5 Werkstofftechnik
Filtern
Dokumenttyp
Sprache
- Englisch (354)
- Mehrsprachig (5)
- Deutsch (1)
- Russisch (1)
Referierte Publikation
- ja (361) (entfernen)
Schlagworte
- Additive manufacturing (21)
- EBSD (16)
- Additive Manufacturing (14)
- Microstructure (14)
- Corrosion (12)
- Residual stress (12)
- Transmission electron microscopy (12)
- Creep (11)
- Glass (9)
- Crystallization (8)
Organisationseinheit der BAM
- 5 Werkstofftechnik (361)
- 5.1 Mikrostruktur Design und Degradation (132)
- 5.2 Metallische Hochtemperaturwerkstoffe (67)
- 5.4 Multimateriale Fertigungsprozesse (63)
- 5.6 Glas (45)
- 5.5 Materialmodellierung (44)
- 5.0 Abteilungsleitung und andere (40)
- 9 Komponentensicherheit (38)
- 5.3 Polymere Verbundwerkstoffe (36)
- 8 Zerstörungsfreie Prüfung (36)
Paper des Monats
- ja (11)
We use pattern matching of experimental and dynamically simulated backscattered Kikuchi diffraction (BKD) patterns to increase the orientation precision of electron backscatter diffraction (EBSD) measurements. In order to quantify the improvement in orientation precision, we analyze the experimental distribution of the kernel average misorientation (KAM) angles. We find that for the same raw data, i.e. the same EBSD data acquisition time budget, the pattern matching approach improves the KAM resolution by an order of magnitude compared to orientation data delivered from the conventional Hough-transform based data analysis. This quantitative improvement enables us to interpret small orientation changes in plastically deformed materials which are hidden in noisy orientation data delivered from the reference EBSD system.
As an application example, we analyze a ferritic-martensitic steel (P92) sample before and after low-cycle fatigue (LCF) loading (±0.3% strain) at 620 °C. Whereas the low precision of the EBSD orientation data from the manufacturer software does not allow a reliable discrimination of the gradually changing microstructure, we find very clear systematic differences of the local microstructure after the pattern matching orientation refinement of the initial, raw pattern data. For the investigated P92 sample, the KAM-angle histograms are well described by two log-normal distributions indicating the already tempered and the remaining and mostly untempered martensite.
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°.
The Bravais lattices and their lattice parameters are blindly determined using electron backscatter diffraction (EBSD) patterns of materials with cubic or tetragonal crystal structures. Since the geometric relationships in a single EBSD pattern are overdetermined, the relative errors of determining the lattice parameters as well as the axial ratios are confined to about 0.7 ± 0.4% and 0.07 ± 0.03%, respectively, for ideal simulated EBSD patterns. The accuracy of the crystal orientation determination reaches about 0.06 ± 0.03°. With careful manual band detection, the accuracy of determining lattice parameters from experimental patterns can be as good as from simulated patterns, although the results from simulated patterns are often better than expermental patterns, which are lower quality and contain uncertain systematic errors. The reasonably high accuracy is obtained primarily because the detection of the diffracting-plane traces and zone axes is relatively accurate. The results here demonstrate that the developed procedure based on the EBSD technique presents a reliable tool for crystallographic characterization of the Bravais lattices of unknown phases.
Thin Sol-Gel Alumina Coating as Protection of a 9% Cr Steel Against Flue Gas Corrosion at 650 °C
(2018)
Samples of sol-gel alumina coated and uncoated P92 steel were exposed to flue gas at 650 °C for 300 h. As result of this treatment a 50 µm thick bi-layered oxide scale had formed on the surface of the uncoated sample. Below the scale a 40 µm thick inner oxidation zone was detected. In contrast, the porous, micron thick alumina coating enabled the formation of a chromium oxide scale with a thickness of some nanometers at the interface between steel substrate and coating. In this case high temperature corrosion of the steel was prevented so far.
Though Ni-base superalloys show a high oxidation and corrosion resistance, coatings could still improve these properties, especially if used at temperatures up to 1000 °C. Here, a coating was prepared by applying a boehmite-sol via dip-coating and a subsequent heat treatment at 600 °C for 30 minutes. To evaluate the coating, the oxidation behavior of bare and alumina coated Ni-base alloy Inconel 625 in air at 900 °C was studied for up to 2000 h. Electron microscopic studies of sample surfaces and cross-sections showed that (i) in the 3.5 µm – 6.3 mm thick scale formed on the bare alloy, Fe and Ni are located as fine precipitates at the grain boundaries of the chromia-rich scale, (ii) Ni and Ti are concentrated to a minor degree at the grain boundaries of the scale, too; and for the coated sample: (iii) the only 1.8 µm thick sol-gel alumina coating slows down the formation of chromia on the alloy surface and reduces the outward diffusion of the alloy constituents. The protective effect of the coating was evidenced by (i) diminished chromium diffusion at grain boundaries resulting in less pronounced string-like protrusions at the outer surface of the coated IN 625, (ii) formation of a Cr-enriched zone above the alloy surface which was thinner than the scale on the uncoated sample, (iii) no detectable Cr-depleted zone at the alloy surface, and (iv) a narrower zone of formation of Kirkendall pores.
Additive manufacturing of metals – and in particular building with laser-based powder bed fusion – is highly flexible and allows high-resolution features and feedstock savings. Meanwhile, though space stations in low Earth orbit are established, a set of visits to the Moon have been performed, and humankind can send out rovers to explore Venus and Mars, none of these milestone missions is equipped with technology to manufacture functional metallic parts or tools in space. In order to advance space exploration to long-term missions beyond low Earth orbit, it will be crucial to develop and employ technology for in-space manufacturing (ISM) and in-situ resource utilisation (ISRU). To use the advantages of laser-based powder bed fusion in these endeavours, the challenge of powder handling in microgravity must be met. Here we present a device capable of building parts using metallic powders in microgravity. This was proven on several sounding rocket flights, on which occasions Zr-based metallic glass parts produced by additive manufacturing in space were built. The findings of this work demonstrate that building parts using powder feedstock, which is more compact to transport into space than wire, is possible in microgravity environments. This thus significantly advances ISRU and ISM and paves the way for future tests in prolonged microgravity settings.
