the proportion of ferrite likely to hold interphase precipitation varies little with cooling rate. However, TEM analyses show that the interphase precipitation refines with increasing cooling rate in this cooling range. With cooling rates in excess of 20 K/s, interphase precipitation is increasingly suppressed due to the increasingly diffusional-displacive nature of the Widmanstatten γ/α transformation that is activated. The present study illustrates that the extent and dimensions of interphase precipitation can be controlled through controlled cooling.

The keyhole mode in laser powder bed fusion (LPBF) additive manufacturing can be associated with excessive porosity and spatter, however, the underlying physics in multilayer build conditions remain unclear. Here, we used ultra-fast synchrotron X-ray imaging to reveal this phenomena. We in investigated melt pool dynamics, keyhole porosity and spatter formation mechanisms and their impact in all layers of the build. We observed that the transient melt pool dynamics associated with the keyhole include: (I) keyhole initiation, (II) keyhole development, and (III) melt pool recovery. Porosity and spatter were associated with stages (II) and (III). We also discovered that droplet spatter can form due to the collapse of the keyhole recoil zone, causing molten particle agglomeration and ejection during stage (III). Our results clarify the transient dynamics behind the keyhole mode in a multi-layer LBPF process and can be used to guide the reduction in porosity and spatter in additive manufacturing.

Interphase precipitation (IPP) of nanoscale carbides in a vanadium-containing high-strength low-alloy steel has been investigated. Small angle neutron scattering (SANS) and transmission electron microscopy (TEM) were employed to characterize the precipitates and their size distributions in Fe-0.047C-0.2V-1.6Mn (in wt.%) alloy samples which had been austenitized, isothermally transformed at 700 °C for between 3 and 600 min and water quenched. TEM confirms that, following heat treatment, rows of vanadium-containing nanoscale interphase precipitates were present. Model-independent analysis of the nuclear SANS signal and model fitting calculations, using oblate spheroid and disc-shapes, were performed. The major axis diameter increased from 18 nm after 3 min to 35 nm after 600 min. Precipitate volume percent increased from 0.09 to 0.22 vol% over the same period and number density fell from 2 × 10 21 to 5 × 10 20 m −3. A limited number of measurements of precipitate maximum diameters from TEM images showed the mean value increased from 8 nm after 5 min to 28 nm after 600 min which is in reasonable agreement with the SANS data.

A novel mathematical approach for the independent quantification of phase fractions in multiple simultaneous phase transformations is introduced. The proposed dilation curve analysis is very general, relying only on raw dilatation data and the density of some of the constituents involved in the transformations. Transformation start and end temperatures and instantaneous phase fractions are accurately measured using this method. As an example, the simultaneous transformation of austenite to bainite and martensite in seven cylindrical AISI 4140 steel samples cooled at rates between 1 and 4 K/s from 1223 K (950 °C) is used to show the feasibility of this new methodology. The martensite and bainite fractions calculated using the presented methodology for all seven samples are in good agreement with the ones measured with quantitative metallography. Hot stage microscopy was also performed on a sample of the same batch, yielding quantitative results consistent with the start temperatures from the analysis proposed.

The size and distribution of interphase precipitates in micro-alloyed steels is a crucial micro-structural feature to control for obtaining the necessary strength in low-cost automotive sheets. In order to optimize both alloy chemistry and thermal processing an enhanced understanding of the interphase precipitation mechanism is required. It is proposed that the evolution of inter-sheet spacing of MC carbides during the γ→α+MC transformation can be explained considering the interfacial segregation and the corresponding dissipation of Gibbs energy inside the moving interphase boundary. The inter-sheet spacing of interphase precipitates is controlled by a complex interplay between the interfacial energy and interfacial segregation, this is presented in form of an analytical model. It is shown that the general trend of refining inter-sheet spacing with growing ferrite half-thickness can be well predicted by the proposed model.