Ingenieurwissenschaften und zugeordnete Tätigkeiten
Filtern
Erscheinungsjahr
Dokumenttyp
Schlagworte
- Electron backscatter diffraction (25)
- EBSD (20)
- SEM (9)
- Pattern matching (6)
- Phase identification (6)
- Simulation (6)
- Orientation relationship (5)
- Steel (5)
- Crystal orientation (4)
- EDX (4)
Organisationseinheit der BAM
- 5 Werkstofftechnik (36)
- 5.1 Mikrostruktur Design und Degradation (33)
- 9 Komponentensicherheit (4)
- 5.2 Metallische Hochtemperaturwerkstoffe (3)
- 5.5 Materialmodellierung (3)
- 9.0 Abteilungsleitung und andere (2)
- 1 Analytische Chemie; Referenzmaterialien (1)
- 1.4 Prozessanalytik (1)
- 5.4 Multimateriale Fertigungsprozesse (1)
- 6 Materialchemie (1)
- 6.1 Oberflächen- und Dünnschichtanalyse (1)
- 8 Zerstörungsfreie Prüfung (1)
- 8.5 Röntgenbildgebung (1)
- 9.3 Schweißtechnische Fertigungsverfahren (1)
- 9.5 Tribologie und Verschleißschutz (1)
Paper des Monats
- ja (1)
Eingeladener Vortrag
- nein (6)
Методом рентгеноструктурного анализа в интервале температур 18—1150 °С определены температурные зависимости периодов кристаллических решеток γ- и γ'-фаз, их размерно-го несоответствия (мисфит) и объемной доли γ'-фазы экспериментального монокристал-лического жаропрочного никелевого сплава. Определены диапазоны температур, в которых происходят интенсивные изменения структурно-фазовых характеристик исследованного сплава.
During the energy transformation from fossil fuels to renewable energy sources, the use of hydrogen as fuel and energy storage can play a key role. This presents new challenges to industry and the scientific community alike. The storage and transport of hydrogen, which is nowadays mainly realized by austenitic stainless steels, remains problematic, which is due to the degradation of mechanical properties and the possibility of phase transformation by hydrogen diffusion and accumulation. The development of materials and technologies requires a fundamental understanding of these degradation processes. Therefore, studying the behavior of hydrogen in austenitic steel contributes to an understanding of the damage processes, which is crucial for both life assessment and safe use of components in industry and transportation. As one of the few tools that is capable of depicting the distribution of hydrogen in steels, time-of-flight secondary ion mass spectrometry was conducted after electrochemical charging. To obtain further information about the structural composition and cracking behavior, electron-backscattered diffraction and scanning electron microscopy were performed. Gathered data of chemical composition and topography were treated employing data fusion, thus creating a comprehensive portrait of hydrogen-induced effects in the austenite grade AISI 304L. Specimens were electrochemically charged with deuterium instead of hydrogen. This arises from the difficulties to distinguish between artificially charged hydrogen and traces existing in the material or the rest gas in the analysis chamber. Similar diffusion and permeation behavior, as well as solubility, allow nonetheless to draw conclusions from the experiments.
A band width determination using the first derivative of the band profile systematically underestimates the true Bragg angle. Corrections are proposed to compensate for the resulting offset Δa/a of the mean lattice parameters derived from as many Kikuchi band widths as possible. For dynamically simulated Kikuchi patterns, Δa/a can reach up to 8% for phases with a high mean atomic number Z, whereas for much more common low-Z materials the offset decreases linearly. A predicted offset Δa/a = f(Z) is therefore proposed, which also includes the unit-cell volume and thus takes into account the packing density of the scatterers in the material. Since Z is not always available for unknown phases, its substitution by Zmax, i.e. the atomic number of the heaviest element in the compound, is still acceptable for an approximate correction. For simulated Kikuchi patterns the offset-corrected lattice parameter deviation is Δa/a < 1.5%. The lattice parameter ratios, and the angles α, β and γ between the basis vectors, are not affected at all.1.5%. The lattice parameter ratios, and the angles , and between the basis vectors, are not affected at all.
The derivation of a crystal structure and its phase-specific parameters from a single wide-angle backscattered Kikuchi diffraction pattern requires reliable extraction of the Bragg angles. By means of the first derivative of the lattice profile, an attempt is made to determine fully automatically and reproducibly the band widths in simulated Kikuchi patterns. Even under such ideal conditions (projection centre, wavelength and lattice plane traces are perfectly known), this leads to a lattice parameter distribution whose mean shows a linear offset that correlates with the mean atomic number Z of the pattern-forming phase. The consideration of as many Kikuchi bands as possible reduces the errors that typically occur if only a single band is analysed. On the other hand, the width of the resulting distribution is such that higher image resolution of diffraction patterns, employing longer wavelengths to produce wider bands or the use of higher interference orders is less advantageous than commonly assumed.
Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird.
Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert.
Gold and platinum-group-metals (PGM) are cycled through Earth's environments by interwoven geological, physical, chemical and biological processes leading to the trans/neoformation of metallic particles in placers.