Processing and cytocompatibility of Cu-doped and undoped fluoride-containing bioactive glasses
(2024)
Sintered or additive-manufactured bioactive glass (BG) scaffolds are highly interesting for bone replacement applications. However, crystallization often limits the high-temperature processability of bioactive glasses (BGs). Thus, the BG composition must combine high bioactivity and processability. In this study, three BGs with nominal molar (%) compositions 54.6SiO2-1.7P2O3-22.1CaO-6.0Na2O-7.9K2O-7.7MgO (13–93), 44.8SiO2-2.5P2O3-36.5CaO-6.6Na2O-6.6K2O-3.0CaF2 (F3) and 44.8SiO2-2.5P2O3-35.5CaO-6.6Na2O-6.6K2O-3.0CaF2-1.0CuO (F3–Cu) were investigated. The dissolution and ion release kinetics were investigated on milled glass powder and crystallized particles (500–600 μm). All glasses showed the precipitation of hydroxyapatite (HAp) crystals after 7 days of immersion in simulated body fluid. No significant differences in ion release from glass and crystalline samples were detected. The influence of surface roughness on cytocompatibility and growth of preosteoblast cells (MC3T3-E1) was investigated on sintered and polished BG pellets. Results showed that sintered BG pellets were cytocompatible, and cells were seen to be well attached and spread on the surface after 5 days of incubation. The results showed an inverse relation of cell viability with the surface roughness of pellets, and cells were seen to attach and spread along the direction of scratches.
Understanding the origins of intrinsic stress in Si nanowires (NWs) is crucial for their successful utilization as transducer building blocks in next-generation, miniaturized sensors based on anoelectromechanical systems (NEMS). With their small size leading to ultrahigh-resonance frequencies and extreme surface-to-volume ratios, silicon NWs raise new opportunities regarding sensitivity, precision, and speed in both physical and biochemical sensing. With silicon optoelectromechanical properties strongly dependent on the level of NW intrinsic stress, various studies have been devoted to the measurement of such stresses generated, for example, as a result of harsh fabrication processes. However, due to enormous NW surface area, even the native oxide that is conventionally considered as a benign surface condition can cause significant stresses. To address this issue, a combination of nanomechanical characterization and atomistic simulation approaches is developed. Relying only on low-temperature processes, the fabrication approach yields monolithic NWs with optimum boundary conditions, where NWs and support architecture are etched within the same silicon crystal. Resulting NWs are characterized by transmission electron microscopy and micro-Raman spectroscopy. The interpretation of results is carried out through molecular dynamics simulations with ReaxFF potential facilitating the incorporation of humidity and temperature, thereby providing a close replica of the actual oxidation environment - in contrast to previous dry oxidation or self-limiting thermal oxidation studies. As a result, consensus on significant intrinsic tensile stresses on the order of 100 MPa to 1 GPa was achieved as a function of NW critical dimension and aspect ratio. The understanding developed herein regarding the role of native oxide played in the generation of NW intrinsic stresses is important for the design and development of silicon-based NEMS.
Laser based powder bed fusion additive manufacturing offers the flexibility to incorporate standard and userdefined scan strategies in a layer or in between the layers for the customized fabrication of metallic components. In the present study, four different scan strategies and their impact on the development of microstructure, texture, and residual stresses in laser powder bed fusion additive manufacturing of a nickel-based superalloy Inconel 718 was investigated. Light microscopy, scanning electron microscopy combined with electron backscatter diffraction, and neutron diffraction were used as the characterization tools. Strong textures with epitaxially grown columnar grains were observed along the build direction for the two individual scan strategies. Patterns depicting the respective scan strategies were visible in the build plane, which dictated the microstructure development in the other planes. An alternating strategy combining the individual strategies in the successive layers and a 67◦ rotational strategy weakened the texture by forming finer microstructural features. Von Mises equivalent stress plots revealed lower stress values and gradients, which translates as lower distortions for the alternating and rotational strategies. Overall results confirmed the scope for manipulating the microstructure, texture, and residual stresses during laser powder bed fusion additive manufacturing by effectively controlling the scan strategies.
Influence of support configurations on the characteristics of selective laser-melted Inconel 718
(2018)
Samples fabricated using two different support configurations by following identical scan strategies during selective laser melting of superalloy Inconel 718 were characterized in this study. Characterization methods included optical microscopy, electron back-scattered diffraction and x-ray diffraction residual stress measurement. For the scan strategy considered, microstructure and residual stress development in the samples were influenced by the support structures. However, crystallographic texture intensity and the texture components formed within the core part of the samples were almost independent of the support. The formation of finer grains closer to the support as well as within the columnar grain boundaries resulted in randomization and texture intensity reduction by nearly half for the sample built on a lattice support. Heat transfer rates dictated by the support configurations in addition to the scan strategy influenced the microstructure and residual stress development in selective laser-melted Inconel 718 samples.
In the present study, microstructure and texture development during single and multiple pass friction stir processing (FSP) of a strain hardenable wrought AlMg alloy (AA5086) was investigated. Subtle differences were observed while comparing with heat treatable alloys in the nucleation mechanism of the recrystallized microstructure observed in the nugget zone. Strain induced boundary migration was the dominant mechanism of microstructure evolution in the alloy, which influenced the crystallographic texture development by weakening it. Micro-texture measurements reveal variations in the crystallographic texture along the thickness of the sample. Recrystallization texture components were observed in the nugget zone indicative of a pronounced static recrystallization in the alloy as compared to the heat treatable alloys. Bulk texture measurements within the nugget zone of the optimally processed sample reveal a relatively dominant C component of shear texture. Average grain size in the nugget zone remained the same and the bulk crystallographic texture components were retained during multiple-pass FSP. The lower strain energies involved and the enhanced recovery processes due to the high temperature materials processing of the alloy during FSP resulted in a stable microstructure and texture. In summary, FSP could be promoted as a competent and suitable secondary processing technique for the bulk production of ultra-fine-grained materials in strain hardenable aluminium alloys.
A double cantilever beam technique in air equipped with ultrasound modulation was used to measure the crack velocity v in borate and silicate glasses. In all glasses v and the stress intensity KI followed the empirical correlation v ~ KIn. Indicated by its smallest KI at v = 1 μm s − 1, KI* = 0.27 MPa m0.5, the silicoborate glass containing 70 mol% B2O3 was found most susceptible to stress-corrosion enhanced crack growth. Contrarily, the sodium calcium magnesium silicate glass appeared least susceptible with KI* = 0.57 MPa m0.5. No clear correlation is evident between KI*, reflecting the stress-corrosion susceptibility, and the hydrolytic resistance for all glasses under study, but values of n obtained from the present study and taken from previous literature for 35 glasses tend to decrease with increasing network modifier ion fraction. Energy dissipation during stress-corrosion enhanced crack propagation is assumed to cause this trend.
