Microstructure and Crystallographic Texture Evolution During the Friction-Stir Processing of a Precipitation-Hardenable Aluminum Alloy

Friction-stir processing (FSP) has been proven as a successful method for the grain refinement of high-strength aluminum alloys. The most important attributes of this process are the fine-grain microstructure and characteristic texture, which impart suitable properties in the as-processed material. In the current work, FSP of the precipitation-hardenable aluminum alloy 2219 has been carried out and the consequent evolution of microstructure and texture has been studied. The as-processed materials were characterized using electron back-scattered diffraction, x-ray diffraction, and electron probe microanalysis. Onion-ring formation was observed in the nugget zone, which has been found to be related to the precipitation response and crystallographic texture of the alloy. Texture development in the alloy has been attributed to the combined effect of shear deformation and dynamic recrystallization. The texture was found heterogeneous even within the nugget zone. A microtexture analysis revealed the dominance of shear texture components, with C component at the top of nugget zone and the B and A(2)* components in the middle and bottom. The bulk texture measurement in the nugget zone revealed a dominant C component. The development of a weaker texture along with the presence of some large particles in the nugget zone indicates particle-stimulated nucleation as the dominant nucleation mechanism during FSP. Grain growth follows the Burke and Turnbull mechanism and geometrical coalescence.

Evolution of Texture and Microstructure in Deformed and Annealed Copper-Iron Multilayer

The effect of multiple phases on the evolution of texture during cold rolling and annealing of a copper-iron multilayer, fabricated by accumulative roll bonding, has been studied. The presence of an iron layer affects the deformation texture of the copper layer only at very large strains. On the other hand, a strong effect of copper on iron is observed at both small and large strains. At smaller strains, the larger deformation carried by the copper suppresses the texture development in the iron, whereas, at higher strains, selection of specific orientation relationship at the interface influences the texture of the iron layer. Shear banding and continuous dynamic recrystallization were found to influence the evolution of texture in the copper layer. The influence of large plastic deformation on the recrystallization behavior of copper is demonstrated with the suppression of typical fcc annealing texture components, described as constrained recrystallization. Evolution of typical annealing texture component is suppressed because of the multilayer microstructure. The plane of the interface formed during deformation is determined by a combination of the rolling texture of individual phases, constrained annealing, and the tendency to form a low-energy interface between the two phases during annealing.

Quartz recrystallization regimes, c-axis texture transitions and fluid inclusion reequilibration in a prograde greenschist to amphibolite facies mylonite zone (Ribeira Shear Zone, SE Brazil)

The crystal-plastic behavior of quartz mylonites from the Ribeira Shear Zone (SE Brazil), a major strike-slip structure that was active during a prograde metamorphic phase related to the Neoproterozoic Brasiliano-Pan African Orogeny, was investigated using a multi-method approach. Geothermobarometry results indicate deformational conditions ranging from similar to 300 to similar to 630 degrees C and 500-700 MPa. A strong correlation between mapped metamorphic zones and a dominance of different dynamic recrystallization mechanisms of quartz occurs within the mylonite zone. Bulging recrystallization (BLG) dominates within the chlorite zone between 300 and 410 degrees C, subgrain rotation recrystallization (SGR) operates within the biotite zone from 410 to 520 degrees C, and grain boundary migration recrystallization (GBM) dominates in the garnet zone above 520 degrees C. The development of quartz c-axis textures is mainly governed by temperature and dynamic recrystallization mechanisms. Textures from BLG zone mylonites are characterized by maxima around Z; SGR zone mylonites display single girdles or asymmetric type I crossed girdles; and GBM zone mylonites comprise maxima around Y and intermediate between X and Z. The scarcity or absence of water-bearing fluid inclusions in quartz mylonites from the SGR and GBM zones, which are dominated by carbonic inclusions, suggests water-deficient conditions, whereas BLG zone mylonites are dominated by water-bearing inclusions. This evidence indicates that water was available in the protoliths but has been eliminated with increasing deformation and deformation temperature. No effect of the water content variation on the quartz microstructural and recrystallized grain size evolution was detected, and little influence on c-axis texture development was observed. Most of the fluid inclusion densities were reequilibrated during the shear zone exhumation history, recording a decompression in the range of 300-500 MPa, while microstructural reequilibration effects related to the prograde metamorphism are largely preserved. Fluid inclusion microstructures and densities from two SGR zone samples preserved evidence for a near isothermal compression within the interior of the Ribeira Shear Zone during the prograde metamorphism. (C) 2009 Elsevier B.V. All rights reserved.

