Search Results (10)

In recent years, electron diffraction (ED) and structural imaging have undergone a major resurgence in the scientific community, driven by continuous advancements in transmission electron microscopy (TEM) instrumentation, such as Cs correctors, direct detection cameras and automation, and the development or expansion of analytical methods, such as cryo-EM, beam precession, 4D Scanning Electron Diffraction, 3D electron diffraction, 4D-STEM, and ptychography [...] Full article

In the Al-Fe binary system, the Al₁₃Fe₃ phase as well as the Al₁₃Fe₄ phase has similar icosahedral building blocks like those appearing in quasicrystals. Therefore, it is of vital importance to clarify the formation process of these two phases. Coexistence of the Al₁₃Fe₃ and Al₁₃Fe₄ phases was discovered from the educts obtained with a nominal atomic ratio of Al/Fe of 9:2 by high-pressure sintering for the first time. Firstly, single crystal X-ray diffraction (SXRD) combined with a scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (EDX) measurement capabilities were adopted to determine the detailed crystal structures of both phases, which were sharply refined with regard to Al₁₃Fe₃ and Al₁₃Fe₄. Secondly, the orientation relationship between Al₁₃Fe₃ and Al₁₃Fe₄ was directly deduced from the SXRD datasets and the coexistence structure model was consequently constructed. Finally, seven pairs of parallel atomic planes and their unique orientation relations were determined from the reconstructed reciprocal space precession images. In addition, the real space structure model of the intergrowth crystal along with one kind of interfacial atomic structure were constructed from the determined orientation relations between two phases. Full article

Although the Al₂Fe phase has similar decagonal-like atomic arrangements as that of the orthorhombic Al₅Fe₂ phase, no evidence for intergrowth samples of Al₂Fe and Al₅Fe₂ has been reported. In the present work, the co-existence of Al₂Fe and Al₅Fe₂ phases has been discovered from the educts obtained with a nominal atomic ratio of Al:Fe of 2:1 by arc melting. First, single-crystal X-ray diffraction (SXRD) as well as scanning electron microscope (SEM) equipped with energy-dispersive X-ray spectroscopy (EDX) measurements have been utilized to determine the exact crystal structures of both phases, which are refined to be Al_12.48Fe_6.52 and Al_5.72Fe₂, respectively. Second, the orientation relationship between Al₂Fe and Al₅Fe₂ has been directly deduced from the SXRD data sets, and the co-existence structure model has been constructed. Finally, four pairs of parallel atomic planes and their unique orientation relations have been determined from the reconstructed reciprocal-space precession images of (0kl), (h0l), and (hk0) layers. In addition, one kind of interface atomic structure model is constructed by the orientation relations between two phases, correspondingly. Full article

Cobalt-Rhenium (Co-Re)-based alloys are currently investigated as potential high-temperature materials with melting temperatures beyond those of nickel-based superalloys. Their attraction stems from the binary Co-Re phase diagram, exhibiting complete miscibility between Co and Re, whereby the melting temperature steadily increases with the Re-content. Thus, depending on the Re-content, one can tune the melting temperature between that of pure Co (1495 °C) and that of pure Re (3186 °C). Current investigations focus on Re-contents of about 15 at.%, which makes melting with standard equipment still feasible. In addition to solid solution strengthening due to the mixture of Co- and Re-atoms, particle strengthening by tantalum carbide (TaC) and titanium carbide (TiC) precipitates turned out to be promising in recent studies. Yet, it is currently unclear which of the two particle types is the best choice for high temperature applications nor has the strengthening mechanism associated with the monocarbide (MC)-precipitates been elucidated. To address these issues, we perform compression tests at ambient and elevated temperatures on the particle-free base material containing 15 at.% of rhenium (Re), 5 at.% of chromium (Cr) and cobalt (Co) as balance (Co-15Re-5Cr), as well as on TaC- and TiC-containing variants. Additionally, transmission electron microscopy is used to analyze the shape of the precipitates and their orientation relationship to the matrix. Based on these investigations, we show that TiC and TaC are equally suited for precipitation strengthening of Co-Re-based alloys and identify climb over the elongated particles as a rate controlling particle strengthening mechanism at elevated temperatures. Furthermore, we show that the Re-atoms are remarkably strong obstacles to dislocation motion, which are overcome by thermal activation at elevated temperatures. Full article

