TEM Orientation Mapping Research Articles

Martensitic transformation induced by cooling NiTi wire under various tensile stresses: Martensite variant microstructures, textures, recoverable strains and plastic strains

Whenever the forward and/or reverse B2 cubic to B19’ monoclinic martensitic transformation in NiTi shape memory alloy wire proceeds under external stress above certain threshold, it generates incremental plastic strains which accumulate during thermomechanical cyclic loading and lead to functional fatigue preventing many promising engineering applications from realization. In this work, unique thermomechanical loading experiments were performed on NiTi shape memory wire with the aim to reveal the mechanism by which the forward martensitic transformation upon cooling under external stress generates plastic strain. Recoverable transformation strains and plastic strains generated by the forward transformation on cooling under various tensile stresses were evaluated, martensite variant microstructures in grains were reconstructed by nanoscale orientation mapping in TEM, martensite textures after cooling at room temperature were evaluated by in-situ synchrotron x-ray diffraction and permanent dislocation defects in martensite were analyzed by TEM. Based on the obtained experimental evidence, it is proposed that the forward martensitic transformation on cooling under stress proceeds via habit plane interfaces between austenite and second order laminate of (001) compound twins in martensite. Depending on the magnitude of the applied stress, the induced martensite reorients, partially detwins and deforms plastically via [100](001) dislocation slip in martensite in extent permitted by the requirement for compatible deformation of grains in nanocrystalline NiTi wire via a single deformation system. During the forward MT upon cooling under highest stresses 600 MPa, the martensite deforms via kwinking deformation enabling generation of large plastic strains 8 %.

Stress induced martensitic transformation in NiTi at elevated temperatures: Martensite variant microstructures, recoverable strains and plastic strains

To shed light on the origin of the loss of functional properties of NiTi with temperature increasing above 100 °C, we have investigated stress induced martensitic transformations in nanocrystalline NiTi shape memory wire by thermomechanical tensile testing supplemented with post-mortem reconstruction of martensite variant microstructures in grains by nanoscale orientation mapping in TEM. The stress induced martensitic transformation generating recoverable transformation strain as well as plastic strain is not completed at the end of the upper stress plateau. The higher is the test temperature, the larger is the volume fraction of retained austenite as well as the plastic strain. The martensite variant microstructures in NiTi wire deformed up to the end of the stress plateau at 120 °C contain partially detwinned single domains of (001) compound twin laminate filling entire grains. It is proposed that the stress induced martensitic transformation proceeds via habit plane interface between austenite and second order laminate of (001) compound twins and that the martensite promptly reorients and deforms plastically by dislocation glide in the [100](001) slip system. When the wire is loaded further beyond the end of the stress plateau, the stress induced martensitic transformation continues and the martensite deforms plastically. It is concluded that the observed gradual loss of superelastic functionality of NiTi with increasing temperature does not originate from the plastic deformation of austenite, as widely assumed in the literature, but that it derives from the loss of resistance of the stress induced martensite to the plastic deformation under increasing stress.

Grain boundary-mediated plasticity in aluminum films unraveled by a statistical approach combining nano-DIC and ACOM-TEM

Nanomechanical on-chip testing is combined with nanoscale in situ digital image correlation and automated crystal orientation mapping in TEM to deliver novel statistically representative quantitative data about the deformation mechanisms in nanocrystalline aluminum films. The films are very ductile, with a rare stable multiple necking process with local strains reaching up to 0.45 and macroscopic elongation up to 0.17. The strain fields with resolution below 100 nm are related to the underlying microstructure and crystallographic orientation maps. This reveals nanoscopic shear bands forming preferentially along GB with high misorientations, tilted at +/− 45° with respect to loading direction. The analysis of these data prove that the strong strain delocalization process is promoted by GB migration and grain rotation, leading to large strain rate sensitivity. The distribution of misorientation angles between grains evolve during deformation. The GBs with misorientation between 20° and 40°, which are the GBs with highest energy, involve the largest strains.