Barium silicate glass powders 4 h milled in CO2 and Ar and sintered in air are studied with microscopy, total carbon analysis, differential thermal Analysis (DTA), vacuum hot extraction mass spectroscopy (VHE-MS), Fourier-transformed infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary-ion mass spectrometry (TOF-SIMS). Intensive foaming of powder compacts is evident, and VHE studies prove that foaming is predominantly caused by carbonaceous species for both milling gases. DTA Shows that the decomposition of BaCO3 particles mix-milled with glass powders occurs at similar temperatures as foaming of compacts. However, no carbonate at the glass surface could be detected by FTIR spectroscopy, XPS, and TOF-SIMS after heating to the temperature of sintering. Instead, CO2 molecules unable to rotate identified by FTIR spectroscopy after milling, probably trapped by mechanical dissolution into the glass bulk. Such a mechanism or microencapsulation in cracks and particle aggregates can explain the contribution of Ar to foaming after intense milling in Ar atmosphere. The amount of CO2 molecules and Ar, however, cannot fully explain the extent of foaming. Carbonates mechanically dissolved beneath the surface or encapsulated in cracks and micropores of particle aggregates are therefore probably the major foaming source.
Due to their high strength-to-weight ratio and excellent fatigue resistance, glass fiber reinforced polymers (GFRP) are used as a construction material in a variety of applications including composite high-pressure gas storage vessels. Thus, an early damage detection of the composite material is of great importance. Material degradation can be determined via measuring the distributed strain profile of the GFRP structures. In this article, swept wavelength interferometry based distributed strain sensing (DSS) was applied for structural health monitoring of internal pressure loaded GFRP tube specimens. Measured strain profiles were compared to theoretical calculation considering Classical Lamination Theory. Reliable strain measurements with millimeter resolution were executed even at elongations of up to 3% in the radial direction caused by high internal pressure load. Material fatigue was localized by damaged-induced strain changes during operation, and detected already at 40% of burst pressure.
Subsurface characterization of high-strength high-interstitial austenitic steels after impact wear
(2018)
The microstructure of the subsurface after impact wear of three high-strength high interstitial austenitic steels has been analysed using transmission electron microscopy (TEM) in alloys with C and N as interstitial elements. In all cases, a nanocrystalline region followed by a transition zone and a cold-worked area are present. Additionally, microhardness and nano-scratching tests were conducted to study the wear-related properties of the impact subsurface and the base material. The results of the microstructural analysis reveal that the following mechanisms are involved during impact wear: abrasion (ploughing), microcrack formation associated with contact fatigue, entrapment and adhesion of SiO2 particles. The analysis of the wear-related properties indicates that the subsurface acts as a self-protective layer that prevents the deterioration of the substrate.
Microplastics are increasingly entering marine, limnic and terrestrial ecosystems worldwide, where they sorb hydrophobic organic contaminants. Here, the sorption behavior of the fuel-related water contaminants benzene, toluene, ethyl benzene and xylene (BTEX) and four tertiary butyl ethers to virgin and via UV radiation aged polypropylene (PP) and polystyrene (PS) pellets was investigated. Changes in material properties due to aging were recorded using appropriate polymer characterization methods, such as differential scanning calorimetry, Fourier transform infrared spectroscopy, gel permeation chromatography, X-ray photoelectron spectroscopy, and microscopy.
Pellets were exposed to water containing BTEX and the ethers at 130-190 mg/L for up to two weeks.
Aqueous sorbate concentrations were determined by headspace gas chromatography. Sorption to the polymers was correlated with the sorbate's Kow and was significant for BTEX and marginal for the ethers.
Due to substantially lower glass transition temperatures, PP showed higher sorption than PS. Aging had no effect on the sorption behavior of PP. PS sorbed less BTEX after aging due to an oxidized surface layer.
Reliable measurement of the size of polydisperse, complex-shaped commercial nanopowders is a difficult but necessary task, e.g., for regulatory requirements and toxicity risk assessment. Suitable methods exist for the accurate characterization of the size of non-aggregated, stabilized, spherical and monodisperse nanoparticles. In contrast, industrial nanoscale powders usually require dedicated sample preparation procedures developed for the analysis method of choice. These nano-powders tend to agglomerate and/or aggregate, a behavior which in combination with an innate broad particle size distribution and irregular shape often significantly alters the achievable accuracy of the measured size parameters. The present study systematically tests two commercially available nanoscale powders using different sample preparation methods for correlative analysis by scanning electron microscopy, dynamic light scattering, Brunauer–Emmet–Teller method and differential mobility analysis. One focus was set on the sample preparation by embedding nanoparticles in carbon-based hot-mounting resin. Literature on this topic is scarce and the accuracy of the data extracted from cross sections of these particles is unclearly stated. In this paper systematic simulations on the deviation of the size parameters of well-defined series of nanoparticles with different shapes from the nominal value were carried out and the contributing factors are discussed.
The steam side oxidation of ferritic–martensitic VM12-SHC steel was investigated under thermo-cyclic conditions in water steam at 620/320 °C and 30 bar with a focus on assessing the influence of pre-oxidation time, specimen geometry and surface finish. The specimens were pre-oxidized under isothermal conditions in water steam at 620 °C and 30 bar for 500 h or 1500 h. After pre-oxidation treatment, all specimens were subjected up to 258 thermal cycles. Three different geometries—rectangular coupons, U-shaped ring segments and ring samples—were investigated to evaluate the influence of open/closed shape, and flat/curved surface on corrosion rate. At the same time, two types of surface finish were considered: “as received” and “ground.” The formation of a protective scale by pre-oxidation was investigated. EBSD and ESMA analyses revealed that the Cr-content of the alloy appeared to be insufficient for obtaining a protective oxide scale under studied conditions, at the same time the anayses confirmed that initial oxidation depends on presence of minor alloying elements as Si and Mn, strong oxide formers which can alter the kinetics and morphology of the corrosion reaction. Moreover, rectangular coupons with small wall thickness and flat surface exhibited the highest corrosion rate, while “ground” curved samples showed only local oxidation. This indicates that for same pre-oxidation time, oxidation kinetics is controlled by curvature.
