Kun Yan

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...

Repeated crack healing in MAX-phase ceramics revealed by 4D in situ synchrotron X-ray tomographic microscopy.

MAX phase materials are emerging as attractive engineering materials in applications where the material is exposed to severe thermal and mechanical conditions in an oxidative environment. The Ti2AlC MAX phase possesses attractive thermomechanical properties even beyond a temperature of 1000 K. An attractive feature of this material is its capacity for the autonomous healing of cracks when operating at high temperatures. Coupling a specialized thermomechanical setup to a synchrotron X-ray tomographic microscopy endstation at the TOMCAT beamline, we captured the temporal evolution of local crack opening and healing during multiple cracking and autonomous repair cycles at a temperature of 1500 K. For the first time, the rate and position dependence of crack repair in pristine Ti2AlC material and in previously healed cracks has been quantified. Our results demonstrate that healed cracks can have sufficient mechanical integrity to make subsequent cracks form elsewhere upon reloading after healing.

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.

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.

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.

Measurement of residual stress shakedown in pressure/tensile armour wires of flexible pipes by neutron diffraction

The manufacture of unbonded flexible pipes (flowlines and risers) involves wrapping steel wires to create pressure and tensile armour layers. The forming of armour wires from vendor supply conditions to a helix shape on the pipe involves significant plastic straining and the wires that are wrapped onto the pipe are not unloaded. Therefore the armour wires in flexible pipes are expected to contain significant residual stress (RS) as a result of the plastic straining and loading during manufacture and placement. This may lead to detrimental effects on the strength, durability and the service integrity of the pipe. It is postulated that the unfavorable RS introduced during pipe manufacture reduces due to stress shakedown during the factory acceptance test (FAT) where the pipe is subjected to a high internal pressure.This paper describes the first attempts to measure RS in the armour wires in unbonded flexible pipes. The key development is the use of a neutron diffraction method which allows the measurement of RS in-situ on the manufactured pipe through the whole wire sections. Pipe samples were prepared exposing the relevant metal layer and the measurements were performed on pipe samples taken before and after performing the pressurized FAT. The effect of the FAT on the shakedown of residual stress in pressure armour wires is discussed. As shown by the measurements, the elastic strains and stresses in the pressure armour wires are much larger in the hoop direction of the pipe (i.e. along the length of the wire) than radial or axial to the pipe. In pre-FAT pipe the hoop stresses are essentially tensile on the extrados and compressive on the intrados. The results have shown that the FAT reduces the hoop strains and stresses to approximately 1/3 of their as manufactured level.© 2015 ASME

D-80 IN-SITU OBSERVATION OF DYNAMIC RECRYSTALLIZATION AND RELATED PHENOMENA IN THE BULK OF ZIRCONIUM ALLOY

The nuclear reactor structural material Zircaloy-4 grade R60804 of nominal composition Zr 1.5%Sn 0.2%Fe 0.1%Cr 0.1%O (in weight %) has been tested under thermo-mechanical load on the high energy X-ray beamline 1-ID at the Advanced Photon Source while diffraction patterns were recorded in-situ and continuously on a sub-second time scale. Multiple heating-cooling cycles were run between 690 K and 1280 K under mechanical load increasing stepwise from 0 N to 225 N. The temperature cycles transform the metal from its low temperature α phase below 1083 K through an α+β phase field into its single β-phase of bcc structure stable above 1253 K and back. Initially, the β-phase precipitates in a fine grain breaking also the coexistent α-grains. After α disappears, grain growth is rapid resulting in only a very few sharp spots on the diffraction rings. Upon cooling, the α-phase reappears and grows into the β-grains and the well known Burgers orientation relationship is observed, i.e. the α-{002} orientation aligns with the β-{110} plane orientation, which can be reversed upon subsequent heating. The β-phase being very ductile and soft shows plastic deformation, which escalates at 225 N and a cross section of 30 mm. While temperature is increased, first we observe grain breakage into sub-grains due to the deformation process, which recovers dynamically. Plastic deformation is faster at higher temperature when new grain orientations pop up and disappear continuously and the system recrystallizes dynamically. The details and fingerprints for the different stages during an in-situ observation from the bulk of a metallic material measured for the first time.