Microstructural characterisation of a bulk, spraycast Al-Fe-Cr-Ti alloy

Legislative and environmental demands are increasing the pressure on transport industries to introduce vehicles with lower weight, greater efficiency and reduced emissions while remaining competitive. For these reason the aerospace, defence and automotive industries worldwide are unanimous in the call for the development of new alloys with a step-change in performance. In the present thesis the results of the thorough microstructural and mechanical properties investigation of a 19 kg spraycast billet of the normally nanoquasicrystalline containing composition Al93Fe3Cr2Ti2 produced at Oxford University along with three binary Al intermetallics: Al3Ti, Al13Cr2 an Al13Fe4 produced by suction casting in the form of 5 mm rods at Sheffield University are presented and discussed.EThOS - Electronic Theses Online ServiceGBUnited Kingdo

Synchrotron X-ray and neutron investigation of the structure and thermal expansion of the monoclinic Al13Cr2 phase

The crystal structure of the Al13Cr2 intermetallic phase at 298 K was studied by synchrotron X-ray and neutron diffraction through the analysis of data collected on bulk samples, one in the as-cast condition, one after annealing at 773 K for 24 h and one for 168 h. Furthermore the thermal expansion behaviour of the structure was investigated for the first time in-situ up to 773 K. The diffraction patterns were analysed using whole pattern fitting techniques using the Le Bail and Pawley methods as well as the Rietveld method. The structure was found to be monoclinic with space group C2=m and lattice parameters a ¼ 25.3101 Å, b ¼ 7.6081 Å, c ¼ 10.9689 Å and b ¼ 128.704+ at 298 K in the as-cast condition. From the temperature variation of the unit cell parameters the principal axes of the thermal expansion tensor were calculated. The largest principal axis has a magnitude of 1:66 105 K1 and lies parallel to b, the second largest lies in the a-c plane at an angle of ∼37° from c in the direction of -a with a value 1:64 105 K1 whereas the smallest lies at ∼53° to c in the direction of þa and has a value of 1:31 105 K1 . Analysis of the behaviour of the icosahedra revealed that their expansion is highly anisotropic and the level of anisotropy is related to the point symmetry of the central Cr atoms

Tracking the evolution of hot tears in aluminium alloys using high-speed X-ray imaging

Hot tears are detrimental defects forming during the final stage of solidification when the remaining liquid loses the capacity to compensate for liquid to solid volume shrinkage. Although a mature semi-quantitative description of hot tearing has been developed, little is known about the dynamic evolution of hot tears as experimental studies have been conducted mostly post-solidification or in semi-static in-situ conditions. Here, we present a methodology to investigate the evolution of hot tears with high spatial and temporal resolution using synchrotron-based X-ray radiography. We develop a novel hot tear detection and tracking algorithm for quantification of hot tear density, area fraction and merging from the analysis of radiographic sequences of the solidification of thin metal samples. The methodology is demonstrated for an Al-5wt%Cu alloy and examples of the results and new insights that can be achieved are described

The mechanism of Fe-rich intermetallic compound formation and growth on inoculants revealed by electron backscattered diffraction and X-ray imaging

Fe-rich intermetallics affect critically the mechanical properties and recyclability of aluminium alloys. Increasing effort has been spent on the inoculation of these intermetallics, hoping to promote a finer distribution. Recently Al-5Ti-1B (wt.%), originally developed to refine -Al, has been shown to refine Al13Fe4, an intermetallic phase present in a variety of Al alloys. However, mechanisms of the formation and growth of the intermetallics on the inoculants are unclear. In this paper, Ti is added to Fe-containing Al alloys to produce a large number of potent Al3Ti particles, the active inoculant in Al-5Ti-1B. We use a combination of electron backscattered diffraction, in situ synchrotron X-ray radiography and post-solidification X-ray computed tomography to investigate the formation and growth of primary Al13Fe4 on Al3Ti inoculants, first in a model Al-Fe alloy, with key insights then confirmed in a high Fe-containing, recycled 6xxx alloy. Crystallographic orientation relationships between Al13Fe4 and Al3Ti are analysed comprehensively, and the formation and growth dynamics of Al13Fe4 on Al3Ti is also unveiled. A strong link is revealed between the formation of Al13Fe4 on Al3Ti and a twinning-related pseudo-symmetry of Al13Fe4. Finally, a potential strategy to refine both intermetallics and -Al in recycled alloys with elevated Fe concentration is proposed

3D Correlative Imaging of Lithium Ion Concentration in a Vertically Oriented Electrode Microstructure with a Density Gradient

The performance of Li+ ion batteries (LIBs) is hindered by steep Li+ ion concentration gradients in the electrodes. Although thick electrodes (≥300 µm) have the potential for reducing the proportion of inactive components inside LIBs and increasing battery energy density, the Li+ ion concentration gradient problem is exacerbated. Most understanding of Li+ ion diffusion in the electrodes is based on computational modeling because of the low atomic number (Z) of Li. There are few experimental methods to visualize Li+ ion concentration distribution of the electrode within a battery of typical configurations, for example, coin cells with stainless steel casing. Here, for the first time, an interrupted in situ correlative imaging technique is developed, combining novel, full-field X-ray Compton scattering imaging with X-ray computed tomography that allows 3D pixel-by-pixel mapping of both Li+ stoichiometry and electrode microstructure of a LiNi0.8 Mn0.1 Co0.1 O2 cathode to correlate the chemical and physical properties of the electrode inside a working coin cell battery. An electrode microstructure containing vertically oriented pore arrays and a density gradient is fabricated. It is shown how the designed electrode microstructure improves Li+ ion diffusivity, homogenizes Li+ ion concentration through the ultra-thick electrode (1 mm), and improves utilization of electrode active materials