Effect of hydriding induced defects on the small-scale plasticity mechanisms in nanocrystalline palladium thin films

Nanoindentation tests performed on nanocrystalline palladium films subjected to hydriding/dehydriding cycles demonstrate a significant softening when compared to the as-received material. The origin of this softening is unraveled by combining in situ TEM nanomechanical testing with automated crystal orientation mapping in TEM and high resolution TEM. The softening is attributed to the presence of a high density of stacking faults and of Shockley partial dislocations after hydrogen loading. The hydrogen induced defects affect the elementary plasticity mechanisms and the mechanical response by acting as preferential sites for twinning/detwinning during deformation. These results are analyzed and compared to previous experimental and simulation works in the literature. This study provides new insights into the effect of hydrogen on the atomistic deformation and cracking mechanisms as well as on the mechanical properties of nanocrystalline thin films and membranes.

Microstructural investigations of materials after severe plastic deformation by means of orientations mapping in TEM and SEM

Qualitative and quantitative microstructure descriptions of crystalline materials are crucial for characterization and better understanding of the mechanisms of deformation and recrystallization processes. In this study orientation mapping in SEM and TEM were applied to investigations of materials after plastic deformations by means of cold rolling and hydrostatic extrusion (HE) methods. Statistical analysis of local orientation, texture and grain boundary characterization were done for chosen materials of different symmetry like cubic aluminium and hexagonal titanium with high resolution capability down to a few square nanometres. It was proved that TEM / Orientation Mapping (OM) investigations can be successfully applied for complementary analysis to conventional SEM/EBSD.

NiTi Shape Memory Marformed Alloy Studied by Electron Beam Precession TEM Orientation Mapping Method

NiTi Shape Memory Marformed Alloy Studied by Electron Beam Precession TEM Orientation Mapping Method

Optimization of Automated Crystal Orientation Mapping in a TEM for Ni4Ti3 Precipitation in All-Round SMA

Automated crystal orientation and phase mapping in TEM are applied to the quantification of Ni4Ti3 precipitates in Ni–Ti shape memory alloys which will be used for the implantation of artificial sphincters operating using the all-round shape memory effect. This paper focuses on the optimization process of the technique to obtain best values for all major parameters in the acquisition of electron diffraction patterns as well as template generation. With the obtained settings, vast statistical data on nano- and microstructures essential to the operation of these shape memory devices become available.

Grain rotations in ultrafine-grained aluminum films studied using in situ TEM straining with automated crystal orientation mapping

In situ TEM straining allows probing deformation mechanisms of ultrafine-grained and nanocrystalline metals. While obtaining statistically meaningful information about microstructural changes using conventional bright-field/dark-field imaging or diffraction is time consuming, automated crystal orientation mapping in TEM (ACOM-TEM) enables tracking orientation changes of hundreds of grains simultaneously. We use this technique to uncover extensive grain rotations during in situ tensile deformation of a freestanding, ultrafine-grained aluminum film (thickness 200nm, mean grain size 180nm). During loading, both the fraction of grains that undergo rotations and the magnitude of their rotations increase with strain. The rotations are partially or fully reversible in a significant fraction of grains during unloading, leading to notable inelastic strain recovery. More surprisingly, the direction of rotation remains unchanged for a small fraction of grains during unloading, despite a sharp reduction in the applied stress. The ACOM-TEM measurements also provide evidence of reversible and irreversible grain/twin boundary migrations in the film. These microstructural observations point to a highly inhomogeneous and constantly evolving stress distribution in the film during both loading and unloading.

Height-resolved quantification of microstructure and texture in polycrystalline thin films using TEM orientation mapping

A method is presented for the quantitative investigation of microstructure and texture evolution in polycrystalline thin films based on in-plane automated crystal orientation mapping in transmission electron microscopy, from the substrate up. To demonstrate the method we apply it to the example of low pressure metal–organic chemical vapor deposited ZnO layers. First, orientation mapping is applied to standard cross-section and plan-view transmission electron microscopy samples of films, illustrating how plan-view samples both reduce the occurrence of grain overlap that is detrimental to reliable orientation mapping and also improve sampling statistics compared to cross-sections. Motivated by this, orientation mapping has been combined with a double-wedge method for specimen preparation developed by Spiecker et al. (2007) [1], which creates a large area plan-view sample that traverses the film thickness. By measuring >10,000 grains in the film, the resulting data give access to grain size, orientation and misorientation distributions in function of height above the substrate within the film, which are, in turn, the inputs necessary for quantitative assessment of growth models and simulations. The orientation data are directly related to microstructural images, allowing correlation of orientations with in-plane and out-of-plane grain sizes and shapes.The spatial correlation of the entire data set gives insights into previously unnoticed growth mechanisms such as the presence of renucleation or preferred misorientations. Finally, the data set can be used to guide targeted, local studies by other transmission electron microscopy techniques. This is demonstrated by the site-specific application of nano-beam diffraction to validate the presence of coherent [21¯1¯0]/(011¯3) twin boundaries first suggested by the orientation mapping.

