Mark H Reid

In situ study of dynamic recrystallization and hot deformation behavior of a multiphase titanium aluminide alloy

Hot-compression tests were conducted in a high-energy synchrotron x-ray beam to study in situ and in real time microstructural changes in the bulk of a β-solidifying titanium aluminide alloy. The occupancy and spottiness of the diffraction rings have been evaluated in order to access grain growth and refinement, orientation relationships, subgrain formation, dynamic recovery, and dynamic recrystallization, as well as phase transformations. This method has been applied to an alloy consisting of two coexisting phases at high temperature and it was found that the bcc β-phase recrystallizes dynamically, much faster than the hcp α-phase, which deforms predominantly through crystallographic slip underpinned by a dynamic recovery process with only a small component of dynamic recrystallization. The two phases deform to a very large extent independently from each other. The rapid recrystallization dynamics of the β-phase combined with the easy and isotropic slip characteristics of the bcc structure explain the ex...

Phase transition and ordering behavior of ternary Ti–Al–Mo alloys using in-situ neutron diffraction

Abstract Neutron diffraction has been used for in-situ investigations to elucidate the phase transformation behavior of two Mo-containing TiAl alloys with compositions of Ti-44Al-3Mo and Ti-44Al-7Mo (in at.%). Five different phases are present in these alloys. These include three ordered phases at room temperature, namely α2, β0 and γ and two disordered phases, and, which occur at higher temperatures. The sequence of the three phase transformations in each alloy has been determined. The phase transformation and disordering/ordering temperatures were determined on heating and cooling from the diffracted peak intensities. The neutron experiments are particularly sensitive to the order–disorder transitions in TiAl alloys, which are compared with the overall phase fractions obtained from previous high energy X-ray diffraction. Hysteresis and undercooling effects are observed for the various phase transformations and depend on the nature of atomic rearrangements.

Defect dynamics in polycrystalline zirconium alloy probed in situ by primary extinction of neutron diffraction

After α + β-zirconium has fully transformed into β-phase upon heating, the intensities of all β-Zr Bragg reflections decrease simultaneously as a function of time. It is shown that this effect represents a transition from the kinematic to the dynamic theory of diffraction due to the ever increasing crystal perfection driven by thermal recovery of the system. The best fitting coherent crystallite size of 30 μm and other microstructural features are verified by in situ laser scanning confocal microscopy. This effect of primary extinction in neutron diffraction has been employed to further investigate the crystal perfection kinetics. Upon further heating, crystal recovery is identified as a process of dislocation annihilation, suffering from lattice friction. Upon cooling, precipitating α-Zr induces strain into the perfect β-crystallites, re-establishing the kinematic diffraction intensities. An Avrami analysis leads to the estimations of nucleation time, consumption of nucleation sites and lower-dimensional growth. Such technique bears great value for further investigation on all metal systems annealed close to the melting temperature.

Effect of microstructural morphology on the mechanical properties of titanium alloys

Different morphologies of ?+? microstructures were obtained in a commercial Ti-6Al-4V alloy by cooling at different rates from the single ?-phase region into the two phase region. The effect of such morphologies on mechanical properties was studied using hot compression tests in a Gleeble thermomechanical simulator. A variety of complex morphologies could be obtained since the cooling rate has a significant influence on the ? to ? phase transformation and the resulting morphological development. While most of the ? phase transformed to colonies of ? at high cooling rates, it was possible to obtain a complex mixture of a colonies, grain boundary a and lamellar structure by decreasing the cooling rate. These complex morphologies each exhibited distinctive mechanical properties and characteristic dynamic phase transformation behaviour during deformation as a function of strain rate.

Morphology and composition changes of spinel (MgAl2O4) inclusions in steel

Abstract In this study, spinel inclusions of close to stoichiometric MgO.Al2O3 composition and known size distribution were added to a liquid steel bath before assessing their reactivity. The inclusions were then tracked for changes in size, morphology and composition with time in an aluminium killed steel at 1600°C, by sampling of the melt followed by automatic SEM based inclusion analysis techniques. The majority of the inclusions in the melt were alumina and complex sulphide inclusions, with the added spinel inclusions being a small proportion of the total inclusions. The proportion of alumina inclusions increased with time. The spinel inclusions were found to be evenly distributed through the melt and there was little change in their average size during the reaction. However, the composition of the inclusions did change, with the Mg/Al mass-% ratio changing from ∼0·5 to 0·08.