Undetected and undesired microstructural variations in components produced by laser powder bed fusion are a major challenge, especially for safety-critical components. In this study, an in-depth analysis of the microstructural features of 316L specimens produced by laser powder bed fusion at different levels of volumetric energy density and different levels of inter layer time is reported. The study has been conducted on specimens with an application relevant build height
(>100 mm). Furthermore, the evolution of the intrinsic preheating temperature during the build-up of specimens was monitored using a thermographic in-situ monitoring set-up. By applying recently determined emissivity values of 316L powder layers, real temperatures could be quantified. Heat accumulation led to preheating temperatures of up to about 600 °C. Significant differences in the preheating temperatures were discussed with respect to the individual process parameter combinations, including the build height. A strong effect of the inter layer time on the heat accumulation was observed. A shorter inter layer time resulted in an increase of the preheating temperature by more than a factor of 2 in the upper part of the specimens compared to longer inter layer times. This, in turn, resulted in heterogeneity of the microstructure and differences in material properties within individual specimens. The resulting differences in the microstructure were analyzed using electron back scatter diffraction and scanning electron microscopy. Results from chemical analysis as well as electron back scatter diffraction measurements indicated stable conditions in terms of chemical alloy composition and austenite phase content for the used set of parameter combinations. However, an increase of the average grain size by more than a factor of 2.5 could be revealed within individual specimens. Additionally, differences in feature size of the solidification cellular substructure were examined and a trend of increasing cell sizes was observed. This trend was attributed to differences in solidification rate and thermal gradients induced by differences in scanning velocity and preheating temperature. A change of the thermal history due to intrinsic preheating could be identified as the main cause of this heterogeneity. It was induced by critical combinations of the energy input and differences in heat transfer conditions by variations of the inter layer time. The microstructural variations were directly correlated to differences in hardness.
The influence of the support structure on residual stress and distortion in SLM Inconel 718 parts
(2018)
The effect of support structure and of removal from the base plate on the residual stress state in selective laser melted IN718 parts was studied by means of synchrotron X-ray diffraction. The residual stresses in subsurface region of two elongated prisms in as-built condition and after removal from the base plate were determined. One sample was directly built on a base plate and another one on a support structure. Also, the distortion on the top surface due to stress release was measured by contact profilometry. High tensile residual stress values were found, with pronounced stress gradient along the hatching direction. In the sample on support, stress redistribution took place after removal from the base plate, as opposed to simple stress relaxation for the sample without support. The sample on support structure showed larger distortion compared to sample without support. We conclude that the use of a support decreases stress values but stress-relieving heat treatments are still needed.
Manufacturing defects, high residual stress (RS), and microstructures affect the structural integrity of laser powder bed fusion (LPBF) Ti-6Al-4V. In this study, the individual effect of these factors on fatigue performance at elevated temperature (300 °C) was evaluated. Material in as-built condition and subjected to post-processing, including two heat treatments and hot isostatic pressing, was investigated. It was found that in the absence of tensile RS, the fatigue life at elevated temperature is primary controlled by the defects; and densification has a much stronger effect than the considered heat treatments on the improvement of the mechanical performance.
Automated computational workflows are a powerful concept that can improve the usability and reproducibility of simulation and data processing approaches. Although used very successfully in bioinformatics, workflow environments in materials science are currently commonly applied in the field of atomistic simulations. This work showcases the integration of a discrete element method (DEM) simulation of powder pressing in the convenient SimStack workflow environment. For this purpose, a Workflow active Node (WaNo) was developed to generate input scripts for the DEM solver using LIGGGHTS Open Source Discrete Element Method Particle Simulation code. Combining different WaNos in the SimStack framework makes it possible to build workflows and loop over different simulation or evaluation conditions. The functionality of the workflows is explained, and the added user value is discussed. The procedure presented here is an example and template for many other simulation methods and issues in materials science and engineering.
A key aspect in the development of multilayer inductors is the magnetic permeability of the ferrite layers. Here, the effects of different processing steps on the permeability of a NiCuZn ferrite is investigated. Dry pressed, tape cast, and co‐fired multilayer samples are analyzed. An automated data pipeline is applied to structure the acquired experimental data according to a domain ontology based on PMDco (Platform MaterialDigital core ontology). Example queries to the ontology show how the determined process‐property correlations are accessible to non‐experts and thus how suitable data for component design can be identified. It is demonstrated how the inductance of co‐fired multilayer inductors is reliably predicted by simulations if the appropriate input data corresponding to the manufacturing process is used.This article is protected by copyright. All rights reserved.
Dielectric strength testing of ceramics can be performed with various setups and parameters. Comparisons of results from different sources are often not meaningful, because the results are strongly dependent on the actual testing procedure. The aim of this study is to quantify the influence of voltage ramp rate, electrode size, electrode conditioning, and sample thickness on the measured AC dielectric strength of a commercial alumina. Mean values, Weibull moduli, and failure probabilities determined in standardized short time tests are evaluated and related to withstand voltage tests. Dielectric strength values in the range from 21.6 to 33.2 kV/mm were obtained for the same material using different testing procedures. Short time tests resulted in small standard deviations (< 2 kV/mm) and high Weibull moduli around 30, while withstand tests at voltage levels with low and virtual zero failure probability in short time tests resulted in large scatter of withstand time and Weibull moduli < 1. The strong decrease in Weibull moduli is attributed to progressive damage from partial discharge and depolarization during AC testing. These findings emphasize the necessity of a thorough documentation of testing procedure and highlight the importance of withstand voltage tests for a comprehensive material characterization.
The fracture surface of slow and continuous crack propagation during environmental stress cracking of a semicrystalline polyethylene exhibits isotropic roughness exponents at the local scale but resolved across the macroscopic fracture surface a clear position dependence is found. The spatially resolved roughness exponent admits values in the range between 0.1 and 0.4, demonstrating nontrivial exponents in the small length-scale regime. Instead, they vary across the fracture surface according to the stress-state distribution, which suggests that the exponents are intimately linked to the locally dominating dissipation processes during craze cracking.
Transformers couple two sections of a circuit by electromagnetic induction. They are widely used to either transform alternating voltage levels or to transmit power or signals across galvanic isolation. Both of these functions are essential for the operation of sensors and controllers. Covering all aspects from idea to circuit performance and from design to manufacture, this paper presents the first comprehensive description of the making of miniaturized, rugged, up-to-100W transformers for embedding into multilayer circuit boards. For circular coils, the well-manageable Ampere-Laplace law is shown to yield reliable designs, predicting correctly the performance of manufactured hardware. This enables fast design without lengthy finite element modelling. In the low-power linear regime, basic relations describe how the device’s characteristics evolve from the material properties and device structure. While scattering Parameters are useful for the analysis of isolated transformers with their intrinsic parasitics, the interaction with the components of the final circuit and the aspects of power and efficiency are addressed by chain matrixes.