Dynamic recrystallization of austenite in Ni-30 Pct Fe model alloy : microstructure and texture evolution

The microstructure and crystallographic texture development in an austenitic Ni-30 pct Fe model alloy was investigated within the dynamic recrystallization (DRX) regime using hot torsion testing. The prominent DRX nucleation mechanism was strain-induced grain boundary migration accompanied by the formation of large-angle sub-boundaries and annealing twins. The increase in DRX volume fraction occurred through the formation of multiple twinning chains. With increasing strain, the pre-existing Σ3 twin boundaries became gradually converted to general boundaries capable of acting as potent DRX nucleation sites. The texture characteristics of deformed grains resulted from the preferred consumption of high Taylor factor components by new recrystallized grains. Similarly, the texture of DRX grains was dominated by low Taylor factor components as a result of their lower consumption rate during the DRX process. The substructure of deformed grains was characterized by “organized,” banded subgrain arrangements, while that of the DRX grains displayed “random,” more equiaxed subgrain/cell configurations.

Texture and substructure characteristics of dynamic recrystallization in a Ni–30%Fe austenitic model alloy

The substructure and texture development during dynamic recrystallization (DRX) of an austenitic Ni–30%Fe model alloy was investigated using hot torsion testing. The current results revealed that the DRX texture was dominated by grains with a low Taylor factor component. This was related to the preferred nucleation and lower consumption rates of these grains during DRX. The substructure of DRX grains was ‘‘random” in character and displayed complex subgrain/cell arrangements that largely depended on grain orientation.

Texture evolution and softening processes in an austenitic Ni-30Fe alloy subjected to hot deformation and subsequent annealing

The current work has investigated the texture development in an austenitic Ni-30Fe model alloy during deformation within the dynamic recrystallization (DRX) regime and after post-deformation annealing. Both the deformed matrix and DRX texture displayed the expected FCC shear components, the latter being dominated by the low Taylor factor grains, which was presumably caused by their lower consumption rate during DRX. The deformed matrix grains were largely characterized by organized, microband structures, while the DRX grains showed more random, complex subgrains/cell arrangements. The latter substructure type proved to be significantly less stable during post-deformation annealing. The recrystallization of the deformed matrix occurred through nucleation and growth of new grains fully replacing the deformed structure, as expected for the classical static recrystallization (SRX). Unlike the DRX grains, the SRX texture was essentially random. By contrast, a novel softening mechanism was revealed during annealing of the fully DRX microstructure. The initial post-dynamic softening stage involved rapid growth of the dynamically formed nuclei and migration of the mobile boundaries in line with the well-established metadynamic recrystallization (MDRX) mechanism, which weakened the starting DRX texture. However, in parallel, the sub-boundaries within the deformed DRX grains progressively disintegrated through dislocation climb and dislocation annihilation, which ultimately led to the formation of dislocation-free grains. Consequently, the weakened DRX texture largely remained preserved throughout the annealing process.

Microstructure and texture evolution during symmetric and asymmetric rolling of a martensitic Ti-6Al-4V alloy

In the current study, the effect of deformation mode (i.e., symmetric vs asymmetric rolling) on the extent of grain refinement and texture development in Ti-6Al-4V was examined through warm rolling of a martensitic starting microstructure. During rolling, the initial martensitic lath structure was progressively fragmented, primarily through continuous dynamic recrystallization. This eventually led to an ultrafine-grained (UFG) microstructure composed of equiaxed grains with a mean size of 180 to 230 nm, mostly surrounded by high-angle grain boundaries. Depending on the rolling reduction and deformation mode (symmetric and asymmetric), the rolled specimens displayed different layer morphologies throughout the specimen thickness: a fully UFG surface layer, a partial UFG transition layer, and a partially fragmented lath interior layer. Due to a higher level of effective strain and continuous rotation of the principle axis, asymmetric rolling resulted in a greater extent of grain refinement compared with symmetric rolling at a given thermomechanical condition. A bulk UFG structure was successfully obtained using 70 pct asymmetric rolling. In addition, the rolling texture exhibited various characteristics throughout the thickness due to a different combination of shear and compressive strains. Principally, the basal texture component was displaced from the normal toward rolling direction during asymmetric rolling, differing from the symmetric rolling textures.

Deformation characterization of superplastic AA7475 alloy

AA7475 alloy was deformed up to 25% elongation in INSTRON at 788K. The grain boundary sliding due to this superplastic deformation was measured by Scanning Electron Microscope. The microstructure and texture development due to this deformation at elevated temperature was analyzed from the Orientation Image Microstructures i.e. the Electron Back Scattered Diffraction Image. The Orientation Image Microstructures revealed that superplastic deformation was associated with recovery and recrystallization in-situ process.