Accurate structure analysis of epitaxial perovskite thin films is a fundamental step towards the ability to tune their physical properties as desired. Precession-assisted electron diffraction tomography (PEDT) has proven to be an effective technique for performing ab initio structure solutions and refinements for this class of materials. As the film thickness or the region of interest (ROI) decrease in size, the capacity to collect PEDT data with smaller electron beams is a key parameter and ROI tracking becomes a major issue. To circumvent this problem, we considered here an alternative approach to acquiring data by combining PEDT with a scan over an area, extracting the intensities collected at different positions and using them to perform accurate structure refinements. As a proof of concept, a Scanning Precession Electron Tomography (SPET) experiment is performed on a 35 nm thick perovskite $PrV{O}_3$(PVO) film deposited on a $SrTi{O}_3$ (STO) substrate. This way, it was possible to detect small changes in the PVO structure along the film thickness, from the variation in unit cell parameters to atomic positions. We believe that SPET has the potential to become the standard procedure for the accurate structure analysis of ROIs as small as 10 nm. Full article

Understanding of the creep behavior Nb and Ta-rich γ-TiAl alloys plays a crucial role towards realization of their potential applications. The present article reports the evolution of microstructural features in the crept γ-TiAl-based Ti-5Al-8Nb-2Cr-0.2B and Ti-45Al-8Ta-0.2C-0.2B-0.2C alloys. Structural characterizations have been carried out using automated crystal orientation mapping (ACOM) along with precession electron diffraction (PED) in a transmission electron microscope, in conjunction with electron back-scattered diffraction (EBSD) in a scanning electron microscope (SEM) and transmission electron microscopy (TEM). Creep behavior of the fourth generation γ-TiAl-based alloys has been comparatively investigated under constant load tensile creep tests performed in the temperature range from 800–850 °C and applied stresses range of 125–200 MPa. It has been demonstrated that the ACOM with PED technique has accurate and reliable diffraction pattern recognition and higher spatial resolution, and supplements effectively the conventional EBSD technique for characterization of complex microstructural features evolved during creep of multiphase (γ + α₂ + β)-based TiAl alloys. The results show that the Nb and Ta additions have distinctly different effects on the microstructural instability and phase transformation during the creep deformation. The formation of the Ta-rich intermetallic phase (Ti₄Al₃Ta, the so-called τ phase) has been detected preferentially along the colony and the γ-α₂ interphase boundaries in the Ta-rich alloy, whilst its isomorph, Ti₄Al₃Nb intermetallic, has hardly been detected in the Nb-rich alloy. Implications of τ-phase formation and related microstructural instabilities have been discussed with respect to the creep behavior of the two alloys. Full article

ACOM/TEM is an automated electron diffraction pattern indexing tool that enables the structure, phase and crystallographic orientation of materials to be routinely determined. The software package, which is part of ACOM/TEM, has substantially evolved over the last fifteen years and has pioneered numerous additional functions with the constant objective of improving its capabilities to make the tremendous amount of information contained in the diffraction patterns easily available to the user. Initially devoted to the analysis of local crystallographic texture, and as an alternative to both X-ray pole figure measurement and EBSD accessories for scanning electron microscopes, it has rapidly proven itself effective to distinguish multiple different phases contained within a given sample, including amorphous phases. Different strategies were developed to bypass the inherent limitations of transmission electron diffraction patterns, such as 180° ambiguities or the complexity of patterns produced from overlapping grains. Post processing algorithms have also been developed to improve the angular resolution and to increase the computing rate. The present paper aims to review some of these facilities. On-going works on 3D reconstruction are also introduced. Full article