While these design rules are similar for multilayer boards of different material (like epoxy, Teflon, ceramics), the manufacturing of ceramic board transformers is considered here in detail. Low-temperature-cofired ceramic (LTCC) boards being sintered at 900 °C are particularly suited for harsh environments with chemical or thermal stress as frequently found at sensor positions. The transformer performance usually benefits from or even requires an integrated ceramic core of higher permeability, a ferrite, to shape the magnetic flux. Methods to sinter ferrites inside a dielectric ceramic multilayerandto measure their performance are therefore described in detail.Asthe sintering behaviour of dielectricandmagnetic ceramics differs considerably, their simultaneous sintering is challenging.However, the sintering temperatures of the usefulMnZnand NiZnCu ferrites can be lowered to that of the dielectric material with only moderate loss of permeability by glass additives. Furthermore, thermal mismatch between materials causes catastrophic failure or at least stress and loss of magnetic performance during cooling to room temperature after sintering. This is avoidable by either adjusting the thermal expansion coefficient of the ferrite or by enclosing the ferrite between stressreleasing separation layers.We present the state of the art in materials development according to the first approach as well as fully functional devices made with the second technique.
Other applications not directly addressed but well related to this work are characterized by low load resistance in relation to the coil resistance of the transformer. Efficient power transmission then requires that technological solutions are applied to achieve the lowest possible resistive loss inside the coils by an enlarged conductor cross-section.
As this is particularly challenging for LTCC boards, a technique is discussed to fabricate conductor traces with a thickness larger than their width.
Soiling of photovoltaic (PV) systems compromises their performance causing a significant power loss and demanding periodical cleaning actions. This phenomenon raises great concerns in the solar energy field, thus leading to notable research efforts over the last decades. Soiling is caused by a dual action of dust deposition and biofouling. However, surprisingly, the microbiological contribution to PV soiling is often overlooked or underestimated. In this study, a variety of qPCR-based methods have been developed to quantify the microbial load of fungi, bacteria and phototrophs on PV panels. These protocols were evaluated by comparison with culturedependent methods, and were implemented with real solar plants for two years. The results show that the developed molecular methods are highly sensitive and reliable to monitor the microbial component of the soiling. Fungal biomass was clearly dominant in all analysed PV modules, while bacteria and phototrophs showed much lower abundance. Light microscopy and qPCR results revealed that melanised microcolonial fungi and phototrophs are the main biofilm-forming microorganisms on the studied solar panels. In particular, the fungal qPCR protocol is proposed as a useful tool for monitoring of PV soiling, and investigating the microbial contribution to specific soiling cases.
The prediction of structural parameters and optoelectronic properties of compound semiconductors is very important. However, calculations often neglect chemical variability and structural defects. In chalcopyrite type semiconductors one of the major defects are copper vacancies (V Cu). The four cation neighbors of the anion determine its position in the chalcopyrite type structure expressed by the Wyckoff position 8d (x, 1/4, 1/8). Intrinsic point defects like V
Cu and anti-sites may cause variations of the Anion position in the middle of the cation tetrahedron, especially in the Anion position Parameter x. For stoichiometric chalcopyrite type compounds a formalism according to the principle of conservation of tetrahedral bonds (CTB) can be applied to calculate the anion position parameter, but it fails in the case of off-stoichiometric chalcopyrites. This case study of chalcopyrite type CuGaS 2 and Mn-substituted GuGaS 2
shows that the experimentally determined anion position Parameter x
deviate from values calculated by CTB approach. The systematic investigation of off-stoichiometric CuGaS 2 and Mn-substituted GuGaS
2 demonstrates the effect of copper vacancies on the average radii of the cation sites (Wyckoff positions 4a and 4b) as well as on the anion position Parameter x. By applying an elaborated CTB Approach implementing copper vacancies an agreement between experimental and calculated anion position Parameter x can be obtained.
Early material damage in equimolar CrMnFeCoNi in mixed oxidizing/sulfiding hot gas atmosphere
(2022)
The challenges to use more varied fuels at medium and high temperatures above 500 °C need to be addressed by tuning the materials toward a better resistance against increased corrosion. As a first step the corrosion processes need to be better understood, especially in the case of the unavoidable and highly corrosive sulfur-based gases. Herein, oxidation/sulfidation of an equimolar CrMnFeCoNi high-entropy alloy is studied at an early stage after hot gas exposure at 600 °C for 6 h in 0.5% SO2 and 99.5% Ar. The oxidation process is studied by means of X-ray diffraction, scanning and transmission electron microscopy, and supported by thermodynamic calculations. It is found that the sulfur does not enter the bulk material but interacts mainly with the fast-diffusing manganese at grain boundary triple junctions at the alloy surface. Submicrometer scaled Cr–S–O-rich phases close to the grain boundaries complete the sulfur-based phase formation. The grains are covered in different Fe-, Mn-, and Cr-based spinels and other oxides.
Misfits of γ- γ’ based Al10Co25Cr8Fe15Ni36Ti6 and its Mo- and Hf-variations are studied up to a temperature of 980 °C and compared with Ni- and Co-based superalloys. The trace elements decrease (Hf) or increase (Mo) the edge radii of the γ’ cuboids without changing their sizes. Atom probe measurements revealed that the Hf alloy prefers the γ’ phase while Mo prefers the γ matrix, leading to a lattice parameters enhancement of both phases, as could be revealed by synchrotron X-ray diffraction. The misfit is influenced in opposite ways: Hf increases the positive misfit, while Mo reduces it at all investigated temperatures.
Superalloy inspired Al10Co25Cr8Fe15Ni36Ti6 compositionally complex alloy is known for its gamma-gamma' microstructure and the third Heusler phase. Variations of this alloy, gained by replacing 0.5 or 1 at. pct Al by the equivalent amount of Mo, W, Zr, Hf or B, can show more phases in addition to this three-phase morphology. When the homogenization temperature is chosen too high, a eutectic phase formation can take place at the grain boundaries, depending on the trace elements: Mo and W do not form eutectics while Hf, Zr and B do. In order to avoid the eutectic formation and the potential implied grain boundary weakening, the homogenization temperature must be chosen carefully by differential scanning calorimetry measurements. A too low homogenization temperature, however, could impede the misorientation alignment of the dendrites in the grain. The influence of grain boundary phases and incomplete dendrite re-orientation are compared and discussed.