Spatial correlation in grain misorientation distribution

Grain misorientation was studied in relation to the nearest neighbor's mutual distance using electron back-scattered diffraction measurements. The misorientation correlation function was defined as the probability density for the occurrence of a certain misorientation between pairs of grains separated by a certain distance. Scale-invariant spatial correlation between neighbor grains was manifested by a power law dependence of the preferred misorientation vs. inter-granular distance in various materials after diverse strain paths. The obtained negative scaling exponents were in the range of -2 +/- 0.3 for high-angle grain boundaries. The exponent decreased in the presence of low-angle grain boundaries or dynamic recrystallization, indicating faster decay of correlations. The correlations vanished in annealed materials. The results were interpreted in terms of lattice incompatibility and continuity conditions at the interface between neighboring grains. Grain-size effects on texture development, as well as the implications of such spatial correlations on texture modeling, were discussed.

Cost-effective wear and oxidation resistant electrodeposited Ni-pumice coating

In the search for newer distributed phases that can be used in Ni-composite coatings, inexpensive and naturally available pumice has been identified as a potential candidate material. The composition of the pumice mineral as determined by Rietveld analysis shows the presence of corundum, quartz, mulllite, moganite and coesite phases. Pumice stone is crushed, ball-milled, dried and dispersed in a nickel sulfamate bath and Ni-pumice coatings are electrodeposited at different current densities and magnetic agitation speeds. Pumice particles are uniformly incorporated in the nickel matrix and Ni-pumice composite coatings with microhardness as high as 540 HK are obtained at the lowest applied current density. In the electrodeposited Ni-pumice coatings, the grain size of Ni increases with the applied current density. The overall intensity of texture development is slightly stronger for the Ni-pumice composite coating compared to plain Ni coating and the texture evolution is possibly not the strongest deciding factor for the enhanced properties of Ni-pumice coatings. The wear and oxidation resistances of Ni-pumice coating are commensurate with that of Ni-SiC coating electrodeposited under similar conditions. (C) 2014 Elsevier B.V. All rights reserved.

Asymmetric rolling of 5182 aluminium alloy and interstitial free steel sheets

This Ph.D. research focuses on asymmetric rolling (ASR), as an alternative method for improving mechanical responses of aluminium-magnesium alloy and interstitial free (IF) steel regarding industrial requirements. Aluminium alloys are attractive materials in various industries due to their appropriate properties such as low density and corrosion resistance; however, their low formability has limited their applications. As formability of aluminium alloys can be improved through texture development, part of this dissertation is dedicated to producing the desired crystallographic texture with the ASR process. Two types of ASR (i.e. reverse and continuous asymmetric rolling) were investigated. The impact of shear deformation imposed by ASR processes on developing the desirable texture and consequently on mechanical behaviours was observed. The developed shear texture increased the normal and also planar anisotropy. Texture evolution during plastic deformation as well as induced mechanical behaviour were simulated using the “self-consistent” and Taylor models. Interstitial free (IF) steel was the second material selected in this dissertation. Since IF steel is one of the most often used materials in automotive industries it was chosen to investigate the effect of shear deformation through ASR on its properties. Two types of reverse and continuous asymmetric rolling were carried out to deform IF steel sheets. The results of optical microscopy and atomic force microscopy observations showed no significant difference between the grains’ morphology of asymmetric and conventionally rolled samples, whereas the obtained results of transmission electron microscopy indicated that fine and equiaxed dislocation cells were formed through the asymmetric rolling process. This structure is due to imposed shear deformation during the ASR process. Furthermore, the mechanical behaviour of deformed and annealed sheets was evaluated through uniaxial tensile tests. Results showed that at low thickness reductions (18%) the asymmetric rolled sample presented higher stress than that of the conventionally rolled sheet; while for higher thickness reductions (60%) the trend was reversed. The texture analyses indicated that intense rolling texture components which developed through 60% thickness reduction of conventional rolling cause a relatively higher stress; on the contrary the fine structure resulting from ASR appears to be the source of higher stress observed after pre-deformation of 18%.