Interfaces such as grain boundaries (GBs) and heterointerfaces (HIs) are known to play a crucial role in structure-property relationships of polycrystalline materials. While several methods have been used to characterize such interfaces, advanced transmission electron microscopy (TEM) and scanning TEM (STEM) techniques have proven to be uniquely powerful tools, enabling quantification of atomic structure, electronic structure, chemistry, order/disorder, and point defect distributions below the atomic scale. This review focuses on recent progress in characterization of polycrystalline oxide interfaces using S/TEM techniques including imaging, analytical spectroscopies such as energy dispersive X-ray spectroscopy (EDXS) and electron energy-loss spectroscopy (EELS) and scanning diffraction methods such as precession electron nano diffraction (PEND) and 4D-STEM. First, a brief introduction to interfaces, GBs, HIs, and relevant techniques is given. Then, experimental studies which directly correlate GB/HI S/TEM characterization with measured properties of polycrystalline oxides are presented to both strengthen our understanding of these interfaces, and to demonstrate the instrumental capabilities available in the S/TEM. Finally, existing challenges and future development opportunities are discussed. In summary, this article is prepared as a guide for scientists and engineers interested in learning about, and/or using advanced S/TEM techniques to characterize interfaces in polycrystalline materials, particularly ceramic oxides. Full article

We report the first results of a combined focused ion beam and high-resolution transmission electron microscopy (FIB/HRTEM) investigation of zoned laurite (RuS₂)-erlichmanite (OS₂) in mantle-hosted chromitites. These platinum-group minerals form isolated inclusions (<50 µm across) within larger crystals of unaltered chromite form the Ojén ultramafic massif (southern Spain). High-magnification electron microscopy (HMEM), high angle-annular dark field (HAADF) and precession electron diffraction (PED) data revealed that microscale normal zoning in laurite consisting of Os-poor core and Os-rich rims observed by conventional micro-analytical techniques like field emission scanning electron microscope and electron microprobe analysis (FE-SEM and EPMA) exist at the nanoscale approach in single laurite crystals. At the nanoscale, Os poor cores consist of relatively homogenous pure laurite (RuS₂) lacking defects in the crystal lattice, whereas the Os-richer rim consists of homogenous laurite matrix hosting fringes (10–20 nm thickness) of almost pure erlichmanite (OsS₂). Core-to-rim microscale zoning in laurite reflects a nonequilibrium during laurite crystal growth, which hampered the intra-crystalline diffusion of Os. The origin of zoning in laurite is related to the formation of the chromitites in the Earth’s upper mantle but fast cooling of the chromite-laurite magmatic system associated to fast exhumation of the rocks would prevent the effective dissolution of Os in the laurite even at high temperatures (~1200 °C), allowing the formation/preservation of nanoscale domains of erlichmanite in laurite. Our observation highlights for the first time the importance of nanoscale studies for a better understanding of the genesis of platinum-group minerals in magmatic ore-forming systems. Full article

The mantle transition zone represents an important layer in the interior of the Earth that is characterized by phase transformations of olivine polymorphs. Constraining the rheology difference between wadsleyite and ringwoodite is important in determining the viscosity contrast at a depth of 520 km. In this study, we perform a post-mortem by transmission electron microscopy of a wadsleyite + ringwoodite aggregate, deformed at high-pressure and high-temperature, in a deformation-DIA apparatus. From orientation maps acquired by scanning precession electron diffraction, we calculate local misorientations and misorientation-gradients, which are used as a proxy of plastic strain. We show that at 17.3 GPa, 1700 K, the plastic responses of wadsleyite and ringwoodite are comparable, although recovery by subgrain boundary migration is more easily activated in wadsleyite. Full article