This paper presents the results of a study of the morphology and structure at the weld interface in a brass–Invar bimetal, which belongs to the class of so-called thermostatic bimetals, or thermobimetals. The structure of the brass–Invar weld interface was analyzed using optical microscopy and scanning electron microscopy (SEM), with the use of energy-dispersive X-ray (EDX) spectrometry and back-scattered electron diffraction (BSE) to identify the phases. The distribution of the crystallographic orientation of the grains at the weld interface was obtained using an e-Flash HR electron back-scatter diffraction (EBSD) detector and a forward-scatter detector (FSD). The results of the study indicated that the weld interface had the wavy structure typical of explosive welding. The wave crests and troughs showed the presence of melted zones consisting of a disordered Cu–Zn–Fe–Ni solid solution and undissolved Invar particles. The pattern quality map showed that the structure of brass and Invar after explosive welding consisted of grains that were strongly elongated towards the area of the highest intensive plastic flow. In addition, numerous deformation twins, dislocation accumulations and shear bands were observed. Thus, based on the results of this study, the mechanism of Cu–Zn–Fe–Ni structure formation can be proposed.
Hydrogen is an attractive energy carrier that requires high effort for safe storage. For ensuring safety, storage cylinders must undergo a challenging approval process. Relevant standards and regulations for composite cylinders used for the transport of hydrogen and for its onboard storage are currently based on deterministic (e.g. ISO 11119-3) or to some respect semi-probabilistic criteria (UN GTR No. 13; with respect to burst strength).
This paper provides a systematic analysis of the load cycle properties resulting from these regulations and standards. Their characteristics are compared with the probabilistic approach of the Federal Institute for Materials Research and Testing BAM. The most important aspect of comparing different concepts is the rate for accepting designs with potentially unsafe or critical safety properties. This acceptance rate is analysed by operating Monte-Carlo simulations over the available range of production properties.
Atomistic deformation simulations in the nominally elastic regime are performed for a model binary glass with strain rates as low as 10 4 /s (corresponding to 0.01 shear strain per 1 μs). A strain rate dependent elastic softening due to a micro-plasticity is observed, which is mediated by thermally-activated localized structural transformations (LSEs). A closer inspection of the atomic-scale structure indicates the material response is distinctly different for two types of local atomic environments. A system spanning iscosahe- drally coordinated substructure responds purely elastically, whereas the remaining substructure admits both elastic and microplastic evolution. This leads to a heterogeneous internal stress distribution which, upon unloading, results in negative creep and complete residual-strain recovery. A detailed structural analysis in terms of local stress, atomic displacement, and SU(2) local bonding topology shows such mi- croscopic processes can result in large changes in local stress and are more likely to occur in geomet- rically frustrated regions characterized by higher free volume and softer elastic stiffness. The thermally- activated LSE activity also mediates structural relaxation, and in this way should be distinguished from stress-driven shear transformation activity which only rejuvenates glass structure. The frequency of LSE activity, and therefore the amount of micro-plasticity, is found to be related to the degree to which the glassy state is relaxed. These insights shed atomistic light onto the structural origins that may govern re- cent experimental observations of significant structural evolution in response to elastic loading protocols.
This manuscript is based on an oral contribution to the TMS 2020 annual meeting and is dedicated to Prof. Peter Liaw, who for decades has shown great interest in serrated plastic flow.
Here we will focus on the case of bulk metallic glasses, and begin with briefly summarizing some aspects of serrated and non-serrated inhomogeneous flow—a phenomenon that has perplexed materials scientists for decades. Four directions of research are identified that emerged out of the desire to fundamentally understand the intermittent inhomogeneous flow response. These research directions gear away from the phenomenological stress–strain behavior but put the underlying shear defect into focus. Unsolved problems and future research topics are discussed.
Due to the different thermal expansion of the constituent materials, cyclic thermal loading of FRP induces alternating stresses in the material at two scales: at the micro scale (level of fibre–matrix-interaction) and at the macro scale (level of the multidirectional laminate). Especially the micro scale effect is not comprehensively investigated yet. Additionally, computational investigations mostly neglect this effect due to the homogenous modelling of the composite material. As this effect is assumed to significantly contribute to the fatigue of FRP at thermal loads, the present paper suggests an experimental and numerical multiscale approach including Experiments at the different involved material scales to separately observe the effects acting at these scales. The approach also includes numerical modelling for each scale to complement the knowledge gained from the Experiments and to create a basis for the consideration of the micro effect even in macroscopic fatigue models treating homogeneous modelled composites. The main focus of the contribution is to bring the overall Approach up for discussion, rather than to present the multiscale modelling details.
Dense ZnO films with a strong c‐axis texture have been deposited on transparent conductive oxide glass, glass, and Si wafers, respectively, with a two‐step pressureless wet chemical method using zinc acetate dihydrate as Zn‐precursor. The crystallographic structure of the films has been studied with XRD and scanning electron microscopy. Optical measurements reveal a high transparency of the ZnO films with a thickness of up to 10 μm. This new cost‐effective route for ZnO film deposition does not require expensive sophisticated equipment and is easily upscaled.
Melting is well understood in terms of the Lindemann criterion, which
essentially states that crystalline materials melt when the thermal vibrationsof their atoms become so vigorous that they shake themselves free of the binding forces. This picture does not necessarily have to hold for glasses, where the nature of the solid–liquid cross-over is highly debated. The Lindemann criterion implies that the thermal expansion coefficients of crystals are inversely proportional to their melting temperatures. Here we find that, in contrast, the thermal expansion coefficient of glasses decreases more strongly with increasing glass temperature, which marks the liquid–solid cross-over in this material class. However, this proportionality returns when the thermal expansion coefficient is scaled by the fragility, a measure of particle cooperativity. Therefore, for a glass to become liquid, it is not sufficient to simply overcome the interparticle binding energies.
Instead, more energy must be invested to break up the typical cooperative particle network that is common to glassy materials. The thermal expansion coefficient of the liquid phase reveals similar anomalous behaviour and is universally enhanced by a constant factor of approximately 3. These universalities allow the estimation of glass temperatures from thermal expansion and vice versa.