The mechanism of Fe-rich intermetallic compound formation and growth on inoculants revealed by electron backscattered diraction and X-ray imaging

Fe-rich intermetallics affect critically the mechanical properties and recyclability of aluminium alloys. Increasing effort has been spent on the inoculation of these intermetallics, hoping to promote a finer distribution. Recently Al-5Ti-1B (wt.%), originally developed to refine α-Al, has been shown to refine Al13Fe4, an intermetallic phase present in a variety of Al alloys. However, mechanisms of the formation and growth of the intermetallics on the inoculants are unclear. In this paper, Ti is added to Fe-containing Al alloys to produce a large number of potent Al3Ti particles, the active inoculant in Al-5Ti-1B. We use a combination of electron backscattered diffraction, in situ synchrotron X-ray radiography and post-solidification X-ray computed tomography to investigate the formation and growth of primary Al13Fe4 on Al3Ti inoculants, first in a model Al-Fe alloy, with key insights then confirmed in a high Fe-containing, recycled 6xxx alloy. Crystallographic orientation relationships between Al13Fe4 and Al3Ti are analysed comprehensively, and the formation and growth dynamics of Al13Fe4 on Al3Ti is also unveiled. A strong link is revealed between the formation of Al13Fe4 on Al3Ti and a twinning-related pseudo-symmetry of Al13Fe4. Finally, a potential strategy to refine both intermetallics and α-Al in recycled alloys with elevated Fe concentration is proposed

Tracking the evolution of hot tears in aluminium alloys using high-speed X-ray imaging

Hot tears are detrimental defects forming during the final stage of solidification when the remaining liquid loses the capacity to compensate for liquid to solid volume shrinkage. Although a mature semi-quantitative description of hot tearing has been developed, little is known about the dynamic evolution of hot tears as experimental studies have been conducted mostly post-solidification or in semi-static in-situ conditions. Here, we present a methodology to investigate the evolution of hot tears with high spatial and temporal resolution using synchrotron-based X-ray radiography. We develop a novel hot tear detection and tracking algorithm for quantification of hot tear density, area fraction and merging from the analysis of radiographic sequences of the solidification of thin metal samples. The methodology is demonstrated for an Al-5wt%Cu alloy and examples of the results and new insights that can be achieved are described

Investigating Metal Solidification with X-ray Imaging

In the last two decades, X-ray imaging techniques have been used increasingly to study metal solidification in real-time as, thanks to advances in X-ray sources (synchrotron and laboratory-based) and detector technology, images can now be obtained with spatio-temporal resolutions sufficient to record key phenomena and extract quantitative information, primarily relating to crystal growth. This paper presents an overview of the research conducted at the University of Oxford over the last 6 years as a partner in the UK’s Future Liquid Metal Engineering (LiME) Manufacturing Hub. The focus is on in situ X-ray radiography to investigate the solidification of Al alloys, including the formation of primary α-Al crystals, and the formation and growth of secondary intermetallic phases. Technologically, the thrust is to understand how to control as-cast phases, structures and element distributions, particularly elements associated with recycling, as a means to facilitate greater recirculation of aluminium alloys. We first present studies on refinement of primary α-Al, including extrinsic grain refinement using inoculation and intrinsic refinement based on dendrite fragmentation. Second, we describe studies on intermetallic phase formation and growth, because intermetallic fraction, morphology and distribution are frequently a limiting factor of alloy mechanical properties and recyclability. Then we present some of the latest progress in studying liquid flow during solidification and associated hot tear formation. Finally, future research directions are described

The mechanism of Fe-rich intermetallic compound formation and growth on inoculants revealed by electron backscattered diffraction and X-ray imaging

Fe-rich intermetallics affect critically the mechanical properties and recyclability of aluminium alloys. Increasing effort has been spent on the inoculation of these intermetallics, hoping to promote a finer distribution. Recently Al-5Ti-1B (wt.%), originally developed to refine -Al, has been shown to refine Al$_{13}$Fe$_4$, an intermetallic phase present in a variety of Al alloys. However, mechanisms of the formation and growth of the intermetallics on the inoculants are unclear. In this paper, Ti is added to Fe-containing Al alloys to produce a large number of potent Al$_3$Ti particles, the active inoculant in Al-5Ti-1B. We use a combination of electron backscattered diffraction, in situ synchrotron X-ray radiography and post-solidification X-ray computed tomography to investigate the formation and growth of primary Al$_{13}$Fe$_4$ on Al$_3$Ti inoculants, first in a model Al-Fe alloy, with key insights then confirmed in a high Fe-containing, recycled 6xxx alloy. Crystallographic orientation relationships between Al$_{13}$Fe$_4$ and Al$_3$Ti are analysed comprehensively, and the formation and growth dynamics of Al$_{13}$Fe$_4$ on Al$_3$Ti is also unveiled. A strong link is revealed between the formation of Al$_{13}$Fe$_4$ on Al$_3$Ti and a twinning-related pseudo-symmetry of Al$_{13}$Fe$_4$. Finally, a potential strategy to refine both intermetallics and -Al in recycled alloys with elevated Fe concentration is proposed