In-situ Straining Analysis by TEM Orientation Mapping (EBSD-like TEM) - Direct Imaging of Deformation Processes in Nanocrystalline Metals

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.

Recrystallization in Ultra-Fine Grain Structures of AA3104 Alloy Processed by ECAP and HPT

The objective of this study was to determine the effect of deformation mode on recrystallization behavior of severely deformed material. Commercial purity AA3104 aluminum alloy was deformed via high pressure torsion and equal channel angular pressing to different strains and then annealed to obtain the state of partial recrystallization. The microstructure and the crystallographic texture were analysed using scanning and transmission electron microscopes equipped with orientation measurement facilities. The nucleation of new grains was observed in bulk recrystallized samples and during in-situ recrystallization in the transmission microscope. Irrespective of the applied deformation mode, a large non-deformable second phase particles strongly influenced strengthening of the matrix through deformation zones around them. It is known that relatively high stored energy stimulates the nucleation of new grains during the recrystalization. In most of the observed cases, the growth of recrystallized grains occurred by the coalescence of neighboring subcells. This process usually led to nearly homogeneous equiaxed grains of similar size. The diameter of grains in the vicinity of large second phase particles was only occasionally significantly larger than the average grain size. Large grains were most often observed in places far from the particles. TEM orientation mapping from highly deformed zones around particles showed that orientations of new grains were not random and only strictly defined groups of orientations were observed.

Microstructural and Textural Aspects of Shear Banding in Plane Strain Deformed Fcc Metals

Periodic crystal lattice rotations within compact clusters of shear bands, developed in copper, have been characterized over a range of scales by optical microscopy, high resolution FEG-SEM-EBSD and TEM orientation mapping, to examine the role of local lattice re-orientation on slip propagation across pre-existing barriers to dislocation motion. Two different cases were analysed in detail. The single crystal analysis addresses the relation between the crystallographic microtexture and microstructure development due to the crystal anisotropy after a strain path change. All the changes in strain path directly lead to crystallite subdivisions and strain localization in the form of macroscopically visible bands of different morphology at the micro scale. The elongated cell substructure formed during primary straining was the source of anisotropy after changing deformation path. It is thought that the presence of this structure (here subcells) as barriers to dislocation motion is crucial for the occurrence of shear banding. The analysis of pure polycrystalline copper has been focused on the influence of local lattice re-orientations within particular grains on slip propagation across grain boundaries. The crystal lattice rotated in such a way that one of the {111} slip planes became nearly parallel to the direction of maximum shear (due to the actual state of anisotropy). A natural consequence of this rotation was the formation of a specific microtexture which facilitated slip propagation across grain boundaries.

Application of orientation imaging to the study of substructural development in cold deformed Al-0.3%Mn single crystal of {110} orientation

A systematic study of the deformation microstructures over 3 perpendicular surfaces was carried out in the present work in order to correlate better the substructure with slip patterns, initial and final crystal orientation, and the macroscopic coordinate system. The microstructure and texture evolution of high purity Al-0.3 wt% Mn alloy of initial near brass {110}<112> (or Bs) orientation, channel-die compressed to the strain level of 1.5, were studied by TEM (including TEM orientation mapping) and high-resolution FEG-SEM/EBSD techniques to observe crystal subdivision deformation patterns at the microscopic scale. The grain orientation dependent structures were analyzed in terms of active slip systems focussing on the crystallography of extended planar boundaries. It was concluded that the type of dislocation structure (one or two sets of microbands) in {110}<112> oriented crystallites, at moderate strains (< 1.5) depended strongly on the crystallographic grain orientation. In this non-ideal initial crystal orientation the applied deformation mode activates a double slip, of which one system predominates and leads to further rotation away from Bs. A general rotation combined with a wide orientation spread is observed after a strain up to 1.5. The microband boundary alignment corresponds very well to the traces of crystallographic {111} planes, on which most of the slip occurs.