Thermal cycling of a Ni-excess NiTi alloy was conducted between 50 °C and liquid nitrogen temperature to induce martensitic transformations and to reverse them after. The starting point was an annealed and slowly cooled state, the end point a sample thermally cycled 1500 times. Positron annihilation lifetime spectra and Coincidence Doppler Broadening profiles were obtained in various states and at various tem- peratures. It was found that the initial state was low in defects with positron lifetimes close to that of bulk NiTi. Cycling lead to a continuous build-up of a defect structure up to 20 0 −50 0 cycles after which saturation was reached. Two types of defects created during cycling were identified, namely pure dislo- cations and vacancies attached to dislocations.
This work presents strong evidence for structural damage accumulation as a function of shear strain admitted by shear bands in a Zr-based bulk metallic glass. Analyzing the shear-band structure of shear- band segments that experienced shear strains covering four orders of magnitude with high-angle annular dark field transmission electron microscopy (HAADF-STEM) reveals strongly scattered data with on overall trend of increasing local volume dilatation with increasing shear strain. Locally, however, a variety of trends is observed, which underlines the strong heterogeneity of structural damage in shear bands in metallic glasses.
The effectiveness of the mechanism of precipitation strengthening in metallic alloys depends on the shapes of the precipitates. Two different material systems are considered: tetragonal γ′′ precipitates in Ni-based alloys and tetragonal θ′ precipitates in Al-Cu-alloys. The shape formation and evolution of the tetragonally misfitting precipitates was investigated by means of experiments and phase-field simulations. We employed the method of invariant moments for the consistent shape quantification of precipitates obtained from the simulation as well as those obtained from the experiment. Two well-defined shape-quantities are proposed: (i) a generalized measure for the particles aspect ratio and (ii) the normalized λ2, as a measure for shape deviations from an ideal ellipse of the given aspect ratio. Considering the size dependence of the aspect ratio of γ′′ precipitates, we find good agreement between the simulation results and the experiment. Further, the precipitates’ in-plane shape is defined as the central 2D cut through the 3D particle in a plane normal to the tetragonal c-axes of the precipitate. The experimentally observed in-plane shapes of γ′′-precipitates can be quantitatively reproduced by the phase-field model.
Grain boundary energy effect on grain boundary segregation in an equiatomic high-entropy alloy
(2020)
Grain boundary (GB) Segregation has a substantial effect on the microstructure evolution and properties of polycrystalline alloys. The mechanism of nanoscale segregation at the various GBs in multicomponent alloys is of great challenge to reveal and remains elusive so far. To address this issue, we studied the GB segregation in a representative equiatomic FeMnNiCoCr high-entropy alloy (HEA) aged at 450 °C. By combining transmission Kikuchi diffraction, atom probe tomography analysis and a density-based thermodynamics modeling, we uncover the nanoscale segregation behavior at a series of well-characterized GBs of different characters. No segregation occurs at coherent twin boundaries; only slight nanoscale segregation of Ni takes place at the low-angle GBs and vicinal \Sigma 29b coincidence site lattice GBs. Ni and Mn show cosegregation of high levels at the general high-angle GBs with a strong depletion in Fe, Cr, and Co. Our density-based thermodynamic model reveals that the highly negative energy of mixing Ni and Mn is the main driving force for nanoscale cosegregation to the GBs. This is further assisted by the opposite segregation of Ni and Cr atoms with a positive enthalpy of mixing. It is also found that GBs of higher interfacial energy, possessing lower atomic densities (higher disorder and free volume), show higher segregation levels. By clarifying the origins of GB segregations in the FeMnNiCoCr HEA, the current work provides fundamental ideas on nanoscale segregation at crystal defects in multicomponent alloys.
Die klassische Metallographie basiert auf Abbildungen einzelner Schliffebenen und kann auf räumliche Formen und Anordnungen des Gefüges nur bedingt schließen. Die Idee, aus metallographischen Serienschliffen dreidimensionale Gefügestrukturen zu rekonstruieren, ist daher naheliegend und nicht neu. Allerdings ist der Aufwand, in Handarbeit viele Einzel-Schliffe zu präparieren und zu Bildstapeln zusammenzusetzen, sehr hoch und steht einer häufigen Anwendung entgegen.
Deshalb wird an der BAM ein Roboter-gestütztes 3D-Metallographie-System entwickelt, das an einer Schliffprobe die Schritte Präparation und Bildeinzug vollautomatisch mit vielen Wiederholungen ausführt. Die Präparation umfasst Schleifen, Polieren und optional Ätzen der Schlifffläche, der Bildeinzug autofokussierte lichtmikroskopische Aufnahmen bei mehreren Vergrößerungsstufen. Der erhaltene Bildstapel wird anschließend vorverarbeitet, segmentiert und in ein 3D-Modell umgesetzt, das einer mikrotomographischen Aufnahme ähnelt, allerdings mit besserer lateraler Auflösung bei großem Volumen. Im Gegensatz zu tomographischen Verfahren besteht die Möglichkeit der Kontrastierung durch klassische chemische Ätzung. Die Integration eines REMs ist geplant. Bislang durchgeführte Arbeiten verdeutlichen die Möglichkeiten der Darstellung von Heißgas-Korrosionsschichten, Grauguss-Werkstoffen und Keramik-basierten mikroelektronischen Strukturen (Vias).
The research focus of this study was set on the corrosion process of condensate as droplets on the surface of carbon steels (X52, X70) martensitic steel UNS S41500, and super austenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the offshore transportation condition in a buried pipeline). The possibility of dew/droplet formation on the steel surface and wetting behavior of corresponding materials were evaluated by contact angle measurement in dense CO2 at 278 K. To observe the effect of impurities (SO2 and O2) on droplet corrosion process, exposure tests were carried out in the mixed atmosphere with a drop, 1 ‑ 10 µL in volume, of CO2 saturated ultra-pure water on steel surface. Comparable exposure tests were carried out with the same gas mixture and the same volume of water, as vapor, to observe the droplet formation and the corrosion process that follows. Effects of surface roughness on the droplet formation and its corrosion process were further studied and showed no significant role upon long time exposure. The results from droplet experiments were compared to those from the bulk electrolyte for the further recommendation on the quality control of gas stream along with the use of carbon steels as transport pipelines in CCS - Carbon Capture and Storage system.