Electromechanical properties of engineered lead free potassium sodium niobate based materials

K0.5Na0.5NbO3 (KNN), is the most promising lead free material for substituting lead zirconate titanate (PZT) which is still the market leader used for sensors and actuators. To make KNN a real competitor, it is necessary to understand and to improve its properties. This goal is pursued in the present work via different approaches aiming to study KNN intrinsic properties and then to identify appropriate strategies like doping and texturing for designing better KNN materials for an intended application. Hence, polycrystalline KNN ceramics (undoped, non-stoichiometric; NST and doped), high-quality KNN single crystals and textured KNN based ceramics were successfully synthesized and characterized in this work. Polycrystalline undoped, non-stoichiometric (NST) and Mn doped KNN ceramics were prepared by conventional ceramic processing. Structure, microstructure and electrical properties were measured. It was observed that the window for mono-phasic compositions was very narrow for both NST ceramics and Mn doped ceramics. For NST ceramics the variation of A/B ratio influenced the polarization (P-E) hysteresis loop and better piezoelectric and dielectric responses could be found for small stoichiometry deviations (A/B = 0.97). Regarding Mn doping, as compared to undoped KNN which showed leaky polarization (P-E) hysteresis loops, B-site Mn doped ceramics showed a well saturated, less-leaky hysteresis loop and a significant properties improvement. Impedance spectroscopy was used to assess the role of Mn and a relation between charge transport – defects and ferroelectric response in K0.5Na0.5NbO3 (KNN) and Mn doped KNN ceramics could be established. At room temperature the conduction in KNN which is associated with holes transport is suppressed by Mn doping. Hence Mn addition increases the resistivity of the ceramic, which proved to be very helpful for improving the saturation of the P-E loop. At high temperatures the conduction is dominated by the motion of ionized oxygen vacancies whose concentration increases with Mn doping. Single crystals of potassium sodium niobate (KNN) were grown by a modified high temperature flux method. A boron-modified flux was used to obtain the crystals at a relatively low temperature. XRD, EDS and ICP analysis proved the chemical and crystallographic quality of the crystals. The grown KNN crystals exhibit higher dielectric permittivity (29,100) at the tetragonal-to-cubic phase transition temperature, higher remnant polarization (19.4 μC/cm2) and piezoelectric coefficient (160 pC/N) when compared with the standard KNN ceramics. KNN single crystals domain structure was characterized for the first time by piezoforce response microscopy. It could be observed that <001> - oriented potassium sodium niobate (KNN) single crystals reveal a long range ordered domain pattern of parallel 180° domains with zig-zag 90° domains. From the comparison of KNN Single crystals to ceramics, It is argued that the presence in KNN single crystal (and absence in KNN ceramics) of such a long range order specific domain pattern that is its fingerprint accounts for the improved properties of single crystals. These results have broad implications for the expanded use of KNN materials, by establishing a relation between the domain patterns and the dielectric and ferroelectric response of single crystals and ceramics and by indicating ways of achieving maximised properties in KNN materials. Polarized Raman analysis of ferroelectric potassium sodium niobate (K0.5Na0.5)NbO3 (KNN) single crystals was performed. For the first time, an evidence is provided that supports the assignment of KNN single crystals structure to the monoclinic symmetry at room temperature. Intensities of A′, A″ and mixed A′+A″ phonons have been theoretically calculated and compared with the experimental data in dependence of crystal rotation, which allowed the precise determination of the Raman tensor coefficients for (non-leaking) modes in monoclinic KNN. In relation to the previous literature, this study clarifies that assigning monoclinic phase is more suitable than the orthorhombic one. In addition, this study is the basis for non-destructive assessments of domain distribution by Raman spectroscopy in KNN-based lead-free ferroelectrics with complex structures. Searching a deeper understanding of the electrical behaviour of both KNN single crystal and polycrystalline materials for the sake of designing optimized KNN materials, a comparative study at the level of charge transport and point defects was carried out by impedance spectroscopy. KNN single crystals showed lower conductivity than polycrystals from room temperature up to 200 ºC, but above this temperature polycrystalline KNN displays lower conductivity. The low temperature (T < 200 ºC) behaviour reflects the different processing conditions of both ceramics and single crystals, which account for less defects prone to charge transport in the case of single crystals. As temperature increases (T > 200 ºC) single crystals become more conductive than polycrystalline samples, in which grain boundaries act as barriers to charge transport. For even higher temperatures the conductivity difference between both is increased due to the contribution of ionic conduction in single crystals. Indeed the values of activation energy calculated to the high temperature range (T > 300 ºC) were 1.60 and 0.97 eV, confirming the charge transport due to ionic conduction and ionized oxygen vacancies in single crystals and polycrystalline KNN, respectively. It is suggested that single crystals with low defects content and improved electromechanical properties could be a better choice for room temperature applications, though at high temperatures less conductive ceramics may be the choice, depending on the targeted use. Aiming at engineering the properties of KNN polycrystals towards the performance of single crystals, the preparation and properties study of (001) – oriented (K0.5Na0.5)0.98Li0.02NbO3 (KNNL) ceramics obtained by templated grain growth (TGG) using KNN single crystals as templates was undertaken. The choice of KNN single crystals templates is related with their better properties and to their unique domain structure which were envisaged as a tool for templating better properties in KNN ceramics too. X-ray diffraction analysis revealed for the templated ceramics a monoclinic structure at room temperature and a Lotgering factor (f) of 40% which confirmed texture development. These textured ceramics exhibit a long range ordered domain pattern consisting of 90º and 180º domains, similar to the one observed in the single crystals. Enhanced dielectric (13017 at TC), ferroelectric (2Pr = 42.8 μC/cm2) and piezoelectric (d33 = 280 pC/N) properties are observed for textured KNNL ceramics as compared to the randomly oriented ones. This behaviour is suggested to be due to the long range ordered domain patterns observed in the textured ceramics. The obtained results as compared with the data previously reported on texture KNN based ceramics confirm that superior properties were found due to ordered repeated domain pattern. This study provides an useful approach towards properties improvement of KNN-based piezoelectric ceramics. Overall, the present results bring a significant contribution to the pool of knowledge on the properties of sodium potassium niobate materials: a relation between the domain patterns and di-, ferro-, and piezo-electric response of single crystals and ceramics was demonstrated and ways of engineering maximised properties in KNN materials, for example by texturing were established. This contribution is envisaged to have broad implications for the expanded use of KNN over the alternative lead-based materials.