SolTrack: an automatic video processing software for in situ interface tracking

High‐Resolution in situ observation of solidification experiments has become a powerful technique to improve the fundamental understanding of solidification processes of metals and alloys. In the present study, high‐temperature laser‐scanning confocal microscopy (HTLSCM) was utilized to observe and capture in situ solidification and phase transformations of alloys for subsequent post processing and analysis. Until now, this analysis has been very time consuming as frame‐by‐frame manual evaluation of propagating interfaces was used to determine the interface velocities. SolTrack has been developed using the commercial software package MATLAB and is designed to automatically detect, locate and track propagating interfaces during solidification and phase transformations as well as to calculate interfacial velocities. Different solidification phenomena have been recorded to demonstrate a wider spectrum of applications of this software. A validation, through comparison with manual evaluation, is included where the accuracy is shown to be very high.

Dynamic Recovery and Recrystallization during Hot-Working in an Advanced TiAl Alloy

Abstract Intermetallic TiAl alloys are light-weight high-temperature materials and intended to partly replace Ni based alloys in jet engines. Due to difficult forming operations, component prices are high and limit the possible field of application. During hot-working, recovery and recrystallization effects determine the microstructural evolution and thereby the mechanical properties of the finished part as well as its behavior during deformation. To study the occurring phenomena, in-situ diffraction experiments with high-energy X-rays were conducted. By means of this method, the dominating processes were identified. The results were validated through electron back scatter diffraction experiments.

Simulation of microsegregation and the solid/liquid interface progression in the concentric solidification technique

A concentric solidification technique was employed to simulate experimentally the segregation of alloying elements during solidification at the centerline of continuously cast steel. Microstructural development of low carbon steel upon solidification has been observed in situ in a laser-scanning confocal microscope. Microscopic analyses following in situ observations, demonstrate that segregation occurring at steel slabs can reasonably be simulated by the use of the concentric solidification technique. The validity of these experimental simulations has been correlated with mathematical analyses using the Thermo-Calc and DICTRA (Diffusion Controlled Transformation) modeling tools. The effect of cooling rate on the sequence of events during solidification of Fe–0.18%C and Fe–4.2 wt%Ni peritectic alloys was studied and compared with the experimental observations.

Disintegration of Northern Cape iron ores under reducing conditions

Abstract Cracking occurs in the first step of gaseous reduction of hematite iron ore, to magnetite, and can lead to the formation of fine material, with deleterious effects on operation of shaft furnaces. To study this, samples of three ore types from the Northern Cape iron ore field in South Africa, and one blended ore from this region, were studied. The methods were high temperature microscopy (during reduction) and quantification of fines formation following reduction disintegration tests. The ore types do differ significantly with regards to their propensity to form fines. Although disintegration is clearly triggered by reduction, no direct correlation could be established between the degree of reduction and the amount of fines generated. Reduction disintegration increased with higher hydrogen percentages (>5%) in the reduction gas, and at higher temperatures (in the 500–700°C range). Disintegration of the samples decreased at temperatures >750°C. There was no correlation between the presence of gangue minerals and fines formation.

Hot Deformation of Cast and Extruded TiAl: An In Situ Diffraction Study

Intermetallic TiAl alloys are a class of innovative high-temperature materials which are developed to replace the substantially denser Ni-base alloys in low-pressure turbine blades of jet engines. By streamlining the production process of these parts, a substantial decrease in production costs can be achieved. To this end, a profound knowledge of the microstructural processes occurring during hot deformation is a prerequisite. To investigate the microstructural development during forming operations, cast and extruded as well as only cast specimens were hot-deformed and the microstructural development investigated in-situ by means of a novel diffraction method. This powder diffraction method utilizes the behavior of individual reflection spots on the Debye-Scherrer rings for deriving the materials response to the deformation imposed. It was found that the behavior of the two specimens is rather similar, although the starting microstructures show pronounced differences.