For reliability and safety issues of injection wells, corrosion resistance of materials used needs to be determined. Herein, representative low-cost materials, including carbon steel X70/1.8977 and low alloyed steel 1.7225, were embedded in mortar to mimic the realistic casing-mortar interface. Two types of cement were investigated: (1) Dyckerhoff Variodur commercial Portland cement, representing a highly acidic resistant cement and (2) Wollastonite, which can react with CO2 and become stable under a CO2 stream due to the carbonation process. Exposure tests were performed under 10 MPa and at 333 K in artificial aquifer fluid for up to 20 weeks, revealing crevice corrosion and uniform corrosion instead of expected pitting corrosion. To clarify the role of cement, simulated pore water was made by dispersing cement powder in aquifer fluid and used as a solution to expose steels. Surface analysis, accompanied by element mapping on exposed specimens and their crosssections, was carried out to trace the chloride intrusion and corrosion process that followed.
To study the effects of condensed acid liquid, hereafter referred to as condensate, on the CO2 transport pipeline steels, gas mixtures containing a varying concentration of H2O, O2, NO2, and SO2, were proposed and resulted in the condensate containing H2SO4 and HNO3 with the pH ranging from 0.5 to 2.5. By exposing the pipeline steel to the synthetic condensate with different concentration of acidic components, the corrosion kinetic is significantly changed. Reaction kinetic was studied using electrochemical methods coupled with water analysis and compared with surface analysis (scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffractometry (XRD)) of corroded coupons. The results showed that, although the condensation of NO2 in the form of HNO3 causes faster general corrosion rate, it is the condensation of SO2 in the form of H2SO4 or the combination of SO2 and NO2 that may cause much more severe problems in the form of localized and pitting corrosions. The resulting corrosion forms were depended on the chemical nature of acids and their concentration at the same investigated pH. The effects of changing CO2 flow rate and renewing condensate on pitting corrosion were further studied.
Poly (ether ether ketone) (PEEK) has a high continuous service temperature, excellent mechanical properties, and good solvent and abrasion resistance, which can be further improved through the addition of carbon nanotubes (CNTs). CNT-PEEK nanocomposites are promising matrices for continuous carbon fibre composites; powder processing can mitigate the high melt viscosities in these systems. In this study, model single fibre (hierarchical) composites were produced by embedding sized and desized carbon fibres in nanocomposite CNTPEEK powders followed by single fibre pull-out tests to assess interfacial characteristics. Carbon fibre-PEEK interfacial shear strength is typically 40–45 MPa. Increasing CNT loadings increased fibre-matrix interfacial shear strength linearly up to ~70 MPa at 5.0 wt%, which was attributed to the CNT-based mechanical modification of the PEEK matrix. Apparent interfacial shear strength was inversely correlated with the embedded fibre length irrespective of carbon fibre sizing or CNT loading, indicating brittle fracture of the fibre-matrix interface.
Pulled out carbon fibres were still coated with the matrix, which indicated strong adhesion at the interface in all samples, likely related to a transcrystalline region. Adhesion was, however, negatively affected by the presence of epoxy sizings. Frictional shear strength was independent of embedded fibre length and CNT content for all samples.
Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. Imaging and the tensile test are run at the highest possible frame rate (0.7 s-1 ) and the lowest possible strain rate (5.5∙10-4 s -1 ). For 0°/90° non-crimp fabrics, the first inter-fiber cracks occur at 380 MPa (strain 0.8 %). Prior to failure at about 760 MPa (strain 2.0 %), we observe the evolution of nearly equidistant (1 mm distance) cracks running across the entire sample in the fully damaged state.
Additive Manufacturing (AM) through the Selective Laser Melting (SLM) route offers ample scope for producing geometrically complex parts compared to the conventional subtractive manufacturing strategies. Nevertheless, the residual stresses which develop during the fabrication can limit application of the SLM components by reducing the load bearing capacity and by inducing unwanted distortion, depending on the boundary conditions specified during manufacturing. The present study aims at characterizing the residual stress states in the SLM parts using different diffraction methods. The material used is the nickel based superalloy Inconel 718. Microstructure as well as the surface and bulk residual stresses were characterized. For the residual stress analysis, X-ray, synchrotron and neutron diffraction methods were used. The measurements were performed at BAM, at the EDDI beamline of -BESSY II synchrotronand the E3 line -BER II neutron reactor- of the Helmholtz-Zentrum für Materialien und Energie (HZB) Berlin. The results reveal significant differences in the residual stress states for the different characterization techniques employed, which indicates the dependence of the residual state on the penetration depth in the sample. For the surface residual stresses, longitudinal and transverse stress components from X-ray and synchrotron agree well and the obtained values were around the yield strength of the material. Furthermore, synchrotron mapping disclosed gradients along the width and length of the sample for the longitudinal and transverse stress components. On the other hand, lower residual stresses were found in the bulk of the material measured using neutron diffraction. The longitudinal component was tensile and decreased towards the boundary of the sample. In contrast, the normal component was nearly constant and compressive in nature. The transversal component was almost negligible. The results indicate that a stress re-distribution takes place during the deposition of the consecutive layers. Further investigations are planned to study the phenomenon in detail.
Epoxy R-Glass Fiber-Reinforced Polymer (GFRP) composite plates were hydrothermally aged at 60 ◦C for 23, 75, and 133 days. The water content reached 0.97 wt%, 1.45 wt% and 1.63 wt%, respectively. The studied GFRP matrix was inert to hydrolysis or chain scission, allowing for investigation of irreversible changes in the fiber-matrix interphase due to hydrothermal aging upon re-drying. During each period, a subset of the specimens was removed from the water bath and dried in a chamber. The weight loss upon drying was explained with epoxy leaching (impurities), sizing-rich interphase hydrolysis, glass fiber surface hydrolysis, accumulated degradation products escaping, and water changing state from bound to free. The influence of hydrothermal aging on the fiber-matrix interfacial properties was investigated. Lower interfacial strength of hydrothermally aged (wet)
samples was attributed to plasticization of the epoxy, plasticization and degradation of the sizing-rich interphase (including formation of hydrolytic flaws), and hydrolytic degradation of the glass fiber surface. The kinetics of epoxy-compatible epoxysilane W2020 sizing-rich interphase hydrolysis provided an estimate of ca. 1.49%, 4.80%, and 8.49% of the total composite interphase degraded after 23, 75, and 133 days, respectively. At these conditions, the interface lost 39%, 48%, and 51% of its strength. Upon re-drying the specimens, a significant part of the interfacial strength was regained. Furthermore, an upward trend was observed, being 13%, 10% and 3% strength, respectively; thus, indicating a possibility of partial recovery of properties.