The placer deposit at Corrego Bom Successo (CBS, Brazil) is one of the few localities worldwide containing secondary gold- and PGM-particles. Placer gold consists of detrital particles from nearby hydrothermal deposits that were transformed in the surface environment. Processes that have affected these particles include shortdistance transport, chemical de-alloying of the primary Gold silver, and (bio)geochemical dissolution/reprecipitation of Gold leading to the formation of pure, secondary gold and the Dispersion of gold nanoparticles. The latter processes are likely mediated by non-living organic matter (OM) and bacterial biofilms residing on the particles. The biofilms are largely composed of metallophillic β- and γ-Proteobacteria. Abundant mobile gold and platinum nanoparticles were detected in surface waters, suggesting similar mobilities of these metals. Earlier hydrothermal processes have led to the formation of coarsely-crystalline, arborescent dendritic potarite (PdHg). On potarite surfaces, biogeochemical processes have then led to the formation of platinum- and palladium-rich micro-crystalline layers, which make up the botryoidal platinum palladium aggregates. Subsequently potarite was dissolved from the core of many aggregates leaving voids now often filled by secondary anatase (TiO2) containing biophilic elements. The presence of fungal structures associated with the anatase suggests that fungi may have contributed to ist formation. For the first time a primary magmatic PGM-particle comprising a mono-crystalline platinum palladium-alloy with platinum iridium osmium inclusions was described from this locality, finally defining a possible primary source for the PGM mineralisation. In conclusion, the formation of modern-day placer gold- and PGM-particles at CBS began 100s ofmillions of years ago bymagmatic and hydrothermal processes. These provided the metal sources for more recent biogeochemical cycling of PGEs and gold that led to the trans/neoformation of gold- and PGM-particles.
Signal optimization for transmission Kikuchi diffraction (TKD) measurements in the scanning electron microscope is investigated by a comparison of different sample holder designs. An optimized design is presented, which uses a metal shield to efficiently trap the electron beam after transmission through the sample. For comparison, a second holder configuration allows a significant number of the transmitted electrons to scatter back from the surface of the sample holder onto the diffraction camera screen. It is shown that the secondary interaction with the sample holder leads to a significant increase in the background level, as well as to additional noise in the final Kikuchi diffraction signal. The clean TKD signal of the optimized holder design with reduced background scattering makes it possible to use small signal changes in the range of 2% of the camera full dynamic range. As is shown by an analysis of the power spectrum, the signal-to-noise ratio in the processed Kikuchi diffraction patterns is improved by an order of magnitude. As a result, the optimized design allows an increase in pattern signal to noise ratio which may lead to increase in measurement speed and indexing reliability.
In the present work, the influence of deuterium on the microstructure of a duplex stainless steel type EN 1.4462 has been characterized by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) supported by scanning electron microscopy (SEM), focused ion beam (FIB), electron back scattered diffraction(EBSD) and energy dispersive x-ray (EDX) investigations. Characterization has been carried out before and after electrochemical charging with deuterium which has been used as a tracer, due to its similar behavior to hydrogen in the steel microstructure. In a first approach, the distribution of the deuterium occurring at temperatures above 58 °C has been visualized. Further it turned out that sub-surface micro blisters are formed in the ferrite-austenite interface, followed by the formation of needle shaped plates and subsequent cracking at the ferrite surface. In the austenite phase, parallel cracking alongside twins and hexagonal close packed (martensitic) regions has been observed. In both phases and even in the apparent interface, cracking has been associated with high deuterium concentrations, as compared to the surrounding undamaged microstructure. Sub-surface blistering in the ferrite has to be attributed to the accumulation and recombination of deuterium at the ferrite-austenite interface underneath the respective ferrite grains and after fast diffusing through this phase. Generally, the present application of chemometric imaging and structural analyses allows characterization of hydrogen assisted degradation at a sub-micron lateral resolution.
The thermal stability of the microstructure of a heat-resistant cobalt alloy, which consists of a γ solid solution strengthened with γ'-phase precipitates, has been studied. The temperature behavior of the dissolution of the hardening γ' phase and the kinetics of its coarsening at 700 and 800°C have been determined. It is found that, during prolonged annealing at 800°C, the γ' → β phase transformation occurs.
The work focuses on the potential of structural and chemical examinations by scanning electron microscopy based methods for archaeometric studies on ceramics. Achieved by a single preparation technique (polished block sections), the feasibility and benefits of electron backscatter diffraction are demonstrated as case studies using polychrome examples of pre-Columbian pottery (Wari, Moche and Cajamarca). Elemental and phase maps allow for separate consideration of clay and temper. Identification of mineral phases and intergrowths of temper particles provide information for clarifying clay procurement and firing techniques with respect to local versus non-local pottery to enlighten trade relations, technological transfer and shared heritage of pre-Columbian cultures.
X-ray stress analysis on crystalline materials is based on the determination of elastic lattice strains. The strains described by the shift of peak positions are converted to stresses by the means of theory of elasticity. The development of the sin2ψ-method of X-ray stress analysis introduced an enormous progress in X-ray stress analysis during the last decades. This report outlines some important elements of X-ray physics and fundamentals of theory of elasticity. The Standard measuring procedure are described and special experimental differences to the common powder diffractometry are outlined.