Modelling the combined effect of grain size and grain shape on plastic anisotropy of metals

Within each columnar grain of a metallic film, the resistance to dislocation glide varies in function of the orientation of the slip plane with regard to the grain long axis. Plastic slip is impeded across grain boundaries and this contributes to the anisotropy of the overall mechanical response. A simplified (Taylor-type) crystal plasticity model is proposed that accounts for such effect of grain shape on the slip system selection. Assuming that dislocation density gradients are normal to the grain boundaries, backstresses developed at the onset of plasticity are estimated based on two definitions of the effective grain boundary spacing ‘‘seen’’ by individual slip systems. The first one reduces to the mean area-to-perimeter ratio of cross-sections of the grain cut parallel to the slip plane. Closed-form expressions of the average backstresses developed inside grains with spheroidal shapes are introduced in the crystal hardening law. The model reproduces the very high plastic anisotropy of electro-deposited pure iron with a strong c-fiber and a refined columnar grain structure [Yoshinaga, N., Sugiura, N., Hiwatashi, S., Ushioda, K., Kada, O., 2008. Deep drawability of electro-deposited pure iron having an extremely sharp h111i//ND texture. ISIJ Int. 48, 667–670]. It also provides valid estimates of the texture development and the influence of grain size on the yield strength.

Deformation behaviour of a commercial pure titanium alloy during hot compression testing

The flow curve behaviour and microstructure evolution of commercially pure titanium (CP-Ti) through uniaxial hot compression was investigated at 850 °C and a strain rate of 0.1/s. Electron back scattered diffraction (EBSD) was employed to characterize the microstructure and crystallographic texture development for different thermomechanical conditions. The stress-strain curves of CP-Ti alloy under hot compression displayed a typical flow behaviour of metals undergoing dynamic recrystallization (DRX), which resulted in grain refinement. The critical strain for the onset of DRX was 0.13 using the double differentiation analysis technique. It was also revealed that the texture was markably altered during hot deformation. © (2014) Trans Tech Publications, Switzerland.

A double inclusion homogenization scheme for polycrystals with hierarchal topologies: Application to twinning in Mg alloys

The present work introduces a double inclusion elasto-plastic self-consistent (DI-EPSC) scheme for topologies in which crystals can contain subdomains (i.e. twins, etc.). The approach yields a direct coupling between the mechanical response of grains and their subdomains via a concentration relationship on mean fields derived from both the Eshelby and the Tanaka-Mori properties. The latent effect caused by twinning on the mechanical response is observed on both initially extruded and non-textured Mg alloys. For twinned grains, it is shown that deformation system activities and plastic strain distributions within twins drastically depend on the interaction with parent domains. Moreover, a quantitative study on the coupled influence of secondary slip activities on the material response is proposed. © 2014 Published by Elsevier Ltd.