During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite.
The advent of simultaneous energy dispersive X-ray spectroscopy (EDS) data collection has vastly improved the phase separation capabilities for electron backscatter diffraction (EBSD) mapping. A major problem remains, however, in distinguishing between multiple cubic phases in a specimen, especially when the compositions of the phases are similar or their particle sizes are small because the EDS interaction volume is much larger than that of EBSD, and the EDS spectra collected during spatial mapping are generally noisy due to time limitations and the need to minimize sample drift. The backscatter electron (BSE) signal is very sensitive to the local composition due to its atomic number (Z) dependence. BSE imaging is investigated as a complimentary tool to EDS to assist phase segmentation and identification in EBSD through examination of specimens of meteorite, Cu dross, and steel oxidation layers. The results demonstrate that the simultaneous acquisition of EBSD patterns, EDS spectra, and the BSE signal can provide new potential for advancing multiphase material characterization in the scanning electron microscope.
The locally varying tetragonality in martensite grains of a high-carbon steel (1.2 mass percent C) was resolved by electron backscatter diffraction (EBSD) with a spatial resolution in the order of 100 nm. Compared to spatially integrating X-ray diffraction, which yielded an average tetragonality fo c/a=1.05, the EBSD measurements in the scanning electron microscope allowed to image a local variation of the lattice papameter ration c/a in the range of 1.02 ≤ c/a ≤ 1.07. The local variation of tetragonality is confirmed by two different EBSD data analysis approaches based on the fitting of simulated to experimental EBSD patterns. The resulting EBSD-based tetragonality maps are pointing to a complex interaction of carbon concentration and local lattice distortions during the formation process of martensitic structures.
Synthesis of Molybdenum and Niobium Mono- and Binary Silicides by the Method of SHS-Metallurgy
(2016)
The process of self-propagating high-temperature synthesis of the Mo–Nb–Si silicides from the powder mixtures has been investigated. Based on performed experiments, the composition of powder mixtures as well as technological parameters are proposed which provide the synthesis of monosilicides MoSi₂, NbSi₂, and binary silicides Mo₁-хNbxSi₂ with different ratios of Nb/Mo by adding different contents of MoO₃ and Nb₂O₅. Microstructure and phase compositions of the obtained silicide ingots are characterized by scanning electron microscopy, electron probe microanalysis, X-ray diffraction, and backscatter electron diffraction.
Kirkendall porosity that forms during interdiffusion in a diffusion couple of nickel-base superalloy CMSX-10 with pure nickel is investigated. The diffusion experiments are conducted at a temperature of 1250 °C, where the strengthening ƴ'-phase ist partially dissolved. The porosity is studied by X-ray sub-μ tomography with a spatial resolution of about 0.35³ μm³ at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France. It is found that depending on the distance from the interface the Kirkendall pores take different shapes: octahedral, rounded pyramidal, drop shaped, dendritic, pear shaped, and joint shapes. Such a variety of pore morphologies indicates a complex multistage process of porosity nucleation and growth under vacancy supersaturation of different degrees. The experimental findings are interpreted on the basis of the results of diffusion modeling. It is shown that the kinetics of porosity growth is essentially influenced by the dissolution of the ƴ'-phase.
A new technique for investigation of interfacial dislocations in nickel-base superalloys by scanning electron microscopy is presented. At high temperatures the pressure of interfacial dislocations against the gamma/gamma'-interface causes grooves. This 'fingerprint of the dislocation network' is visualized by deep selective etching, which removes the gamma'-phase down to the gamma/gamma'-interface. Compared with transmission electron microscopy, the proposed method has important advantages: observation of large sample areas, no superposition of dislocations lying in different specimen depths, possibility of three-dimensional view of dislocation configurations, information about the dislocation mobility, reduced time for preparation and visualization. The method can be applied for multiphase materials where the interface is grooved by interfacial dislocations.
Roaldite – Fe4N – has been identified in the São Julião de Moreira iron meteorite using electron backscatter diffraction (EBSD) and simultaneously acquired energy-dispersive x-ray spectroscopy (EDS). Mean-periodic-number images derived from raw EBSD patterns confirm this phase by an even higher spatial resolution compared to EDS.
Roaldite appears in the form of systematically and repetitively aligned plates. Despite the locally heavy plastic deformation, it is shown that the origin of the oriented precipitation of roaldite is linked to the orientation of the kamacite matrix. Roaldite can be considered to be precipitated from kamacite using an inverse Kurdjumov-Sachs (K-S) or Nishiyama-Wassermann (N-W) orientation relationship. A more accurate discrimination is impossible due to the accumulated shock deformation, which blurs the local reference orientation of kamacite. The habit plane of roaldite is found to be {112}R, which is most likely parallel to {120}K of kamacite. Some of the roaldite plates contain two orientation variants which repeatedly alternate. Their misorientation angle is about 12°.